CN105111932A - Production method of reactive organosilicon waterproofing agent - Google Patents
Production method of reactive organosilicon waterproofing agent Download PDFInfo
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Abstract
The invention discloses a production method of a reactive organosilicon waterproofing agent, which comprises the following steps: 1) adding a certain amount of deionized water into a mixture containing a nonionic emulsifier and an anionic emulsifier, and stirring at 50-95 DEG C for 20-60 minutes to obtain an emulsifier-water mixture system; 2) regulating the pH value of the emulsifier-water mixture system in the step 1) to greater than or equal to 1 and smaller than 7 or greater than 7 and smaller than or equal to 14 with a pH regulator; 3) proportionally adding an organosilicon ring body and alkoxy silane or mixture thereof into the emulsifier-water mixture system in the step 2); and 4) after finishing charging, stirring for polymerization at 50-95 DEG C for 30-480 minutes. The method has the advantages of cheap and accessible raw materials, and is simple to operate, easy to implement and convenient for property regulation. The prepared product has the advantages of uniform dispersion, favorable stability, favorable weather resistance, high adhesion, favorable washing fastness, energy saving, environment friendliness, favorable reproducibility and the like.
Description
Technical field
The invention belongs to chemistry and material science, particularly a kind of production method of response type waterproofing agent of organosilicon.
Background technology
Organosilicon is nontoxic, harmless and have excellent high-low temperature resistant and the performance such as hydrophobic, and in current many building materials water-proof materials, result of use is best.In earlier stage, waterproofing agent of organosilicon is solvent-borne type, and use cost is high, contaminate environment.Along with the development of science and technology, present stage adopts the aqueous product of low-cost and pollution-less to substitute.
Aqueous product is often methyl siliconic acid salt and emulsion class two kinds in the market.Methyl siliconic acid salt good water solubility, use cost is low, but methyl silicate is easily with water loss, and validity period is short, and in strong basicity corrosion material contaminate environment.Emulsion-type waterproofing agent is usually through organosilicon linear polymer: methyl-silicone oil, hydroxy silicon oil, Silicon Containing Hydrogen wet goods emulsification preparation, this kind of Product Activity functional group is few, rear difficulty and base material is used to form effective covalent linkage, cause this kind of keeping life short, at concrete, gypsum, adopts outer addition manner use can affect the strength of materials, weak effect in the materials such as all kinds of sheet materials; The product stability difference simultaneously adopting emulsification method to obtain easily layering loses usability.For improving the above-mentioned shortcoming of this series products, the product result of use adopting silane dispersing method to obtain subsequently is good, but cost is high, poor stability.Therefore, the defect that anxious a kind of stability yet-to-be developed is high, validity period is long emulsion type products overcomes above-mentioned two series products.
Summary of the invention
The object of the invention is for above-mentioned present situation, aim to provide that a kind of stability is high, validity period is long, at concrete, gypsum, can not reduce the production method of the emulsion-type waterproofing agent of organosilicon of the intensity of material when the method for mixing in adopting in the materials such as all kinds of sheet materials uses.
The object of the invention is to be achieved through the following technical solutions:
A production method for response type waterproofing agent of organosilicon, concrete grammar is as follows:
1) mixture containing nonionic emulsifying agent and anionic emulsifier is added a certain amount of deionized water, at 50 ~ 95 DEG C, stir 20 ~ 60min, obtain emulsifying agent water mixed system;
2) by pH adjusting agent by step 1) emulsifying agent water mixed system pH value be adjusted to 1≤pH < 7 or 7 < pH≤14;
3) organosilicon ring body is added step 2 by a certain percentage respectively or after mixing with organoalkoxysilane) emulsifying agent water mixed system in;
4) after having fed in raw material within the scope of 50 ~ 95 DEG C, stirred polyase 13 0 ~ 480min, to have obtained final product.
Further, organosilicon ring body: organoalkoxysilane: emulsifying agent: the mass ratio of water is: 1 ~ 10:25 ~ 60:0.1 ~ 20:30 ~ 90.
Further, the mixture of described nonionic emulsifying agent and anionic emulsifier is one or more mixtures formed in one or more and anionic emulsifier in nonionic emulsifying agent.
