WO2017070921A1 - Two-component, addition-type, anti-sedimenttation conductive silicone rubber and preparation method thereof - Google Patents

Abstract

Disclosed are a two-component, addition-type, anti-sedimentation conductive silicone rubber formed by mixing a component A and a component B in a mass ratio of 1:1, and a preparation method thereof, wherein the component A includes a base material: 20-60 parts, hydrosilicone oil: 2-10 parts, an inhibitor: 0.005-1 part, a diluent: 5-15 parts, a coupling agent: 0.005-2 parts, and modified conductive powder: 40-75 parts, and the component B includes a base material: 10-60 parts, a platinum catalyst: 0.0001-0.0005 part, a coupling agent: 0.005-2 parts, and modified conductive powder: 40-75 parts. The addition-type, anti-sedimentation conductive silicone rubber, as an adhesive for FIP dispensing, can prevent the conductive adhesive from sedimenting during storage and transportation, the vulcanized adhesive strip has excellent toughness, good adhesiveness to various plastic and metal substrates, especially to an aluminum plate.

Description

Two-component additive forming anti-settling conductive silica gel and preparation method thereof Technical field

The invention relates to a conductive silica gel and a preparation method thereof, in particular to an anti-settling conductive silica gel and a preparation method thereof, and belongs to the field of organic absorbing materials required for electromagnetic shielding interface.

Background technique

With the development of modern high-tech, the electromagnetic interference (EMI) and electromagnetic compatibility (EMC) problems caused by electromagnetic waves are becoming more and more serious, which not only cause interference and damage to electronic instruments and equipment, but also affect their normal work, and also pollute the environment and harm humans. Health; in addition, electromagnetic wave leakage will also jeopardize the security of national information security and military core secrets. Therefore, exploring efficient electromagnetic shielding materials to prevent electromagnetic interference and electromagnetic compatibility caused by electromagnetic waves is of great significance for improving the safety and reliability of electronic products and equipment and ensuring the safety and smoothness of information communication systems, network systems and transmission systems.

There are many conductive glues on the market, but there are several fatal defects: First, the shelf life is very short, usually only about 3 months, and if improperly stored or placed for a long time, there will be no glue, resulting in products. Unable to use; Second, the storage stability is poor. After storage for a period of time, the conductive powder will settle, resulting in complicated sizing process and poor electrical conductivity. Third, the bonding performance on the flange surface is poor.

In view of the shortage of the above electromagnetic shielding materials and the shortage of conductive glue, the development of conductive glue with electromagnetic shielding effect has become an urgent problem.

Summary of the invention

The invention aims at the deficiencies of the existing conductive glue, and provides a two-component addition-forming anti-settling conductive silica gel and a preparation method thereof.

The technical solution of the present invention to solve the above technical problems is as follows:

Two-component additive anti-settling conductive silica gel characterized by being composed of component A and component B

The mass ratio is 1:1, and the component A comprises the following raw materials by weight:

The component B comprises the following raw materials by weight:

The base material is prepared by dehydrating and blending 80-120 parts of vinyl silicone oil, 50-70 parts of fumed silica, 3-8 parts of hexamethyldisilazane and 0.2-1 part of distilled water;

The modified conductive powder refers to a conductive powder whose surface is coated with a coupling agent.

Further, the vinyl silicone oil refers to a polydiorganosiloxane liquid glue containing a vinyl group, and the molecular weight of the silicone liquid glue is 2 to 50 w.

Further, the conductive powder refers to pure silver conductive powder, pure nickel conductive powder, nickel-coated graphite conductive powder, silver-clad aluminum conductive powder, silver-clad copper conductive powder, silver-coated nickel conductive powder, silver-clad glass conductive powder. One or a mixture of two or more.

Further, the inhibitor is 2-methyl-3-butynyl-2-ol, 3-methyl-1-ethynyl-3-ol, 3,5-dimethyl-1-hexynyl- 3-alcohol, 1-ethynyl-1-cyclohexanol and polyvinylpolysiloxane At least one of the alkane.

Further, the diluent is at least one of dimethyl silicone oil, tetramethyltetravinylcyclotetrasiloxane, octamethylcyclotetrasiloxane or hexamethyldisiloxane.

Further, the hydrogen-containing silicone oil refers to one or a mixture of two or more of methyl hydrogen silicone oil, methylphenyl silicone oil, and hydroxyl hydrogen-containing silicone oil.

Further, the coupling agent is a silane coupling agent A-171, a titanate coupling agent KR-TTS, an aluminate coupling agent DL-411, an epoxy group, a hydroxyl group, a nitrile group, a carbonyl group, an ester group. One or a mixture of two or more of the silane coupling agents.

The beneficial effects of the invention are:

1) The additive anti-settling conductive silica gel of the invention has stable storage property, and has excellent electrical and physical properties, weather resistance, high and low temperature resistance, etc. after vulcanization;

2) The additive anti-settling conductive silicone rubber provided by the invention is used as FIP dispensing to prevent sedimentation of the conductive adhesive during storage and transportation; the vulcanized strip has excellent toughness; in various plastics And the metal substrate has good adhesion, especially to the aluminum plate.

The invention also claims a method for preparing the above two-component additive anti-settling conductive silica gel, comprising the following steps:

1) Conductive powder drying: drying the conductive powder to remove moisture;

2) Conductive powder coating: the powder obtained in the step 1) is subjected to a surface treatment by a wet method, that is, the coupling agent is mixed with a 95% ethanol solution to be hydrolyzed, and then the conductive powder is added thereto, and the obtained mixture is subjected to After thorough stirring and mixing, the water is heated to volatilize the ethanol to obtain a conductive powder coated with a coupling agent on the surface, that is, the modified conductive powder;

3) Preparation of anti-settling type base material: 80-120 parts of vinyl silicone oil, 50-70 parts of fumed silica, 3-8 parts of hexamethyldisilazane and 0.2-1 part of distilled water are placed in a vacuum kneader Internally, dewatering and blending at 100-150 ° C and pressure <0.01 MPa to obtain an anti-settling type base;

4) Preparation of component A: 20 to 60 parts of the base material obtained in the step 3), 2 to 10 parts of the hydrogen-containing silicone oil, 0.005 to 1 part of the inhibitor, 5 to 15 parts of the diluent, 0.005 to 2 parts of the coupling agent, and 40 to 75 parts of the modified conductive powder are uniformly mixed;

5) Preparation of component B: taking 20 to 60 parts of the base material obtained in step 3), 0.0001 to 0.0005 parts of platinum catalyst, 5 to 15 parts of diluent, 0.005 to 2 parts of coupling agent, and modified conductive powder 40 to 75 Mix and mix evenly;

6) Mixing: After mixing the component A and the component B in a mass ratio of 1:1, the mixture is degassed under a pressure of <0.01 MPa for 20 to 40 minutes to obtain an anti-settling conductive silica gel.

Further, the conductive powders described in steps 1) and 2) are pure silver conductive powder, pure nickel conductive powder, nickel-coated graphite conductive powder, silver-clad aluminum conductive powder, silver-clad copper conductive powder, silver-coated nickel conductive powder, One or a mixture of two or more of the silver-clad glass conductive powder.

Further, the vinyl silicone oil described in the step 3) means a polydiorganosiloxane liquid gel containing a vinyl group having a molecular weight of 2 to 50 w.

