CN1903898A - Siloxane containing water soluble polymer emulsion and redispersible emulsion powder and its preparation method - Google Patents
Siloxane containing water soluble polymer emulsion and redispersible emulsion powder and its preparation method Download PDFInfo
- Publication number
- CN1903898A CN1903898A CN 200610036627 CN200610036627A CN1903898A CN 1903898 A CN1903898 A CN 1903898A CN 200610036627 CN200610036627 CN 200610036627 CN 200610036627 A CN200610036627 A CN 200610036627A CN 1903898 A CN1903898 A CN 1903898A
- Authority
- CN
- China
- Prior art keywords
- emulsion
- water
- soluble polymers
- monomer
- methacrylate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Processes Of Treating Macromolecular Substances (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The present invention discloses water-soluble polymer emulsion containing siloxane and redispersable emulsion powder and their preparation method. The space-stable silicon-containing water-soluble polymer emulsion is obtained by using vinyl multifunctional organic siloxane functional monomer and alkyl methacrylate, hydroxyalkyl ester, alkyl acrylate and carboxylic acid cross-linking monomer through emulsion polymerization mode. Its redispersable emulsion powder is made up by using space-stable siloxane-containing water-soluble mother body polymer emulsion through a specific spray-drying process. The invented products can be extensively used in building field.
Description
Technical field
The invention belongs to water-soluble polymers emulsion field, what relate in particular to a kind of spatial stability contains siloxanes water-soluble polymers emulsion and redispersable latex powder and preparation method thereof.
Background technology
Along with science and technology development, people are more and more deep to the understanding of environment protection and Sustainable development.In coatings industry, replacing with serious pollution solvent based coating with water-borne coatings, powder coating is trend of the times, and water-borne coatings has obtained using widely.But the building water emulsion coating that uses is made up of polymer emulsion, color stuffing, various auxiliary agent and water now, and wherein auxiliary agent and water are used in order to produce with accumulating coating, account for the over half of coating weight and price.Major part is water (accounting for 60%) in the aqueous architectural latex coating, and solid content only accounts for 40%, and storage and use liquid latex coating need be used a large amount of storage tanks, and the recycling of these plastics or irony storage tank also needs lot of manpower and material resources.So not only increased cost, and caused the waste of resource, also contaminate environment.
According to coating Water-borne modification and the high development trend of containing admittedly, people's imagination will be mixed into dry powder paint with color stuffing after the polymer emulsion drying in recent years, add the water stirring during use and can be made into traditional emulsion paint now, have existing with the same performance of coating.Dry powder paint has solved an emulsion paint stability and the high difficult problem of carrying cost, makes emulsion paint be able to pack and sell with a kind of prescription form stable and low carrying cost.Dry powder paint is different from existing various architectural latex coating, it is a solid, can be as the cement paper bag packing, do not need metal bucket or plastic tank packing, both saved some used industrial chemicals of existing emulsion paint, the volatile organic compounds (VOC) that causes environmental pollution can be reduced again, zero VOC building coating can be made.Dry powder paint is a building coating of new generation, is the great revolution of building coating.
" dry powder paint " is the coating material technology of coating circle.The gordian technique of this coating system is to prepare the redispersible polymer latex powder---can instant (dispersion) in water and certain water-proof powder film forming material is arranged, the mixture of it and color stuffing can redispersion in water, energy cold cross-linking film forming has the same performance of current emulsion paint during use.Though existing in the world a few countries is developed " redispersable latex powder " of the Vinyl Acetate Copolymer-vinyl with certain water dispersible and film forming ability, but because degree of scatter is limited, film forming properties does not reach the degree that can be used as " dry powder paint " filmogen; And, the characteristics of this kind redispersable latex powder water tolerance and ion stability difference have been determined owing to raw material itself.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, what a kind of spatial stability was provided contains siloxanes water-soluble polymers emulsion.
Another object of the present invention is to provide a kind of preparation method who contains siloxanes water-soluble polymers emulsion of this spatial stability.
A further object of the present invention is to provide a kind of redispersible polymer latex powder.
The present invention also aims to provide a kind of preparation method of this redispersible polymer latex powder.
Adopt following technology to realize for addressing the above problem the inventor:
Of the present invention contain each component of siloxanes water-soluble polymers emulsion and the quality percentage composition as follows:
Alkyl acrylate 25～50%
Alkyl methacrylate 25～50%
Hydroxy alkyl ester 2～10%
Carboxylic acid cross-linking monomer 2～10%
Vinyl polyfunctional group organo-siloxane function monomer 1～10%
Described alkyl acrylate be in methyl acrylate, ethyl propenoate, propyl acrylate, butyl acrylate, vinylformic acid pentyl ester, Ethyl acrylate, the Isooctyl acrylate monomer any one or more than one.
Described alkyl methacrylate be in methyl methacrylate, Jia Jibingxisuanyizhi, propyl methacrylate, butyl methacrylate, methacrylic acid pentyl ester, n octyl methacrylate, the Isooctyl methacrylate any one or more than one.
Described hydroxy alkyl ester be in 2-Hydroxy ethyl acrylate, vinylformic acid-3-hydroxy propyl ester, vinylformic acid-2-hydroxyl butyl ester, vinylformic acid-5-hydroxyl pentyl ester, the vinylformic acid-own ester of 6-hydroxyl, methacrylic acid-2-hydroxy methacrylate, the methacrylic acid-2-hydroxy propyl ester any one.
