CN100381535C - Anti-fouling single-component room temperature sealing silicone sulfide glue and its production process - Google Patents
Anti-fouling single-component room temperature sealing silicone sulfide glue and its production process Download PDFInfo
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Abstract
The present invention relates to anti-fouling single-component room temperature sealing silicone sulfide glue and a preparation method thereof, which is characterized in that the glue is prepared from the following components: 5 to 30 portions by weight of silicon oil with a Si-H molecular end radical, and dry oil addition product (short for antifouling agent)as anti-fouling components, 100 portions by weight of alpha, omega-dihydroxy polysiloxane, and 70 to 130 portions by weight of active calcium carbonate. The components are added into a vacuum stirrer, dewatered and mixed at the temperature of 100 to 150 DEG C and the vacuum degree of 0.06 to 0.099MPa for 30 to 200 minutes; then, the mixture is cooled to obtain a base material; subsequently, 5 to 15 portions by weight of crosslinking agent, 0.5 to 5 portions by weight of silane coupling agent and 0.5 to 1.5 portions by weight of catalyst are added into a high-speed dispersing stirrer filled with the base material or a planetary stirrer filled with the base material, and are stirred for reaction at the vacuum degree of 0.06 to 0.099MPa and the rotation speed of 200 to 600 rpm for 30 to 150 minutes; and thus, the anti-fouling single-component room temperature sealing silicone sulfide glue is prepared.
Description
Technical field
The present invention relates to a kind of anti-fouling single-component room temperature sealing silicone sulfide glue and manufacture method thereof, belong to high molecule sealing materials and manufacturing field thereof.
Background technology
Room temperature sealing silicone sulfide glue at room temperature need not heating, illumination or other special conditions, and the moisture in the ingress of air can vulcanize and is elastomerics, has the characteristics very easily of using.Seal gum after the sulfuration has excellent high and low temperature resistance, excellent water tolerance, and performances such as remarkable weather-resistant and anti-ozone, ultraviolet ray have work-ing life of many decades.Multiple base materials such as aluminium alloy, glass, metal, stone material, cement are had good and persistent cohesiveness, and good elasticity is a resist displacement ability etc.Therefore silicone sealant is widely used in building trade, particularly in the curtain wall decoration industry.As everyone knows, the very easily dust suction of silicone sealant surface after the sulfuration, simultaneously since in the silicone sealant oiliness softening agent and a small amount of lower-molecular substance slowly ooze out the pollution that causes buildings periphery base material.In order to reduce silicone sealant surface deposition dust and to the pollution of buildings periphery base material, the Japanese Patent spy opens clear 62-1750,62-7763 and add siccative oil such as tung oil, hydrogenated castor oil in prescription, though prevent contaminative, but seal gum siccative oil in preservation is slowly separated out from seal gum, thereby influence the quality guaranteed period of seal gum, simultaneously the variable color easily of seal gum surface; U.S. Pat 4460740, US 4695603 and Japanese Patent spy open clear 56-76453,56-76542 report and add tensio-active agent in sizing materials, this way has temporary transient antifouling effect, seal gum surface deposition dust reduces, but can influence the cohesiveness of silicone sealant to base material greatly; US 5357025 adds the siloxanes agent that contains fluorocarbon radicals, and the room temperature sealing silicone sulfide glue of the siloxanes agent of fluorocarbon radicals and siccative oil such as tung oil, the shared preparation of hydrogenated castor oil makes the sulfuration encapsulant surface form siccative oil oxidation products layer, plays antifouling effect.But the exposure in atmosphere of this siccative oil oxidation products layer can fade away, and the effect of cleaning also loses gradually, and the surface again can dust suction, mildews, and cost is higher simultaneously.
Summary of the invention
The objective of the invention is provides a kind of anti-fouling single-component room temperature sealing silicone sulfide glue and manufacture method thereof at the deficiencies in the prior art.Being characterized in adopting exposed terminated groups is that the silicone oil and the siccative oil affixture (abbreviation stain control agent) of Si-H base is anti-pollution composition, with α, alpha, omega-dihydroxy polysiloxane, treated carbonates, linking agent, silane coupling agent and catalyst reaction make anti-fouling single-component room temperature sealing silicone sulfide glue.
Purpose of the present invention is realized that by following technical measures wherein said starting material umber is parts by weight except that specified otherwise.