Further, described nonionic emulsifying agent is: op is serial, AEO is serial, Span is serial or tween is serial.
Further, described anionic emulsifier is SDBS, DBSA or SDS.
Further, described pH adjusting agent is: one or more in acetic acid, hydrochloric acid, sulfuric acid, phosphoric acid, Witco 1298 Soft Acid, sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate, volatile salt, bicarbonate of ammonia, ammoniacal liquor, ammonia.
Further, described step 3) in by organosilicon ring body and organoalkoxysilane, the mode added in emulsifying agent water mixed system is disposable reinforced, the mode of batch charging or continuous charging, feed time is 0 ~ 120min.
Further, described organoalkoxysilane is:
1rSi (OR)
3,
2rSi (OR)
3,
3r
4r (OR)
2, R is one or more in methyl, ethyl, propyl group, sec.-propyl;
Wherein
1r is C
1 ~ 18saturated alkyl and aryl radical or
1r=OR;
2r is the one in acryloxypropyl, vinyl, allyl group, aminopropyl, chloropropyl, γ-glycidyl ether oxygen base;
3r with
4r is: the one in saturated alkyl and aryl radical, acryloxypropyl, vinyl, allyl group, aminopropyl, chloropropyl, γ-glycidyl ether oxygen base;
3r with
4r can identical can be different.
Further, described organosilicon ring body is: D
4octamethylcyclotetrasiloxane, D
3hexamethyl cyclotrisiloxane, DMC organosilicon ring body mixture, D
4 vieight vinyl cyclotetrasiloxanes, D
3 visix vinyl cyclotrisiloxane, DMC
vicontaining one or more in the organosilicon ring body mixture of vinyl.
The production method of a kind of response type waterproofing agent of organosilicon provided by the invention, low raw-material cost is easy to get, operation is simple, performance is convenient to adjustment, obtained polymer emulsion is uniformly dispersed, favorable reproducibility, preparation process is pollution-free, the product obtained is easy to use, good waterproof performance, can large-scale industrial production be carried out, waterproof or the maintenance demands such as stone material, timber, gypsum, concrete, coating, historical relic, textiles can be met.
Embodiment
The embodiment of the present invention provides a kind of production method of response type waterproofing agent of organosilicon.Concrete grammar is as follows:
1) mixture containing nonionic emulsifying agent and anionic emulsifier is added a certain amount of deionized water, at 50 ~ 95 DEG C, stir 20 ~ 60min, obtain emulsifying agent water mixed system.
2) by pH adjusting agent by step 1) emulsifying agent water mixed system pH value be adjusted to 1≤pH < 7 or 7 < pH≤14.
3) by organosilicon ring body and organoalkoxysilane by a certain percentage respectively or after mixing in 50 ~ 95 DEG C of temperature ranges, add step 2) emulsifying agent water mixed system in.Organosilicon ring body: organoalkoxysilane: emulsifying agent: the mass ratio of water is: 1 ~ 10:25 ~ 60:0.1 ~ 20:30 ~ 90.
4) after having fed in raw material within the scope of 50 ~ 95 DEG C, stirred polyase 13 0 ~ 480min, to have obtained final product.
The open loop of organosilicon ring body need effectively be controlled the open loop of silane ring body and rate of polymerization with organoalkoxysilane copolymerization, the hydrolysis of alkoxyl silicone group in organoalkoxysilane, polycondensation and with the rates of polymerization such as ring body open-loop products copolymerization, and then control the product polymerization degree and structure, to obtain the product of different performance.To control between all kinds of monomer the most effective means of hydrolytie polycondensation speed by adjusting the potential of hydrogen of system and temperature.Under non-neutral condition, silane ring body effectively can obtain difunctionality linear siloxane by open loop polycondensation increase molecular weight; And with organoalkoxysilane copolymerization; The slight change of pH-value also can cause the hydrolytie polycondensation speed of various monomer and a great difference of product.Therefore, control the homopolymerization of all kinds of monomer and copolymerization rate by controlling the pH-value of emulsion system and obtain the different product of structure, control the different performance of product.Therefore the present invention's pH adjusting agent emulsifying agent water mixed system pH value is adjusted to 1 ~ 14 (PH ≠ 7).