Described carboxylic acid cross-linking monomer be in vinylformic acid, the methacrylic acid any one.
Described vinyl polyfunctional group organo-siloxane function monomer be in vinyltrimethoxy silane, vinyl methoxyl group diethoxy silane, vinyltriethoxysilane, vinyl oxyethyl group diisopropoxy silane, the vinyl silane triisopropoxide any one.
The preparation method's step that contains siloxanes water-soluble polymers emulsion of the present invention is as follows:
Step 1: preparation seed microemulsion
Earlier water, emulsifying agent are joined in the reactor that thermometer, heating temperature controller, agitator, filling tube, azeotropic condensing reflux pipe are housed, dispersed with stirring 10～20 minutes, add aforesaid propylene acid alkyl ester quality 5～20%, above-mentioned alkyl methacrylate quality 5～20%, 5～20% and above-mentioned carboxylic acid cross-linking monomer quality of above-mentioned hydroxy alkyl ester quality 5～40%, be warming up to 75～85 ℃, add the Potassium Persulphate initiator again, react after 15～30 minutes, faint blue light appears in emulsion, restir 5～20 minutes promptly forms transparent seed microemulsion;
The total mass of described water equates that with the monomer total mass step 1 consumption accounts for 20～50% of water total mass;
The total mass of described emulsifying agent is 1～3% of a monomer total mass, and the step 1 consumption accounts for 10～50% of emulsifying agent total mass;
The total mass of described Potassium Persulphate initiator is 0.4～1.0% of a monomer total mass, and the step 1 consumption accounts for 20～50% of total mass;
Step 2: preparation contains siloxanes water-soluble polymers emulsion
Above-mentioned vinyl polyfunctional group organosilicon functional monomer and remaining alkyl acrylate, alkyl methacrylate, hydroxy alkyl ester, carboxylic acid cross-linking monomer, water and emulsifying agent mixed stirred 10～30 minutes, make it fully emulsified, obtain monomer pre-emulsion; In 3～5 hours, pre-emulsion and remaining Potassium Persulphate initiator be added drop-wise in the reactor continuously react with the seed microemulsion, temperature of reaction maintains 75～85 ℃, reaction finishes, be incubated 1～2 hour, be cooled to 40～60 ℃, the pH value of regulating emulsion is 7～9, filter discharging, promptly get and contain siloxanes water-soluble polymers emulsion.
Each component of redispersible polymer latex powder and quality percentage composition are as follows:
Contain siloxanes water-soluble polymers emulsion 85～95%
Protective colloid 3～10%
Anti-caking agent 1～5%.
Described protective colloid is the graft copolymer of silicon sol, ether of cellulose, polyvinyl alcohol, polyacrylamide, polyvinylpyrrolidone, aldehydes modified polyvinyl alcohol, modified polyacrylic acid, starch and derivative thereof, ethylene oxide, on quadrol in the grafted ethylene oxide copolymer any one or more than one.
Described anti-caking agent be in lime, ground dolomite, diatomite, pure aluminium silicate, kaolin, talcum powder, clay, the silicon-dioxide any one or more than one.
Preparation method's step of redispersible polymer latex powder is as follows:
Step 1: the preparation of sprayable emulsion
Take by weighing the protective colloid of 3～10 mass parts, adding water stirs up to dissolving fully, make solid content and be 30～50% protective colloid solution, what add 85～95 mass parts in above-mentioned protective colloid solution contains siloxanes water-soluble polymers emulsion, stirred 5～10 minutes, the last anti-caking agent that adds 1～5 mass parts in above-mentioned mixed solution stirred 10～30 minutes, made and treated spray-dried emulsion;
Step 2: the spraying drying of emulsion
The spraying drying inlet temperature that spray-dryer is set is that 150 ± 10 ℃, temperature out are that 70 ± 10 ℃, hot blast wind speed are 0.5～8m
3/ min, feeding speed 20～80ml/min, atomizer rotating speed (control droplet size) are 200～400rpm, start heating system then, when treating that out temperature rises to set(ting)value, start the spraying drying that feeder system, atomization system and negative pressure system carry out emulsion, collect at last, can obtain the redispersible polymer latex powder.
