CN105111932B - A kind of production method of response type waterproofing agent of organosilicon - Google Patents
A kind of production method of response type waterproofing agent of organosilicon Download PDFInfo
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- CN105111932B CN105111932B CN201510531110.5A CN201510531110A CN105111932B CN 105111932 B CN105111932 B CN 105111932B CN 201510531110 A CN201510531110 A CN 201510531110A CN 105111932 B CN105111932 B CN 105111932B
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Abstract
The invention discloses a kind of production method of response type waterproofing agent of organosilicon, specific method is as follows：1) a certain amount of deionized water will be added in containing the mixture of nonionic emulsifier and anion emulsifier, 20~60min is stirred at 50~95 DEG C, obtains emulsifier water mixed system；2) the emulsifier water mixed system pH value of step 1) is adjusted to 1≤pH ＜, 7 or 7 ＜ pH≤14 with pH adjusting agent；3) organosilicon ring body is added in the emulsifier water mixed system of step 2) respectively or after mixing by a certain percentage with alkoxy silane；4) feed after the completion of in the range of 50~95 DEG C, stirring 0~480min of polyase 13 to get.Low raw-material cost of the present invention is easy to get, operation is simple, performance is conveniently adjusted, product obtained have dissipate uniformly, stability is good, good weatherability, strong adhesive force, washability are good, energy conservation and environmental protection, high repeatability and other advantages.
Description
Technical field
The invention belongs to chemistry and materials science field, more particularly to a kind of producers of response type waterproofing agent of organosilicon
Method.
Background technology
Organosilicon is nontoxic, harmless and with excellent high-low temperature resistant and the performances such as hydrophobic, in current many building materials waterproof materials
Using effect is best in material.Early period, waterproofing agent of organosilicon are solvent-borne type, and use cost is high, pollutes environment.With the hair of science and technology
Exhibition is substituted at this stage using the aqueous product of low-cost and pollution-less.
Aqueous product is often two kinds of methane-siliconic acid salt and type of latex type currently on the market.Methane-siliconic acid salt good water solubility,
Use cost is low, but methyl silicate, easily with water loss, the term of validity is short, and pollutes environment in strong basicity corrosion material.Breast
Liquid type waterproofing agent often passes through organosilicon linear polymer：Prepared by the emulsifications such as methyl-silicone oil, hydroxy silicon oil, containing hydrogen silicone oil, this kind of production
Product active function groups are few, difficult after use to form effective covalent bond with base material, cause this kind of product term of validity short, in concrete, stone
The strength of materials can be influenced using outer addition manner use in the materials such as cream, all kinds of plates, effect is poor；It is obtained simultaneously using emulsification method
Usability is lost in the product stability difference easily layering arrived.To improve the disadvantages mentioned above of this kind of product, the silane side of disperseing then is used
The product using effect that method obtains is good but of high cost, and stability is poor.Therefore, a kind of anxious stability yet-to-be developed is high, term of validity length
Emulsion type products overcome the defects of above-mentioned two classes product.
The content of the invention
The purpose of the present invention is be directed to above-mentioned present situation, it is desirable to provide a kind of stability is high, the term of validity is long, in concrete, stone
Cream, all kinds of plates will not reduce the emulsion-type waterproofing agent of organosilicon of the intensity of material when the method use mixed in materials in
Production method.
The purpose of the present invention is what is be achieved through the following technical solutions：
A kind of production method of response type waterproofing agent of organosilicon, specific method are as follows：
1) a certain amount of deionized water will be added in containing the mixture of nonionic emulsifier and anion emulsifier, 50~
20~60min is stirred at 95 DEG C, obtains emulsifier water mixed system；
2) the emulsifier water mixed system pH value of step 1) is adjusted to 1≤pH ＜, 7 or 7 ＜ pH≤14 with pH adjusting agent；
3) the emulsifier water of step 2) is added in after organosilicon ring body being distinguished or mixed by a certain percentage with alkoxy silane
In mixed system；
4) feed after the completion of in the range of 50~95 DEG C, stirring 0~480min of polyase 13 to get.
Further, organosilicon ring body：Alkoxy silane：Emulsifier：The mass ratio of water is：1~10：25~60：0.1~
20：30~90.
Further, the mixture of the nonionic emulsifier and anion emulsifier is one kind in nonionic emulsifier
Or a variety of one or more mixtures formed with anion emulsifier.