Again organosilicon ring body or various silane are added to step 2 respectively or after mixing) emulsifying agent water mixed system in mode disposable reinforced for adopting, the mode of batch charging or continuous charging, feed time is 0 ~ 120min.Join in the emulsifying agent after PH adjustment and deionized water mixed solution, then obtain response type waterproofing agent of organosilicon through stirring 30 ~ 480min.
In suitable emulsifying agent aqueous systems, the product solvability after copolymerization changes, and with emulsifying agent and micellar phase mutual effect thereof, forms stable emulsion particle, finally obtains stable response type waterproofing agent of organosilicon.And by the copolymerization between different monomers, obtain the response type waterproofing agent of organosilicon of different structure and performance, meet the demand in the field such as the manufacturing of stone material, textiles, concrete, gypsum, timber, coating, historical relic's protection, all kinds of sheet material.
With specific embodiment in detail the present invention is described in detail below:
The production method of embodiment 1 one kinds of response type waterproofing agent of organosilicon
By 1.5 parts of op-10,2 parts of SDBS and 50 part deionized waters add in reactor jointly, stir 20min, obtain emulsifying agent water mixed system at 50 DEG C; With acetic acid by emulsifying agent water mixed system pH regulator to 5; 25 parts of Union carbide A-162s are added drop-wise to continuously in above-mentioned reactor in 40min, then once add 10 parts of DMC, then stir polymerization 60min in 50 DEG C of constant temperature and obtain the emulsion of oyster white with blue light.
The production method of embodiment 2 one kinds of response type waterproofing agent of organosilicon
By 1.9 parts of AEO-9,2.2 parts of SDBS and 50 part deionized waters add in reactor jointly, stir 30min, obtain emulsifying agent water mixed system at 70 DEG C, with hydrochloric acid by emulsifying agent water mixed system pH regulator to 4.The mixture of 40 parts of methyltrimethoxy silanes and 8 parts of DMC is added drop-wise to continuously in above-mentioned reactor in 50min, then stirs polymerization 120min in 70 DEG C of constant temperature and obtain the emulsion of oyster white with blue light.
The production method of embodiment 3 one kinds of response type waterproofing agent of organosilicon
By 1.2 parts of op-10,2.5 parts of SDBS and 55 part deionized waters add in reactor jointly, stir 60min, obtain emulsifying agent water mixed system at 75 DEG C, with Witco 1298 Soft Acid by emulsifying agent water mixed system pH regulator to 1.By 60 parts of propyl-triethoxysilicanes and 10 parts of D
4mixture be added drop-wise to continuously in 60min in above-mentioned reactor, then stir polymerization 60min in 75 DEG C of constant temperature and obtain the emulsion of oyster white with blue light.
The production method of embodiment 4 one kinds of response type waterproofing agent of organosilicon
By 0.51 part of op-7,4 parts of SDBS and 60 part deionized waters add in reactor jointly, stir 60min, obtain emulsifying agent water mixed system at 85 DEG C, with sulfuric acid by emulsifying agent water mixed system pH regulator to 2.By 40 parts of propyl trimethoxy silicanes and 9 parts of D
4 vImixture be added drop-wise to continuously in 30min in above-mentioned reactor, then stir polyase 13 20min in 85 DEG C of constant temperature and obtain the emulsion of oyster white with blue light.
The production method of embodiment 5 one kinds of response type waterproofing agent of organosilicon
By 1.5 parts of op-10,2.3 parts of SDS and 80 part deionized waters add in reactor jointly, stir 30min, obtain emulsifying agent water mixed system at 90 DEG C, with Witco 1298 Soft Acid by emulsifying agent water mixed system pH regulator to 3.By 30 parts of octyltri-ethoxysilane and 9 parts of D
3mixture be added drop-wise to continuously in 30min in above-mentioned reactor, then stir polymerization 220min in 90 DEG C of constant temperature and obtain the emulsion of oyster white with blue light.
The production method of embodiment 6 one kinds of response type waterproofing agent of organosilicon
By 1.4 parts of op-10,1.35 parts of SDS and 50 part deionized waters add in reactor jointly, stir 30min, obtain emulsifying agent water mixed system at 65 DEG C, with sulfuric acid by emulsifying agent water mixed system pH regulator to 2.By 40 parts of propyl-triethoxysilicanes, 6 parts of dimethyl diethoxy TMOSs and 8 parts of DMC
vImixture be added drop-wise to continuously in 30min in above-mentioned reactor, so stir polymerization 480min in 65 DEG C of constant temperature and obtain the emulsion of oyster white with blue light.
