CN110818893A - Polymerization production method of antibacterial nylon 6 slices - Google Patents
Polymerization production method of antibacterial nylon 6 slices Download PDFInfo
- Publication number
- CN110818893A CN110818893A CN201910916061.5A CN201910916061A CN110818893A CN 110818893 A CN110818893 A CN 110818893A CN 201910916061 A CN201910916061 A CN 201910916061A CN 110818893 A CN110818893 A CN 110818893A
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- Prior art keywords
- pressure
- heating
- reaction
- solution
- caprolactam
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- 229920002292 Nylon 6 Polymers 0.000 title claims abstract description 33
- 238000006116 polymerization reaction Methods 0.000 title claims abstract description 31
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 29
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 14
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 claims abstract description 46
- 238000010438 heat treatment Methods 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 230000001681 protective effect Effects 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000001816 cooling Methods 0.000 claims abstract description 17
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 13
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 12
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims abstract description 10
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- 238000007599 discharging Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000005711 Benzoic acid Substances 0.000 claims abstract description 5
- 235000010233 benzoic acid Nutrition 0.000 claims abstract description 5
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 5
- 150000001408 amides Chemical class 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 3
- 239000003242 anti bacterial agent Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 230000000845 anti-microbial effect Effects 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/40—Polyamides containing oxygen in the form of ether groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/08—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino-carboxylic acids
- C08G69/14—Lactams
- C08G69/16—Preparatory processes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0806—Silver
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polyamides (AREA)
Abstract
The invention relates to a polymerization production method of antibacterial nylon 6 slices, which comprises the following steps: 1) adding amide, nano-silver and deionized water into a high-pressure reaction kettle, filling protective gas to replace air, heating for reaction, cooling and reducing pressure to remove water, and performing hydrolysis reaction on caprolactam to obtain a solution A; 2) putting the solution A and ethylene glycol into a polymerization reactor, filling protective gas into the polymerization reactor to replace air, heating, adding concentrated sulfuric acid, continuously heating for reaction at normal pressure, then reducing pressure, removing water, keeping pressure and heat, continuously reacting, and cooling to obtain a solution B; 3) adding caprolactam and benzoic acid or acetic acid into a polymerization reactor, heating under protective atmosphere, maintaining pressure, heating and pressurizing for reaction, then cooling and depressurizing, continuing to react, discharging, extracting and drying to obtain the antibacterial nylon 6 slice. The invention has the advantages that: on the premise of ensuring the mechanical property of the nylon 6 slice, the antibacterial property of the nylon 6 slice is improved.
Description
Technical Field
The invention relates to a polymerization production method of an antibacterial nylon 6 slice.
Background
Along with the improvement of living standard of people, the requirement on the environment is higher and higher. Antimicrobial materials have become an emerging industry. The antibacterial material is characterized by inhibiting the growth and reproduction of bacteria and keeping the environment clean and sanitary in the long-term use process.
In the prior art, the antibacterial property of nylon 6 is realized, and an inorganic antibacterial agent is generally added into a nylon 6 matrix. However, the addition of the inorganic antibacterial agent can improve the antibacterial performance of nylon 6 and greatly reduce the mechanical performance of nylon 6.
Disclosure of Invention
The invention provides a polymerization production method of antibacterial nylon 6 slices, aiming at overcoming the defects in the prior art, realizing the antibacterial property of the nylon 6 slices during polymerization production and ensuring that the mechanical property of the nylon 6 slices is not influenced.
