JP2001262121A - Modified silicone-based sealant composition excellent in thixotropy - Google Patents

Abstract

PROBLEM TO BE SOLVED: To obtain a modified silicone-based sealant composition added with excellent thixotropy and presenting no dropping without using any swelling process. SOLUTION: This sealant composition is obtained by using a modified silicone polymer as a main component and compounding a polybutene having 300-4000 molecular weight together with calcium carbonate treated with a fatty acid.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a modified silicone sealing material composition having excellent thixotropic properties, and more particularly, to use a polybutene having a specific molecular weight and a fatty acid-treated calcium carbonate in combination to use any swelling process. Without,
The present invention relates to a modified silicone-based sealing material composition having excellent thixotropic properties and having no sagging.

[0002]

2. Description of the Related Art A modified silicone-based sealant composition containing a modified silicone polymer as a main component is a one-component type cured by moisture curing; a base containing the modified silicone polymer and a curing agent. There are two types of catalyst-containing curing agents, which are used for waterproofing high-rise buildings and housing-related waterproofing, and their demand is steadily increasing. By the way, when applying such waterproofing, dripping at the time of application becomes a serious problem, and conventionally, hydrogenated castor oil or polyamide-based wax is used, but generally the productivity of swelling and dissolving is extremely poor,
In addition, there is a limit in excellent thixotropic properties required for anti-drooping. SUMMARY OF THE INVENTION An object of the present invention is to provide a modified silicone-based sealing material composition having excellent thixotropic properties without using a swelling step at all and having no sagging.

[0003]

Means for Solving the Problems The present inventors have made intensive studies to achieve the above object, and found that polybutene having a specific molecular weight compatible with the modified silicone polymer and calcium carbonate treated with fatty acid were used in combination. Even without using a swelling step, excellent thixotropic properties can be expressed,
Moreover, even when applied in a high-temperature atmosphere of 50 ° C. or more, the anti-dripping effect can be sufficiently exhibited, and it is found that this is a unique effect that cannot be achieved from the conventional swelling type. Was completed.

[0004] That is, the present invention provides a modified silicone-based sealing material composition comprising a modified silicone polymer as a main component and a combination of polybutene having a molecular weight of 300 to 4000 and fatty acid-treated calcium carbonate. It is.

[0005] The modified silicone polymer used in the present invention is a polyoxyalkylene ether having a main chain skeleton and having a hydrolyzable group (for example, a hydroxyl group,
A liquid polymer having a silyl group or a silanol group having a halogen group, an alkoxy group, a mercapto group, etc. is referred to, and among them, a polymer having a polyoxypropylene ether as a main chain and a molecular weight of 8,000 to 15,000 is preferable.

The polybutene used in the present invention is compatible with the above-mentioned modified silicone polymer as a main component and has a viscous liquid or wax having a molecular weight of 300 to 4000. The waxy material may be used in combination with a viscous liquid.

The fatty acid-treated calcium carbonate used in the present invention is known per se, for example, having a particle size of 0.02 to 0.02.
Light calcium carbonate having a surface of about 10 μm is treated with a fatty acid (such as stearic acid, lauric acid, or oleic acid).

[0008]

BEST MODE FOR CARRYING OUT THE INVENTION The modified silicone-based sealing material composition according to the present invention is composed of a system containing the above-mentioned modified silicone polymer as a main component and blending the above-mentioned polybutene and fatty acid-treated calcium carbonate in combination. Can be divided into two modes of a one-component type and a two-component type constituted by the following components. Here, the amount of the polybutene to be used in combination with the above is generally selected from the range of 2 to 30% (% by weight, the same applies hereinafter), preferably the range of 5 to 20% of the total amount of the sealing material composition. If it is less than 2%, thixotropic properties are not sufficiently developed, and if it exceeds 30%, bleeding and the like tend to be remarkable, which tends to be a practical problem. The amount of the fatty acid-treated calcium carbonate to be used may be generally selected in the range of 10 to 80%, preferably 30 to 60%, based on the total amount of the sealing material composition. If it is less than 10%, the thixotropic effect is not sufficient, and if it exceeds 80%, there is no problem with thixotropic, but the viscosity is too high and the workability remains problematic.