The production method of embodiment 7 one kinds of response type waterproofing agent of organosilicon
By 4.33 parts of op-10,2.34 parts of SDS and 50 part deionized waters add in reactor jointly, stir 30min, obtain emulsifying agent water mixed system at 70 DEG C, with acetic acid, emulsifying agent water mixed system PH are adjusted to 3.By 26 parts of propyl-triethoxysilicanes, 4 parts of aminomethyl phenyl diethoxy TMOSs and 7 parts of D
3mixture join at twice in 60min in above-mentioned reactor, then stir polyase 13 00min in 70 DEG C of constant temperature and obtain the emulsion of oyster white with blue light.
The production method of embodiment 8 one kinds of response type waterproofing agent of organosilicon
By 2.6 parts of op-7,3.5 parts of SDS and 60 part deionized waters add in reactor jointly, stir 30min, obtain emulsifying agent water mixed system at 83 DEG C, with Witco 1298 Soft Acid, emulsifying agent water mixed system PH are adjusted to 4.By 36 parts of acryloxypropyl triethoxyl silanes, 2 parts of methyl triethoxy TMOSs and 5 parts of D
4mixture be added drop-wise to continuously in 60min in above-mentioned reactor, then stir 260min in 83 DEG C of constant temperature and obtain the copolymer resins emulsion of oyster white with blue light.
The production method of embodiment 9 one kinds of response type waterproofing agent of organosilicon
By 3.48 parts of op-10,2.3 parts of SDS and 65 part deionized waters add in reactor jointly, stir 20min, obtain emulsifying agent water mixed system at 50 DEG C, with hydrochloric acid by emulsifying agent water mixed system pH regulator to 3.By 38 parts of γ-glycydoxy three TMOSs and 9 parts of D
4mixture 0min be disposablely added in above-mentioned reactor, then stir polymerization 160min in 50 DEG C of constant temperature and obtain the emulsion of oyster white with blue light.
The production method of embodiment 10 1 kinds of response type waterproofing agent of organosilicon
Example 10, by 3.58 parts of op-10,2.1 parts of Span60,0.3 part of SDBS and 54 part deionized water adds in reactor jointly, stirs 20min, obtain emulsifying agent water mixed system at 36 DEG C, with sodium hydroxide by emulsifying agent water mixed system pH regulator to 9.By 28 parts of aminopropyl trimethoxysilane and 9 parts of D
3mixture be added drop-wise to continuously in 60min in above-mentioned reactor, then stir polymerization 220min in 36 DEG C of constant temperature and obtain the emulsion of oyster white with blue light.
The production method of embodiment 11 1 kinds of response type waterproofing agent of organosilicon
By 0.48 part of op-10,3.1 parts of Tween, 0.4 part of SDS and 77 part deionized water adds in reactor jointly, stirs 20min, obtain emulsifying agent water mixed system at 95 DEG C, with potassium hydroxide by emulsifying agent water mixed system pH regulator to 12.By 16 parts of γ-glycydoxy three TMOSs, 9 parts of aminopropyl three TMOSs and 8 parts of D
3 vimixture be added drop-wise to continuously in 30min in above-mentioned reactor, then stir polymerization 120min in 95 DEG C of constant temperature and obtain the emulsion of oyster white with blue light.
The production method of embodiment 12 1 kinds of response type waterproofing agent of organosilicon
By 0.46 part of op-10,1.05 parts of Tween, 1.3 parts of SDS and 77 part deionized waters add in reactor jointly, stir 20min, obtain emulsifying agent water mixed system at 60 DEG C, with Witco 1298 Soft Acid by emulsifying agent water mixed system pH regulator to 1.By 26 parts of γ-glycydoxy three TMOSs, 4 parts of dimethyldiethoxysilanes and 8 parts of D
4mixture be added dropwise to continuously in 30min in above-mentioned reactor, then stir polyase 13 20min in 60 DEG C of constant temperature and obtain the emulsion of oyster white with blue light.