The technical solution of the invention is as follows: a polymerization production method of antibacterial nylon 6 slices comprises the following steps:
1) adding the following components in a high-pressure reaction kettle in a mass ratio of (2.5-4.0) to (0.15-0.25): 1, filling protective gas into caprolactam, nano silver and deionized water to replace air, heating to 230 ℃ in 215-1.1 MPa, reacting for 2.5-3.5 hours, cooling to 125 ℃ in 115-0 ℃, reducing the pressure to remove water, and performing hydrolysis reaction on caprolactam to obtain a solution A;
2) putting the solution A prepared in the step 1) and glycol with the molecular weight of 500-9000 into a polymerization reactor according to the mass ratio of 1:3-1:5, filling protective gas into the polymerization reactor to replace air, adding concentrated sulfuric acid which is 0.6-0.8% of the total weight of the solution A when the temperature is increased to 92-96 ℃, continuously heating to 110-120 ℃, carrying out normal pressure reaction for 2.5-3.5 hours, then reducing the pressure to-0.03-0.04 MPa to remove water, keeping the pressure, keeping the temperature at 110-120 ℃, continuously reacting for 1.5-2.5 hours, and cooling to obtain a solution B;
3) adding benzoic acid or acetic acid accounting for 0.3-0.4% of the total weight of caprolactam and caprolactam into the polymerization reactor in the step 2), heating at the speed of 9-10 ℃/10min under the protective atmosphere, keeping the pressure at 0.04-0.06MPa, heating to 265-275 ℃, carrying out pressurized reaction for 2.5-3.5 hours, then cooling to 245-255 ℃, reducing the pressure to-0.03-0.04 MPa, continuing the reaction for 1.2-1.8 hours, discharging, extracting and drying to obtain the antibacterial nylon 6 slice.
Preferably, the breaking elongation of the antibacterial nylon 6 slice is 45-50%, and the notch impact strength is 32-38J/m.
The invention has the advantages that: the caprolactam which is a main production raw material is prepared into a modifying reagent and added into a polymerization production system of the nylon 6 slice, the preparation process is simple, the effect is obvious, the antibacterial property is good, the breaking elongation performance and the notch impact strength of the product are improved, the tensile strength and the bending modulus can be comparable to those of an unmodified product, and the product has excellent comprehensive performance. On the premise of ensuring the mechanical property of the nylon 6 slice, the antibacterial property of the nylon 6 slice is improved.
Detailed Description
The present invention will be described in further detail with reference to examples and specific embodiments.
Example 1
A polymerization production method of antibacterial nylon 6 slices comprises the following steps:
1) adding a mixture of the components in a mass ratio of 2.5: 0.25: 1, filling protective gas into caprolactam, nano silver and deionized water to replace air, heating to 215 ℃, reacting for 3.5 hours under the pressure of 1.1MPa, cooling to 125 ℃, reducing the pressure to remove water, and performing hydrolysis reaction on the caprolactam to obtain a solution A;
2) putting the solution A prepared in the step 1) and glycol with the molecular weight of 500 into a polymerization reactor according to the mass ratio of 1:3, filling protective gas into the polymerization reactor to replace air, adding concentrated sulfuric acid with the weight of 0.6% of the total weight of the solution A when the temperature is raised to 92 ℃, continuously raising the temperature to 110 ℃, reacting for 2.5 hours under normal pressure, then reducing the pressure to-0.04 MPa to remove water, keeping the pressure, keeping the temperature at 120 ℃, continuously reacting for 2.5 hours, and cooling to obtain a solution B;
3) adding benzoic acid accounting for 0.4 percent of the total weight of caprolactam and caprolactam into the polymerization reactor in the step 2), heating at the speed of 10 ℃/10min under the protective atmosphere, keeping the pressure at 0.06MPa, heating to 265 ℃, carrying out pressurized reaction for 2.5 hours, then cooling to 245 ℃, reducing the pressure to-0.04 MPa, continuing the reaction for 1.8 hours, discharging, extracting and drying to obtain the antibacterial nylon 6 slice.
The elongation at break of the obtained antibacterial nylon 6 slice is 45 percent, and the notch impact strength is 32J/m.
