CN100595250C - Method for manufacturing mono-component water-dispersing room temperature dewatering silicon sulfide ketone seal gum - Google Patents
Method for manufacturing mono-component water-dispersing room temperature dewatering silicon sulfide ketone seal gum Download PDFInfo
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- CN100595250C CN100595250C CN200710049060A CN200710049060A CN100595250C CN 100595250 C CN100595250 C CN 100595250C CN 200710049060 A CN200710049060 A CN 200710049060A CN 200710049060 A CN200710049060 A CN 200710049060A CN 100595250 C CN100595250 C CN 100595250C
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Abstract
The present invention relates to a manufacturing method of single component water dispersivity room temperature evaporated sulfuration silicones sealing gum. The manufacturing method is characterizedin that the method includes the steps as follows: wherein the raw materials are all parts by weight; 100 shares of anion hydroxide radical silicon oil, 1.5 to 6 shares of anion active agent, 0 to 6 shares of non-ion active agent and 60 to 150 shares of de-ionized water are processed in a high pressure viscolizer for one to three times, the mixture is added into a reaction kettle with a blender, and the mixture reacts for 24 to 72 hours under the temperature of 5 to 80 degree centigrade, then 0.5 to 20 shares of metal alkaline silicate or silica sol and 0.02 to 5 shares of stanniferous catalyzing compound are added for curing 2 to 3 days to get Alpha and Omega to (dihydroxy) dimer organic siloxane polymer latex; the latex, 0 to 5 shares of organic silicon resin acceptor, 50 to 180 shares ofinorganic filler, 0.1 to 1 shares of thickening agent and 0.1 to 1 shares of foam killer are added into a kneader for evenly mixing to get single component water dispersivity room temperature evaporated sulfuration silicones sealing gum.
Description
Technical field
The present invention relates to a kind of mono-component water-dispersing room temperature dewatering silicon sulfide ketone seal gum and manufacture method thereof, belong to high molecule sealing materials and manufacturing field thereof.
Background technology
U.S. Pat 2,891,920 disclose and carry out the polydiorganosiloxane letex polymerization and make the emulsion film forming method of dewatering under the tensio-active agent existence condition, can be used to prepare protective membrane.Hyde thinks, make this emulsion under envrionment conditions, have sufficient intensity after the dehydrated crosslinking film forming to reach the purpose of use, just must make the molecular weight of polydiorganosiloxane reach one, and under this ultra-high molecular weight condition, this emulsion is extremely unstable than higher value.Hyde points out, prepare stable polydiorganosiloxane emulsion, preferred acid catalyzer when adopting anion surfactant, preferred bases catalyzer when adopting cats product, adopt the nonionogenic tenside soda acid all can, prepared emulsion can several years of storage.Yet the preparation of this protective membrane that Hyde proposes is not used widely.
U.S. Pat 3,294,725 disclose a kind of preparation method of comparatively stable polydiorganosiloxane emulsion, use Witco 1298 Soft Acid to be catalyzer, the emulsion of preparation gained is neutralized to the pH value near 7 with an alkali metal salt, no matter emulsion whether with the filler blend, all can obtain more stable water dispersion.Add the pH value hereinto in the property emulsion and be 8.5 silicon sol, sneak into the organo-silicon coupling agent of trifunctional again,, can obtain silicon rubber film behind the dehydrated crosslinking as methyltrimethoxy silane.
U.S. Pat 3,706,695 disclose a kind of preparation method of silicone dispersion system, and the employing white carbon black is a reinforced filling, and the polydiorganosiloxane emulsion is basic filmogen, can make the silicon rubber of conductivity.Huebner further specifies, and should comprise also in this silicone aqueous systems that the organo-metallic enriched material is that catalyzer and alkyltrialkoxysilaneand are linking agent.This silicone aqueous systems can make silicon rubber with practical value after the dehydration in one to two week after preparation, yet, after in case the silicone aqueous systems stores the long period, the silicon rubber performance of dehydration gained is just undesirable, need add catalyzer and linking agent once more, therefore, the silicone aqueous systems of stability in storage be made, two-pack must be formulated as.
Above patent proposed the preparation method of silicone elastica preferably, and obtained relevant application, but insufficiently is:
(1) the one-component shelf lives not long, must be mixed with two-pack,
It is (2) can not room temperature dehydration crosslinked or need long time,
(3) filler and α, ω～(dihydroxyl) polydiorganosiloxane polymer emulsion ratio is unreasonable, increases the content of filler, and the performance of product descends again greatly, no practical value.