The present invention compared with prior art has following advantage and beneficial effect:
(1) in conventional emulsion polymerization, emulsifying agent is lower molecular weight parents materials, emulsifying agent is that physical adsorption is on the emulsion particle surface, in the drying process, low molecular weight emulsifier easily produces migration and breaks away from the emulsion particle surface, cause the surfactant on emulsion particle surface to lack, thereby do not have the redispersion performance when latex powder is disperseed again in water; And among the present invention, stablize the emulsifying agent of emulsion particle and protective colloid and emulsion particle surface and have stronger reactive force, it is not produced with the emulsion particle surface in spray-drying process separates, and emulsifying agent that the present invention adopts and protective colloid have stronger water-soluble, can satisfy stability and latex powder in water the again dispersive redispersion performance of emulsion particle in dispersion system;
(2) the redispersion process of realization spraying drying latex powder, must adopt special-purpose emulsion to carry out spraying drying, contain in the preparation of siloxanes water-soluble polymers emulsion in the present invention, selected a kind of polymer substance of good water solubility to make the protection colloid, on water-soluble polymer, there is the graftomer long-chain, whole molecule has parents' structure, its hydrophilic segment is the water-soluble polymer part in the structure, hydrophobic is polymers grafted long-chain part, and this long-chain part is similar to polymer architecture in the emulsion particle, according to the similar compatibility rule, have that hydrophobic part can be anchored on the emulsion particle surface in the polymkeric substance of parents' structure, and its hydrophilic segment stretches in the water, makes the emulsion particle stable dispersion in dispersion medium; The bonding force of this grappling is a kind of Chemical bond power, its intensity is much larger than physical adsorption power, in the emulsion spray-drying process, but parents' structural polymer mortise is on the emulsion particle surface, thereby for latex powder redispersion process provides material guarantee, but and by in polymer lateral chain, introducing the siloxanyl monomers of cold cross-linking, by crosslinked film forming water tolerance and the intensity improved;
(3) the redispersible polymer latex powder solid content height (near 100%) of the present invention's preparation, the difficulty that can reduce conveying, stores, can use the papery packing, both reduced packing cost, also reduced industrial waste, and stability in storage is good, and the shelf lives is long, not can because of water freeze or volatilize go bad; The more important thing is it can be in water dissolving rapidly, homodisperse, again form latex, can be widely used in zero VOC dry powder paint, terrace mending mortar, gravity flow self-leveling floor mortar, wall and floor tile adhesive agent, sealing mortar, building putty powder, plastering material, heat insulating board binding material, concrete repair mortar, jointing agent and powder coating, powder adhesive etc. with former matrix polymer emulsion same performance.
Embodiment
In order to understand the present invention better, the present invention is done to describe further below in conjunction with embodiment.
Embodiment 1
1) contains the synthetic of siloxanes water-soluble polymers emulsion
Set of monomers becomes butyl acrylate, methyl methacrylate, methacrylic acid, methacrylic acid-2-hydroxy methacrylate, vinyl silane triisopropoxide, and its component prescription is as follows:
| Form | Quality (g) | |
| 1 2 3 4 5 6 7 8 | Methyl methacrylate (MMA) methacrylic acid (MAA) butyl acrylate (BA) methacrylic acid-2-hydroxy methacrylate (HEMA) vinyl silane triisopropoxide C-1706 emulsifying agent potassium peroxydisulfate (K2S 2O 8) initiator water | 14 4 25 2 5 0.5 0.2 50 |
Step 1: preparation seed microemulsion
Earlier 50% water, 50% emulsifying agent are joined in the reactor that thermometer, heating temperature controller, agitator, filling tube, azeotropic condensing reflux pipe are housed, dispersed with stirring 20 minutes, add 20% butyl acrylate, 20% methyl methacrylate, methacrylic acid-2-hydroxy methacrylate of 20% and 5% methacrylic acid, be warming up to 75 ℃, add 50% Potassium Persulphate initiator again, react after 30 minutes, faint blue light appears in emulsion, restir 15 minutes promptly forms transparent seed microemulsion;
Step 2: preparation contains siloxanes water-soluble polymers emulsion
The water of the emulsifying agent of vinyl silane triisopropoxide C-1706 monomer and remaining butyl acrylate of 80%, 80% methyl methacrylate, methacrylic acid-2-hydroxy methacrylate of 80%, 95% methacrylic acid and 50% and 50% is mixed in-rises stirred 30 minutes, make it fully emulsified, obtain monomer pre-emulsion; In 5 hours, pre-emulsion and remaining 50% Potassium Persulphate initiator be added drop-wise in the reactor continuously react with the seed microemulsion, temperature of reaction maintains 80 ℃, reaction finishes, be incubated 1 hour, be cooled to 40 ℃, the pH value of regulating emulsion is 7, filter discharging, promptly get and contain siloxanes water-soluble polymers emulsion.
2) preparation of redispersible polymer latex powder
Protective colloid is a polyvinylpyrrolidone, and anti-caking agent is a diatomite, and its component prescription is as follows
| Form | Quality (g) | |
| 1 2 3 | Contain siloxanes water-soluble polymers emulsion polyvinylpyrrolidone diatomite | 90 6 4 |
Step 1: the preparation of sprayable emulsion
Take by weighing the polyvinylpyrrolidone protective colloid of 6g, adding water stirs up to dissolving fully, make solid content and be 30% protective colloid solution, in above-mentioned protective colloid solution, add and contain siloxanes water-soluble polymers emulsion 90g, stirred 5 minutes, in above-mentioned mixed solution, add 4g diatomite at last, stirred 10 minutes, make and treat spray-dried emulsion;
Step 2: the spraying drying of emulsion
The spraying drying inlet temperature that spray-dryer is set is that 150 ℃, temperature out are that 70 ℃, hot blast wind speed are 1.5m
3/ min, feeding speed 20ml/min, atomizer rotating speed are 200rpm, start heating system then, when treating that out temperature rises to set(ting)value, start the spraying drying that feeder system, atomization system and negative pressure system carry out emulsion, the gained rubber powder is further used 80 mesh sieve vibrosieves, collect at last, can obtain the redispersible polymer latex powder.