Further, the nonionic emulsifier is：Op series, AEO series, Span series or tween series.
Further, the anion emulsifier is SDBS, DBSA or SDS.
Further, the pH adjusting agent is：Acetic acid, hydrochloric acid, sulfuric acid, phosphoric acid, dodecyl benzene sulfonic acid, sodium hydroxide,
One or more of potassium hydroxide, sodium carbonate, sodium acid carbonate, ammonium carbonate, ammonium hydrogen carbonate, ammonium hydroxide, ammonia.
Further, organosilicon ring body and alkoxy silane are added in emulsifier water mixed system in the step 3)
Mode is the mode of disposable charging, batch charging or continuous charging, and feed time is 0~120min.
Further, the alkoxy silane is：1RSi(OR)3,2RSi(OR)3,3R4R(OR)2, R is methyl, ethyl, third
One or more of base, isopropyl；
Wherein1R is C1~18Saturated alkyl and aryl radical or1R=OR；2R is acryloxypropyl, vinyl, allyl
One kind in base, aminopropyl, chloropropyl, γ-glycidol ether oxygroup；3R with4R is:Saturated alkyl and aryl radical, acryloyl
One kind in oxygen propyl group, vinyl, pi-allyl, aminopropyl, chloropropyl, γ-glycidol ether oxygroup；3R with4R can it is identical can not
Together.
Further, the organosilicon ring body is：D4Octamethylcy-clotetrasiloxane, D3Hexamethyl cyclotrisiloxane, DMC have
Machine silicon ring body mixture, D4 viEight vinyl cyclotetrasiloxanes, D3 ViSix vinyl cyclotrisiloxane, DMCviContaining the organic of vinyl
One or more of silicon ring body mixture.
A kind of production method of response type waterproofing agent of organosilicon provided by the invention, low raw-material cost are easy to get, operate letter
Single easy, performance is conveniently adjusted, and polymer emulsion obtained is uniformly dispersed, favorable reproducibility, and preparation process is pollution-free, obtained production
Product are easy to use, good waterproof performance, can carry out large-scale industrial production, can meet stone material, timber, gypsum, concrete, coating,
The waterproofs such as historical relic, textile or maintenance demand.
Specific embodiment
The embodiment of the present invention provides a kind of production method of response type waterproofing agent of organosilicon.Specific method is as follows：
1) mixture containing nonionic emulsifier and anion emulsifier is added into a certain amount of deionized water, 50~95
20~60min is stirred at DEG C, obtains emulsifier water mixed system.
2) the emulsifier water mixed system pH value of step 1) is adjusted to 1≤pH ＜, 7 or 7 ＜ pH≤14 with pH adjusting agent.
3) after organosilicon ring body being distinguished or is mixed by a certain percentage with alkoxy silane in 50~95 DEG C of temperature ranges,
It adds in the emulsifier water mixed system of step 2).Organosilicon ring body：Alkoxy silane：Emulsifier：The mass ratio of water is：1~
10：25~60：0.1~20：30~90.
4) feed after the completion of in the range of 50~95 DEG C, stirring 0~480min of polyase 13 to get.
The open loop of silane ring body and rate of polymerization, alkane need to be effectively controlled by the open loop of organosilicon ring body and with alkoxy silane copolymerization
The hydrolysis of alkoxyl silicone group in oxysilane, polycondensation and its with ring body open-loop products copolymerization etc. rates of polymerization, and then control production
The object degree of polymerization and structure, to obtain the product of different performance.Acid-base value and temperature by adjusting system are all kinds of monomers of control
Between the most effective mode of hydrolytie polycondensation rate.Under the conditions of non-neutral, silane ring body can effectively open loop polycondensation increase molecular weight obtain
Bifunctionality linear siloxane；And it is copolymerized with alkoxy silane；The slight change of pH-value also results in the hydrolysis of various monomers
A great difference of polycondensation rate and product.Therefore, by control the pH-value of emulsion system control the homopolymerization of all kinds of monomers and
Copolymerization rate and obtain the different product of structure, control the different performance of product.Therefore the present invention is mixed with pH adjusting agent emulsifier water
System pH is closed to adjust to 1~14 (PH ≠ 7).