Summary of the invention
The objective of the invention is to provide a kind of manufacture method of mono-component water-dispersing room temperature dewatering silicon sulfide ketone seal gum at the deficiencies in the prior art.
Purpose of the present invention is realized that by following technical measures wherein said raw material umber is parts by weight except that specified otherwise.
The manufacture method of mono-component water-dispersing room temperature dewatering silicon sulfide ketone seal gum may further comprise the steps:
(1) 100 parts of hydroxy silicon oils, 1.5～6 portions of anion surfactants, 0～6 portion of nonionogenic tenside, 60～150 parts of deionized waters are joined in the reactor that has agitator, mix.To handle 1～3 time in this mixed solution immigration high pressure homogenizer, again mixture is added in the aforesaid reaction vessel, in 5～80 ℃ of reactions of temperature 24～72 hours, in reactant, add 0.5～20 part of alkaline metal silicate or silicon sol and 0.02～5 part of stanniferous catalytic cpd, slaking obtained α, ω～(dihydroxyl) polydiorganosiloxane polymer emulsion on the 2nd～3 under the room temperature;
(2) will stir in above-mentioned polymer emulsion, 0～5 part of organo-silicon coupling agent, 50～180 parts of mineral fillers, 0.1～1 part of thickening material and 0.1～1 part of adding kneader of defoamer or the planetary stirrer, obtain mono-component water-dispersing room temperature dewatering silicon sulfide ketone seal gum.
Wherein the structural formula of hydroxy silicon oil is
N=6～20, R is CH
3-, CH
3CH
2-, CH
2=CH-or C
6H
5-, R can be identical, also can be different.The dry matter content of emulsion is 40%～70%, dry-matter α, and ω～(dihydroxyl) polydiorganosiloxane molecular weight is 300,000～900,000, the pH value is 8～12.
Anion surfactant is at least a in Witco 1298 Soft Acid, Sodium dodecylbenzene sulfonate, the sodium lauryl sulphate; Nonionogenic tenside is C
8～40Polyxyethylated alkylphenol in any.
Silicon sol is the dispersion liquid of colloid silica in water, and solid content is 40%～60%, and the pH value is 3～10.
The stanniferous catalytic cpd is at least a in dibutyl tin dilaurate, dibutyl tin acetate, dibutyl two stannous octoates or the stannous octoate.
Organo-silicon coupling agent is at least a in vinyltrimethoxy silane, vinyltriethoxysilane, isobutyl-Trimethoxy silane, isobutyl-triethoxyl silane, n-octyl triethoxyl silane, phenyltrimethoxysila,e, gamma-methyl allyl acyloxypropyl trimethoxysilane, γ-(2,3 epoxies, third oxygen) propyl trimethoxy silicane.
Mineral filler is at least a in lime carbonate, white carbon black, hydrated aluminum oxide, aluminum oxide, magnesium hydroxide, titanium dioxide, silicon powder, the white lime.
Thickening material is any among Walocel MT 20.000PV, Natvosol, the DSX3116.DSX3116 buys from Shenzhen Haichuan Chemical Technology Co., Ltd.
Defoamer is Foamaster-75, buys from Shenzhen Haichuan Chemical Technology Co., Ltd.
The mono-component water-dispersing room temperature dewatering silicon sulfide ketone seal gum that adopts method for preparing to obtain.
Thickening material and defoamer are additive well known to those skilled in the art, can use jointly, and its precondition is that these additives do not have a negative impact to obtaining of realization of the present invention and excellent results.
Mono-component water-dispersing room temperature dewatering silicon sulfide ketone seal gum is used for bonding to aluminium, glass, pottery.After aluminium or ceramic surface cleaned up, applying glue 1cm thereon after 14 days, manually can't go up from aluminium or pottery it is torn, and its satisfactory mechanical property press GB/T528-92 and tested.The mono-component water-dispersing room temperature dewatering silicon sulfide ketone seal gum secluding air still is a paste after storing 1 year, but dehydrated crosslinking.
The present invention has following advantage
(1) environmental protection practicality, its sulfidation is not emitted the organic molecule material, and is free from environmental pollution.
(2) stable storing, the solvent-borne type silicone sealant shelf lives is 3～12 months; The water-dispersing room temperature dewatering silicon sulfide ketone seal gum shelf lives is 6～12 months.
(3) easy to use, not dehydration sulfureted a very long time can also be soluble in water more fully before, is convenient to cleaning.
