CN103819127B - Preparation method of efficient organic silicon emulsion water-proofing agent for reinforcing cement mortar concrete - Google Patents
Preparation method of efficient organic silicon emulsion water-proofing agent for reinforcing cement mortar concrete Download PDFInfo
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- CN103819127B CN103819127B CN201410029344.5A CN201410029344A CN103819127B CN 103819127 B CN103819127 B CN 103819127B CN 201410029344 A CN201410029344 A CN 201410029344A CN 103819127 B CN103819127 B CN 103819127B
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Abstract
The invention relates to a preparation method of an efficient organic silicon emulsion water-proofing agent for reinforcing cement mortar concrete. The preparation method comprises the following steps: firstly adding octene and isopropanol in a three-necked flask, filling the flask with nitrogen, heating in water bath, reacting under a reflux condition, and depressurizing to steam out octyl triethoxysilane; adding methyl triethoxysilane and a dimethyl siloxane ring body in the three-necked flask, using a catalyst to balance the solution, performing hydrolysis on the solution, reacting to obtain a partial hydrolysis prepolymer of methyl silicone resin; at last, weighing octyl triethoxysilane and a methyl silicone resin prepolymer, adding a non-ionic surfactant alkyl alcohol polyoxyethylene ether, fully stirring the solution uniformly, adding water to emulsify the solution, and adding a buffer solution to obtain a waterproof emulsion; or, adding water in a emulsification kettle, adding the non-ionic surfactant and the buffer solution in the kettle, starting a high-speed shearing machine, slowly adding octyl triethoxysilane and the silicon resin prepolymer in the kettle, and emulsifying the substances to obtain the same waterproof emulsion. The efficient organic silicon emulsion water-proofing agent has the characteristics of high water seepage pressure resistance and the like.
Description
Technical field
The invention belongs to sand-cement slurry overall enhanced water-resisting agent technical field, relate to the preparation method that a kind of sand-cement slurry concrete strengthens efficient organic silicon emulsion water-resisting agent.
Background technology
Cement products comprises sand-cement slurry, and cement concrete, in forming and hardening process, due to the hydration of cement, forms many pores, and they are very easily by water permeation, due to the effect of repeatedly expanding with heat and contract with cold, cement products is ftractureed.Macro-corrosion gas is contained as sulfurous gas in air acid rain and seawater, carbonic acid gas and chlorion, they penetrate in the pore of cement products with water, destroy cement structures, corrosion reinforcing bar, the cement products life-span is shortened dramatically, and what have causes house, the building collapsings such as bridge, make people's lives and properties be subject to unnecessary loss.Therefore, how to ensure cement products especially component long-term safety use, extending its work-ing life is one of vital task of building materials department.
Before more than 70 years, people just with chlorosilane process masonry wood surface, make its surface refuse water, and anti-sealing infiltrates in goods, as described in US2412470.Because releasing hydrogenchloride when it is hydrolyzed, there is corrosive nature to base material, having stimulation to human body.The sixties in last century people adopt not chloride silane and polysiloxane as building materials water-resisting agent, and silane is alkylalkoxy silane mainly, as organoalkoxysilanes such as methyl, ethyl, propyl group, butyl, octyl groups.Polysiloxane comprises containing hydrogen silicone oil, hydroxy silicon oil, epoxy silicon oil and silicone resin etc.Rise to the seventies in last century, it is found that octyl group silane and octyltri-ethoxysilane are optimal building surface water-resisting agents.Many patents adopt the octyltri-ethoxysilane process cement products of 100%, make octyl group permselective silane to cement products as 1 ~ 10mm inside concrete, water can not be permeated into, depth of penetration changes with the density strength of concrete product, the finer and close intensity of goods is larger, and the octyl group permselective silane degree of depth is more shallow.For high-grade concrete, even if the octyl group silane of 100% also permeates less than 2mm, as extra large work standard-required infiltration is greater than 2mm, people have to separately think scheme.Because waterproof layer is less than 2mm, mean that waterproof reliability is not enough, because waterproof layer also can slowly wear away by external influence in life-time service process.Except water method is refused on surface, people's idea adds water-resisting agent in cement concrete, makes its integral waterproofing.As Chinese Patent Application No. 200410058200, US2008/0271643A just adopts water reducer to add in concrete together with fatty acid hydrophober, make concrete integral waterproofing, but waterproof effect is not good, ageing resistance and resistance to microbial attack poor; And for example Chinese patent 03116917 and 01128085 etc. adopt naphthalene water reducer to add organosilicon and other additive, make integral waterproofing, but the overall water repellency of concrete is poor, because naphthalene water reducer wetting ability is too strong.Chinese patent 98124422, Authorization Notice No. CN1106363c is the patent of being applied in China by German Degussa company, the emulsion adopting silicoorganic compound and organic-silicon-modified tensio-active agent to prepare joins in concrete, make its integral waterproofing, water-repellancy and anti-sodium-chlor perviousness are significantly improved, but how have no the change of concrete anti-compression brute force.