The production method of embodiment 13 1 kinds of response type waterproofing agent of organosilicon
By 0.5 part of op-7,0.5 part of AEO-9,1.4 parts of SBDS and 64 part deionized waters add in reactor jointly, stir 20min, with acetic acid, pH of mixed is adjusted to 3 at 55 DEG C.By 24 parts of γ-glycydoxy three TMOSs, 5 parts of aminomethyl phenyl dimethoxysilane and 6 parts of D
3mixture 0min once join in above-mentioned reactor, then stir polymerization 420min in 55 DEG C of constant temperature and obtain the emulsion of oyster white with blue light.
The production method of embodiment 14 1 kinds of response type waterproofing agent of organosilicon
By 0.46 part of AEO-10,2.4 parts of SBDS and 44 part deionized waters add in reactor jointly, stir 20min, obtain emulsifying agent water mixed system at 30 DEG C, with sulfuric acid by emulsifying agent water mixed system pH regulator to 6.The mixture of 10 parts of γ-glycydoxy three TMOSs, 3 parts of aminomethyl phenyl dimethoxysilane, 7 parts of dimethyldiethoxysilanes and 4 parts of DMC is added drop-wise to continuously in above-mentioned reactor in 30min, then stirs polymerization 220min in 30 DEG C of constant temperature and obtain the copolymer emulsion of oyster white with blue light.
The production method of embodiment 15 1 kinds of response type waterproofing agent of organosilicon
By 4.36 parts of op-10,0.35 part of SBDS and 30 part deionized water adds in reactor jointly, stirs 20min, obtain emulsifying agent water mixed system at 80 DEG C, with hydrochloric acid by emulsifying agent water mixed system pH regulator to 1.By 14 parts of phenyl triethoxysilanes, 11 parts of Union carbide A-162s and 4 parts of D
4mixture be added drop-wise at twice in 60min in above-mentioned reactor, then stir 420min in 80 DEG C of constant temperature and obtain the emulsion of oyster white with blue light.
The production method of embodiment 16 1 kinds of response type waterproofing agent of organosilicon
By 2.45 parts of op-10,1.37 parts of SBDS and 60 part deionized waters add in reactor jointly, stir 20min, obtain emulsifying agent water mixed system at 67 DEG C, with potassium hydroxide by emulsifying agent water mixed system pH regulator to 11.By 14 parts of aminopropyl triethoxysilanes, 15 parts of Union carbide A-162s and 6 parts of D
4mixture be added drop-wise to continuously in 30min in above-mentioned reactor, then stir polymerization 120min in 67 DEG C of constant temperature and obtain the emulsion of oyster white with blue light.
The production method of embodiment 17 1 kinds of response type waterproofing agent of organosilicon
By 1.25 parts of op-10,0.37 part of SBDS and 70 part deionized water adds in reactor jointly, stirs 20min, obtain emulsifying agent water mixed system at 75 DEG C, with Witco 1298 Soft Acid by emulsifying agent water mixed system pH regulator to 6.By 14 parts of Union carbide A-162s, the mixture of 6 parts of methyl vinyl diethoxysilane and 3 parts of DMC is disposable in 0min to be added in above-mentioned reactor, then stirs polyase 13 50min in 75 DEG C of constant temperature and obtains the copolymer resins emulsion of oyster white with blue light.
The production method of embodiment 18 1 kinds of response type waterproofing agent of organosilicon
By 1.45 parts of op-10,0.4 part of SDS and 60 part deionized water adds in reactor jointly, stirs 20min, obtain emulsifying agent water mixed system at 87 DEG C, with Witco 1298 Soft Acid by emulsifying agent water mixed system pH regulator to 3.By 15 parts of propyl trimethoxy silicanes, 11 parts of methyl vinyl diethoxysilane and 3 parts of D
3 vimixture join at twice in 30min in above-mentioned reactor, then stir polyase 13 20min in 87 DEG C of constant temperature and obtain the emulsion of oyster white with blue light.