(4) Du Te cementability, this water-dispersing room temperature dewatering silicon sulfide ketone seal gum can adhere to the wet basis material, also can applying glue again after it is solidified with intensity.
Embodiment
Below by embodiment the present invention is carried out concrete description; be necessary to be pointed out that at this; present embodiment only is 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 1
(1) with 100 parts of hydroxy silicon oils, 1.5 parts of Witco 1298 Soft Acids, 1.5 parts of Sodium dodecylbenzene sulfonatees and 66 parts of deionized waters join in the reactor that has agitator, mix.To handle 3 times in this mixed solution immigration high pressure homogenizer, again mixture is added in the aforesaid reaction vessel, in 30 ℃ of reactions of temperature 48 hours, add 1.5 parts of nonionogenic tenside OP-10, adding amount of dry matter in 25 ℃ of temperature in reactant is 6.7 parts of 50% sodium silicate aqueous solutions, adds 1.3 parts of amount of dry matters again and be 40% dibutyl tin dilaurate water miscible liquid, mix, room temperature reaction 48 hours makes α, ω～(dihydroxyl) polydiorganosiloxane polymer emulsion.
(2) 25 ℃ of temperature, with above-mentioned emulsion, 150 parts in the lime carbonate of particle diameter below 6.5 μ m, 1 part of Natvosol, 1 part of Foamaster-75 defoamer stirs in the adding planetary stirrer, makes the mono-component water-dispersing room temperature dewatering silicon sulfide ketone seal gum of paste, by standard GB/T528-92 sample preparation, record after 14 days that mechanical property is detailed to be shown in Table 1.
Embodiment 2
(1) with 100 parts of hydroxy silicon oils, 6 parts of Witco 1298 Soft Acids and 66 parts of deionized waters join in the reactor that has agitator, mix.To handle 3 times in this mixed solution immigration high pressure homogenizer, again mixture is added in the aforesaid reaction vessel, in 5 ℃ of reactions of temperature 24 hours, adding amount of dry matter in 25 ℃ of temperature in reactant is 6.7 parts of 50% sodium silicate aqueous solutions, add 1.3 parts of amount of dry matters again and be 40% dibutyl tin acetate water miscible liquid, mix room temperature reaction 48 hours, make α, ω～(dihydroxyl) polydiorganosiloxane polymer emulsion.
(2) 25 ℃ of temperature, with above-mentioned emulsion, 0.5 part of gamma-methyl allyl acyloxypropyl trimethoxysilane, 0.5 part of γ-(2,3 epoxies, third oxygen) propyl trimethoxy silicane, 150 parts in the lime carbonate of particle diameter below 6.5 μ m, 1 part of Natvosol stirs in 1 part of adding of Foamaster-75 defoamer planetary stirrer, makes the mono-component water-dispersing room temperature dewatering silicon sulfide ketone seal gum of paste, by standard GB/T528-92 sample preparation, record after 14 days that mechanical property is detailed to be shown in Table 1.
Embodiment 3
(1) with 100 parts of hydroxy silicon oils, 2 parts of Witco 1298 Soft Acids and 66 parts of deionized waters join in the reactor that has agitator, mix.To handle 3 times in this mixed solution immigration high pressure homogenizer, again mixture is added in the aforesaid reaction vessel, in 5 ℃ of reactions of temperature 24 hours, add 1.5 parts of nonionogenic tenside OP-10, adding amount of dry matter in 25 ℃ of temperature in reactant is 1 part of 50% sodium silicate aqueous solution, adds 5 parts of amount of dry matters again and be 40% dibutyl two stannous octoate water miscible liquids, mix, room temperature reaction 48 hours makes α, ω～(dihydroxyl) polydiorganosiloxane polymer emulsion.
(2) 25 ℃ of temperature, with above-mentioned emulsion, 2 parts of vinyltrimethoxy silanes, 142 parts of magnesium hydroxides, 1 part of Natvosol stirs in 1 part of adding of Foamaster-75 defoamer planetary stirrer, makes the mono-component water-dispersing room temperature dewatering silicon sulfide ketone seal gum of paste, by standard GB/T528-92 sample preparation, record after 14 days that mechanical property is detailed to be shown in Table 1.