Organosilicon ring body or various silane are added in the emulsifier water mixed system of step 2) respectively or after mixing again
Mode is using the mode of disposable charging, batch charging or continuous charging, and feed time is 0~120min.It is added to PH tune
In emulsifier and deionized water mixed liquor after section, then agitated 30~480min obtains response type waterproofing agent of organosilicon.
In suitable emulsifier aqueous systems, the product dissolubility after copolymerization changes, with emulsifier and its micellar phase
Interaction forms stable emulsion particle, finally obtains stable response type waterproofing agent of organosilicon.It and can be by between different monomers
Copolymerization, obtain different structure and the response type waterproofing agent of organosilicon of performance, meet stone material, textile, concrete, gypsum, timber,
The demand in the fields such as coating, historical relic's protection, the manufacturing of all kinds of plates.
The present invention is described in detail with specific embodiment below：
A kind of production method of 1 response type waterproofing agent of organosilicon of embodiment
By 1.5 parts of op-10,2 parts of SDBS and 50 part of deionized waters are added in reactor jointly, and 20min is stirred at 50 DEG C,
Obtain emulsifier water mixed system；Emulsifier water mixed system pH is adjusted to 5 with acetic acid；25 parts of methyltriethoxysilane are existed
It is continuously added drop-wise in above-mentioned reactor in 40min, then once adds in 10 parts of DMC, then in 50 DEG C of constant temperature stirring polymerization 60min
Obtain the lotion that milky carries blue light.
A kind of production method of 2 response type waterproofing agent of organosilicon of embodiment
By 1.9 parts of AEO-9,2.2 parts of SDBS and 50 part of deionized waters are added in reactor, stirred at 70 DEG C jointly
30min obtains emulsifier water mixed system, is adjusted emulsifier water mixed system pH to 4 with hydrochloric acid.By 40 parts of methyl trimethoxy oxygen
The mixture of base silane and 8 parts of DMC are continuously added drop-wise in above-mentioned reactor in 50min, then in 70 DEG C of constant temperature stirring polymerizations
120min obtains the lotion that milky carries blue light.
A kind of production method of 3 response type waterproofing agent of organosilicon of embodiment
By 1.2 parts of op-10,2.5 parts of SDBS and 55 part of deionized waters are added in reactor, stirred at 75 DEG C jointly
60min obtains emulsifier water mixed system, is adjusted emulsifier water mixed system pH to 1 with dodecyl benzene sulfonic acid.By 60 part third
Ethyl triethoxy silicane alkane and 10 parts of D4Mixture be continuously added drop-wise in above-mentioned reactor in 60min, then in 75 DEG C of constant temperature
Stirring polymerization 60min obtains the lotion that milky carries blue light.
A kind of production method of 4 response type waterproofing agent of organosilicon of embodiment
By 0.51 part of op-7,4 parts of SDBS and 60 part of deionized waters are added in reactor jointly, and 60min is stirred at 85 DEG C,
Emulsifier water mixed system is obtained, is adjusted emulsifier water mixed system pH to 2 with sulfuric acid.By 40 parts of propyl trimethoxy silicanes and
9 parts of D4 VIMixture be continuously added drop-wise in above-mentioned reactor in 30min, then obtained in 85 DEG C of constant temperature stirring polyase 13 20min
The lotion of blue light is carried to milky.
A kind of production method of 5 response type waterproofing agent of organosilicon of embodiment
By 1.5 parts of op-10,2.3 parts of SDS and 80 part of deionized waters are added in reactor, stirred at 90 DEG C jointly
30min obtains emulsifier water mixed system, is adjusted emulsifier water mixed system pH to 3 with dodecyl benzene sulfonic acid.It is pungent by 30 parts
Ethyl triethoxy silicane alkane and 9 parts of D3Mixture be continuously added drop-wise in above-mentioned reactor in 30min, then stirred in 90 DEG C of constant temperature
It mixes polymerization 220min and obtains the lotion that milky carries blue light.
A kind of production method of 6 response type waterproofing agent of organosilicon of embodiment
By 1.4 parts of op-10,1.35 parts of SDS and 50 part of deionized waters are added in reactor, stirred at 65 DEG C jointly
30min obtains emulsifier water mixed system, is adjusted emulsifier water mixed system pH to 2 with sulfuric acid.By 40 parts of propyl triethoxies
Silane, 6 parts of dimethyl diethoxy oxysilane and 8 parts of DMCVIMixture above-mentioned reactor is continuously added drop-wise in 30min
In, so lotion of the milky with blue light is obtained in 65 DEG C of constant temperature stirring polymerization 480min.