Embodiment 2
1) contains the synthetic of siloxanes water-soluble polymers emulsion
Set of monomers becomes ethyl propenoate, butyl methacrylate, vinylformic acid, the vinylformic acid-own ester of 6-hydroxyl, vinyltrimethoxy silane, and its component prescription is as follows:
| Form | Quality (g) | |
| 1 2 3 4 5 6 7 8 | Ethyl propenoate, (EA) vinylformic acid, (AA) butyl methacrylate, (BA) vinylformic acid-own ester vinyltrimethoxy silane of 6-hydroxyl emulsifying agent Potassium Persulphate, (K 2S 2O 8) initiator water | 14 4 24 4 4 1.5 0.4 50 |
Step 1: preparation seed microemulsion
Earlier 20% water, 20% emulsifying agent are joined in the reactor that thermometer, heating temperature controller, agitator, filling tube, azeotropic condensing reflux pipe are housed, dispersed with stirring 10 minutes, the ethyl propenoate of adding 10%, 5% butyl methacrylate, vinylformic acid-own ester of 6-hydroxyl of 10%, 40% vinylformic acid, be warming up to 80 ℃, add 20% Potassium Persulphate initiator again, react after 15 minutes, faint blue light appears in emulsion, restir 5 minutes promptly forms transparent seed microemulsion;
Step 2: preparation contains siloxanes water-soluble polymers emulsion
The water of the emulsifying agent of vinyltrimethoxy silane monomer and remaining ethyl propenoate of 90%, 95% butyl methacrylate, vinylformic acid-own ester of 6-hydroxyl of 90%, 60% vinylformic acid and 80% and 80% mixed stirred 10 minutes, make it fully emulsified, obtain monomer pre-emulsion; In 3.5 hours, pre-emulsion and remaining 80% Potassium Persulphate initiator be added drop-wise in the reactor continuously react with the seed microemulsion, temperature of reaction maintains 85 ℃, reaction finishes, be incubated 2 hours, be cooled to 50 ℃, the pH value of regulating emulsion is 9, filter discharging, promptly get and contain siloxanes water-soluble polymers emulsion.
2) preparation of redispersible polymer latex powder
Protective colloid is a polyvinyl alcohol, and anti-caking agent is a kaolin, and its component prescription is as follows:
| Form | Quality (g) | |
| 1 2 3 | Contain siloxanes water-soluble polymers emulsion polyvinyl alcohol kaolin | 95 4 1 |
Step 1: the preparation of sprayable emulsion
Take by weighing the polyvinyl alcohol protective colloid of 4g, adding water stirs up to dissolving fully, make solid content and be 50% protective colloid solution, in above-mentioned protective colloid solution, add and contain siloxanes water-soluble polymers emulsion 95g, stirred 10 minutes, in above-mentioned mixed solution, add 1g kaolin at last, stirred 30 minutes, make and treat spray-dried emulsion;
Step 2: the spraying drying of emulsion
The spraying drying inlet temperature that spray-dryer is set is that 140 ℃, temperature out are that 60 ℃, hot blast wind speed are 7.5m
3/ min, feeding speed 80ml/min, atomizer rotating speed are 400rpm, start heating system then, when treating that out temperature rises to set(ting)value, start the spraying drying that feeder system, atomization system and negative pressure system carry out emulsion, the gained rubber powder is further used 80 mesh sieve vibrosieves, collect at last, can obtain the redispersible polymer latex powder.
Embodiment 3
1) contains the synthetic of siloxanes water-soluble polymers emulsion
Set of monomers becomes Isooctyl acrylate monomer, butyl methacrylate, Jia Jibingxisuanyizhi, vinylformic acid, methacrylic acid-2-hydroxy propyl ester, vinyl oxyethyl group diisopropoxy silane, and its component prescription is as follows:
| Form | Quality (g) | |
| 1 2 3 4 5 6 7 8 9 | Isooctyl acrylate monomer butyl methacrylate EMA acrylic acid methacrylic acid-2-hydroxy propyl ester vinyl ethyoxyl diisopropoxy silane emulsifying agent potassium peroxydisulfate (K2S 2O 8) initiator water | 15 10 15 3 3 4 1.0 0.5 50 |
Step 1: preparation seed microemulsion
Earlier 50% water, 35% emulsifying agent are joined in the reactor that thermometer, heating temperature controller, agitator, filling tube, azeotropic condensing reflux pipe are housed, dispersed with stirring 20 minutes, add 5% Isooctyl acrylate monomer, 8% butyl methacrylate, 10% Jia Jibingxisuanyizhi, 25% vinylformic acid, 15% methacrylic acid-2-hydroxy propyl ester again, be warming up to 82 ℃, add 30% Potassium Persulphate initiator again, react after 15 minutes, faint blue light appears in emulsion, restir 20 minutes promptly forms transparent seed microemulsion;
Step 2: preparation contains siloxanes water-soluble polymers emulsion
The water of the emulsifying agent of vinyl oxyethyl group diisopropoxy silane monomer and remaining Isooctyl acrylate monomer of 95%, 92% butyl methacrylate, 90% Jia Jibingxisuanyizhi, 75% vinylformic acid, 85% methacrylic acid-2-hydroxy propyl ester and 65% and 50% mixed stirred 25 minutes, make it fully emulsified, obtain monomer pre-emulsion; In 3 hours, pre-emulsion and remaining 70% Potassium Persulphate initiator be added drop-wise in the reactor continuously react with the seed microemulsion, temperature of reaction maintains 78 ℃, reaction finishes, be incubated 1 hour, be cooled to 60 ℃, the pH value of regulating emulsion is 7.5, filter discharging, promptly get and contain siloxanes water-soluble polymers emulsion.