The production method of embodiment 19 1 kinds of response type waterproofing agent of organosilicon
By 3.35 parts of op-10,1.44 parts of SDBS and 30 part deionized waters add in reactor jointly, at 60 DEG C, stir 20min, obtain emulsifying agent water mixed system Witco 1298 Soft Acid and phosphoric acid quality than being that the mixture of 1:1 is by emulsifying agent water mixed system pH regulator to 3.By 28 parts of vinyl front three ethylsilane and 4 parts of D
4 vIdivide in 30min with the mixture of 5 parts of DMC and join for three times in above-mentioned reactor, then stir polymerization 120min in 60 DEG C of constant temperature and obtain the emulsion of oyster white with blue light.
The production method of embodiment 20 1 kinds of response type waterproofing agent of organosilicon
By 2.7 parts of op-10,1.12 part DBSA, 0.1 part of Span60,0.35 part of SDBS and 36 part deionized water adds in reactor jointly, 20min is stirred at 56 DEG C, obtaining emulsifying agent water mixed system, is that the mixture of 1:1 is by emulsifying agent water mixed system pH regulator to 9 with the mass ratio of sodium bicarbonate and sodium carbonate.By 3.5 parts of Union carbide A-162s, 25 parts of aminopropyl trimethoxysilane, 4 parts of D
4be added drop-wise to continuously in 60min in above-mentioned reactor with the mixture of 5 parts of DMC, then stir polymerization 120min in 56 DEG C of constant temperature and obtain the emulsion of oyster white with blue light.
The production method of embodiment 21 1 kinds of response type waterproofing agent of organosilicon
By 4.32 parts of op-10,3.11 part DBSA, 0.34 part of SDBS and 67 part deionized water adds in reactor jointly, at 56 DEG C, stir 20min, and the mass ratio obtaining emulsifying agent water mixed system volatile salt and bicarbonate of ammonia is that emulsifying agent and water mixture system pH are adjusted to 8 by the mixture of 1:0.7.By 1 part of propyl-triethoxysilicane, 24 parts of chloropropyl triethoxysilanes and 5 parts of DMC
vimixture join continuously in 30min in above-mentioned reactor, then stir polymerization 110min in 56 DEG C of constant temperature and obtain the copolymer resins emulsion of oyster white with blue light.
The production method of embodiment 22 1 kinds of response type waterproofing agent of organosilicon
By 0.37 part of op-10,0.22 part of DBSA, 0.41 part of SDBS and 50 part deionized water adds in reactor jointly, stirs 20min, obtain emulsifying agent water mixed system at 80 DEG C.With ammoniacal liquor by emulsifying agent water mixed system pH regulator to 9.By 3 parts of amine propyl-triethoxysilicanes, 22 parts of r-chloropropyl trimethoxyl silanes and 7 parts of DMC
vimixture join continuously in 30min in above-mentioned reactor, then stir polymerization 110min in 80 DEG C of constant temperature and obtain the copolymer resins emulsion of oyster white with blue light.
The production method of embodiment 23 1 kinds of response type waterproofing agent of organosilicon
By 2.33 parts of op-10,0.12 part of DBSA, 0.25 part of SDBS and 55 part deionized water adds in reactor jointly, stirs 20min, obtain emulsifying agent water mixed system at 70 DEG C, with ammonia by emulsifying agent water mixed system pH regulator to 8.The mixture of 12 parts of γ-glycydoxy three TMOSs and 13 parts of r-chloropropyl trimethoxyl silanes is joined continuously in above-mentioned reactor in 120min, then adds 4 parts of D
4continue reaction 400min and obtain the emulsion of oyster white with blue light.
The production method of embodiment 24 1 kinds of response type waterproofing agent of organosilicon
By 0.32 part of AEO-10,0.11 part of DBSA, 1.34 parts of SDBS and 77 part deionized waters add in reactor jointly, at 66 DEG C, stir 20min, obtaining emulsifying agent water mixed system, is that the mixture of 1:0.7 is by emulsifying agent water mixed system pH regulator to 8 with the mass ratio of volatile salt and bicarbonate of ammonia.By 2 parts of tetraethoxys, 23 parts of octyl group Trimethoxy silanes and 8 parts of D
4mixture join continuously in 30min in above-mentioned reactor, then stir polymerization 450min in 66 DEG C of constant temperature and obtain the emulsion of oyster white with blue light.