Example 2
A polymerization production method of antibacterial nylon 6 slices comprises the following steps:
1) adding a mixture of the components in a mass ratio of 4.0: 0.15: 1, filling protective gas into caprolactam, nano silver and deionized water to replace air, heating to 230 ℃, reacting for 2.5 hours under the pressure of 0.9MPa, cooling to 115 ℃, reducing the pressure to remove water, and performing hydrolysis reaction on the caprolactam to obtain a solution A;
2) putting the solution A prepared in the step 1) and glycol with the molecular weight of 9000 into a polymerization reactor according to the mass ratio of 1:5, filling protective gas into the polymerization reactor to replace air, adding concentrated sulfuric acid with the weight of 0.8% of the total weight of the solution A when the temperature is raised to 96 ℃, continuously raising the temperature to 120 ℃, reacting at normal pressure for 3.5 hours, then reducing the pressure to-0.03 MPa to remove water, keeping the pressure, keeping the temperature at 110 ℃, continuously reacting for 1.5 hours, and cooling to obtain a solution B;
3) adding acetic acid accounting for 0.3 percent of the total weight of caprolactam and caprolactam into the polymerization reactor in the step 2), heating at the speed of 9 ℃/10min under the protective atmosphere, keeping the pressure at 0.04-MPa, heating to 275 ℃, pressurizing for reaction for 3.5 hours, then cooling to 255 ℃, reducing the pressure to-0.03 MPa, continuing the reaction for 1.2 hours, discharging, extracting and drying to obtain the antibacterial nylon 6 slice.
The obtained antibacterial nylon 6 slice has the elongation at break of 50 percent and the notch impact strength of 38J/m.
Example 3
A polymerization production method of antibacterial nylon 6 slices comprises the following steps:
1) adding a mixture of the components in a mass ratio of 3.0: 0.2: 1, filling protective gas into caprolactam, nano silver and deionized water to replace air, heating to 220 ℃, reacting for 3 hours under the pressure of 1.0MPa, cooling to 120 ℃, reducing the pressure to remove water, and performing hydrolysis reaction on the caprolactam to obtain a solution A;
2) putting the solution A prepared in the step 1) and glycol with the molecular weight of 6000 into a polymerization reactor according to the mass ratio of 1:4, filling protective gas into the polymerization reactor to replace air, adding concentrated sulfuric acid with the weight of 0.7% of the total weight of the solution A when the temperature is raised to 94 ℃, continuously raising the temperature to 115 ℃, reacting for 3 hours under normal pressure, then reducing the pressure to-0.03 MPa to remove water, keeping the pressure, keeping the temperature at 115 ℃, continuously reacting for 2 hours, and reducing the temperature to obtain a solution B;
3) adding benzoic acid accounting for 0.35 percent of the total weight of caprolactam and caprolactam into the polymerization reactor in the step 2), heating at the speed of 9 ℃/10min under the protective atmosphere, keeping the pressure at 0.05MPa, heating to 270 ℃, pressurizing for reaction for 3 hours, then cooling to 250 ℃, reducing the pressure to-0.03 MPa, continuing the reaction for 1.5 hours, discharging, extracting and drying to obtain the antibacterial nylon 6 slice.
The obtained antibacterial nylon 6 slice has the elongation at break of 48 percent and the notch impact strength of 35J/m.
All the above components are prior art, and those skilled in the art can use any model and existing design that can implement their corresponding functions.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various changes and modifications can be made without departing from the inventive concept of the present invention, and these changes and modifications are all within the scope of the present invention.
Claims (2)
1. A polymerization production method of antibacterial nylon 6 slices is characterized by comprising the following steps:
1) adding the following components in a high-pressure reaction kettle in a mass ratio of (2.5-4.0) to (0.15-0.25): 1, filling protective gas into caprolactam, nano silver and deionized water to replace air, heating to 230 ℃ in 215-1.1 MPa, reacting for 2.5-3.5 hours, cooling to 125 ℃ in 115-0 ℃, reducing the pressure to remove water, and performing hydrolysis reaction on caprolactam to obtain a solution A;
2) putting the solution A prepared in the step 1) and glycol with the molecular weight of 500-9000 into a polymerization reactor according to the mass ratio of 1:3-1:5, filling protective gas into the polymerization reactor to replace air, adding concentrated sulfuric acid which is 0.6-0.8% of the total weight of the solution A when the temperature is increased to 92-96 ℃, continuously heating to 110-120 ℃, carrying out normal pressure reaction for 2.5-3.5 hours, then reducing the pressure to-0.03-0.04 MPa to remove water, keeping the pressure, keeping the temperature at 110-120 ℃, continuously reacting for 1.5-2.5 hours, and cooling to obtain a solution B;
3) adding benzoic acid or acetic acid accounting for 0.3-0.4% of the total weight of caprolactam and caprolactam into the polymerization reactor in the step 2), heating at the speed of 9-10 ℃/10min under the protective atmosphere, keeping the pressure at 0.04-0.06MPa, heating to 265-275 ℃, carrying out pressurized reaction for 2.5-3.5 hours, then cooling to 245-255 ℃, reducing the pressure to-0.03-0.04 MPa, continuing the reaction for 1.2-1.8 hours, discharging, extracting and drying to obtain the antibacterial nylon 6 slice.
