CN104446125A - Organosilicon waterproofing agent of solid powder and preparation method of organosilicon waterproofing agent - Google Patents

Organosilicon waterproofing agent of solid powder and preparation method of organosilicon waterproofing agent Download PDF

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Publication number
CN104446125A
CN104446125A CN201410732607.9A CN201410732607A CN104446125A CN 104446125 A CN104446125 A CN 104446125A CN 201410732607 A CN201410732607 A CN 201410732607A CN 104446125 A CN104446125 A CN 104446125A
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water
agent
organosilicon
silane
waterproofing agent
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Pending
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CN201410732607.9A
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Chinese (zh)
Inventor
周宇鹏
周涛
滕青艺
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Guangzhou seeco Chemical Technology Co Ltd
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NANXIONG TRIPOD CHEMICAL Co Ltd
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Abstract

The invention relates to an organosilicon waterproofing agent of solid powder. Silicane and polysiloxane are taken as waterproofing agents; a nonionic surfactant is taken as an emulsifier; polycarboxylate is taken as a cement water-reducing agent and a dispersing agent; a water-soluble polymer is adopted as a colloid protectant and a cement anti-cracking agent; and ultrafine silica is taken as a dispersing carrier, so that the organosilicon waterproofing agent has good dispersity in water, and further has good mixing uniformity with aggregates such as cement and quartz sand. The nonionic surfactant is added as the emulsifier; meanwhile, the polycarboxylate dispersing agent and water-soluble polyvinyl alcohol are added as the colloid protectants, so that the silicane and the polysiloxane in the waterproofing agent are always wrapped by the emulsifier, the dispersing agent and the colloid protectants until contacting the cement; and water-repellent silicon is formed by hydrolytic polycondensation in an alkaline water medium.

Description

A kind of pressed powder waterproofing agent of organosilicon and preparation method thereof
Technical field
The invention belongs to water-resisting agent technical field, relate to a kind of pressed powder waterproofing agent of organosilicon and preparation method thereof.
Background technology
Silane and polysiloxane are the excellent water-resisting agents of building materials, and they can penetrate in the internal structure of porous building materials, and under the effect of moisture content, hydrolytie polycondensation forms the web-like silicon resin that vapour refuses water, prevent penetration by liquid water and do not stop steam through.These waterproofing agent of organosilicon can be solvent type, also emulsion-type can be made, the advantage of solvent type water-resisting agent is that seepage force is strong, but with organic solvent, transport uses dangerous, and price is also more expensive, the water-resisting agent of emulsion-type is without flammable solvent, use water as thinner, but seepage force is poor, waterproof effect is not as good as solvent type water-resisting agent.No matter be solvent-borne type or emulsion-type waterproofing agent, be all liquid, packed and transported is all not too convenient.
External as US Patent No. 8431646B 2(2013.03.30), Degussa company of Germany adopts water-soluble polymers emulsification waterproofing agent of organosilicon, then obtain the free-pouring waterproofing agent of organosilicon being easy to be scattered in water by spraying dry, the spray drying device that this method is expensive, it is high to invest large energy consumption.The US Patent No. 6268423B of Wa Ke company of Germany application 1, employing silicon-dioxide is carrier, then mixes with silane, siloxanes, obtains Powdered water-resisting agent, the powdery water-resisting agent obtained by this method, is also not easily scattered in water, after mixing, disperses uneven with powders such as cement, after cement solidification, waterproof effect is not good, and affects the intensity of cement products.
Summary of the invention
For overcoming above-mentioned technical disadvantages; the invention provides a kind of pressed powder waterproofing agent of organosilicon and preparation method thereof; it adopts nonionogenic tenside to be emulsifying agent; take water-soluble high-molecular compound as the protective material of emulsion; with polycarboxylate cement water reducer for dispersion intensifier; again with the large silicon-dioxide of specific surface area for carrier, make the Powdered waterproofing agent of organosilicon of easy wetting and dispersing in water.Join in cement concrete and sand-cement slurry and be mixed together → aquation, cement concrete and sand-cement slurry integral waterproofing is made after solidification, make the water-intake rate reduction of cement products etc. 80%, intensity improves more than 20%, and in anti-sealing, chlorion is to the erosion of hardware in cement concrete.