A kind of production method of 7 response type waterproofing agent of organosilicon of embodiment
By 4.33 parts of op-10,2.34 parts of SDS and 50 part of deionized waters are added in reactor, stirred at 70 DEG C jointly
30min obtains emulsifier water mixed system, is adjusted emulsifier water mixed system PH to 3 with acetic acid.By 26 parts of propyl triethoxies
Silane, 4 parts of aminomethyl phenyl diethoxy oxysilane and 7 parts of D3Mixture be added to above-mentioned reaction at twice in 60min
In device, then lotion of the milky with blue light is obtained in 70 DEG C of constant temperature stirring polyase 13 00min.
A kind of production method of 8 response type waterproofing agent of organosilicon of embodiment
By 2.6 parts of op-7,3.5 parts of SDS and 60 part of deionized waters are added in reactor jointly, and 30min is stirred at 83 DEG C,
Emulsifier water mixed system is obtained, is adjusted emulsifier water mixed system PH to 4 with dodecyl benzene sulfonic acid.By 36 parts of acryloyl-oxies
Propyl-triethoxysilicane, 2 parts of methyl triethoxy oxysilane and 5 parts of D4Mixture be continuously added drop-wise in 60min
It states in reactor, then obtains copolymer resins lotion of the milky with blue light in 83 DEG C of constant temperature stirring 260min.
A kind of production method of 9 response type waterproofing agent of organosilicon of embodiment
By 3.48 parts of op-10,2.3 parts of SDS and 65 part of deionized waters are added in reactor, stirred at 50 DEG C jointly
20min obtains emulsifier water mixed system, is adjusted emulsifier water mixed system pH to 3 with hydrochloric acid.By 38 parts of γ-glycidols
Three oxysilane of ether oxygen base propyl and 9 parts of D4Mixture 0min be disposably added in above-mentioned reactor, then in 50 DEG C of constant temperature
Stirring polymerization 160min obtains the lotion that milky carries blue light.
A kind of production method of 10 response type waterproofing agent of organosilicon of embodiment
Example 10, by 3.58 parts of op-10,2.1 parts of Span60,0.3 part of SDBS and 54 part of deionized water adds in reactor jointly
In, stir 20min at 36 DEG C, obtain emulsifier water mixed system, with sodium hydroxide by emulsifier water mixed system pH adjust to
9.By 28 parts of aminopropyl trimethoxysilanes and 9 parts of D3Mixture be continuously added drop-wise in above-mentioned reactor in 60min, then
Lotion of the milky with blue light is obtained in 36 DEG C of constant temperature stirring polymerization 220min.
A kind of production method of 11 response type waterproofing agent of organosilicon of embodiment
By 0.48 part of op-10,3.1 parts of Tween, 0.4 part of SDS and 77 part of deionized water is added in reactor jointly, 95
20min is stirred at DEG C, obtains emulsifier water mixed system, is adjusted emulsifier water mixed system pH to 12 with potassium hydroxide.By 16
Three oxysilane of part γ-glycydoxy, 9 parts of three oxysilane of aminopropyl and 8 parts of D3 viMixture in 30min
It is inside continuously added drop-wise in above-mentioned reactor, then obtains breast of the milky with blue light in 95 DEG C of constant temperature stirring polymerization 120min
Liquid.
A kind of production method of 12 response type waterproofing agent of organosilicon of embodiment
By 0.46 part of op-10,1.05 parts of Tween, 1.3 parts of SDS and 77 part of deionized waters are added in reactor jointly, 60
20min is stirred at DEG C, obtains emulsifier water mixed system, is adjusted emulsifier water mixed system pH to 1 with dodecyl benzene sulfonic acid.
By 26 parts of three oxysilane of γ-glycydoxy, 4 parts of dimethyl diethoxysilanes and 8 parts of D4Mixture exist
It is continuously added dropwise in above-mentioned reactor in 30min, then obtains milky with indigo plant in 60 DEG C of constant temperature stirring polyase 13 20min
The lotion of light.