Embodiment 4
(1) with 100 parts of hydroxy silicon oils, 1.5 parts of Witco 1298 Soft Acids, 0.25 part of Sodium dodecylbenzene sulfonate, 0.25 part of sodium lauryl sulphate and 100 parts of deionized waters join in the reactor that has agitator, mix.To handle 3 times in this mixed solution immigration high pressure homogenizer, again mixture is added in the aforesaid reaction vessel, in 30 ℃ of reactions of temperature 48 hours, add 5 parts of nonionogenic tenside OP-10, adding amount of dry matter in 25 ℃ of temperature in reactant is 6.7 parts of 50% sodium silicate aqueous solutions, adds 1.3 parts of amount of dry matters again and be 40% dibutyl tin dilaurate water miscible liquid, mix, room temperature reaction 48 hours makes α, ω～(dihydroxyl) polydiorganosiloxane polymer emulsion.
(2) 25 ℃ of temperature, with above-mentioned emulsion, 1 part of vinyltrimethoxy silane, 149 parts in the lime carbonate of particle diameter below 6.5 μ m, 1 part of silicon powder, 1 part of Natvosol, stir in 1 part of adding of Foamaster-75 defoamer planetary stirrer, make the mono-component water-dispersing room temperature dewatering silicon sulfide ketone seal gum of paste, by standard GB/T528-92 sample preparation, record after 14 days that mechanical property is detailed to be shown in Table 1.
Embodiment 5
(1) with 100 parts of hydroxy silicon oils, 1.5 parts of Witco 1298 Soft Acids, 0.5 part of Sodium dodecylbenzene sulfonate and 150 parts of deionized waters join in the reactor that has agitator, mix.To handle 3 times in this mixed solution immigration high pressure homogenizer, again mixture is added in the aforesaid reaction vessel, in 5 ℃ of reactions of temperature 24 hours, add 1.5 parts of nonionogenic tenside OP-10, adding amount of dry matter in 25 ℃ of temperature in reactant is 6.7 parts of 50% sodium silicate aqueous solutions, adds 1.3 parts of amount of dry matters again and be 40% dibutyl tin dilaurate water miscible liquid, mix, room temperature reaction 48 hours makes α, ω～(dihydroxyl) polydiorganosiloxane polymer emulsion.
(2) 25 ℃ of temperature, with the lime carbonate of above-mentioned emulsion particle diameter below 6.5 μ m, 170 parts, 1 part of Walocel MT 20.000PV, stir in 1 part of adding of Foamaster-75 defoamer planetary stirrer, make the mono-component water-dispersing room temperature dewatering silicon sulfide ketone seal gum of paste, by standard GB/T528-92 sample preparation, record after 14 days that mechanical property is detailed to be shown in Table 1.
Embodiment 6
(1) with 100 parts of hydroxy silicon oils, 2 parts of Witco 1298 Soft Acids and 66 parts of deionized waters join in the reactor that has agitator, mix.To handle 3 times in this mixed solution immigration high pressure homogenizer, again mixture is added in the aforesaid reaction vessel, in 5 ℃ of reactions of temperature 24 hours, add 2 parts of nonionogenic tenside OP-10, adding amount of dry matter in 25 ℃ of temperature in reactant is 18 parts of 50% sodium silicate aqueous solutions, adds 0.05 part of amount of dry matter again and be 40% stannous octoate emulsion, mix, room temperature reaction 48 hours makes α, ω～(dihydroxyl) polydiorganosiloxane polymer emulsion.
(2) 25 ℃ of temperature, with above-mentioned emulsion, 5 parts of vinyltrimethoxy silanes, 100 parts in the lime carbonate of particle diameter below 6.5 μ m, 50 parts of silicon powders, 1 part of DSX3116 thickening material, stir in 1 part of adding of Foamaster-75 defoamer planetary stirrer, make the mono-component water-dispersing room temperature dewatering silicon sulfide ketone seal gum of paste, by standard GB/T528-92 sample preparation, record after 14 days that mechanical property is detailed to be shown in Table 1.
Table 1
Claims (9)
1, the manufacture method of mono-component water-dispersing room temperature dewatering silicon sulfide ketone seal gum is characterized in that this method may further comprise the steps, the wherein raw materials used parts by weight that are:
(1) with 100 parts of hydroxy silicon oil, 1.5～6 portions of anion surfactants, 0～6 portion of nonionogenic tenside, 60～150 parts of deionized waters join in the reactor that has agitator, mix, to handle 1～3 time in this mixed solution immigration high pressure homogenizer, again mixture is added in the aforesaid reaction vessel, in 5～80 ℃ of reactions of temperature 24～72 hours, in reactant, add 0.5～20 part of alkaline metal silicate and 0.02～5 part of stanniferous catalytic cpd, slaking obtained α, ω～(dihydroxyl) polydiorganosiloxane polymer emulsion on the 2nd～3 under the room temperature;
(2) will stir in above-mentioned polymer emulsion, 0～5 part of organo-silicon coupling agent, 50～180 parts of mineral fillers, 0.1～1 part of thickening material and 0.1～1 part of adding kneader of defoamer or the planetary stirrer, obtain mono-component water-dispersing room temperature dewatering silicon sulfide ketone seal gum;
Wherein, the structural formula of hydroxy silicon oil is
N=6～20, R is CH
3-, CH
3CH
2-, CH
2=CH-or C
6H
5-, R can be identical, also can be different, and the dry matter content of emulsion is 40%～70%, dry-matter α, ω～(dihydroxyl) polydiorganosiloxane molecular weight is 300,000～900,000, the pH value is 8～12.