The recipe ingredient of anti-fouling single-component room temperature sealing silicone sulfide glue is:
5～30 parts of stain control agents
α, 100 parts of alpha, omega-dihydroxy polysiloxane
70～130 parts of treated carbonatess
5～15 parts of linking agents
0.5～5 part of silane coupling agent
0.5～1.5 part of catalyzer
Wherein stain control agent is that exposed terminated groups is the silicone oil of Si-H base
N=15～25, with the affixture of siccative oil, siccative oil is tung oil, hydrogenated castor oil.
α, alpha, omega-dihydroxy polysiloxane structure formula is
N=50～2000, R is CH
3-, CH
3CH
2-or C
6H
5-.R can be identical, also can be different, and R is preferably methyl.
Linking agent is at least a in methyl tributanoximo silane, vinyl tributanoximo silane and the phenyl tributanoximo silane.
Silane coupling agent is at least a in γ-(2,3 epoxies, third oxygen) propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane, γ-An Bingjisanyiyangjiguiwan and N-(β aminoethyl)-γ-aminopropyl front three (second) TMOS.
Catalyzer is any in dibutyl tin dilaurate, dibutyl tin acetate or dibutyl two stannous octoates.
The manufacture method of anti-fouling single-component room temperature sealing silicone sulfide glue:
A. with α, alpha, omega-dihydroxy polysiloxane 100 weight parts, treated carbonates 70～130 weight parts add in the vacuum mixer, in 100～150 ℃ of temperature, vacuum tightness is 0.06～0.099MPa, dehydration blend 30～150 minutes, cool off base-material;
B. stain control agent is synthetic: the end group that adds the following formula structure in the there-necked flask that agitator, thermometer, reflux exchanger are housed is the silicone oil of Si-H base
N=15～25,20～40 weight parts, toluene 50～100 weight parts, siccative oil 10～20 weight parts, 0.1% isopropyl alcohol solution of chloroplatinic acid, 1～4 weight part was warming up to 90～110 ℃ of reactions after 3～5 hours, extracted toluene out and got stain control agent;
C. at room temperature, above-mentioned base-material is added in the high speed dispersion stirrer, add stain control agent 5～30 weight parts, linking agent 5～15 weight parts again, silane coupling agent 0.5～5 weight part and catalyzer 0.5～1.5 weight part, in vacuum tightness 0.06～0.099MPa, rotating speed 20～600rpm stirring reaction was made anti-fouling single-component room temperature sealing silicone sulfide glue in 30～150 minutes.
Anti-fouling single-component room temperature sealing silicone sulfide glue is tested every performance by JC/T882; Test result is detailed to be shown in Table 1.Wherein anti-pollution test is that anti-fouling single-component room temperature sealing silicone sulfide glue is filled in (wide 20mm in 2 white porcelain plate gaps, dark 10mm), after at room temperature solidifying 14 days, place at 45 ° of inclination angles outdoor, the pollution condition of observing rubber surface and porcelain plate periphery.3 months, 6 months, 9 months result also is shown in Table 1.
The present invention has following advantage:
1. adopt exposed terminated groups be the silicone oil of Si-H base and siccative oil add product (abbreviation stain control agent) for preventing pollutant component, the part unsaturated group of siccative oil makes seal gum surface form oxidation products, thereby prevents seal gum surface dust suction and the pollution of buildings periphery base material is had anti-fouling effect preferably.
2. adopting exposed terminated groups is that the silicone oil of Si-H base and the adduct of siccative oil (abbreviation stain control agent) are for preventing pollutant component, can not influence the package stability of seal gum, because this stain control agent molecule has the Si-O-Si skeleton structure, good with the seal gum consistency, can from system, not move.
3. adopt neutral curing system, bonded base material is not had corrosion, excellent in adhesion.
4. anti-fouling single-component room temperature sealing silicone sulfide glue has good physical and mechanical property.
5. anti-fouling single-component room temperature sealing silicone sulfide glue can be deployed into shades of colour with customer requirements, and single component is easy to use.
6. production process does not have three wastes generation, and is environmentally friendly.
Embodiment
Below by the embodiment description concrete to the present invention; be necessary to be pointed out that at this following examples only are used for the present invention is further specified; can not be interpreted as limiting the scope of the invention, the person skilled in the art in this field can make some nonessential improvement and adjustment according to the content of the invention described above.