2. The method for producing the antibacterial nylon 6 chip by polymerization as claimed in claim 1, wherein the elongation at break of the antibacterial nylon 6 chip is 45-50%, and the notched impact strength is 32-38J/m.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910916061.5A CN110818893A (en) | 2019-09-26 | 2019-09-26 | Polymerization production method of antibacterial nylon 6 slices |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910916061.5A CN110818893A (en) | 2019-09-26 | 2019-09-26 | Polymerization production method of antibacterial nylon 6 slices |
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| CN110818893A true CN110818893A (en) | 2020-02-21 |
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| CN201910916061.5A Pending CN110818893A (en) | 2019-09-26 | 2019-09-26 | Polymerization production method of antibacterial nylon 6 slices |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021203240A1 (en) * | 2020-04-07 | 2021-10-14 | 江苏弘盛新材料股份有限公司 | Anti-static and anti-microbial nylon 6 and preparation method therefor |
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| CN102382296A (en) * | 2011-08-17 | 2012-03-21 | 浙江华建尼龙有限公司 | Production process for preparing fiber-grade nylon 6 chips with extracted aqueous concentrated solution and apparatus thereof |
| CN102702509A (en) * | 2012-05-17 | 2012-10-03 | 上海仕天工程塑料有限公司 | Silver-containing nylon 6-based composite resin material and preparation method thereof |
| CN105669969A (en) * | 2016-02-01 | 2016-06-15 | 东华大学 | Nylon 6 polymerization method and direct spinning method of melt of polymer obtained with nylon 6 polymerization method |
| US9764964B2 (en) * | 2012-01-17 | 2017-09-19 | Shanghai Genius Advanced Material (Group) Co., Ltd. | Application of lactam as solvent in nanomaterial preparation |
| US10092486B2 (en) * | 2009-09-18 | 2018-10-09 | International Flavors & Fragrances Inc. | Polyurea or polyurethane capsules |
| CN108774318A (en) * | 2018-07-12 | 2018-11-09 | 中仑塑业（福建）有限公司 | A kind of antistatic nylon 6 and preparation method thereof |
| CN109880079A (en) * | 2019-03-27 | 2019-06-14 | 江苏弘盛新材料股份有限公司 | A kind of antistatic antibiotic nylon 6 and preparation method thereof |
-
2019
- 2019-09-26 CN CN201910916061.5A patent/CN110818893A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10092486B2 (en) * | 2009-09-18 | 2018-10-09 | International Flavors & Fragrances Inc. | Polyurea or polyurethane capsules |
| CN102382296A (en) * | 2011-08-17 | 2012-03-21 | 浙江华建尼龙有限公司 | Production process for preparing fiber-grade nylon 6 chips with extracted aqueous concentrated solution and apparatus thereof |
| US9764964B2 (en) * | 2012-01-17 | 2017-09-19 | Shanghai Genius Advanced Material (Group) Co., Ltd. | Application of lactam as solvent in nanomaterial preparation |
| CN102702509A (en) * | 2012-05-17 | 2012-10-03 | 上海仕天工程塑料有限公司 | Silver-containing nylon 6-based composite resin material and preparation method thereof |
| CN105669969A (en) * | 2016-02-01 | 2016-06-15 | 东华大学 | Nylon 6 polymerization method and direct spinning method of melt of polymer obtained with nylon 6 polymerization method |
| CN108774318A (en) * | 2018-07-12 | 2018-11-09 | 中仑塑业（福建）有限公司 | A kind of antistatic nylon 6 and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021203240A1 (en) * | 2020-04-07 | 2021-10-14 | 江苏弘盛新材料股份有限公司 | Anti-static and anti-microbial nylon 6 and preparation method therefor |
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Application publication date: 20200221 |