Further, the coupling agent in the mixture of the coupling agent and the 95% ethanol solution described in the step 2) accounts for 2 to 10% by weight, and the coupling agent has a mass of 10 to 20% by weight of the absorbing agent.

Further, the inhibitor described in the step 4) is 2-methyl-3-butynyl-2-ol, 3-methyl-1-ethynyl-3-ol, 3,5-dimethyl-1- At least one of hexynyl-3-ol, 1-ethynyl-1-cyclohexanol, and polyvinylpolysiloxane.

Further, the diluents described in steps 4) and 5) are in dimethyl silicone oil, tetramethyltetravinylcyclotetrasiloxane, octamethylcyclotetrasiloxane or hexamethyldisiloxane. At least one.

Further, the hydrogen-containing silicone oil described in the step 4) means one or a mixture of two or more of methyl hydrogen silicone oil, methylphenyl silicone oil, and hydroxyl hydrogen-containing silicone oil.

Further, the coupling agent described in the steps 3) and 4) is a silane coupling agent A-171, a titanate coupling agent KR-TTS, an aluminate coupling agent DL-411, an epoxy group, and a hydroxyl group. One or a mixture of two or more of a cyano group, a carbonyl group, and an ester group.

The beneficial effects of the preparation method of the two-component anti-settling silicon-based conductive silica gel of the invention are as follows:

1) The process flow is simple, the raw materials used are cheap and easy to obtain, and easy to implement;

2) The obtained product is used as FIP dispensing to prevent the sedimentation of the conductive adhesive during storage and transportation; the vulcanized strip has excellent toughness; and has good adhesion on various plastic and metal substrates. Sex, especially for aluminum sheets.

detailed description

The principles and features of the present invention are described in the following examples, which are intended to illustrate the invention and are not intended to limit the scope of the invention.

Example 1:

A two-component additive anti-settling conductive silica gel is prepared by mixing A component and B component at a mass ratio of 1:1, and the component A comprises the following raw materials by weight: base material: 20 parts, methyl group Hydrogen silicone oil: 2 parts, inhibitor 2-methyl-3-butynyl-2-ol: 0.005 parts, dimethyl silicone oil: 5 parts, silane coupling agent A-171: 0.005 parts, modified pure silver conductive powder 40 parts, the B component comprises the following raw materials by weight: base: 20 parts, platinum catalyst: 0.0001 parts, dimethyl silicone oil: 5 parts, silane coupling agent A-171:1 parts, modified pure Silver conductive powder: 40 parts, the base material is a vinyl silicone oil having a molecular weight of 2 W: 50 parts, a vinyl silicone oil having a molecular weight of 10 W: 50 parts, a hydrophobic white carbon black R972: 60 parts, hexamethyldisilane nitrogen Alkane: 5 parts, distilled water: 0.5 parts by dehydration blending, the modified pure silver conductive powder refers to a pure silver conductive powder having a surface coated with a silane coupling agent A-171.

The preparation method of the above two-component additive anti-settling conductive silica gel is as follows:

1) The conductive powder is dried, and 10-30 um of pure silver conductive powder is placed in a blast drying oven and dried at 80 ° C for 1 hour;

2) Conductive powder coating, the surface of the conductive powder obtained in the step 1) is subjected to wet surface treatment, that is, the silane coupling agent A-171 is mixed with a 95% ethanol solution to be hydrolyzed for 30 minutes, wherein the silane couple is divided by weight. The crosslinking agent A-171 accounts for 5wt%, and then the conductive powder is added to the mixed solution of the silane coupling agent A-171 and ethanol, and the silane coupling agent A-171 is 15wt% of the weight of the conductive powder, and is fully stirred and mixed for 30min. Thereafter, the ethanol is evaporated by heating in a water bath of 80 ° C to obtain a pure silver conductive powder coated with a layer of coupling agent A-171 on the surface;

3) Preparation of anti-settling type base material: vinyl silicone oil having a molecular weight of 2 W: 50 parts, vinyl silicone oil having a molecular weight of 10 W: 50 parts, hydrophobic white carbon black R972: 60 parts, hexamethyldisilazane: 5 parts, distilled water: 0.5 parts were placed in a vacuum kneader, and dehydrated and blended at 100 ° C and a pressure of 0.008 MPa to obtain an anti-settling type base;

4) Preparation of component A: base material obtained in step 3): 20 parts, methyl hydrogen silicone oil: 2 parts, inhibitor 2-methyl-3-butynyl-2-ol: 0.005 parts, dimethyl Silicone oil: 5 parts, silane coupling agent A-171: 0.005 parts, pure silver conductive powder obtained in step 2): 40 parts, placed in a double planetary mixer and stirred for 1 hour;

5) Preparation of component B: taking the base material obtained in step 3): 20 parts, platinum catalyst: 0.0001 parts, dimethyl silicone oil: 5 parts, silane coupling agent A-171:1 parts, obtained in step 2) Modified silver-silver conductive powder: 40 parts, placed in a double planetary mixer and stirred for 1 hour;

6) Mixing: A component and a component B were uniformly mixed at a mass ratio of 1:1, and then defoamed under a pressure of 0.005 MPa for 30 minutes to obtain an anti-settling conductive silica gel.

Example 2:

A two-component addition-forming anti-settling conductive silica gel is prepared by mixing A component and B component at a mass ratio of 1:1, and the component A comprises the following raw materials by weight: base material: 40 parts, methyl group Hydrogen silicone oil: 6 parts, inhibitor 2-methyl-3-butynyl-2-ol: 0.5 parts, dimethyl silicone oil: 10 parts, silane coupling agent A-171:1 parts, modified pure nickel conductive powder : 60 parts, the B component comprises the following raw materials by weight: base: 40 parts, platinum catalyst: 0.0003 parts, dimethyl silicone oil: 10 parts, silane coupling agent A-171:1 parts, modified pure Nickel conductive powder: 65 parts, the base material is a vinyl silicone oil having a molecular weight of 10 W: 50 parts, a vinyl silicone oil having a molecular weight of 20 W: 50 parts, a hydrophobic white carbon black R972: 60 parts, hexamethyldisilane nitrogen Alkane: 5 parts, distilled water: 0.5 parts by dehydration blending, the modified pure nickel conductive powder refers to a pure nickel conductive powder having a surface coated with a silane coupling agent A-171.