A one-component modified silicone polymer is blended with a predetermined amount of polybutene and a fatty acid-treated calcium carbonate, and, if necessary, a viscosity adjusting solvent, an antioxidant (hindered amine, hindered phenol, benzotriazole, etc.), and an adhesive. (Mercaptoalkoxysilane, aminoalkoxysilane,
Epoxy alkoxysilane, etc.), curing catalyst (divalent tin,
Organic heavy metal compounds such as tetravalent tin, bismuth, and manganese, such as stannous octate and tin acetylacetonate;
Amines such as triethylenediamine, N-alkylpiperazine, laurylamine), a tack remover and the like in an appropriate range.

A two-component modified silicone polymer, a base containing polybutene and a fatty acid-treated calcium carbonate, and a viscosity adjusting solvent, an antioxidant, an adhesive, and the like, if necessary, a curing catalyst and, if necessary, a filler (Heavy calcium carbonate, magnesium carbonate, clay, talc, bentonite, zinc oxide, etc.), plasticizers (phthalic diesters, epoxidized hexahydrophthalic diesters, alkylenedicarboxylic diesters, alkylbenzenes, etc.) And a curing agent.

Preferred examples of the mixing ratio of each component in the sealing material composition of the present invention are shown below. "%" Indicates the amount in the total amount of the sealing material composition in the case of the one-component type, and the amount in the total amount of the base or curing agent in the case of the two-component type. 1-component type: % modified silicone polymer 15-35 polybutene 5-20 fatty acid-treated calcium carbonate 30-60 viscosity adjusting solvent 2-5 anti-aging agent 0.1-5 adhesive agent 0.1-5 curing catalyst 0. 1-3

In the case of the two-component type: (base) % modified silicone polymer 15-35 polybutene 5-20 fatty acid-treated calcium carbonate 30-60 viscosity adjusting solvent 0.1-5 antioxidant 0.1-5 adhesive 0.1 to 5 (curing agent) Curing catalyst 0.5 to 10 Heavy calcium carbonate 50 to 80 Plasticizer 10 to 30 In addition to the components of the preferred examples, a coloring agent (titanium oxide, organic When there is an increase in viscosity due to the passage of time, a wetting modifier, a wetting dispersant, or the like may be appropriately selected and blended.

[0013]

Next, the present invention will be described more specifically with reference to examples and comparative examples. Example 1 (two-component type) (1) Base Modified silicone polymer [manufactured by Kaneka Chemical Industry Co., Ltd .;
810 "] 500 g into a planetary mixer,
Next, polybutene having an average molecular weight of 350 [Idemitsu Petrochemical
300 g of "Polybutene OH" manufactured by K.K.) and uniformly mixed. Thereafter, 1000 g of fatty acid-treated calcium carbonate [manufactured by Shiroishi Calcium Co., Ltd., "Biscolite R"] is added, and the mixture is stirred and dispersed. 3 g of "Ilganox 1010" and 1 g of an adhesive were added,
Continue stirring. After 10 minutes of stirring, the stirring was stopped, and a solvent for adjusting the viscosity [Isopor H, manufactured by Exxon Chemical Co., Ltd.] 50
g, and the mixture is subjected to vacuum degassing and stirring for 10 minutes to obtain a base. (2) Curing agent Curing catalyst: 10 g of tin acetylacetonate, 100 g of heavy calcium carbonate and 50 g of plasticizer: diisononyl phthalate were put into a planetary mixer, mixed for 10 minutes, and then subjected to vacuum defoaming and stirring for 10 minutes. Obtain a curing agent.

Comparative Example 1 (two-component type) (1) Base 500 g of a modified silicone polymer ("S-810") is charged into a planetary mixer, and then 300 g of diisononyl phthalate is charged and uniformly mixed. afterwards,
Fatty acid-treated calcium carbonate ("Viscolite R") 10
Then, 30 g of hydrogenated castor oil [“Dispalon # 305” manufactured by Kusumoto Chemical Co., Ltd.] was added.
Is added, and the temperature is increased to 60 ° C. with uniform stirring to swell for 1 hour. After the swelling, the temperature was lowered to 20 ° C., and then the same amount and the same amount of the antioxidant and the same adhesive as in Example 1 were added. Further, the same amount and the same amount of the viscosity adjusting solvent as in Example 1 were added. Run for a minute to get the base. (2) Curing agent Same as in Example 1.

Comparative Example 2 (two-component type) (1) Base In Example 1, polybutene 30 having an average molecular weight of 350 was used.
A base is obtained in the same manner except that 300 g of diisononyl phthalate is used instead of 0 g. (2) Curing agent Same as in Example 1. Comparative Example 3 (two-component type) (1) Base In Example 1, polybutene 30 having an average molecular weight of 350 was used.
300 g of 2-ethylhexyl adipate instead of 0 g
A base is obtained in the same manner except that is used. (2) Curing agent Same as in Example 1.