The present invention solves the technological method that its technical problem adopts: a kind of pressed powder waterproofing agent of organosilicon; it with silane and polysiloxane for water-resisting agent; take nonionogenic tenside as emulsifying agent; take polycarboxylate as cement water reducing agent and dispersion agent; taking water-soluble polymers as colloid protective agent and cement anticracking agent, take superfine silicon dioxide as dispersible carrier.
The preparation method of above-mentioned pressed powder waterproofing agent of organosilicon, the steps include:
Choose the water-soluble high-molecular compound of 100 parts according to weight ratio and add the nonionogenic tenside that weight part is 8 parts wherein, and stir, then the silane of 80 parts is taken, after the polysiloxane of 40 parts mixes, add in polyvinyl alcohol aqueous phase several times, each add-on is 10-20 part, open high-shear emulsion machine, emulsification is carried out with the speed of 2000-4000 rev/min, after oil phase adds, add the polycarboxylate aqueous solution of 12 parts again, high speed shear 5 minutes again, obtain the organic silicon water-proofing agent emulsion containing organosilicon 50%, again emulsion is added in carrier to stir evenly and just obtains pressed powder water-resisting agent.
Described silane comprises the alkylalkoxy silane of various carbon chain lengths, as Union carbide A-162, propyl-triethoxysilicane, butyl triethoxyl silane, octyltri-ethoxysilane, dodecyl triethoxysilane or their mixture.
Described polysiloxane is the hydrolysis prepolymer of various silane.
Described emulsifying agent be various nonionogenic tenside as alkyl alcohol ethoxylates, polyoxyethylene carboxylate class, the HLB value of emulsifying agent between 9 ~ 13, the consumption of emulsifying agent be silane siloxanes total amount 5 ~ 10% between.
Described water-soluble high-molecular compound comprises polyvinyl alcohol, Soxylat A 25-7 and carbohydrate as cellulose family, modified starch series, first-selected water-soluble polymers is polyvinyl alcohol, polyvinyl alcohol can use high molecular, also can with low-molecular-weight, the present invention adopts low-molecular-weight polyvinyl alcohol to be good.
The invention has the beneficial effects as follows: there is good dispersity in water; simultaneously good with the mixing uniformity of the aggregate such as cement, quartz sand feature; the present invention adds nonionogenic tenside and makees emulsifying agent; add polycarboxylate salt dispersant and water-soluble poval as protective colloid simultaneously; silane siloxanes emulsified dose all the time, dispersion agent and protective colloid in water-resisting agent are wrapped up; until and cements, hydrolytie polycondensation under alkaline aqueous medium, forms the silicone resin refusing water.
Embodiment
Below in conjunction with embodiment, the present invention is further described.
A kind of pressed powder waterproofing agent of organosilicon; it is with silane and polysiloxane for water-resisting agent, and being emulsifying agent with nonionogenic tenside, take polycarboxylate as cement water reducing agent and dispersion agent; taking water-soluble polymers as colloid protective agent and cement anticracking agent, take superfine silicon dioxide as dispersible carrier.
The preparation method of above-mentioned pressed powder waterproofing agent of organosilicon, the steps include:
Choose the water-soluble high-molecular compound of 100 parts according to weight ratio and add the nonionogenic tenside that weight part is 8 parts wherein, and stir, then the silane of 80 parts is taken, after the polysiloxane of 40 parts mixes, add in polyvinyl alcohol aqueous phase several times, each add-on is 10-20 part, open high-shear emulsion machine, emulsification is carried out with the speed of 2000-4000 rev/min, after oil phase adds, add the polycarboxylate aqueous solution of 12 parts again, then high speed shear 5 minutes, obtain the organic silicon water-proofing agent emulsion containing organosilicon 50%.Again emulsion is added in support powder and stirs evenly, just obtain pressed powder water-resisting agent.