The preparation method of the above two-component additive anti-settling conductive silica gel is as follows:

1) The conductive powder is dried, and 10-30 um of pure nickel conductive powder is placed in a blast drying oven and dried at 80 ° C for 1 hour;

2) Conductive powder coating, the surface of the conductive powder obtained in the step 1) is subjected to wet surface treatment, that is, the silane coupling agent A-171 is mixed with a 95% ethanol solution to be hydrolyzed for 30 minutes, wherein the silane couple is divided by weight. The crosslinking agent A-171 accounts for 2wt%, and then the conductive powder is added to the mixed solution of the silane coupling agent A-171 and ethanol. The silane coupling agent A-171 is 10wt% of the weight of the conductive powder, and after mixing for 30 minutes with sufficient stirring , heating in a water bath of 80 ° C to evaporate the ethanol to obtain a pure nickel conductive powder coated with a layer of coupling agent A-171;

3) Preparation of anti-settling type base material: vinyl silicone oil having a molecular weight of 10 W: 50 parts, vinyl silicone oil having a molecular weight of 20 W: 50 parts, hydrophobic white carbon black R972: 60 parts, hexamethyldisilazane: 5 parts, distilled water: 0.5 parts were placed in a vacuum kneader, dehydrated and blended at 120 ° C, pressure 0.005Mpa to obtain anti-settling type base;

4) Preparation of component A: base material obtained in step 3): 40 parts, methylhydrogen silicone oil: 6 parts, inhibitor 2-methyl-3-butynyl-2-ol: 0.5 part, dimethyl Silicone oil: 10 parts, silane coupling agent A-171:1 parts, pure nickel conductive powder obtained in step 2): 60 parts, placed in a double planetary mixer and stirred for 1 hour;

5) Preparation of component B: taking the base material obtained in step 3): 40 parts, platinum catalyst: 0.0003 parts, dimethyl silicone oil: 10 parts, silane coupling agent A-171:1 parts, obtained in step 2) Modified pure nickel conductive powder: 65 parts, placed in a double planetary mixer and stirred for 1 hour;

6) Mixing: A component and a component B were uniformly mixed at a mass ratio of 1:1, and then defoamed under a pressure of 0.005 MPa for 30 minutes to obtain an anti-settling conductive silica gel.

Example 3:

A two-component addition-forming anti-settling conductive silica gel is prepared by mixing A component and B component at a mass ratio of 1:1, and the component A comprises the following raw materials by weight: base material: 60 parts, hydroxyl group Hydrogen silicone oil: 10 parts, inhibitor 3-methyl-1-ethynyl-3-ol: 1 part, tetramethyltetravinylcyclotetrasiloxane: 15 parts, titanate coupling agent KR-TTS: 2 parts, Modified nickel-coated graphite conductive powder: 75 parts, the B component comprises the following raw materials by weight: base: 60 parts, platinum catalyst: 0.0005 parts, tetramethyltetravinylcyclotetrasiloxane: 15 parts, Titanate coupling agent KR-TTS: 2 parts, modified nickel-coated graphite conductive powder: 75 parts, the base material is composed of a vinyl silicone oil having a molecular weight of 20 W: 80 parts, and a hydrophobic white carbon black R972: 50 parts. Hexamethyldisilazane: 5 parts, distilled water: 0.8 parts by dehydration blending, the modified nickel-coated graphite conductive powder refers to nickel-coated graphite conductive powder coated with a titanate coupling agent KR-TTS .

The preparation method of the above two-component additive anti-settling conductive silica gel is as follows:

1) The conductive powder is dried, and 30-50 um of nickel-coated graphite conductive powder is placed in a blast drying oven and dried at 80 ° C for 1 hour;

2) Conductive powder coating, the surface of the conductive powder obtained in the step 1) is subjected to a wet surface treatment, that is, the titanate coupling agent KR-TTS is mixed with a 95% ethanol solution to be hydrolyzed for 30 minutes, wherein by weight, The titanate coupling agent KR-TTS accounts for 2wt%, and then the conductive powder is added to the mixed solution of the titanate coupling agent KR-TTS and ethanol. The titanate coupling agent KR-TTS is 15wt of the weight of the conductive powder. %, after thorough stirring and mixing for 30 min, it is heated in a water bath of 80 ° C to evaporate the ethanol to obtain a nickel-coated graphite conductive powder coated with a coupling agent on the surface;

3) Preparation of anti-settling type base material: vinyl silicone oil having a molecular weight of 20 W: 80 parts, hydrophobic white carbon black R972: 50 parts, hexamethyldisilazane: 5 parts, distilled water: 0.8 parts, placed under vacuum kneading In the machine, dewatering and blending at 120 ° C, pressure 0.006Mpa to obtain anti-settling type base;

4) Preparation of component A: base material obtained in step 3): 60 parts, hydroxy-containing silicone oil: 10 parts, inhibitor 3-methyl-1-ethynyl-3-ol: 1 part, tetramethyl Tetravinylcyclotetrasiloxane: 15 parts, titanate coupling agent: 2 parts, modified nickel-coated graphite conductive powder obtained in step 2): 75 parts, placed in a double planetary mixer and stirred for 1 hour;

5) Preparation of component B: taking the base material obtained in step 3): 60 parts, platinum catalyst: 0.0005 parts, Titanate coupling agent KR-TTS: 2 parts, modified nickel-coated graphite conductive powder: 75 parts, placed in a double planetary mixer and stirred for 1 hour;

6) Mixing: A component and a component B were uniformly mixed at a mass ratio of 1:1, and then defoamed under a pressure of 0.005 MPa for 30 minutes to obtain an anti-settling conductive silica gel.

Example 4:

A two-component addition-forming anti-settling conductive silica gel is prepared by mixing A component and B component at a mass ratio of 1:1, and the component A comprises the following raw materials by weight: base material: 20 parts, hydroxyl group Hydrogen silicone oil: 6 parts, inhibitor 3-methyl-1-ethynyl-3-ol: 0.5 part, tetramethyltetravinylcyclotetrasiloxane: 15 parts, titanate coupling agent KR-TTS: 1 part, modified silver-clad aluminum conductive powder: 60 parts, the B component comprises the following raw materials by weight: base: 20 parts, platinum catalyst: 0.0005 parts, tetramethyltetravinylcyclotetrasiloxane: 15 parts, titanate coupling agent KR-TTS: 2 parts, modified silver-clad aluminum conductive powder: 75 parts, the base material is made of vinyl silicone oil having a molecular weight of 20 W: 120 parts, hydrophobic white carbon black R972: 70 parts, hexamethyldisilazane: 8 parts, distilled water: 0.8 parts by dehydration blending, the modified silver-clad aluminum conductive powder refers to a silver package with a surface coated with a titanate coupling agent KR-TTS Aluminum conductive powder.

The preparation method of the above two-component additive anti-settling conductive silica gel is as follows:

1) The conductive powder is dried, and 30-50 um of silver-clad aluminum conductive powder is placed in a blast drying oven and dried at 80 ° C for 1 hour;

2) Conductive powder coating, the surface of the conductive powder obtained in the step 1) is subjected to a wet surface treatment, that is, the titanate coupling agent KR-TTS is mixed with a 95% ethanol solution to be hydrolyzed for 30 minutes, wherein by weight, The titanate coupling agent KR-TTS accounts for 8wt%, and then the conductive powder is added to the mixed solution of the titanate coupling agent KR-TTS and ethanol. The titanate coupling agent KR-TTS is the silver-clad aluminum conductive powder. 15wt% of the weight, after thorough stirring and mixing for 30min, placed in a water bath of 80 ° C to evaporate the ethanol to obtain a silver-clad aluminum conductive powder coated with a coupling agent on the surface;

3) Preparation of anti-settling type base material: vinyl silicone oil having a molecular weight of 20 W: 120 parts, hydrophobic white carbon black R972: 70 parts, hexamethyldisilazane: 8 parts, distilled water: 0.8 parts, placed under vacuum kneading Inside the machine, Dewatering and blending at 100 ° C and a pressure of 0.006 MPa to obtain an anti-settling type base;

4) Preparation of component A: base material obtained in step 3): 20 parts, hydroxy-containing silicone oil: 6 parts, inhibitor 3-methyl-1-ethynyl-3-ol: 0.5 part, tetramethyl Tetravinylcyclotetrasiloxane: 15 parts, titanate coupling agent KR-TTS: 1 part, modified silver-clad aluminum conductive powder: 60 parts, placed in a double planetary mixer and stirred for 1 hour;

5) Preparation of component B: taking the base obtained in step 3): 20 parts, platinum catalyst: 0.0005 parts, tetramethyltetravinylcyclotetrasiloxane: 15 parts, titanate coupling agent KR-TTS : 2 parts, modified silver-clad aluminum conductive powder: 75 parts, placed in a double planetary mixer and stirred for 1 hour;

6) Mixing: After mixing the component A and the component B in a mass ratio of 1:1, the mixture was degassed under a pressure of 0.005 MPa for 40 minutes to obtain an anti-settling conductive silica gel.