2) preparation of redispersible polymer latex powder
Protective colloid is a modified polyacrylic acid, and anti-caking agent is silicon-dioxide and diatomite, and its component prescription is as follows:
| Form | Quality (g) | |
| 1 2 3 4 | Contain the emulsion modified polyacrylic acid diatomite silicon dioxide of siloxanes water-soluble polymers | 86 10 2 2 |
Step 1: the preparation of sprayable emulsion
Take by weighing the modified polyacrylic acid protective colloid of 10g, adding water stirs up to dissolving fully, make solid content and be 40% protective colloid solution, in above-mentioned protective colloid solution, add and contain siloxanes water-soluble polymers emulsion 86g, stirred 8 minutes, in above-mentioned mixed solution, add 2g diatomite and 2g silicon-dioxide anti-caking agent at last, stirred 24 minutes, make and treat spray-dried emulsion;
Step 2: the spraying drying of emulsion
The spraying drying inlet temperature that spray-dryer is set is that 160 ℃, temperature out are that 80 ℃, hot blast wind speed are 4.5m
3/ min, feeding speed 60ml/min, atomizer rotating speed are 270rpm, start heating system then, when treating that out temperature rises to set(ting)value, start the spraying drying that feeder system, atomization system and negative pressure system carry out emulsion, the gained rubber powder is further used 80 mesh sieve vibrosieves, collect at last, can obtain the redispersible polymer latex powder.
Embodiment 4
1) contains the synthetic of siloxanes water-soluble polymers emulsion
Set of monomers becomes butyl acrylate, Ethyl acrylate, methacrylic acid pentyl ester, methacrylic acid, vinylformic acid-5-hydroxyl pentyl ester, vinyl methoxyl group diethoxy silane, and its component prescription is as follows:
| Form | Quality (g) |
| 1 2 3 4 5 6 7 8 9 | Butyl acrylate Hexyl 2-propenoate methacrylic acid pentyl ester metering system acid acrylic acid-5-hydroxyl pentyl ester vinyl methoxyl group diethoxy silane emulsifying agent potassium peroxydisulfate initator water | 12 10 21 1 4 2 1.2 0.3 50 |
Step 1: preparation seed microemulsion
Earlier 40% water, 40% emulsifying agent are joined in the reactor that thermometer, heating temperature controller, agitator, filling tube, azeotropic condensing reflux pipe are housed, dispersed with stirring 15 minutes, add 10% butyl acrylate, 10% Ethyl acrylate, 15% methacrylic acid pentyl ester, 36% methacrylic acid, 10% vinylformic acid-5-hydroxyl pentyl ester again, be warming up to 75 ℃, add 40% Potassium Persulphate initiator again, react after 25 minutes, faint blue light appears in emulsion, restir 10 minutes promptly forms transparent seed microemulsion;
Step 2: preparation contains siloxanes water-soluble polymers emulsion
The water of the emulsifying agent of vinyl oxyethyl group diisopropoxy silane monomer and remaining 90% butyl acrylate, 90% Ethyl acrylate, 85% methacrylic acid pentyl ester, 64% methacrylic acid, 90% vinylformic acid-5-hydroxyl pentyl ester and 60% and 60% mixed stirred 30 minutes, make it fully emulsified, obtain monomer pre-emulsion; In 4 hours, pre-emulsion and remaining 60% Potassium Persulphate initiator be added drop-wise in the reactor continuously react with the seed microemulsion, temperature of reaction maintains 75 ℃, reaction finishes, be incubated 1.5 hours, be cooled to 45 ℃, the pH value of regulating emulsion is 7.5, filter discharging, promptly get and contain siloxanes water-soluble polymers emulsion.
2) preparation of redispersible polymer latex powder
Protective colloid is silicon sol and polyacrylamide, and anti-caking agent is a lime, and its component prescription is as follows:
| Form | Quality (g) |
| 1 2 3 4 | Contain siloxanes water-soluble polymers emulsion silicon sol polyacrylamide lime | 92 2 2 4 |
Step 1: the preparation of sprayable emulsion
Take by weighing the silicon sol of 2g and the polyacrylamide protective colloid of 2g, adding water stirs up to dissolving fully, make solid content and be 45% protective colloid solution, in above-mentioned protective colloid solution, add and contain siloxanes water-soluble polymers emulsion 92g, stirred 10 minutes, in above-mentioned mixed solution, add 4g lime at last, stirred 12 minutes, make and treat spray-dried emulsion;
Step 2: the spraying drying of emulsion
The spraying drying inlet temperature that spray-dryer is set is that 140 ℃, temperature out are that 60 ℃, hot blast wind speed are 0.5m
3/ min, feeding speed 36ml/min, atomizer rotating speed are 210rpm, start heating system then, when treating that out temperature rises to set(ting)value, start the spraying drying that feeder system, atomization system and negative pressure system carry out emulsion, the gained rubber powder is further used 80 mesh sieve vibrosieves, collect at last, can obtain the redispersible polymer latex powder.