Described silane comprises the alkylalkoxy silane of various carbon chain lengths, as Union carbide A-162, propyl-triethoxysilicane, butyl triethoxyl silane, octyltri-ethoxysilane, dodecyl triethoxysilane or their mixture.
Described polysiloxane is the hydrolysis prepolymer of various silane.
Described emulsifying agent be various nonionogenic tenside as alkyl alcohol ethoxylates, polyoxyethylene carboxylate class, the HLB value of emulsifying agent between 9 ~ 13, the consumption of emulsifying agent be silane siloxanes total amount 5 ~ 10% between.
Described water-soluble high-molecular compound comprises polyvinyl alcohol, Soxylat A 25-7 and carbohydrate as cellulose family, modified starch series, first-selected water-soluble polymers is polyvinyl alcohol, polyvinyl alcohol can use high molecular, also can with low-molecular-weight, the present invention adopts low-molecular-weight polyvinyl alcohol to be good.
Embodiment 1: add fatty alcohol-polyoxyethylene ether mixing nonionogenic tenside 8 grams in PVAC polyvinylalcohol-0588 aqueous solution of 100 gram 20%, its HLB value is 10.3, stir, separately take octyltri-ethoxysilane 80 grams, methyl silicon resin prepolymer polysiloxane 40 grams, after mixing, (each 10-20 gram) adds in polyvinyl alcohol aqueous phase several times, open high-shear emulsion machine, emulsification is carried out with the speed of 2000-4000 rev/min, after oil phase adds, add the polycarboxylate dehydragent aqueous solution of 12 gram 40% again, high speed shear 5 minutes again, obtain the stable emulsion containing organosilicon 50%, by this water-resisting agent emulsion 100 grams, being added drop-wise to specific surface area is 180m 2in the precipitated silica powders 50 grams of/g, stir, make it in water, be easy to dispersion, without particle, occur without oil droplet, obtain the powder containing waterproofing agent of organosilicon 34%.
The PVA-0588 aqueous solution of embodiment 2:100 gram 20%, add this dish-tween blending emulsifiers 6 grams, their HLB value is 10.6, take octyltri-ethoxysilane 60 grams in addition, methyl silicon resin prepolymer 60 grams, after mixing, (each 10-20 gram) adds in PVA-emulsifying agent mixing aqueous phase several times, emulsification 20 minutes in high-speed shearing emulsion machine, after add the polycarboxylate dehydragent of 14 gram 40%, homogenizing 5 minutes again, obtain the emulsion containing water-resisting agent 50%, the water-resisting agent emulsion obtained 100 grams is added dropwise to specific surface area 150m 2in the precipitated silica 50 grams of/g, stir, obtain the powdery waterproofing agent of organosilicon being easy to disperse in water, containing waterproofing agent of organosilicon 34%.
Take cement (425 #) 150 grams, quartz sand (100 order) 300 grams, mixes, 100 grams, another title water, add the powder waterproofing agent 1.8 grams of example 1 and example 2 or 3.6 grams, after abundant dispersed with stirring, be added in cement-sand compound, abundant scraper stirs evenly, then fall note to three diameters be 50cm, the degree of depth is in the plastic disc of 2cm, ambient temperatare one evening, steeped from second day in water and soak one week, after taking-up dries one week, survey sand-cement slurry disk at the bubbly water water-intake rate of 48 hours.Separately do the test block 3 not adding powdery water-resisting agent and do control sample, maintenance under similarity condition, survey at the bubbly water water-intake rate of 48 hours equally, as shown in the table:
powdery water-resisting agent is on the impact of waterproof mortar water-intake rate:
As can be seen from the above table, the water-intake rate of powdery water-resisting agent of the present invention to sand-cement slurry has reduction clearly, by JC474-2008 standard, just make the water-intake rate of sand-cement slurry reduce by more than 65% when the dosage of this powdery water-resisting agent in sand-cement slurry is few, be up to state standards first grade level.