2, the manufacture method of mono-component water-dispersing room temperature dewatering silicon sulfide ketone seal gum according to claim 1 is characterized in that anion surfactant is at least a in Witco 1298 Soft Acid, Sodium dodecylbenzene sulfonate, the sodium lauryl sulphate; Nonionogenic tenside is C
8～40Polyxyethylated alkylphenol in any.
3, the manufacture method of mono-component water-dispersing room temperature dewatering silicon sulfide ketone seal gum according to claim 1 is characterized in that the stanniferous catalytic cpd is at least a in dibutyl tin dilaurate, dibutyl tin acetate, dibutyl two stannous octoates or the stannous octoate.
4, the manufacture method of mono-component water-dispersing room temperature dewatering silicon sulfide ketone seal gum according to claim 1, it is characterized in that organo-silicon coupling agent is at least a in vinyltrimethoxy silane, vinyltriethoxysilane, isobutyl-Trimethoxy silane, isobutyl-triethoxyl silane, n-octyl triethoxyl silane, phenyltrimethoxysila,e, gamma-methyl allyl acyloxypropyl trimethoxysilane, γ-(2,3 epoxies, third oxygen) propyl trimethoxy silicane.
5, the manufacture method of mono-component water-dispersing room temperature dewatering silicon sulfide ketone seal gum according to claim 1 is characterized in that mineral filler is at least a in lime carbonate, white carbon black, hydrated aluminum oxide, aluminum oxide, magnesium hydroxide, titanium dioxide, silicon powder, the white lime.
6, the manufacture method of mono-component water-dispersing room temperature dewatering silicon sulfide ketone seal gum according to claim 1 is characterized in that thickening material is any among Walocel MT 20.000PV, Natvosol, the DSX3116.
7, the manufacture method of mono-component water-dispersing room temperature dewatering silicon sulfide ketone seal gum according to claim 1 is characterized in that defoamer is Foamaster-75.
8, the mono-component water-dispersing room temperature dewatering silicon sulfide ketone seal gum that adopts one of claim 1～7 described method manufacturing to obtain.
9, be used for bonding to aluminium, glass and pottery as mono-component water-dispersing room temperature dewatering silicon sulfide ketone seal gum as described in the claim 8.
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| CN101805518B (en) * | 2009-02-12 | 2012-05-09 | 深圳国宝造币有限公司 | Organosilicon polymer and film forming method thereof on metal surface |
| CN101638518B (en) * | 2009-09-09 | 2011-06-29 | 成都硅宝科技股份有限公司 | Room-temperature vulcanized silicone rubber resisting acid-gas corrosion and high temperature and preparation method thereof |
| CN102816350B (en) * | 2012-07-30 | 2014-06-11 | 华南理工大学 | Wet mixing method for preparing natural rubber/carbon black-nano silica rubber compound |
| CN102912644B (en) * | 2012-10-16 | 2014-07-09 | 淮安凯悦科技开发有限公司 | Skin-tendering siloxane pasty composition and preparation method thereof |
| CN105440539A (en) * | 2015-12-10 | 2016-03-30 | 无锡普瑞腾传动机械有限公司 | Constructional organic silicon sealant |
| CN105585999A (en) * | 2016-03-02 | 2016-05-18 | 广东杰果新材料有限公司 | Condensed type two-component pouring sealant for LED optical lens and preparation method thereof |
| CN109762512A (en) * | 2019-01-14 | 2019-05-17 | 深圳微巨石英科技有限公司 | Aqueous glass cement of waterproof quartz and preparation method thereof |
| CN112080247B (en) * | 2020-09-02 | 2022-04-29 | 圣戈班汇杰(杭州)新材料有限公司 | Water-based silicone adhesive capable of bonding RTV silicone adhesive |
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