Performance test The base and the curing agent were mixed at a ratio of 10: 1 (weight ratio) and subjected to the following performance tests. The results are shown in Table 1 below. i) Viscosity measurement The viscosity (× 10 ⁴ cps) of each of the base alone and the base / hardener mixture (sealing material) is measured at 20 ° C. ii) Sagging test A sealing material having a thickness of 10 mm is applied to a stainless steel vertical surface at 20 ° C., and the sagging distance (mm) and the slip moving distance (mm) after 30 minutes are measured. Incidentally, at 40 ° C. and 50 ° C.
In case of ℃, adjust the temperature of the sealing material and stainless steel,
The test was performed in the temperature atmosphere.

[0017]

[Table 1]

Example 2 (1 component type) Modified silicone polymer [manufactured by Asahi Glass Industry Co., Ltd., "ESS"
-410 ”] into a planetary mixer, and then 200 g of polybutene having an average molecular weight of 950 (“ Polybutene 100H ”, manufactured by Idemitsu Petrochemical Co., Ltd.), and uniformly mixed. Thereafter, 600 g of fatty acid-treated calcium carbonate [manufactured by Takehara Chemical Co., Ltd., "Neolite SP"] was charged and uniformly mixed and dispersed, and then 3 g of "Tinuvin 327" and 3 g of "Ilganox 1010" were used as anti-aging agents.
Was further added, 2 g of an adhesive agent, 3 g of a stabilizer, and 50 g of a viscosity adjusting solvent (“Isoper H”) were added, and the mixture was subjected to vacuum degassing and stirring for 20 minutes. After the atmospheric pressure was released, 30 g of pigment and finally a curing catalyst: dibutyl Tin dilaurate [Nitto Kasei
2 g of “DBTDL” manufactured by K.K.) to obtain a one-component sealing material.

Comparative Example 4 (one-component type) Modified silicone polymer ("ESS-2410") 40
0 g was put into a planetary mixer, then 100 g of diisononyl phthalate and 100 g of 2-ethylhexyl trimellitate were added, and further a polyamide-based wax ["Dispalon # 6500" manufactured by Kusumoto Chemicals, Ltd.]
After adding 30 g and stirring and mixing, 600 g of fatty acid-treated calcium carbonate [manufactured by Takehara Chemical Co., Ltd., "Neolite T"] is added, and the temperature is raised from room temperature (20 ° C.) to 90 while stirring and mixing.
The mixture was heated to 90 ° C. and mixed and stirred at 90 ° C. for 1 hour. After 1 hour, the temperature was lowered from 90 ° C. to 20 ° C. with cooling water. Finally, the same amount of an antioxidant, a cohesive agent, a stabilizer and a solvent for adjusting viscosity as in Example 2 were further added, and a pigment and a curing catalyst were added.
Mix and stir to obtain a one-component sealing material.

Comparative Example 5 (Single Component Type) The same procedure as in Comparative Example 4 was repeated except that the polyamide-based wax (“Disparon # 6500”) was omitted and the mixing and stirring of the components were performed only at 20 ° C. Obtain a shaped sealant. Each one-component type sealing material was subjected to the same performance test as in Example 1, and the results were shown in Table 2 below.
Shown in

[0021]

[Table 2]

[0022]

From the results in Tables 1 and 2, the sealing material composition of the present invention is a one-component type or a two-component type (Examples 1 and 2).
In both cases, compared to the conventional swelling type (Comparative Examples 1 and 4), it is recognized that the dripping prevention effect, particularly the same effect in a 50 ° C. atmosphere, is particularly excellent.

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Claims (4)

[Claims] 1. A modified silicone-based sealing material composition comprising a modified silicone polymer as a main component and a combination of polybutene having a molecular weight of 300 to 4000 and fatty acid-treated calcium carbonate. 2. The modified silicone sealant composition according to claim 1, which is a one-component type. 3. The modified composition according to claim 1, which is a two-component type comprising a modified silicone polymer-containing base and a curing catalyst containing a curing catalyst, wherein polybutene and fatty acid-treated calcium carbonate are blended on the base side. Silicone sealant composition. 4. The modified silicone-based sealing according to claim 1, wherein 2 to 30% by weight of polybutene and 30 to 60% by weight of fatty acid-treated calcium carbonate are blended in the total amount of the sealing material composition. Material composition.