Embodiment 3: powdery waterproofing agent of organosilicon finds after at room temperature depositing half a year that its dispersiveness in water does not change substantially, powdery water-resisting agent shelf-stable is described, does not have hydrolytie polycondensation.
Embodiment 4: do not add emulsifying water, sees in the water of powdery water-resisting agent dispersed.Silane siloxanes mixing water-resisting agent 80 grams, blending emulsifiers (1303 add 1306) 10 grams, adds powdery polycarboxylic acid salt water reducer 10 grams after mixing, being added to 100 grams of specific surface areas is 150m 2in the precipitated silica powders of/g, be uniformly mixed, pack.The ratio being 0.5% in water-resisting agent powder/sand-cement slurry on a small quantity of taking out is scattered in water, and stir and see the dispersiveness of water-resisting agent powder in water, moistening dispersion effect is good, forms the oyster white aqueous solution after stirring.
Embodiment 5: be added with the different preventing pigment of powdery water-reducing agent to the impact of sand-cement slurry water-repellancy.
In plastic containers, claim cement (325 #) 150 grams, add silica powder (100 order) 300 grams, mix, claim 120 grams, water to add water-proofing powder 3 grams (2% of cement amount), stir and water-proofing powder is fully disperseed, then add in cement-mortar, fully stir evenly, then pour in three plastic discs shaping, with water curing after 7 days, under room temperature, drying one week, then dries, weighs at 60 DEG C, then soak in deionized water, survey water-intake rate after 48 days, compare with control sample, result is as follows:
mortar adds the water-intake rate simultaneous test data sheet of different water-proofing powder and hydrophobic powder
Note 1:1 #~ 3 #for not adding the mortar of water-proofing powder, sample as a comparison;
Note 2:4 #~ 6 #for being added with the waterproof mortar of invention water-proofing powder;
Note 3:7 #~ 9 #for being added with the waterproof mortar of German Lockwood water-proofing powder;
Note 4:10 #~ 12 #for being added with the waterproof mortar of commercial hydrophobic powder;
Note 5: above water-proofing powder add-on is 0.66% of mortar dry weight.
As can be seen from the above table, be added with the water-proofing powder of this patent, dosage is after 0.66% of sand-cement slurry dry weight, and the water-intake rate solidifying rear sand-cement slurry is 15.6% with the water-intake rate ratio not adding water-proofing powder, and be up to state standards premium grads level.The water-intake rate ratio adding import water-proofing powder is 38.3%, and the water-intake rate adding the sand-cement slurry of commercial hydrophobic powder does not reach national standard, defective.Illustrate that water-proofing powder prepared by this patent is better than import water-proofing powder, and be much better than commercial hydrophobic powder.
The resistance to compression being added with the waterproof mortar of powder waterproofing agent is powerful through Guangdong Province's building materials test Spot detection, and after 28 days, resistance to compression brute force improves more than 20%, and national standard is be not less than not add 90% of water-resisting agent.After testing, the water pressure resistance being added with the waterproof mortar of water-resisting agent than be greater than 300%(with do not add water-resisting agent waterproof mortar water resistant seepage water pressure compared with).

Claims (6)

1. a pressed powder waterproofing agent of organosilicon; it is characterized in that: it with silane and polysiloxane for water-resisting agent; take nonionogenic tenside as emulsifying agent; take polycarboxylate as cement water reducing agent and dispersion agent; taking water-soluble polymers as colloid protective agent and cement anticracking agent, take superfine silicon dioxide as dispersible carrier.