Can realize the present invention preferably by above embodiment.
Claims (10)
1. one kind contains siloxanes water-soluble polymers emulsion, it is characterized in that each component and quality percentage composition are as follows:
Alkyl acrylate 25～50%
Alkyl methacrylate 25～50%
Hydroxy alkyl ester 2～10%
Carboxylic acid cross-linking monomer 2～10%
Vinyl polyfunctional group organo-siloxane function monomer 1～10%
2. the siloxanes water-soluble polymers emulsion that contains according to claim 1, it is characterized in that described alkyl acrylate be in methyl acrylate, ethyl propenoate, propyl acrylate, butyl acrylate, vinylformic acid pentyl ester, hexyl acrylate, the Isooctyl acrylate monomer any one or more than one.
3. the siloxanes water-soluble polymers emulsion that contains according to claim 1, it is characterized in that described alkyl methacrylate be in methyl methacrylate, Jia Jibingxisuanyizhi, propyl methacrylate, butyl methacrylate, methacrylic acid pentyl ester, n octyl methacrylate, the Isooctyl methacrylate any one or more than one.
4. the siloxanes water-soluble polymers emulsion that contains according to claim 1, it is characterized in that described hydroxy alkyl ester be 2-Hydroxy ethyl acrylate, vinylformic acid-3-hydroxy propyl ester, vinylformic acid-2-hydroxyl butyl ester, vinylformic acid-5-hydroxyl pentyl ester, vinylformic acid-6-hydroxyl in ester, methacrylic acid-2-hydroxy methacrylate, the methacrylic acid-2-hydroxy propyl ester any one.
5. the siloxanes water-soluble polymers emulsion that contains according to claim 1, it is characterized in that described vinyl polyfunctional group organo-siloxane function monomer be in vinyltrimethoxy silane, vinyl methoxyl group diethoxy silane, vinyltriethoxysilane, vinyl oxyethyl group diisopropoxy silane, the vinyl silane triisopropoxide any one.
6. the described preparation method who contains siloxanes water-soluble polymers emulsion of claim 1 is characterized in that step is as follows:
Step 1: preparation seed microemulsion
Earlier water, emulsifying agent are joined in the reactor that thermometer, heating temperature controller, agitator, filling tube, azeotropic condensing reflux pipe are housed, dispersed with stirring 10～20 minutes, add aforesaid propylene acid alkyl ester quality 5～20%, above-mentioned alkyl methacrylate quality 5～20%, 5～20% and above-mentioned carboxylic acid cross-linking monomer quality of above-mentioned hydroxy alkyl ester quality 5～40%, be warming up to 75～85 ℃, add the Potassium Persulphate initiator again, react after 15～30 minutes, faint blue light appears in emulsion, restir 5～20 minutes promptly forms transparent seed microemulsion;
The total mass of described water equates that with the monomer total mass step 1 consumption accounts for 20～50% of water total mass;
The total mass of described emulsifying agent is 1～3% of a monomer total mass, and the step 1 consumption accounts for 10～50% of total mass;
The total mass of described Potassium Persulphate initiator is 0.4～1.0% of a monomer total mass, and the step 1 consumption accounts for 20～50% of total mass;
Step 2: preparation contains siloxanes water-soluble polymers emulsion
Above-mentioned vinyl polyfunctional group organosilicon functional monomer and remaining alkyl acrylate, alkyl methacrylate, hydroxy alkyl ester, carboxylic acid cross-linking monomer, water and emulsifying agent mixed stirred 10～30 minutes, make it fully emulsified, obtain monomer pre-emulsion; In 3～5 hours, pre-emulsion and remaining Potassium Persulphate initiator be added drop-wise in the reactor continuously react with the seed microemulsion, temperature of reaction maintains 75～85 ℃, reaction finishes, be incubated 1～2 hour, be cooled to 40～60 ℃, the pH value of regulating emulsion is 7～9, filter discharging, promptly get and contain siloxanes water-soluble polymers emulsion.
7. redispersible polymer latex powder is characterized in that each component and quality percentage composition are as follows:
Contain siloxanes water-soluble polymers emulsion 85～95%
Protective colloid 3～10%
Anti-caking agent 1～5%.
8. redispersible polymer latex powder according to claim 7, it is characterized in that described protective colloid be the graft copolymer of silicon sol, ether of cellulose, polyvinyl alcohol, polyacrylamide, polyvinylpyrrolidone, aldehydes modified polyvinyl alcohol, modified polyacrylic acid, starch and derivative thereof, ethylene oxide, on quadrol in the grafted ethylene oxide copolymer any one or more than one.
9. redispersible polymer latex powder according to claim 7, it is characterized in that described anti-caking agent be in lime, ground dolomite, diatomite, pure aluminium silicate, kaolin, talcum powder, clay, the silicon-dioxide any one or more than one.