Embodiment
Synthesizing of stainproofing agent
Stain control agent I is synthetic: the end group Si-H silicone oil that adds the following formula structure in the there-necked flask that agitator, thermometer, reflux exchanger are housed
N=20,20 weight parts, toluene 50 weight parts, tung oil 20 weight parts, 0.1% isopropyl alcohol solution of chloroplatinic acid, 1 weight part.Be warming up to 100 ℃ of reactions and got transparent liquid in 5 hours, extract toluene out and get stain control agent I.
Stain control agent II is synthetic: the end group Si-H silicone oil that adds the following formula structure in the there-necked flask that agitator, thermometer, reflux exchanger are housed
N=20,30 weight parts, toluene 80 weight parts, hydrogenated castor oil 25 weight parts, 0.1% isopropyl alcohol solution of chloroplatinic acid, 1 weight part.Be warming up to 100 ℃ of reactions and got transparent liquid in 4 hours, extract toluene out and get stain control agent II.
Embodiment 1: viscosity is the α of 50PaS during with 25 ℃, and alpha, omega-dihydroxy polydimethyl siloxane 100 weight parts, treated carbonates 70 weight parts add in the vacuum mixer, and in 130 ℃ of temperature, vacuum tightness is 0.09MPa, dehydration blend 100 minutes, cool off base-material.Under the room temperature, in the high speed dispersion stirrer of above-mentioned base-material is housed, with stain control agent I, 5 weight parts, methyl tributanoximo silane 12 weight parts, γ-An Bingjisanyiyangjiguiwan 0.5 weight part, dibutyl tin dilaurate 1.2 weight parts add in the high speed dispersion stirrer, in vacuum tightness 0.09MPa, rotating speed 600rpm stirring reaction 60 minutes is made anti-fouling single-component room temperature sealing silicone sulfide glue.
Embodiment 2: viscosity is the α of 30PaS during with 25 ℃, and alpha, omega-dihydroxy polysiloxane 100 weight parts, treated carbonates 100 weight parts add in the vacuum mixer, and in 120 ℃ of temperature, vacuum tightness is 0.085MPa, dehydration blend 120 minutes, cool off base-material.Under the room temperature, in the high speed dispersion stirrer of above-mentioned base-material is housed, with stain control agent I, 30 weight parts, methyl tributanoximo silane 7 weight parts, vinyl tributanoximo silane 2 weight parts, γ-An Bingjisanyiyangjiguiwan 4 weight parts, dibutyl tin dilaurate 0.7 weight part, add in the high speed dispersion stirrer, in vacuum tightness 0.09MPa, rotating speed 600rpm stirring reaction was made anti-fouling single-component room temperature sealing silicone sulfide glue in 60 minutes.
Embodiment 3: viscosity is the α of 10PaS during with 25 ℃, and alpha, omega-dihydroxy polydimethyl siloxane 100 weight parts, treated carbonates 130 weight parts add in the vacuum mixer, and in 110 ℃ of temperature, vacuum tightness is 0.080MPa, dehydration blend 150 minutes, cool off base-material.Under the room temperature, in the high speed dispersion stirrer of above-mentioned base-material is housed, with stain control agent II, 20 weight parts, phenyl tributanoximo silane 7 weight parts, γ-(2,3 epoxies, third oxygen) propyl trimethoxy silicane 2 weight parts and dibutyl tin acetate 1 weight part, add in the high speed dispersion stirrer, in vacuum tightness 0.09MPa, rotating speed 600rpm stirring reaction was made anti-fouling single-component room temperature sealing silicone sulfide glue in 60 minutes.
Comparison example 1: viscosity is the α of 50PaS during with 25 ℃, and alpha, omega-dihydroxy polydimethyl siloxane 100 weight parts, treated carbonates 70 weight parts add in the vacuum mixer in 110 ℃ of temperature, and vacuum tightness is 0.09MPa, dehydration blend 100 minutes, cool off base-material.Under the room temperature, in the high speed dispersion stirrer of above-mentioned base-material is housed, with methyl tributanoximo silane 12 weight parts, γ-An Bingjisanyiyangjiguiwan 0.5 weight part and dibutyl tin dilaurate 1.2 weight parts, add in the high speed dispersion stirrer, in vacuum tightness 0.09MPa, rotating speed 600rpm stirring reaction was made single-component room temperature sealing silicone sulfide glue in 60 minutes.