A kind of production method of 13 response type waterproofing agent of organosilicon of embodiment
By 0.5 part of op-7,0.5 part of AEO-9,1.4 parts of SBDS and 64 part of deionized waters are added in reactor jointly, at 55 DEG C
Lower stirring 20min is adjusted pH of mixed to 3 with acetic acid.By 24 parts of three oxysilane of γ-glycydoxy, 5 parts
Aminomethyl phenyl dimethoxysilane and 6 parts of D3Mixture 0min be once added in above-mentioned reactor, then in 55 DEG C of constant temperature
Stirring polymerization 420min obtains the lotion that milky carries blue light.
A kind of production method of 14 response type waterproofing agent of organosilicon of embodiment
By 0.46 part of AEO-10,2.4 parts of SBDS and 44 part of deionized waters are added in reactor, stirred at 30 DEG C jointly
20min obtains emulsifier water mixed system, is adjusted emulsifier water mixed system pH to 6 with sulfuric acid.By 10 parts of γ-glycidols
Three oxysilane of ether oxygen base propyl, 3 parts of aminomethyl phenyl dimethoxysilanes, 7 parts of dimethyl diethoxysilanes and 4 parts of DMC
Mixture is continuously added drop-wise in 30min in above-mentioned reactor, then obtains milky in 30 DEG C of constant temperature stirring polymerization 220min
Copolymer emulsion with blue light.
A kind of production method of 15 response type waterproofing agent of organosilicon of embodiment
By 4.36 parts of op-10,0.35 part of SBDS and 30 part of deionized water is added in reactor, stirred at 80 DEG C jointly
20min obtains emulsifier water mixed system, is adjusted emulsifier water mixed system pH to 1 with hydrochloric acid.By 14 parts of phenyl triethoxies
Silane, 11 parts of methyltriethoxysilane and 4 parts of D4Mixture be added drop-wise at twice in above-mentioned reactor in 60min, so
Lotion of the milky with blue light is obtained after 80 DEG C of constant temperature stirring 420min.
A kind of production method of 16 response type waterproofing agent of organosilicon of embodiment
By 2.45 parts of op-10,1.37 parts of SBDS and 60 part of deionized waters are added in reactor, stirred at 67 DEG C jointly
20min obtains emulsifier water mixed system, is adjusted emulsifier water mixed system pH to 11 with potassium hydroxide.By 14 parts of aminopropyls
Triethoxysilane, 15 parts of methyltriethoxysilane and 6 parts of D4Mixture above-mentioned reactor is continuously added drop-wise in 30min
In, then lotion of the milky with blue light is obtained in 67 DEG C of constant temperature stirring polymerization 120min.
A kind of production method of 17 response type waterproofing agent of organosilicon of embodiment
By 1.25 parts of op-10,0.37 part of SBDS and 70 part of deionized water is added in reactor, stirred at 75 DEG C jointly
20min obtains emulsifier water mixed system, is adjusted emulsifier water mixed system pH to 6 with dodecyl benzene sulfonic acid.By 14 parts of first
The mixture of ethyl triethoxy silicane alkane, 6 parts of methyl vinyl diethoxysilanes and 3 parts of DMC are disposably added in 0min
It states in reactor, then obtains copolymer resins lotion of the milky with blue light in 75 DEG C of constant temperature stirring polyase 13 50min.
A kind of production method of 18 response type waterproofing agent of organosilicon of embodiment
By 1.45 parts of op-10,0.4 part of SDS and 60 part of deionized water is added in reactor, stirred at 87 DEG C jointly
20min obtains emulsifier water mixed system, is adjusted emulsifier water mixed system pH to 3 with dodecyl benzene sulfonic acid.By 15 part third
Base trimethoxy silane, 11 parts of methyl vinyl diethoxysilanes and 3 parts of D3 ViMixture added at twice in 30min
Into above-mentioned reactor, then lotion of the milky with blue light is obtained in 87 DEG C of constant temperature stirring polyase 13 20min.
A kind of production method of 19 response type waterproofing agent of organosilicon of embodiment
By 3.35 parts of op-10,1.44 parts of SDBS and 30 part of deionized waters are added in reactor, stirred at 60 DEG C jointly
20min, it is 1 to obtain emulsifier water mixed system dodecyl benzene sulfonic acid and phosphoric acid quality ratio:1 mixture mixes emulsifier water
Zoarium system pH is adjusted to 3.By 28 parts of vinyl front three ethylsilanes and 4 parts of D4 VIDivide three in 30min with the mixture of 5 parts of DMC
It is secondary to be added in above-mentioned reactor, then lotion of the milky with blue light is obtained in 60 DEG C of constant temperature stirring polymerization 120min.