It should be noted last that, above embodiment is only in order to illustrate technical scheme of the present invention and unrestricted, although with reference to example to invention has been detailed description, those of ordinary skill in the art is to be understood that, can modify to technical scheme of the present invention or equivalent replacement, and not departing from the spirit and scope of technical solution of the present invention, it all should be encompassed in the middle of right of the present invention.
Claims (9)
1. a production method for response type waterproofing agent of organosilicon, is characterized in that: concrete grammar is as follows:
1) mixture containing nonionic emulsifying agent and anionic emulsifier is added a certain amount of deionized water, at 50 ~ 95 DEG C, stir 20 ~ 60min, obtain emulsifying agent water mixed system;
2) by pH adjusting agent by step 1) emulsifying agent water mixed system pH value be adjusted to 1≤pH < 7 or 7 < pH≤14;
3) organosilicon ring body is added step 2 by a certain percentage respectively or after mixing with organoalkoxysilane) emulsifying agent water mixed system in;
4) after having fed in raw material within the scope of 50 ~ 95 DEG C, stirred polyase 13 0 ~ 480min, to have obtained final product.
2. production method as claimed in claim 1, is characterized in that: organosilicon ring body: organoalkoxysilane: emulsifying agent: the mass ratio of water is: 1 ~ 10:25 ~ 60:0.1 ~ 20:30 ~ 90.
3. production method as claimed in claim 1, is characterized in that: the mixture of described nonionic emulsifying agent and anionic emulsifier is one or more mixtures formed in one or more and the anionic emulsifier in nonionic emulsifying agent.
4. production method as claimed in claim 1, is characterized in that: described nonionic emulsifying agent is: op is serial, AEO is serial, Span is serial or tween is serial.
5. production method as claimed in claim 1, is characterized in that: described anionic emulsifier is SDBS, DBSA or SDS.
6. production method as claimed in claim 1, is characterized in that: described pH adjusting agent is: one or more in acetic acid, hydrochloric acid, sulfuric acid, phosphoric acid, Witco 1298 Soft Acid, sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate, volatile salt, bicarbonate of ammonia, ammoniacal liquor, ammonia.
7. production method as claimed in claim 1, it is characterized in that: described step 3) in by organosilicon ring body and organoalkoxysilane, the mode added in emulsifying agent water mixed system is disposable reinforced, the mode of batch charging or continuous charging, feed time is 0 ~ 120min.
8. production method as claimed in claim 1, is characterized in that: described organoalkoxysilane is:
1rSi (OR)
3,
2rSi (OR)
3,
3r
4r (OR)
2, R is one or more in methyl, ethyl, propyl group, sec.-propyl;
Wherein
1r is C
1 ~ 18saturated alkyl and aryl radical or
1r=OR;
2r is the one in acryloxypropyl, vinyl, allyl group, aminopropyl, chloropropyl, γ-glycidyl ether oxygen base;
3r with
4r is: the one in saturated alkyl and aryl radical, acryloxypropyl, vinyl, allyl group, aminopropyl, chloropropyl, γ-glycidyl ether oxygen base;
3r with
4r can identical can be different.
9. production method as claimed in claim 1, is characterized in that: described organosilicon ring body is: D
4octamethylcyclotetrasiloxane, D
3hexamethyl cyclotrisiloxane, DMC organosilicon ring body mixture, D
4 vieight vinyl cyclotetrasiloxanes, D
3 visix vinyl cyclotrisiloxane, DMC
vicontaining one or more in the organosilicon ring body mixture of vinyl.
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| 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 |
| WO2022128994A1 (en) | 2020-12-18 | 2022-06-23 | Evonik Operations Gmbh | Dilution-stable aqueous compositions for the mass hydrophobization of mineral building materials |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1670056A (en) * | 2005-03-07 | 2005-09-21 | 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 |
| CN101280345A (en) * | 2008-01-22 | 2008-10-08 | 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 |
-
2015
- 2015-08-26 CN CN201510531110.5A patent/CN105111932B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1670056A (en) * | 2005-03-07 | 2005-09-21 | 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 |
| CN101280345A (en) * | 2008-01-22 | 2008-10-08 | 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 |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| WO2022128994A1 (en) | 2020-12-18 | 2022-06-23 | Evonik Operations Gmbh | Dilution-stable aqueous compositions for the mass hydrophobization of mineral building materials |
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| CN105111932B (en) | 2018-06-05 |
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