Example 5:

A two-component addition-forming anti-settling conductive silica gel is prepared by mixing A component and B component at a mass ratio of 1:1, and the component A comprises the following raw materials by weight: base material: 60 parts, phenyl group Hydrogen-containing silicone oil: 2 parts, inhibitor 3,5-dimethyl-1-hexynyl-3-ol: 0.005 parts, octamethylcyclotetrasiloxane: 10 parts, aluminate coupling agent DL- 411:1 parts, modified silver-clad copper conductive powder: 40 parts, the B component comprises the following raw materials by weight: binder: 60 parts, platinum catalyst: 0.0001 parts, octamethylcyclotetrasiloxane: 15 Parts, aluminate coupling agent DL-411: 0.005 parts, modified silver-clad copper conductive powder: 40 parts, the base material consists of vinyl silicone oil with a molecular weight of 30 W: 120 parts, hydrophobic white carbon black R972: 70 a portion, hexamethyldisilazane: 8 parts, distilled water: 0.8 parts by dehydration blending, the modified silver-coated copper conductive powder refers to a silver-coated copper coated with an aluminate coupling agent DL-411 Conductive powder.

The preparation method of the above two-component additive anti-settling conductive silica gel is as follows:

1) The conductive powder is dried, and 50-80 um of silver-clad copper conductive powder is placed in a blast drying oven and dried at 80 ° C for 1 hour;

2) Conductive powder coating, the surface of the conductive powder obtained in the step 1) is subjected to wet surface treatment, that is, the silane coupling agent KH-560 is mixed with a 95% ethanol solution to be hydrolyzed for 30 minutes, wherein the silane is separated by weight. The coupling agent KH-560 accounts for 15% by weight, and then the conductive powder is added to the mixed solution of the silane coupling agent KH-560 and ethanol. The silane coupling agent KH-560 is 20wt% of the weight of the conductive powder, and is fully stirred and mixed for 30min. After that, the mixture is heated in a water bath of 80 ° C to evaporate the ethanol to obtain a silver-coated copper conductive powder coated with a coupling agent on the surface;

3) Preparation of anti-settling type base material: vinyl silicone oil having a molecular weight of 30 W: 120 parts, hydrophobic white carbon black R972: 70 parts, hexamethyldisilazane: 8 parts, distilled water: 0.8 parts, placed under vacuum kneading In the machine, dewatering and blending at 100 ° C, pressure 0.002Mpa to obtain anti-settling type base;

4) Preparation of component A: base material obtained in step 3): 60 parts, phenyl hydrosilane oil: 2 parts, inhibitor 3,5-dimethyl-1-hexynyl-3-ol: 0.005 , octamethylcyclotetrasiloxane: 10 parts, aluminate coupling agent DL-411:1 parts, modified silver-coated copper conductive powder obtained in step 2): 40 parts, placed in a double planetary mixer Stir and mix for 1 hour;

5) Preparation of component B: taking the base material obtained in the step 3): 60 parts, platinum catalyst: 0.0001 part, octamethylcyclotetrasiloxane: 15 parts, aluminate coupling agent DL-411: 0.005 parts The modified silver-clad copper conductive powder obtained in the step 2): 40 parts, placed in a double planetary mixer and stirred for 1 hour;

6) Mixing: After mixing the component A and the component B in a mass ratio of 1:1, the mixture was degassed under a pressure of 0.005 MPa for 40 minutes to obtain an anti-settling conductive silica gel.

Example 6

A two-component addition-forming anti-settling conductive silica gel is prepared by mixing A component and B component at a mass ratio of 1:1, and the component A comprises the following raw materials by weight: base material: 20 parts, phenyl group Hydrogen-containing silicone oil: 10 parts, inhibitor 3,5-dimethyl-1-hexynyl-3-ol: 1 part, octamethylcyclotetrasiloxane: 10 parts, 1, 1, 3, 3- Tetramethyl-1,3 bis[3-(oxiranylmethoxy)propyl]disiloxane: 2 parts, modified silver-coated nickel conductive powder: 75 parts, the B component includes the following weight Raw materials: base: 20 parts, platinum catalyst: 0.0005 parts, octamethylcyclotetrasiloxane: 10 parts, 1,1,3,3-tetramethyl-1,3 bis[3-(epoxy Ethylmethoxy)propyl]disiloxane: 2 parts, modified silver-coated nickel conductive powder: 60 parts, the base material is made of vinyl silicone oil having a molecular weight of 40 W: 120 parts, hydrophobic white carbon black R972 :70 copies, Hexamethyldisilazane: 3 parts, distilled water: 0.3 parts by dehydration blending, the modified silver-coated nickel conductive powder refers to a silver-coated nickel conductive powder having a surface coated with a silane coupling agent KH-171.

The preparation method of the above two-component additive anti-settling conductive silica gel is as follows:

1) The conductive powder is dried, and 100-120 um of silver-coated nickel conductive powder is placed in a blast drying oven and dried at 80 ° C for 1 hour;

2) Conductive powder coating, the surface of the conductive powder obtained in the step 1) is subjected to wet surface treatment, that is, the silane coupling agent KH-171 is mixed with a 95% ethanol solution to be hydrolyzed for 30 minutes, wherein the silane couple is divided by weight. The bonding agent KH-171 accounts for 10% by weight, and then the conductive powder is added to the mixed solution of the silane coupling agent KH-171 and ethanol, and the silane coupling agent KH-171 is 20wt% of the weight of the conductive powder, and is fully stirred and mixed for 30 minutes. After that, it is heated in a water bath of 80 ° C to evaporate the ethanol to obtain a silver-coated nickel conductive powder coated with a layer of a silane coupling agent KH-171;

3) Preparation of anti-settling type base material: vinyl silicone oil having a molecular weight of 40 W: 120 parts, hydrophobic white carbon black R972: 70 parts, hexamethyldisilazane: 3 parts, distilled water: 0.3 parts, placed under vacuum kneading In the machine, dewatering and blending at 150 ° C, pressure 0.002Mpa to obtain anti-settling type base;

4) Preparation of component A: base material obtained in step 3): 20 parts, phenyl hydrosilane oil: 10 parts, inhibitor 3,5-dimethyl-1-hexynyl-3-ol: 1 , octamethylcyclotetrasiloxane: 10 parts, 1,1,3,3-tetramethyl-1,3 bis[3-(oxiranylmethoxy)propyl]disiloxane: 2 parts, modified silver-coated nickel conductive powder obtained in step 2): 75 parts, placed in a double planetary mixer and stirred for 1 hour;

5) Preparation of component B: The base obtained in the step 3): 20 parts, platinum catalyst: 0.0005 parts, octamethylcyclotetrasiloxane: 10 parts, 1,1,3,3-tetramethyl- 1,3 bis[3-(oxiranylethyloxy)propyl]disiloxane: 2 parts, modified silver-coated nickel conductive powder obtained in the step 2): 60 parts, placed in a double planetary mixer Stir and mix for 1 hour;

6) Mixing: After mixing the component A and the component B in a mass ratio of 1:1, the mixture was degassed under a pressure of 0.005 MPa for 40 minutes to obtain an anti-settling conductive silica gel.