A kind of production method of 20 response type waterproofing agent of organosilicon of embodiment
2.7 parts of op-10,1.12 parts of DBSA, 0.1 part of Span60,0.35 part of SDBS are added in jointly with 36 parts of deionized waters
In reactor, 20min is stirred at 56 DEG C, obtains emulsifier water mixed system, is 1 with the mass ratio of sodium acid carbonate and sodium carbonate:1
Mixture emulsifier water mixed system pH is adjusted to 9.By 3.5 parts of methyltriethoxysilane, 25 parts of aminopropyl trimethoxies
Base silane, 4 parts of D4It is continuously added drop-wise in above-mentioned reactor in 60min with the mixture of 5 parts of DMC, is then stirred in 56 DEG C of constant temperature
It mixes polymerization 120min and obtains the lotion that milky carries blue light.
A kind of production method of 21 response type waterproofing agent of organosilicon of embodiment
By 4.32 parts of op-10,3.11 parts of DBSA, 0.34 part of SDBS and 67 part of deionized water is added in reactor jointly,
20min is stirred at 56 DEG C, the mass ratio for obtaining emulsifier water mixed system ammonium carbonate and ammonium hydrogen carbonate is 1:0.7 mixture will
Emulsifier is adjusted with aqueous mixtures system pH to 8.By 1 part of propyl-triethoxysilicane, 24 parts of chloropropyl triethoxysilanes
With 5 parts of DMCViMixture be added continuously in 30min in above-mentioned reactor, then in 56 DEG C of constant temperature stirring polymerization 110min
Obtain the copolymer resins lotion that milky carries blue light.
A kind of production method of 22 response type waterproofing agent of organosilicon of embodiment
By 0.37 part of op-10,0.22 part of DBSA, 0.41 part of SDBS and 50 part of deionized water is added in reactor jointly,
20min is stirred at 80 DEG C, obtains emulsifier water mixed system.Emulsifier water mixed system pH is adjusted to 9 with ammonium hydroxide.By 3 parts of amine
Propyl-triethoxysilicane, 22 parts of r-chloropropyl trimethoxyl silanes and 7 parts of DMCviMixture be added continuously in 30min
It states in reactor, then obtains copolymer resins lotion of the milky with blue light in 80 DEG C of constant temperature stirring polymerization 110min.
A kind of production method of 23 response type waterproofing agent of organosilicon of embodiment
By 2.33 parts of op-10,0.12 part of DBSA, 0.25 part of SDBS and 55 part of deionized water is added in reactor jointly,
20min is stirred at 70 DEG C, obtains emulsifier water mixed system, is adjusted emulsifier water mixed system pH to 8 with ammonia.By 12 parts
The mixture of three oxysilane of γ-glycydoxy and 13 parts of r-chloropropyl trimethoxyl silanes is continuous in 120min
It is added in above-mentioned reactor, then adds in 4 parts of D4The reaction was continued, and 400min obtains the lotion that milky carries blue light.
A kind of production method of 24 response type waterproofing agent of organosilicon of embodiment
By 0.32 part of AEO-10,0.11 part of DBSA, 1.34 parts of SDBS and 77 part of deionized waters are added in reactor jointly,
20min is stirred at 66 DEG C, obtains emulsifier water mixed system, is 1 with the mass ratio of ammonium carbonate and ammonium hydrogen carbonate:0.7 mixture
Emulsifier water mixed system pH is adjusted to 8.By 2 parts of ethyl orthosilicates, 23 parts of octyl group trimethoxy silanes and 8 parts of D4Mixing
Object is added continuously in 30min in above-mentioned reactor, and then obtaining milky in 66 DEG C of constant temperature stirring polymerization 450min carries
The lotion of blue light.
It should be noted last that more than specific embodiment is merely illustrative of the technical solution of the present invention and unrestricted,
Although the present invention is described in detail with reference to example, it will be understood by those of ordinary skill in the art that, it can be to the present invention
Technical solution be modified or replaced equivalently, without departing from the spirit and scope of technical solution of the present invention, should all cover
Among scope of the presently claimed invention.