2. the preparation method of above-mentioned pressed powder waterproofing agent of organosilicon, is characterized in that step is:
Choose the water-soluble high-molecular compound of 100 parts according to weight ratio and add the nonionogenic tenside that weight part is 8 parts wherein, and stir, then the silane of 80 parts is taken, after the polysiloxane of 40 parts mixes, add in polyvinyl alcohol aqueous phase several times, each add-on is 10-20 part, open high-shear emulsion machine, emulsification is carried out with the speed of 2000-4000 rev/min, after oil phase adds, add the polycarboxylate aqueous solution of 12 parts again, high speed shear 5 minutes again, obtain the organic silicon water-proofing agent emulsion containing organosilicon 50%, again emulsion is added in carrier to stir evenly and just obtains pressed powder water-resisting agent.
3. pressed powder waterproofing agent of organosilicon as claimed in claim 1, it is characterized in that: described silane comprises the alkylalkoxy silane of various carbon chain lengths, as Union carbide A-162, propyl-triethoxysilicane, butyl triethoxyl silane, octyltri-ethoxysilane, dodecyl triethoxysilane or their mixture.
4. pressed powder waterproofing agent of organosilicon as claimed in claim 1, is characterized in that: described polysiloxane is the hydrolysis prepolymer of various silane.
5. pressed powder waterproofing agent of organosilicon as claimed in claim 1, it is characterized in that: described emulsifying agent is that various nonionogenic tenside is as alkyl alcohol ethoxylates, polyoxyethylene carboxylate class, the HLB value of emulsifying agent between 9 ~ 13, the consumption of emulsifying agent be silane siloxanes total amount 5 ~ 10% between.
6. pressed powder waterproofing agent of organosilicon as claimed in claim 1, it is characterized in that: described water-soluble high-molecular compound comprises polyvinyl alcohol, Soxylat A 25-7 and carbohydrate as cellulose family, modified starch series, first-selected water-soluble polymers is polyvinyl alcohol, polyvinyl alcohol can use high molecular, also can with low-molecular-weight, the present invention adopts low-molecular-weight polyvinyl alcohol to be good.
CN201410732607.9A 2014-12-07 2014-12-07 Organosilicon waterproofing agent of solid powder and preparation method of organosilicon waterproofing agent Pending CN104446125A (en)

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CN104891854A (en) * 2015-05-11 2015-09-09 江苏科幸新材料股份有限公司 Water repellent, preparation method therefor and exterior wall thermal-insulation material
CN105064604A (en) * 2015-07-21 2015-11-18 安徽美克思科技有限公司 Anti-bacterial waterproof internal wall plate
CN105060737A (en) * 2015-07-21 2015-11-18 江苏科幸新材料股份有限公司 Water repellent as well as preparation method and application thereof
CN105236818A (en) * 2015-09-08 2016-01-13 唐山滦硕无机硅化物有限公司 Organic silicon water-proof powder, preparation method and application thereof
CN105693134A (en) * 2015-12-29 2016-06-22 江苏苏博特新材料股份有限公司 Functional concrete admixture
CN105693135A (en) * 2015-12-25 2016-06-22 江苏苏博特新材料股份有限公司 Cement concrete inner-doping waterproof agent and preparing method thereof
CN105712658A (en) * 2015-12-29 2016-06-29 江苏苏博特新材料股份有限公司 Concrete admixture for inhibiting corrosion medium transmission in ocean environment
CN106116244A (en) * 2016-06-28 2016-11-16 安徽真信涂料有限公司 A kind of preparation method of alkoxy silane hydrophobic powder