Example 7

A two-component addition-forming anti-settling conductive silica gel is prepared by mixing A component and B component at a mass ratio of 1:1, and the component A comprises the following raw materials by weight: base material: 60 parts, phenyl group Hydrogen-containing silicone oil: 6 parts, inhibitor 3,5-dimethyl-1-hexynyl-3-ol: 0.5 part, hexamethyldisiloxane: 5 parts, 1,1,3,3-four Methyl-1,3 bis[3-(oxiranylmethoxy)propyl]disiloxane: 0.005 parts, modified silver-clad glass conductive powder: 60 parts, the B component includes the following parts by weight Raw material: base: 60 parts, platinum catalyst: 0.0001 part, hexamethyldisiloxane: 10 parts, 1,1,3,3-tetramethyl-1,3 bis[3-(oxiranylethyl) Methoxy)propyl]disiloxane: 1 part, modified silver-clad glass conductive powder: 40 parts, the base material is a vinyl silicone oil having a molecular weight of 2 W: 60 parts, a vinyl silicone oil having a molecular weight of 40 W: 60 Part, hydrophobic white carbon black R972: 70 parts, hexamethyldisilazane: 8 parts, distilled water: 0.8 parts by dehydration blending, the modified absorbing silicon carbide refers to the surface coated with titanate Silver-coated glass conductive powder of KR-TTS.

The preparation method of the above two-component additive anti-settling conductive silica gel is as follows:

1) The conductive powder is dried, and the 120-150 um silver-clad glass conductive powder is placed in a blast drying oven and dried at 80 ° C for 1 hour;

2) Conductive powder coating, the surface of the conductive powder obtained in the step 1) is subjected to a wet surface treatment, that is, the titanate coupling agent KR-TTS is mixed with a 95% ethanol solution to be hydrolyzed for 30 minutes, wherein by weight, The titanate coupling agent KR-TTS accounts for 10% by weight, and then the conductive powder is added to the mixed solution of the titanate coupling agent KR-TTS and ethanol. The titanate coupling agent KR-TTS is 20wt of the weight of the conductive powder. %, after thorough stirring and mixing for 30 min, placed in a water bath at 80 ° C to evaporate the ethanol to obtain a conductive powder coated with a layer of titanate coupling agent KR-TTS;

3) Preparation of anti-settling type base material: vinyl silicone oil having a molecular weight of 2 W: 60 parts, vinyl silicone oil having a molecular weight of 10 W: 60 parts, hydrophobic white carbon black R972: 70 parts, hexamethyldisilazane: 8 Parts, distilled water: 0.8 parts of dehydration is placed in a vacuum kneader, dehydrated and blended at 100 ° C, pressure 0.002Mpa to obtain anti-settling type base;

4) Preparation of component A: the base material obtained in the step 3): 60 parts, phenyl hydrosilane oil: 6 parts, Formulation 3,5-Dimethyl-1-hexynyl-3-ol: 0.5 part, hexamethyldisiloxane: 5 parts, 1,1,3,3-tetramethyl-1,3 bis [ 3-(oxiranylmethoxy)propyl]disiloxane: 0.005 parts, modified silver-clad glass conductive powder: 60 parts, placed in a double planetary mixer and stirred for 1 hour;

5) Preparation of component B: taking the base material obtained in the step 3): 60 parts, platinum catalyst: 0.0001 part, hexamethyldisiloxane: 10 parts, tetramethyl-1, 3 bis [3- (ring Oxyethyl methoxy) propyl] disiloxane: 1 part, modified silver-coated glass conductive powder: 40 parts, placed in a double planetary mixer and stirred for 1 hour;

6) Mixing: After mixing the component A and the component B in a mass ratio of 1:1, the mixture was degassed under a pressure of 0.005 MPa for 40 minutes to obtain an anti-settling conductive silica gel.

Example 8

A two-component addition-forming anti-settling conductive silica gel is prepared by mixing A component and B component at a mass ratio of 1:1, and the component A comprises the following raw materials by weight: base material: 40 parts, phenyl group Hydrogenated silicone oil: 2 parts, inhibitor 1-ethynyl-1-cyclohexanol: 0.005 parts, hexamethyldisiloxane: 15 parts, titanate coupling agent KR-TTS: 2 parts, modified silver Glass-coated conductive powder: 40 parts, the B component comprises the following raw materials by weight: base: 40 parts, platinum catalyst: 0.0003 parts, hexamethyldisiloxane: 5 parts, titanate coupling agent KR -TTS: 0.005 parts, modified silver-clad glass conductive powder: 40 parts, the base material is a vinyl silicone oil having a molecular weight of 50 W: 120 parts, hydrophobic white carbon black R972: 70 parts, hexamethyldisilazane: 3 parts, distilled water: 0.8 parts by dehydration blending, the modified silver-coated glass conductive powder refers to a silver-clad glass conductive powder whose surface is coated with a silane coupling agent A-174.

The preparation method of the above two-component anti-settling type silicon-based conductive silica gel is as follows:

1) The conductive powder is dried, and the 150-200 um silver-clad glass conductive powder is placed in a blast drying oven and dried at 80 ° C for 1 hour;

2) Conductive powder coating, the surface of the conductive powder obtained in the step 1) is subjected to wet surface treatment, that is, the silane coupling agent A-174 is mixed with a 95% ethanol solution to be hydrolyzed for 30 minutes, wherein the silane couple is divided by weight. The crosslinking agent A-174 accounts for 5% by weight, and then the conductive powder is added to the mixture of the silane coupling agent A-174 and ethanol. In the solution, the silane coupling agent A-174 is 20wt% of the weight of the conductive powder, and after being fully stirred and mixed for 30 minutes, it is heated in a water bath of 80 ° C to evaporate the ethanol to obtain a surface coated with a silane coupling agent A-174. Conductive powder

3) Preparation of anti-settling type base material: vinyl silicone oil having a molecular weight of 50 W: 120 parts, hydrophobic white carbon black R972: 70 parts, hexamethyldisilazane: 3 parts, distilled water: 0.8 parts dehydrated in a vacuum In the kneading machine, dewatering and blending at 100 ° C and a pressure of 0.002 MPa to obtain an anti-settling type base;

4) Preparation of component A: base material obtained in step 3): 40 parts, phenyl hydrosilane oil: 2 parts, inhibitor 1-ethynyl-1-cyclohexanol: 0.005 parts, hexamethyldisiloxane Oxygenane: 15 parts, titanate coupling agent KR-TTS: 2 parts, modified silver-coated glass conductive powder obtained in step 2): 40 parts, placed in a double planetary mixer and stirred for 1 hour;

5) Preparation of component B: taking the base material obtained in the step 3): 40 parts, platinum catalyst: 0.0003 parts, hexamethyldisiloxane: 5 parts, titanate coupling agent KR-TTS: 0.005 parts, Modified silver-clad glass conductive powder: 40 parts, placed in a double planetary mixer and stirred for 1 hour;

6) Mixing: After mixing the component A and the component B in a mass ratio of 1:1, the mixture was degassed under a pressure of 0.005 MPa for 40 minutes to obtain an anti-settling conductive silica gel.