Summary of the invention
For overcoming above-mentioned technical disadvantages, the invention provides a kind of based on octyltri-ethoxysilane and methyl silicon resin prepolymer, with the nonionogenic tenside emulsifying agent that market has easily been bought, through high-shear emulsifying, the sand-cement slurry concrete obtaining shelf-stable strengthens efficient organic silicon emulsion water-resisting agent
.
The present invention solves the technological method that its technical problem adopts: a kind of sand-cement slurry concrete strengthens the preparation method of efficient organic silicon emulsion water-resisting agent, and its step is as follows:
The first step: the synthesis of octyltri-ethoxysilane, octene 200g is added in 500ml there-necked flask, Virahol 50g, is filled with nitrogen, and heating in water bath is to 80 DEG C, with the aqueous isopropanol of Platinic chloride for catalyzer, drip three ethoxy silane 150g, react several hours under reflux, normal pressure steams Virahol, decompression steams octyltri-ethoxysilane, and yield is more than 90%;
Second step: the synthesis of methyl silicon resin prepolymer, in 500ml there-necked flask, add Union carbide A-162 200g, dimethyl siloxane ring body 100g, take trifluoromethanesulfonic acid as catalyzer 10g, add the hydrolysis of 50g water balance some hours at 50 DEG C ~ 70 DEG C after, decompression steams the ethanol of hydrolysis, through intensification pre-polymerization, filters the partial hydrolysis prepolymer obtaining methyl silicon resin;
3rd step: the emulsification of octyltri-ethoxysilane and methyl silicon resin prepolymer, take octyltri-ethoxysilane 140g and methyl silicon resin prepolymer 60g, add nonionogenic tenside alkyl alcohol ethoxylates 20g, pour high speed shearing homogenizing device into stir, then slowly add water 280g emulsification in high speed shearing homogenizing device, start retrogradation, along with adding of water, emulsion is by thick slowly thinning, after water injection, add damping fluid sodium bicarbonate 0.5g again, the pH value of emulsion is made to remain on 6.0-8.0, obtain the water-proof emulsion that active matter content is 30% ~ 60%, this emulsion is through centrifugal test, without layering, thermal stability test is carried out at 40 DEG C, 15 days not stratified, thickening is not obvious, room temperature is placed, 6 months not stratified, or first in emulsifying kettle, add water 280kg, by nonionogenic tenside 20kg, damping fluid adds in still, open high-speed shearing machine, slowly add octyltri-ethoxysilane 140kg and silicone prepolymer 60kg several times, each add-on is 3kg ~ 5kg, high speed shear makes emulsion temperature raise, chuck leads to water coolant, high-speed shearing machine gap is opened, each 3min ~ 10min, until add all oil phases, reemulsification 30min, just the water-proof emulsion that the 3rd step is identical is obtained, emulsion is through centrifugal test, thermal stability test is qualified, thermal stability test is stored 15 days at 45 DEG C, without layering, without obvious thickening, be equivalent at room temperature store half a year.
The invention has the beneficial effects as follows: the octyltri-ethoxysilane of employing contains the oxyethyl group of three facile hydrolysiss, in alkaline concrete, facile hydrolysis is three silicone hydroxyl, silicon dioxde reaction in they and Calucium Silicate powder is combined into net vertical body structure, methyl silicon resin prepolymer is also incorporated into tridimensional network with inorganic silicon dioxide in the same fashion, product strong mass is improved, in addition, nonionogenic tenside in organic silicon emulsion is also the concrete softening agent of sand-cement slurry, dispersion agent and water reducer, the mobility of cement admixture is increased, make cement products structure tightr, pore reduces, powerful raising, and refuse the octyl group of water in capillary hole wall proper alignment, unanimously outwardly, refuse water in outward, this water-resisting agent not only makes sand-cement slurry concrete strengthening improve more than 20% like this, and integral waterproofing, all waterproof from the inside to surface, so by the water-resisting agent emulsion of this invention, as long as with 2% of cement, after the abundant hydration and sclerosis of cement products, sand-cement slurry concrete 48 hours water-intake rates are 45%, far below 65% of the acceptable end product of national Specification, water resistant seepage water pressure is do not add water-resisting agent 300%, resistance to compression is powerful for not add 124% of water-resisting agent.
subordinate list explanation
Fig. 1 is test result schematic diagram of the present invention;
Fig. 2 is the comparison test figure of the present invention and other water-resisting agents.