Comparison example 2: viscosity is the α of 30PaS during with 25 ℃, and alpha, omega-dihydroxy polysiloxane 100 weight parts, treated carbonates 100 weight parts add in the vacuum mixer, and in 110 ℃ of temperature, vacuum tightness is 0.085MPa, dehydration blend 120 minutes, cool off base-material.Under the room temperature, in the high speed dispersion stirrer of above-mentioned base-material is housed, with methyl tributanoximo silane 7 weight parts, vinyl tributanoximo silane 2 weight parts, γ-An Bingjisanyiyangjiguiwan 4 weight parts and dibutyl tin dilaurate 0.7 weight part, add in the high speed dispersion stirrer, in vacuum tightness 0.09MPa, rotating speed 600rpm stirring reaction was made single-component room temperature sealing silicone sulfide glue in 60 minutes.
Make silicone sealant, the product performance test result is detailed to be shown in Table 1.
Table 1 anti-fouling single-component room temperature sealing silicone sulfide glue The performance test results
Claims (8)
1. anti-fouling single-component room temperature sealing silicone sulfide glue; The recipe ingredient that it is characterized in that sealing glue is by weight:
5～30 parts of stain control agents
α, 100 parts of alpha, omega-dihydroxy polysiloxane
70～130 parts of treated carbonatess
5～15 parts of linking agents
0.5～5 part of silane coupling agent
0.5～1.5 part of catalyzer
Wherein stain control agent is that exposed terminated groups is the silicone oil of Si-H,
N=15～25 are with the affixture of siccative oil.
2. according to the described anti-fouling single-component room temperature sealing silicone sulfide glue of claim 1, it is characterized in that siccative oil is tung oil or hydrogenated castor oil.
3. according to the described anti-fouling single-component room temperature sealing silicone sulfide glue of claim 1, it is characterized in that α, alpha, omega-dihydroxy polysiloxane structure formula is
N=50～2000, R is CH
3-, CH
3CH
2-or C
6H
5-, R can be identical, also can be different.
4. according to the described anti-fouling single-component room temperature sealing silicone sulfide glue of claim 1, it is characterized in that α, the R in the alpha, omega-dihydroxy polysiloxane structure is a methyl.
5. according to the described anti-fouling single-component room temperature sealing silicone sulfide glue of claim 1, it is characterized in that linking agent is at least a in methyl tributanoximo silane, vinyl tributanoximo silane and the phenyl tributanoximo silane.
6. according to the described anti-fouling single-component room temperature sealing silicone sulfide glue of claim 1, it is characterized in that silane coupling agent is at least a in γ-(2,3 epoxies, third oxygen) propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane, γ-An Bingjisanyiyangjiguiwan and N-(β aminoethyl)-γ-aminopropyl front three (second) TMOS.
7. according to the described anti-fouling single-component room temperature sealing silicone sulfide glue of claim 1, it is characterized in that catalyzer is any in dibutyl tin dilaurate, dibutyl tin acetate or dibutyl two stannous octoates.
8. according to the manufacture method of the described anti-fouling single-component room temperature sealing silicone sulfide glue of one of claim 1～7, it is characterized in that this method contains following steps:
A. with α, alpha, omega-dihydroxy polysiloxane 100 weight parts, treated carbonates 70～130 weight parts add in the vacuum mixer, in 100～150 ℃ of temperature, vacuum tightness is 0.06～0.099MPa, dehydration blend 30～150 minutes, cool off base-material;
B. stain control agent is synthetic: the end group that adds the following formula structure in the there-necked flask that agitator, thermometer, reflux exchanger are housed is the silicone oil of Si-H base
N=15～25,20～40 weight parts, toluene 50～100 weight parts, siccative oil 10～20 weight parts, 0.1% isopropyl alcohol solution of chloroplatinic acid, 1～4 weight part was warming up to 90～110 ℃ of reactions after 3～5 hours, extracted toluene out and got stain control agent;
At room temperature, above-mentioned base-material is added in the high speed dispersion stirrer, add stain control agent 5～30 weight parts, linking agent 5～15 weight parts again, silane coupling agent 0.5～5 weight part and catalyzer 0.5～1.5 weight part, in vacuum tightness 0.06～0.099MPa, rotating speed 20～600rpm stirring reaction 30～150 minutes is made anti-fouling single-component room temperature sealing silicone sulfide glue.
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| CN101812281B (en) * | 2009-10-23 | 2012-07-25 | 郑州中原应用技术研究开发有限公司 | Sealant with neutral and transparent silicone structure |
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| EP0733672A1 (en) * | 1995-03-22 | 1996-09-25 | ERNST SONDERHOFF GmbH & Co. KG | Method of manufacturing a (foamed) silicone elastomer, especially for sealing purposes |
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