Example 9

A two-component addition-forming anti-settling conductive silica gel is prepared by mixing A component and B component at a mass ratio of 1:1, and the component A comprises the following raw materials by weight: base material: 40 parts, phenyl group Hydrogen-containing silicone oil: 10 parts, inhibitor 1-ethynyl-1-cyclohexanol: 1 part, hexamethyldisiloxane: 5 parts, aluminate coupling agent DL-411: 0.005 parts, modified silver Nickel-coated conductive powder: 75 parts, the B component includes the following raw materials by weight: base: 40 parts, platinum catalyst: 0.0001 parts, hexamethyldisiloxane: 5 parts, aluminate coupling agent DL -411: 0.005 parts, modified silver-coated nickel conductive powder: 75 parts, the base material is a vinyl silicone oil having a molecular weight of 2 W: 60 parts, a vinyl silicone oil having a molecular weight of 50 W: 60 parts, and a hydrophobic white carbon black R972: 70 parts, hexamethyldisilazane: 8 parts, distilled water: 0.8 parts by dehydration blending, the modified silver-coated nickel conductive powder refers to silver coated with an aluminate coupling agent DL-411 Nickel-plated conductive powder.

The preparation method of the above two-component additive anti-settling conductive silica gel is as follows:

1) The conductive powder is dried, and 150-200 um of silver-coated nickel conductive powder is placed in a blast drying oven and dried at 80 ° C for 1 hour;

2) Conductive powder coating, wet-surface treatment of the silver-coated nickel conductive powder obtained in the step 1), that is, the aluminate coupling agent DL-411 is mixed with a 95% ethanol solution to be hydrolyzed for 30 minutes, wherein by weight The aluminate coupling agent DL-411 accounts for 5 wt%, and then the conductive powder is added to a mixed solution of the aluminate coupling agent DL-411 and ethanol, and the aluminate coupling agent DL-411 is a conductive powder. 20 wt% of the weight, after thorough stirring and mixing for 30 min, placed in a water bath at 80 ° C to evaporate the ethanol to obtain a silver-coated nickel conductive powder coated with a layer of aluminate coupling agent DL-411;

3) Preparation of anti-settling type base material: vinyl silicone oil having a molecular weight of 2 W: 60 parts, vinyl silicone oil having a molecular weight of 10 W: 60 parts, hydrophobic white carbon black R972: 70 parts, hexamethyldisilazane: 8 parts, distilled water: 0.8 parts of dehydration is placed in a vacuum kneader, dehydrated and blended at 100 ° C, pressure 0.002Mpa to obtain anti-settling type base;

4) Preparation of component A: base material obtained in step 3): 40 parts, methylphenyl silicone oil: 10 parts, inhibitor 1-ethynyl-1-cyclohexanol: 1 part, hexamethyldisiloxane Oxytomane: 5 parts, aluminate coupling agent DL-411: 0.005 parts, modified silver-coated nickel conductive powder obtained in step 2): 75 parts, placed in a double planetary mixer and stirred for 1 hour;

5) Preparation of component B: taking the base material obtained in the step 3): 40 parts, platinum catalyst: 0.0001 parts, hexamethyldisiloxane: 5 parts, aluminate coupling agent DL-411: 0.005 parts, The modified silver-coated nickel conductive powder obtained in the step 2): 75 parts, placed in a double planetary mixer and stirred and mixed for 1 hour;

6) Mixing: After mixing the component A and the component B in a mass ratio of 1:1, the mixture was degassed under a pressure of 0.005 MPa for 40 minutes to obtain an anti-settling conductive silica gel.

Comparative Example 1:

The components of Example 1 were prepared at room temperature, base: 20 parts, methyl hydrogen silicone oil: 2 parts, Inhibitor 2-methyl-3-butynyl-2-ol: 0.005 parts, dimethyl silicone oil: 5 parts, silane coupling agent A-171: 0.005 parts, 10-30 um pure silver conductive powder: 40 parts, Stirring and mixing for 1 hour to obtain component A, base: 20 parts, platinum catalyst: 0.0003 parts, dimethyl silicone oil: 10 parts, silane coupling agent A-171:1 parts, 10-30 um pure silver conductive powder: 40 parts, stirred and mixed for 1 hour to obtain component B, which is composed of vinyl silicone oil having a molecular weight of 2 W: 50 parts, vinyl silicone oil having a molecular weight of 10 W: 50 parts, hydrophobic white carbon black R972: 60 parts stirring The mixture was obtained by mixing and mixing the component A and the component B in a mass ratio of 1:1 to obtain a conductive silica gel.

Comparative Example 2:

The components of Example 2 were prepared at room temperature, base: 40 parts, methylhydrogen silicone oil: 6 parts, inhibitor 2-methyl-3-butynyl-2-ol: 0.5 part, dimethicone : 10 parts, silane coupling agent A-171:1 parts, 10-30um pure nickel conductive powder: 60 parts, stirred and mixed for 1 hour to obtain component A, base material: 40 parts, platinum catalyst: 0.0003 parts, two Methyl silicone oil: 10 parts, silane coupling agent A-171:1 parts, 10-30um pure nickel conductive powder: 65 parts, stirred and mixed for 1 hour to obtain component B, the base material is made of vinyl with a molecular weight of 10W Silicone oil: 50 parts, vinyl silicone oil having a molecular weight of 20 W: 50 parts, hydrophobic white carbon black R972: 60 parts by stirring and mixing, and component A and component B are uniformly mixed at a mass ratio of 1:1 to obtain a conductive silica gel.

Comparative Example 3:

The components of Example 3 were prepared at room temperature, base: 60 parts, hydroxy-containing silicone oil: 10 parts, inhibitor 3-methyl-1-ethynyl-3-ol: 1 part, tetramethyltetra Vinyl cyclotetrasiloxane: 15 parts, titanate coupling agent KR-TTS: 2 parts, 30-50um nickel-coated graphite conductive powder: 75 parts, stirred and mixed for 1 hour to obtain component A, the base material: 60 parts, platinum catalyst: 0.0005 parts, tetramethyltetravinylcyclotetrasiloxane: 15 parts, titanate coupling agent KR-TTS: 1 part, 30-50 um of nickel-coated graphite conductive powder: 75 parts, The mixture was stirred for 1 hour to obtain a component B, which was obtained by stirring and mixing a vinyl silicone oil having a molecular weight of 20 W: 80 parts, and a hydrophobic white carbon black R972: 50 parts. The mass ratio of the component A and the component B was 1 by mass. : 1 Mix well to obtain conductive silica gel.