Embodiment
Below in conjunction with subordinate list and embodiment, the present invention is further described.
Sand-cement slurry concrete strengthens a preparation method for efficient organic silicon emulsion water-resisting agent, and its step is as follows:
The first step: the synthesis of octyltri-ethoxysilane, octene 200g is added in 500ml there-necked flask, Virahol 50g, is filled with nitrogen, and heating in water bath is to 80 DEG C, with the aqueous isopropanol of Platinic chloride for catalyzer, drip three ethoxy silane 150g, react several hours under reflux, normal pressure steams Virahol, decompression steams octyltri-ethoxysilane, and yield is more than 90%;
Second step: the synthesis of methyl silicon resin prepolymer, in 500ml there-necked flask, add Union carbide A-162 200g, dimethyl siloxane ring body 100g, take trifluoromethanesulfonic acid as catalyzer 10g, add the hydrolysis of 50g water balance some hours at 50 DEG C ~ 70 DEG C after, decompression steams the ethanol of hydrolysis, through intensification pre-polymerization, filters the partial hydrolysis prepolymer obtaining methyl silicon resin;
3rd step: the emulsification of octyltri-ethoxysilane and methyl silicon resin prepolymer, take octyltri-ethoxysilane 140g and methyl silicon resin prepolymer 60g, add nonionogenic tenside alkyl alcohol ethoxylates 20g, pour high speed shearing homogenizing device into stir, then slowly add water 280g emulsification in high speed shearing homogenizing device, start retrogradation, along with adding of water, emulsion is by thick slowly thinning, after water injection, then add sodium bicarbonate 0.5g. and make the pH value of emulsion remain on 6.0-8.0.Obtain the water-proof emulsion that active matter content is 30% ~ 60%, this emulsion, through centrifugal test, without layering, carries out thermal stability test at 40 DEG C, and 15 days not stratified, and thickening is not obvious, and room temperature is placed, and 6 months not stratified; Or first in emulsifying kettle, add water 280kg, by nonionogenic tenside 20kg, damping fluid adds in still, opens high-speed shearing machine, slowly add octyltri-ethoxysilane 140kg and methyl silicon resin prepolymer 60kg several times, each add-on is 3kg ~ 5kg.High speed shear makes emulsion temperature raise, and chuck leads to water coolant, and high-speed shearing machine gap is opened, each 3min ~ 10min, until add all oil phases, reemulsification 30min, just obtains the water-proof emulsion identical with the 3rd step, emulsion is through centrifugal test, thermal stability test is qualified, and thermal stability test is stored 15 days at 45 DEG C, without layering, without obvious thickening, be equivalent at room temperature store half a year.
See table 1, add water-resisting agent of the present invention in sand-cement slurry, not only do not make the resistance to compression brute force of sand-cement slurry reduce, improve more than 20% than the brute force not adding water-resisting agent on the contrary, water demand ratio is far below the water demand ratio of the acceptable end product of national Specification.
See table 2, various water-resisting agent is weighed 1% ~ 2% by cement be added to the water, the ratio of the water and cement based composite materials that are added with water-resisting agent is that the water cement ratio of 35 ~ 40:100 mixes, then automatic levelling in mould is poured into, maintenance 14 days under the environment of relative temperature >=95% in second day, then its surperficial water repellency and water-intake rate is tested, according to form 2, the waterproof effect that octyl group silane adds resin emulsion is best, absorb water after 48 hours, water-intake rate ratio is less than 50%, reaches the requirement of national standard JC/T474 ~ 2008 first grade; Be 64% with the water-intake rate ratio that the 3%PVA aqueous solution adds octyl group silane and resin emulsion for water, still reach the requirement of GB first grade, and powerful increasing amount the most nearly 130%; Immersion 48 hours water-intake rates of methylate three ethoxy silane emulsion and calcium stearate water-resisting agent are 66%, reach the requirement of GB salable product; Containing hydrogen silicone oil emulsion can not add in sand-cement slurry and concrete, because oneself being cross-linked after its hydrolysis, incompatible with cement, destroys hydrated cementitious structure.