Claims (6)
1. a kind of production method of response type waterproofing agent of organosilicon, it is characterised in that：Specific method is as follows：
1) a certain amount of deionized water will be added in containing the mixture of nonionic emulsifier and anion emulsifier, at 50~95 DEG C
20~60min of lower stirring, obtains emulsifier water mixed system；
2) the emulsifier water mixed system pH value of step 1) is adjusted to 1≤pH ＜, 7 or 7 ＜ pH≤14 with pH adjusting agent；
3) the emulsifier water that step 2) is added in after organosilicon ring body being distinguished or mixed by a certain percentage with alkoxy silane mixes
In system；
4) feed after the completion of in the range of 50~95 DEG C, stirring 0~480min of polyase 13 to get；
Organosilicon ring body：Alkoxy silane：Emulsifier：The mass ratio of water is：1~10：25~60：0.1~20：30~90；
The alkoxy silane is：1RSi(OR)3,2RSi(OR)3,3R4R(OR)2, R is methyl, in ethyl, propyl, isopropyl
It is one or more of；
Wherein1R is C1~18Saturated alkyl and aryl radical or1R=OR；2R is acryloxypropyl, vinyl, pi-allyl, ammonia
One kind in propyl, chloropropyl, γ-glycidol ether oxygroup；3R with4R is:Saturated alkyl and aryl radical, acryloyl-oxy third
One kind in base, vinyl, pi-allyl, aminopropyl, chloropropyl, γ-glycidol ether oxygroup；3R with4R is identical or different；
The organosilicon ring body is：D4Octamethylcy-clotetrasiloxane, D3Hexamethyl cyclotrisiloxane, the mixing of DMC organosilicons ring body
Object, D4 viEight vinyl cyclotetrasiloxanes, D3 ViSix vinyl cyclotrisiloxane, DMCviOrganosilicon ring body mixture containing vinyl
One or more of.
2. production method as described in claim 1, it is characterised in that：The nonionic emulsifier and anion emulsifier it is mixed
Object is closed as the one or more in nonionic emulsifier and one or more mixtures formed in anion emulsifier.
3. production method as described in claim 1, it is characterised in that：The nonionic emulsifier is：Op is serial, AEO is serial,
Span series or tween series.
4. production method as described in claim 1, it is characterised in that：The anion emulsifier is SDBS, DBSA or SDS.
5. production method as described in claim 1, it is characterised in that：The pH adjusting agent is：Acetic acid, hydrochloric acid, sulfuric acid, phosphorus
Acid, dodecyl benzene sulfonic acid, sodium hydroxide, potassium hydroxide, sodium carbonate, sodium acid carbonate, ammonium carbonate, ammonium hydrogen carbonate, ammonium hydroxide, ammonia
One or more of.
6. production method as described in claim 1, it is characterised in that：By organosilicon ring body and alkoxyl silicone in the step 3)
Alkane adds to the mode in emulsifier water mixed system as disposable charging, the mode of batch charging or continuous charging, feed time
For 0~120min.
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| CN107916072A (en) * | 2017-10-31 | 2018-04-17 | 广州广微包装科技有限公司 | A kind of spray-type watery water-proofing agent and preparation method thereof |
| CN110003724A (en) * | 2019-02-25 | 2019-07-12 | 薛银福 | A kind of strong concrete interfacial agents and preparation method thereof |
| CN110982425A (en) * | 2019-11-29 | 2020-04-10 | 湖北新四海化工股份有限公司 | Environment-friendly self-crosslinking ceramic antifouling agent and preparation method thereof |
| CN116601127A (en) | 2020-12-18 | 2023-08-15 | 赢创运营有限公司 | Dilution-stable aqueous composition for the bulk hydrophobization of inorganic building materials |
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| CN1297591C (en) * | 2005-03-07 | 2007-01-31 | 华明扬 | Process for preparing anion composite modified organosilicon emulsion |
| CN100999583A (en) * | 2006-12-22 | 2007-07-18 | 中国林业科学研究院林产化学工业研究所 | Mfg. process of organic silican polymer emulsion |
| CN101280345B (en) * | 2008-01-22 | 2012-04-25 | 浙江传化股份有限公司 | Anion organosilicon emulsion smoothing agent for leather and preparation thereof |
| CN103003333A (en) * | 2010-07-22 | 2013-03-27 | 道康宁公司 | Process for making polysiloxane emulsions |
| CN103755961A (en) * | 2013-12-20 | 2014-04-30 | 中科院广州化学有限公司 | Polysiloxane microemulsion, and preparation method and application thereof |
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