Comparative Example 4:

The components of Example 4 were prepared at room temperature, base: 20 parts, hydroxyl-containing silicone oil: 6 parts, inhibitor 3-methyl-1-ethynyl-3-ol: 0.5 part, tetramethyltetra Vinyl cyclotetrasiloxane: 15 parts, titanate coupling agent KR-TTS: 1 part, 30-50um of silver-clad aluminum conductive powder: 60 parts, stirred and mixed for 1 hour to obtain component A, the base material: 20 parts, platinum catalyst: 0.0005 parts, tetramethyltetravinylcyclotetrasiloxane: 15 parts, titanate coupling agent KR-TTS: 2 parts, 30-50um of silver-clad aluminum conductive powder: 75 parts, The mixture was stirred for 1 hour to obtain a component B. The base material was obtained by mixing and mixing a vinyl silicone oil having a molecular weight of 20 W: 120 parts, and a hydrophobic white carbon black R972: 70 parts. The mass ratio of the component A and the component B was 1 by mass. : 1 Mix well to obtain conductive silica gel.

Comparative Example 5:

The components of Example 5 were prepared at room temperature, base: 60 parts, phenyl hydrosilane oil: 2 parts, inhibitor 3,5-dimethyl-1-hexynyl-3-ol: 0.005 parts , octamethylcyclotetrasiloxane: 10 parts, aluminate coupling agent DL-411:1 parts, 50-80um silver-coated copper conductive powder: 40 parts, stirred and mixed for 1 hour to obtain component A, base Material: 60 parts, platinum catalyst: 0.0001 parts, octamethylcyclotetrasiloxane: 15 parts, aluminate coupling agent DL-411: 0.005 parts, 50-80 um silver-coated copper conductive powder: 40 parts, stirring The mixture was mixed for 1 hour to obtain a component B. The base material was obtained by mixing and mixing a vinyl silicone oil having a molecular weight of 30 W: 120 parts, and a hydrophobic white carbon black R972: 70 parts. The mass ratio of the component A and the component B was 1: 1 Mix well to obtain conductive silica gel.

Comparative Example 6:

The components of Example 6 were prepared at room temperature, base: 20 parts, phenyl hydrosilane oil: 10 parts, inhibitor 3,5-dimethyl-1-hexynyl-3-ol: 1 part Octamethylcyclotetrasiloxane: 10 parts, 1,1,3,3-tetramethyl-1,3 bis[3-(oxiranylmethoxy)propyl]disiloxane: 2 50 parts, 50-80um silver-coated nickel conductive powder: 75 parts, stirred and mixed for 1 hour to obtain component A, base material: 20 parts, platinum catalyst: 0.0005 parts, octamethylcyclotetrasiloxane: 10 parts, 1 1,1,3,3-tetramethyl-1,3 bis[3-(oxiranylmethoxy)propyl]disiloxane: 2 parts, 50-80 um silver-coated nickel conductive powder: 60 parts Stir Mix and mix for 1 hour to obtain component B. The base material is obtained by mixing and mixing vinyl silicone oil of molecular weight: 40 parts, hydrophobic type white carbon black R972: 70 parts, and mixing component A and component B by mass ratio. : 1 Mix well to obtain conductive silica gel.

Comparative Example 7:

The components of Example 7 were prepared at room temperature, base: 60 parts, phenyl hydrosilane oil: 6 parts, inhibitor 3,5-dimethyl-1-hexynyl-3-ol: 0.5 parts Hexamethyldisiloxane: 5 parts, 1,1,3,3-tetramethyl-1,3 bis[3-(oxiranylmethoxy)propyl]disiloxane: 0.005 parts 80-120um silver-coated glass conductive powder: 60 parts, stirred and mixed for 1 hour to obtain component A, base material: 60 parts, platinum catalyst: 0.0001 parts, hexamethyldisiloxane: 10 parts, tetramethyl -1,3 bis[3-(oxiranylmethoxy)propyl]disiloxane: 1 part, 80-120 um of silver-coated glass conductive powder: 40 parts, stirred and mixed for 1 hour to obtain component B, The base material is obtained by mixing vinyl chloride oil having a molecular weight of 2 W: 60 parts, vinyl silicone oil having a molecular weight of 40 W: 60 parts, hydrophobic white carbon black R972: 70 parts, and mixing the components A and B by mass ratio. 1:1 mixed to obtain conductive silica gel.

Comparative Example 8:

The components of Example 8 were prepared at room temperature, base: 40 parts, phenyl hydrosilane oil: 2 parts, inhibitor 1-ethynyl-1-cyclohexanol: 0.005 parts, hexamethyldisiloxane Alkane: 15 parts, titanate coupling agent KR-TTS: 2 parts, 150-200um silver-coated glass conductive powder: 40 parts, stirred and mixed for 1 hour to obtain component A, base material: 40 parts, platinum catalyst: 0.0003 parts, hexamethyldisiloxane: 5 parts, titanate coupling agent KR-TTS: 0.005 parts, 150-200um silver-coated glass conductive powder: 40 parts, stirred and mixed for 1 hour to obtain component B, The base material is obtained by mixing 50 W of vinyl silicone oil: 120 parts, hydrophobic type white carbon black R972: 70 parts, and mixing the component A and the component B in a mass ratio of 1:1 to obtain a conductive silica gel.

Comparative Example 9:

The components of Example 9 were prepared at room temperature, base: 40 parts, phenyl hydrosilane oil: 10 parts, inhibitor 1-ethynyl-1-cyclohexanol: 1 part, hexamethyldisiloxane Alkane: 5 parts, aluminate coupling Agent DL-411: 0.005 parts, 150-200um silver-coated nickel conductive powder: 75 parts, stirred and mixed for 1 hour to obtain component A, base material: 40 parts, platinum catalyst: 0.0001 parts, hexamethyldisiloxane : 5 parts, aluminate coupling agent DL-411: 0.005 parts, 150-200um of silver-coated nickel conductive powder: 75 parts, stirred and mixed for 1 hour to obtain component B, the base material is made of vinyl silicone oil with a molecular weight of 2W : 60 parts, a vinyl silicone oil having a molecular weight of 50 W: 60 parts, and a hydrophobic white carbon black R972: 70 parts obtained by stirring and mixing, and the component A and the component B are uniformly mixed at a mass ratio of 1:1 to obtain a conductive silica gel.

To verify the performance of the products of the invention, we conducted the following tests:

(1) Volume resistivity test

The two electrodes of the resistor are pressed onto a molded piece having a thickness of 2 mm and a length and a width of 25.4 mm, and the resistance is obtained. The solid product resistivity is the product of the measured resistance value and the thickness, and the unit is Ω*cm. . The results are shown in Table 1. The obtained one-component high-temperature vulcanization conductive glue has good electrical conductivity.

(2) Bond strength test

The products prepared in Preparation Examples 1 to 9 and Comparative Examples 1 to 9 were spotted on a aluminum substrate by a dispenser to a strip of 1 mm high and 25 mm long, and after vulcanization at 160 ° C for 1 h, standard weights were used. The fixture was tested for adhesion and its bond strength to the aluminum substrate was calculated. The results are shown in Table 1. It shows that the one-component high-temperature vulcanization conductive glue of the present invention has good adhesion to the aluminum plate.