The octyltri-ethoxysilane adopted contains the oxyethyl group of three facile hydrolysiss, in alkaline concrete, facile hydrolysis is three silicone hydroxyl, silicon dioxde reaction in they and Calucium Silicate powder is combined into net vertical body structure, methyl silicon resin prepolymer is also incorporated into tridimensional network with inorganic silicon dioxide in the same fashion, product strong mass is improved, in addition, nonionogenic tenside in organic silicon emulsion is also the concrete softening agent of sand-cement slurry, dispersion agent and water reducer, the mobility of cement admixture is increased, make cement products structure tightr, pore reduces, powerful raising, and refuse the octyl group of water in capillary hole wall proper alignment, unanimously outwardly, refuse water in outward.This water-resisting agent not only makes sand-cement slurry concrete strengthening improve more than 20%, and integral waterproofing like this, from the inside to surface all waterproof.So by the water-resisting agent emulsion of this invention, as long as with 2% of cement, after the abundant hydration and sclerosis of cement products, sand-cement slurry concrete 48 hours water-intake rates are 45%, far below 65% of the acceptable end product of national Specification, water resistant seepage water pressure is do not add water-resisting agent 300%, and resistance to compression is powerful for not add 124% of water-resisting agent.
Claims (1)
1. sand-cement slurry concrete strengthens a preparation method for efficient organic silicon emulsion water-resisting agent, it is characterized in that step is as follows:
The first step: the synthesis of octyltri-ethoxysilane, octene 200g is added in 500ml there-necked flask, Virahol 50g, is filled with nitrogen, and heating in water bath is to 80 DEG C, with the aqueous isopropanol of Platinic chloride for catalyzer, drip three ethoxy silane 150g, react several hours under reflux, normal pressure steams Virahol, decompression steams octyltri-ethoxysilane, and yield is more than 90%;
Second step: the synthesis of methyl silicon resin prepolymer, in 500ml there-necked flask, add Union carbide A-162 200g, dimethyl siloxane ring body 100g, take trifluoromethanesulfonic acid as catalyzer 10g, add the hydrolysis of 50g water balance some hours at 50 DEG C ~ 70 DEG C after, decompression steams the ethanol of hydrolysis, through intensification pre-polymerization, filters the partial hydrolysis prepolymer obtaining methyl silicon resin;
3rd step: the emulsification of octyltri-ethoxysilane and methyl silicon resin prepolymer, take octyltri-ethoxysilane 140g and methyl silicon resin prepolymer 60g, add nonionogenic tenside alkyl alcohol ethoxylates 20g, pour high speed shearing homogenizing device into stir, then slowly add water 280g emulsification in high speed shearing homogenizing device, start retrogradation, along with adding of water, emulsion is by thick slowly thinning, after water injection, add damping fluid sodium bicarbonate 0.5g again, the pH value of emulsion is made to remain on 6.0-8.0, obtain the water-proof emulsion that active matter content is 30% ~ 60%, this emulsion is through centrifugal test, without layering, thermal stability test is carried out at 40 DEG C, 15 days not stratified, thickening is not obvious, room temperature is placed, 6 months not stratified, or first in emulsifying kettle, add water 280kg, by nonionogenic tenside 20kg, damping fluid adds in still, open high-speed shearing machine, slowly add octyltri-ethoxysilane 140kg and methyl silicon resin prepolymer 60kg several times, each add-on is 3kg ~ 5kg, high speed shear makes emulsion temperature raise, chuck leads to water coolant, high-speed shearing machine gap is opened, each 3min ~ 10min, until add all oil phases, reemulsification 30min, just the water-proof emulsion that the 3rd step is identical is obtained, emulsion is through centrifugal test, thermal stability test is qualified, thermal stability test is stored 15 days at 45 DEG C, without layering, without obvious thickening, be equivalent at room temperature store half a year.
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| CN115180870A (en) * | 2022-07-12 | 2022-10-14 | 常州绿玛特建筑科技有限公司 | Concrete compaction reinforcing agent |
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Denomination of invention: Preparation method of efficient organic silicon emulsion water-proofing agent for reinforcing cement mortar concrete Effective date of registration: 20190625 Granted publication date: 20150624 Pledgee: Bank of China, Limited by Share Ltd, Shaoguan branch Pledgor: Nanxiong Ding Cheng New Material Technology Co., Ltd. Registration number: 2019440000238 |