CN106186803A (en) * 2016-07-25 2016-12-07 江苏苏博特新材料股份有限公司 A kind of silane paste concrete protectant of high hydrophobicity and preparation method thereof
CN106892680A (en) * 2017-02-27 2017-06-27 广西青龙化学建材有限公司 GRC component special-purpose protecting agents and preparation method thereof
CN108002741A (en) * 2017-12-06 2018-05-08 马鞍山拓锐金属表面技术有限公司 A kind of preparation method of silane microcapsules solid powder waterproofing agent
CN108729235A (en) * 2018-07-05 2018-11-02 南雄鼎成新材料科技有限公司 A kind of preparation method and application of single-component low temperature solidification superhydrophobic fabric waterproofing agent
CN110590225A (en) * 2019-09-30 2019-12-20 南京曙光精细化工有限公司 Method for improving dispersibility of n-propyl trialkoxysilane
CN112777984A (en) * 2021-01-08 2021-05-11 黄河勘测规划设计研究院有限公司 Curing agent for damming material of silty dam in loess region
CN112939512A (en) * 2020-12-28 2021-06-11 李泽亮 Green and environment-friendly dry powder waterproof agent for cement
CN113292882A (en) * 2019-07-25 2021-08-24 河南聚研材料科技有限公司 Slow-release silane powder and preparation method and application thereof
CN115650631A (en) * 2022-10-13 2023-01-31 北京富瑞勒斯科技开发有限公司 Concrete waterproof compacting agent and preparation method thereof
CN115772339A (en) * 2022-12-23 2023-03-10 厦门安隆达消防材料有限公司 Non-intumescent steel structure fireproof coating composition

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CN105064604A (en) * 2015-07-21 2015-11-18 安徽美克思科技有限公司 Anti-bacterial waterproof internal wall plate
CN105060737A (en) * 2015-07-21 2015-11-18 江苏科幸新材料股份有限公司 Water repellent as well as preparation method and application thereof
CN105236818B (en) * 2015-09-08 2017-07-28 唐山滦硕无机硅化物有限公司 Organic silicon water-proofing powder
CN105236818A (en) * 2015-09-08 2016-01-13 唐山滦硕无机硅化物有限公司 Organic silicon water-proof powder, preparation method and application thereof
CN105693135A (en) * 2015-12-25 2016-06-22 江苏苏博特新材料股份有限公司 Cement concrete inner-doping waterproof agent and preparing method thereof
CN105693135B (en) * 2015-12-25 2018-02-23 江苏苏博特新材料股份有限公司 A kind of cement concrete internal doping type waterproofing agent and preparation method thereof
CN105712658A (en) * 2015-12-29 2016-06-29 江苏苏博特新材料股份有限公司 Concrete admixture for inhibiting corrosion medium transmission in ocean environment
CN105693134A (en) * 2015-12-29 2016-06-22 江苏苏博特新材料股份有限公司 Functional concrete admixture
CN106116244A (en) * 2016-06-28 2016-11-16 安徽真信涂料有限公司 A kind of preparation method of alkoxy silane hydrophobic powder
CN106186803A (en) * 2016-07-25 2016-12-07 江苏苏博特新材料股份有限公司 A kind of silane paste concrete protectant of high hydrophobicity and preparation method thereof
CN106186803B (en) * 2016-07-25 2018-08-31 江苏苏博特新材料股份有限公司 A kind of silane paste concrete protectant of high hydrophobicity and preparation method thereof
CN106892680A (en) * 2017-02-27 2017-06-27 广西青龙化学建材有限公司 GRC component special-purpose protecting agents and preparation method thereof
CN108002741A (en) * 2017-12-06 2018-05-08 马鞍山拓锐金属表面技术有限公司 A kind of preparation method of silane microcapsules solid powder waterproofing agent
CN108729235A (en) * 2018-07-05 2018-11-02 南雄鼎成新材料科技有限公司 A kind of preparation method and application of single-component low temperature solidification superhydrophobic fabric waterproofing agent
CN113292882A (en) * 2019-07-25 2021-08-24 河南聚研材料科技有限公司 Slow-release silane powder and preparation method and application thereof
CN113292882B (en) * 2019-07-25 2022-10-21 中交一公局第七工程有限公司 Slow-release silane powder and preparation method and application thereof
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