(3) Anti-settling test

The products prepared in Preparation Examples 1 to 9 and Comparative Examples 1 to 9 were stored at 0 to 5 ° C for 6 months, and the change in viscosity of the upper and lower layers was tested. The test was tested by a rheometer, and the instrument was equipped with two plates and plates. The pitch was 0.5 mm and the test temperature was 23 °C. The results are shown in Table 1, which shows that the one-component chamber high vulcanization conductive paste of the present invention has good anti-settling properties.

(4) Tear strength performance test

The products prepared in Preparation Examples 1 to 9 and Comparative Examples 1 to 9 were made into a sample having a thickness of 2 mm, baked at 160 ° C for 1 hour, and then punched into a crescent-shaped sample, which was then tested on a stretching machine. The tear strength of the coupon. The results are shown in Table 1, which shows that the one-component chamber high vulcanization conductive glue of the present invention has good tear strength.

(5) Elongation at break

The products prepared in Preparation Examples 1 to 9 and Comparative Examples 1 to 9 were made into a sample having a thickness of 2 mm, baked at 160 ° C for 1 hour, and then punched into a dumbbell-shaped swatch and then tested on a stretching machine. The elongation at break of the swatch. The elongation at break is the percentage of elongation of the swatch at the point of break.

According to the results of the data in Table 1, the conductive silica gel prepared by the present invention has good electrical conductivity, cohesiveness, anti-settling property, tear strength and elongation at break.

The above are only the preferred embodiments of the present invention, and are not intended to limit the present invention. Any modifications, equivalents, improvements, etc., which are within the spirit and scope of the present invention, should be included in the protection of the present invention. Within the scope.

Table 1: Product performance test data obtained in Examples 1-9 and Comparative Examples 1-9

Claims (10)

A two-component addition-formation anti-settling conductive silica gel characterized in that a component A and a component B are mixed at a mass ratio of 1:1, and the component A comprises the following raw materials by weight:

The component B comprises the following raw materials by weight:

The base material is prepared by dehydrating and blending 80-120 parts of vinyl silicone oil, 50-70 parts of fumed silica, 3-8 parts of hexamethyldisilazane and 0.2-1 part of distilled water; The modified conductive powder refers to a conductive powder whose surface is coated with a coupling agent. The two-component additive anti-settling conductive silica gel according to claim 1, wherein the conductive powder refers to pure silver conductive powder, pure nickel conductive powder, nickel-coated graphite conductive powder, and silver-coated aluminum conductive material. One or a mixture of two or more of powder, silver-clad copper conductive powder, silver-coated nickel conductive powder, and silver-clad glass conductive powder, and the powder has a particle diameter of 10 to 200 um. The two-component additive anti-settling conductive silica gel according to claim 1, wherein the inhibitor is 2-methyl-3-butynyl-2-ol, 3-methyl-1- Ethynyl-3-ol, 3, At least one of 5-dimethyl-1-hexynyl-3-ol, 1-ethynyl-1-cyclohexanol, and polyvinylpolysiloxane. The two-component additive anti-settling conductive silica gel according to claim 1, wherein the diluent is dimethyl silicone oil, tetramethyltetravinylcyclotetrasiloxane, and octamethyl ring. At least one of tetrasiloxane or hexamethyldisiloxane, wherein the hydrogen-containing silicone oil refers to one or more of methyl hydrogen silicone oil, methylphenyl silicone oil, and hydroxyl hydrogen silicone oil. The coupling agent is a silane coupling agent A-171, a titanate coupling agent KR-TTS, an aluminate coupling agent DL-411, an epoxy group, a hydroxyl group, a nitrile group, a carbonyl group, an ester group. One or a mixture of two or more of the silane coupling agents. A method for preparing a two-component additive anti-settling conductive silica gel, comprising the steps of: 1) Conductive powder drying: drying the conductive powder to remove moisture; 2) Conductive powder coating: the powder obtained in the step 1) is subjected to a surface treatment by a wet method, that is, the coupling agent is mixed with a 95% ethanol solution to be hydrolyzed, and then the conductive powder is added thereto, and the obtained mixture is subjected to After thorough stirring and mixing, the water is heated to volatilize the ethanol to obtain a conductive powder coated with a coupling agent on the surface, that is, the modified conductive powder; 3) Preparation of anti-settling type base material: 80-120 parts of vinyl silicone oil, 50-70 parts of fumed silica, 3-8 parts of hexamethyldisilazane and 0.2-1 part of distilled water are placed in a vacuum kneader Internally, dewatering and blending at 100-150 ° C and pressure <0.01 MPa to obtain an anti-settling type base; 4) Preparation of component A: 20 to 60 parts of the base material obtained in the step 3), 2 to 10 parts of the hydrogen-containing silicone oil, 0.005 to 1 part of the inhibitor, 5 to 15 parts of the diluent, and 0.005 to 2 parts of the coupling agent. 40 to 75 parts of the modified conductive powder are stirred and mixed uniformly; 5) Preparation of component B: taking 20 to 60 parts of the base material obtained in step 3), 0.0001 to 0.0005 parts of platinum catalyst, 5 to 15 parts of diluent, 0.005 to 2 parts of coupling agent, and modified conductive powder 40 to 75 Mix and mix evenly; 6) Mixing: After mixing the component A and the component B in a mass ratio of 1:1, the mixture is degassed under a pressure of <0.01 MPa for 20 to 40 minutes to obtain an anti-settling conductive silica gel. The method for preparing a two-component additive anti-settling conductive silica gel according to claim 5, wherein the vinyl silicone oil in the step 3) is a polydiorganosiloxane liquid containing a vinyl group. The gum has a molecular weight of 2 to 50 w. The method for preparing a two-component additive anti-settling conductive silica gel according to claim 5, wherein the conductive powder refers to pure silver conductive powder, pure nickel conductive powder, nickel-coated graphite conductive powder, and silver. One or a mixture of two or more of aluminum-clad conductive powder, silver-clad copper conductive powder, silver-coated nickel conductive powder, and silver-clad glass conductive powder, and the powder has a particle diameter of 10 to 200 μm. The method for preparing a two-component additive anti-settling conductive silica gel according to claim 5, wherein the coupling agent in the mixture of the coupling agent and the 95% ethanol solution in the step 2) accounts for 2~ 10wt%, the mass of the coupling agent is 10-20% by weight of the absorbing agent. The method for preparing a two-component additive anti-settling conductive silica gel according to any one of claims 5-8, wherein the inhibitor in the step 4) is 2-methyl-3-butyl Alkynyl-2-ol, 3-methyl-1-ethynyl-3-ol, 3,5-dimethyl-1-hexynyl-3-ol, 1-ethynyl-1-cyclohexanol and polyethene At least one of the polysiloxanes, the hydrogen-containing silicone oil refers to one or a mixture of two or more of methylhydrogen silicone oil, methylphenyl silicone oil, and hydroxyl hydrogen-containing silicone oil. The method for preparing a two-component additive anti-settling conductive silica gel according to any one of claims 5-8, wherein the diluent described in steps 4) and 5) is dimethicone, At least one of tetramethyltetravinylcyclotetrasiloxane, octamethylcyclotetrasiloxane or hexamethyldisiloxane, the coupling agent is a silane coupling agent A-171, titanium One or a mixture of two or more of an acid ester coupling agent KR-TTS, an aluminate coupling agent DL-411, a silane coupling agent containing an epoxy group, a hydroxyl group, a nitrile group, a carbonyl group, and an ester group.