10. the preparation method of the described redispersible polymer latex powder of claim 7 is characterized in that step is as follows:
Step 1: the preparation of sprayable emulsion
Take by weighing the protective colloid of 3～10 mass parts, adding water stirs up to dissolving fully, make solid content and be 30～50% protective colloid solution, what add 85～95 mass parts in above-mentioned protective colloid solution contains siloxanes water-soluble polymers emulsion, stirred 5～10 minutes, the last anti-caking agent that adds 1～5 mass parts in above-mentioned mixed solution stirred 10～30 minutes, made and treated spray-dried emulsion;
Step 2: the spraying drying of emulsion
The spraying drying inlet temperature that spray-dryer is set is that 150 ± 10 ℃, temperature out are that 70 ± 10 ℃, hot blast wind speed are 0.5～8m
3/ min, feeding speed 20～80ml/min, atomizer rotating speed (control droplet size) are 200～400rpm, start heating system then, when treating that out temperature rises to set(ting)value, start the spraying drying that feeder system, atomization system and negative pressure system carry out emulsion, collect at last, can obtain the redispersible polymer latex powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100366278A CN100460427C (en) | 2006-07-21 | 2006-07-21 | Siloxane containing water soluble polymer emulsion and redispersible emulsion powder and its preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100366278A CN100460427C (en) | 2006-07-21 | 2006-07-21 | Siloxane containing water soluble polymer emulsion and redispersible emulsion powder and its preparation method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1903898A true CN1903898A (en) | 2007-01-31 |
| CN100460427C CN100460427C (en) | 2009-02-11 |
Family
ID=37673278
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006100366278A Expired - Fee Related CN100460427C (en) | 2006-07-21 | 2006-07-21 | Siloxane containing water soluble polymer emulsion and redispersible emulsion powder and its preparation method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100460427C (en) |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102101960A (en) * | 2010-12-24 | 2011-06-22 | 大连工业大学 | High-hydroxy silicon-acrylate aqueous glass coating emulsion and synthesis method thereof |
| CN101735752B (en) * | 2008-11-18 | 2011-08-10 | 曾军 | Building gelatine powder |
| CN102226072A (en) * | 2011-05-06 | 2011-10-26 | 同济大学 | Preparation method of organic silicon microcapsule powder waterproof agent |
| CN101508852B (en) * | 2009-03-18 | 2011-12-21 | 中国科学院广州化学研究所 | Glass-hard organosilicon protective coating, preparation and uses thereof |
| CN102559099A (en) * | 2010-12-31 | 2012-07-11 | 第一毛织株式会社 | Adhesive composition and polarizer film comprising same |
| CN101631808B (en) * | 2007-02-14 | 2012-09-05 | 瓦克化学股份公司 | Redispersible core-shell polymers and a process for preparing them |
| CN106519126A (en) * | 2016-10-27 | 2017-03-22 | 华南理工大学 | Fluorosilicone-modified polyacrylate emulsion as well as preparing method and application thereof |
| CN107998977A (en) * | 2017-11-20 | 2018-05-08 | 桂林理工大学 | A kind of preparation method and applications of controllable hydrophobic selectivity modified kaolinite |
| CN109153880A (en) * | 2016-09-30 | 2019-01-04 | 环保纸有限公司 | With environmental protection, waterproof and paper and coating material of oil preventing performance and preparation method thereof |
| CN109608645A (en) * | 2018-11-06 | 2019-04-12 | 富思特新材料科技发展股份有限公司 | A kind of preparation method of self-dispersing micron order hydrophobic powder |
| CN110760147A (en) * | 2019-10-10 | 2020-02-07 | 江苏兆佳建材科技有限公司 | Preparation method of redispersible latex powder |
| CN113321442A (en) * | 2021-07-12 | 2021-08-31 | 广州建涂堡建材有限公司 | Method for preparing redispersible latex powder by taking modified silicone-acrylic emulsion as raw material |
| CN115819808A (en) * | 2023-01-10 | 2023-03-21 | 安徽皖维花山新材料有限责任公司 | Water-resistant redispersible latex powder and preparation method thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1206251C (en) * | 2003-03-06 | 2005-06-15 | 华南理工大学 | Acrylate micro-emulsion with high solid content, its preparation method and use |
| CN1282677C (en) * | 2004-09-21 | 2006-11-01 | 华南理工大学 | Hydroxyl acrylic acid emulsion with microgel nuclear structure and preparation process and application thereof |
-
2006
- 2006-07-21 CN CNB2006100366278A patent/CN100460427C/en not_active Expired - Fee Related
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101631808B (en) * | 2007-02-14 | 2012-09-05 | 瓦克化学股份公司 | Redispersible core-shell polymers and a process for preparing them |
| CN101735752B (en) * | 2008-11-18 | 2011-08-10 | 曾军 | Building gelatine powder |
| CN101508852B (en) * | 2009-03-18 | 2011-12-21 | 中国科学院广州化学研究所 | Glass-hard organosilicon protective coating, preparation and uses thereof |
| CN102101960B (en) * | 2010-12-24 | 2013-06-05 | 大连工业大学 | High-hydroxy silicon-acrylate aqueous glass coating emulsion and synthesis method thereof |
| CN102101960A (en) * | 2010-12-24 | 2011-06-22 | 大连工业大学 | High-hydroxy silicon-acrylate aqueous glass coating emulsion and synthesis method thereof |
| CN102559099A (en) * | 2010-12-31 | 2012-07-11 | 第一毛织株式会社 | Adhesive composition and polarizer film comprising same |
| CN102559099B (en) * | 2010-12-31 | 2015-02-18 | 第一毛织株式会社 | Adhesive composition and polarizer film comprising same |
| CN102226072A (en) * | 2011-05-06 | 2011-10-26 | 同济大学 | Preparation method of organic silicon microcapsule powder waterproof agent |
| CN109153880A (en) * | 2016-09-30 | 2019-01-04 | 环保纸有限公司 | With environmental protection, waterproof and paper and coating material of oil preventing performance and preparation method thereof |
| CN106519126A (en) * | 2016-10-27 | 2017-03-22 | 华南理工大学 | Fluorosilicone-modified polyacrylate emulsion as well as preparing method and application thereof |
| CN106519126B (en) * | 2016-10-27 | 2019-07-16 | 华南理工大学 | A kind of fluorinated silicone modified polyacrylate dispersion and the preparation method and application thereof |
| CN107998977A (en) * | 2017-11-20 | 2018-05-08 | 桂林理工大学 | A kind of preparation method and applications of controllable hydrophobic selectivity modified kaolinite |
| CN107998977B (en) * | 2017-11-20 | 2020-06-05 | 桂林理工大学 | Preparation method and application of controllable hydrophobic selectively modified kaolinite |
| CN109608645A (en) * | 2018-11-06 | 2019-04-12 | 富思特新材料科技发展股份有限公司 | A kind of preparation method of self-dispersing micron order hydrophobic powder |
| CN110760147A (en) * | 2019-10-10 | 2020-02-07 | 江苏兆佳建材科技有限公司 | Preparation method of redispersible latex powder |
| CN113321442A (en) * | 2021-07-12 | 2021-08-31 | 广州建涂堡建材有限公司 | Method for preparing redispersible latex powder by taking modified silicone-acrylic emulsion as raw material |
| CN115819808A (en) * | 2023-01-10 | 2023-03-21 | 安徽皖维花山新材料有限责任公司 | Water-resistant redispersible latex powder and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100460427C (en) | 2009-02-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1903898A (en) | Siloxane containing water soluble polymer emulsion and redispersible emulsion powder and its preparation method | |
| CN100343293C (en) | Fluorosilicone modified acrylic emulsion for weather resistant antifouling paint | |
| CN100345874C (en) | Organosilicon modified acrylate emulsion for ambient temperature crosslinked aqueous paint and method for preparing same | |
| CN1206251C (en) | Acrylate micro-emulsion with high solid content, its preparation method and use | |
| CN1040333C (en) | Synthesis of latex capsules | |
| CN101173021A (en) | Acrylic acid series nucleocapsid polymer emulsion and re-dispersible emulsion powder, and method for producing thereof | |
| CN101033360A (en) | Method of preparing organic/inorganic hybridization reactivity semi-interpenetrating network structure emulsion | |
| CN1908022A (en) | Process for preparing room temperature self-crosslinking acrylic ester emulsion modified by inorganic nano particle | |
| CN1946750A (en) | Vinyl chloride resin composition and method for preparation thereof | |
| CN1300191C (en) | Process for preparing nano silicon dioxide-acrylate composite emulsion | |
| CN106519126A (en) | Fluorosilicone-modified polyacrylate emulsion as well as preparing method and application thereof | |
| CN112029362B (en) | Preparation method of core-shell structure nano particles and hardened water-based acrylic resin coating | |
| CN107118650B (en) | Silica sol/polyacrylate emulsion containing hydroxyl-amino resin baking varnish and preparation method thereof | |
| CN1347926A (en) | Forming method of polymer hydro-dispersing liquid | |
| CN102702419B (en) | Preparation method of montmorillonite-modified crosslinked acrylate-hybridized core-shell emulsion | |
| CN104358107B (en) | Preparation method of fluorescent super-hydrophobic difunctional nanofiber membrane | |
| CN101648792A (en) | Protecting mortar of express highway roadbed surface hard-face terrace | |
| CN104262552A (en) | Silica sol/silicone acrylate core-shell nanocomposite emulsion and preparation method thereof | |
| CN1084199A (en) | The improved acrylic acid series caulking joint of adhesive performance composition | |
| CN1120187C (en) | Water redispersible power of film-forming polymers having a core/shell structure | |
| CN102796230A (en) | Method for preparing silicone acrylic emulsion with high solid content and high silicon content | |
| CN102190754A (en) | Acrylate emulsion, waterproof acrylate re-dispersible latex powder prepared from same, and preparation method for latex powder | |
| CN1670049A (en) | Process for preparing polyolefin and vinyl monomer graft copolymer | |
| CN101775105B (en) | Preparation method of high-impact polyacrylate grafting vinyl chloride emulsion copolymer resin | |
| CN1385447A (en) | Organic silicon-acrylate nano emulsion |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| EE01 | Entry into force of recordation of patent licensing contract |
Assignee: Guangdong Carpoly Chemical Group Co., Ltd. Assignor: South China University of Technology Contract record no.: 2011440000849 Denomination of invention: Siloxane containing water soluble polymer emulsion and redispersible emulsion powder and its preparation method Granted publication date: 20090211 License type: Common License Open date: 20070131 Record date: 20110805 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20090211 Termination date: 20200721 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |