CN101168584A - Redispersable latex powder emulsion, redispersable latex powder and preparation method thereof - Google Patents
Redispersable latex powder emulsion, redispersable latex powder and preparation method thereof Download PDFInfo
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- CN101168584A CN101168584A CNA200710046594XA CN200710046594A CN101168584A CN 101168584 A CN101168584 A CN 101168584A CN A200710046594X A CNA200710046594X A CN A200710046594XA CN 200710046594 A CN200710046594 A CN 200710046594A CN 101168584 A CN101168584 A CN 101168584A
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Abstract
The invention provides re-dispersible emulsion powder emulsion and re-dispersible emulsion powder and the preparation method thereof. The re-dispersible emulsion powder emulsion is obtained by vinyl ester, (methyl) styrene, and (methyl) acrylic ester through the emulsion polymerization way, and added polyvinyl alcohol is modified polyvinyl alcohol. The re-dispersible emulsion powder can be obtained through being dried in the way of conventional spray drying. The re-dispersible emulsion powder can widely used for the building fields of dry mix sand slurry, powder coating, etc. The re-dispersible emulsion powder of the invention adopts the modified polyvinyl alcohol as protective colloid, and compared with the ordinary re-dispersible emulsion powder, the re-dispersible emulsion powder has excellent adhesive property, and is a high performance and environmental protective product which can meet the requirements of building concrete and building mortar. The product is used in the building concrete and the mortar, and the workability and the cohesive force of the building concrete and the mortar can be obviously enhanced.
Description
Technical field
The present invention relates to redispersable latex powder emulsion and redispersable latex powder.
Background technology
At present, the existing over one hundred year history of the scale operation of cement material and application is characterized in as hard as flint, and very strong ultimate compression strength is arranged, easily water is in harmonious proportion, and generates hydrated product, has the good hydraulicity, excellent in durability, and easy to use, but its extensibility is very low, and permeability resistance is poor, easily shrinkage cracking.
Be to improve impermeability, frost resistance and the thermotolerance of cement material, reduce or thoroughly stop cement material cracking problem.Adding redispersible in cement material is that the polymer based powder composition is well known in water and with homopolymer or multipolymer.Such powdery compositions of dispersion is by preparing corresponding water containing plastic dispersed system spraying drying in hot gas flow.
Chinese patent CN1139944A has described a kind of redispersible in water and based on the dispersed powders of water-soluble polymers, and this powder comprises silicoorganic compound.Adopt the redispersable latex powder water tolerance of this method preparation relatively good, but cementability is poor.
Chinese patent CN1903898A has described a kind of siloxanes water-soluble polymers emulsion and redispersable latex powder and preparation method thereof of containing.Adopt the redispersable latex powder stability of this method preparation relatively good, but cementability is poor.
Summary of the invention
The objective of the invention is to propose a kind of redispersable latex powder emulsion and redispersable latex powder, to overcome the defective of prior art;
Another object of the present invention provides a kind of preparation method of redispersable latex powder emulsion.
The preparation method of redispersable latex powder emulsion of the present invention comprises the steps:
A) 0～100 parts by weight of ethylene base ester, 0～100 weight part (methyl) acrylate, 0～100 weight part (methyl) vinylbenzene and 0～2 weight part molecular weight regulator are mixed and made into mix monomer, total amount is 100 weight parts;
B) mix monomer with 80～100 weight part step a) mixes with 0.2～2 weight part reactive emulsifier, 0.2～2 weight part initiator and 35～100 weight parts waters, is made into mixing solutions;
C) mix monomer with 0～20 weight part step a) adds in the organic siloxane modified polyvinyl alcohol of 2-10 weight part, 0.1～2 weight part reactive emulsifier, 0.1～2 weight part initiator and 32～62 weight parts waters, reacted 0.1～1.0 hour under 50 ℃～90 ℃ conditions, drip b then) mixing solutions of step, the dropping time is 2～5 hours, reacted 0.5～3.0 hour, and obtained the redispersable latex powder emulsion;
The weight solid content of described redispersable latex powder emulsion is 40%～60%, and median size is 100nm～400nm, pH value 3～6;
Said vinyl ester is selected from the vinyl acetate or the tertiary ethylene carbonate of 1 to 10 carbon atom, non-branch or branching type alkyl carboxylic acid;
Said (methyl) acrylate is selected from vinyl cyanide, methyl acrylate, ethyl propenoate, n-butyl acrylate, isobutyl acrylate, ethyl acrylate, vinylformic acid-2-hydroxyl ethyl ester, vinylformic acid-2-hydroxypropyl acrylate, methyl methacrylate, Jia Jibingxisuanyizhi, n-BMA, methacrylic acid-2-ethylhexyl, 2-hydroxyethyl methacrylate, methacrylic acid-2-hydroxypropyl acrylate, acrylic or methacrylic acid C
8～C
16Alkyl ester;
Said molecular weight regulator is at least a in ethyl thioglycolate, Thiovanic acid butyl ester, mercaptoethanol, 2 mercapto ethanol or the tert-dodecyl mercaptan;
Said initiator is selected from least a in Potassium Persulphate, Sodium Persulfate or the ammonium persulphate;
Said reactive emulsifier is selected from least a in allyl polyethenoxy ether ammonium sulfate, allyl polyethenoxy ether or the vinyl Soxylat A 25-7;
Said organic siloxane modified polyvinyl alcohol can prepare by the following method:
40～80 weight account polyethylene alcohol, 100～400 weight parts waters and 20～60 weight part organo-siloxanes are mixed, 80～95 ℃ of reactions 0.5～5 hour, can obtain modified polyvinyl alcohol, 83～99 moles of % of organic siloxane modified polyvinyl alcohol alcoholysis degree of gained, molecular weight 500～10000g/mol;
Said organo-siloxane is selected from least a in vinyl three TMOSs, vinyl methoxyl group diethoxy alkane, vinyltriethoxysilane, the vinyl oxyethyl group diisopropoxy silane;
Above-mentioned redispersable latex powder emulsion can be used for preparing redispersable latex powder, the said redispersable latex powder of the present invention, the component that comprises following parts by weight: 100 parts of redispersable latex powder emulsions (over dry), 3～10 parts of modified polyvinyl alcohols (over dry), 2～15 parts of anti-caking agents, above-mentioned parts by weight are benchmark with the butt component;
Said (over dry) refers to not moisture.
Said anti-caking agent is at least a in diatomite, pure aluminium silicate, talcum powder, attapulgite, kaolin or the silicon-dioxide;
To make emulsion to be sprayed after the said components mixing, adopt spray drying process to obtain described redispersable latex powder.Conventional spray-drying equipment of employing this area and ordinary method are treated sprayable emulsion and are carried out spraying drying.The spraying drying inlet temperature that spray-drier is set is that 180 ℃, temperature out are that 75 ℃ of hot blast wind speed are 4m
3/ min, feeding speed are 50ml/min, atomizer rotating speed 300rpm, start heating system then, when treating that out temperature arrives set(ting)value, start the spraying drying that feeder system, atomization system and negative pressure system carry out emulsion.
As everyone knows, add organic silicon emulsion or on the polymkeric substance long-chain, introduce siloxanyl monomers and can improve the emulsion film forming water tolerance, but improve little for the cohesive force of emulsion.And the present invention adopts organic-silicon-modified polyvinyl alcohol as protective colloid, unexpectedly, adds the water tolerance that this modified polyvinyl alcohol can not only improve emulsion, also increases significantly for the cohesiveness of emulsion.
Redispersable latex powder of the present invention adopts modified polyvinyl alcohol as protective colloid, compares with common redispersable latex powder, has excellent cementability, is a kind of product that can satisfy building concrete, building mortar high-performance, environmental protection.This product uses in building concrete and mortar, can obviously improve workability, the cohesive force of building concrete, mortar.
Embodiment
Embodiment 1
1) preparation of modified polyvinyl alcohol A:
With the 40g polyvinyl alcohol (molecular weight: 500g/mol, alcoholysis degree: 83 moles of %), 100g deionized water, 60g vinyl three TMOSs mix, and is warming up to 80 ℃ of reactions 5 hours, reduces to 25 ℃, discharging, standby.
2) the redispersable latex powder emulsion is synthetic:
A) 98g vinyl-acetic ester, 2g ethyl thioglycolate are mixed and made into mix monomer, standby.
B) the 80g mix monomer is joined in the aqueous solution of 2g allyl polyethenoxy ether vitriol, 0.2g Potassium Persulphate and 100g deionized water high-speed stirring 30 minutes.Standby.
C) 20 parts of mix monomers are added in the aqueous solution of using 64.3g deionized water dissolving 20g modified polyvinyl alcohol A, 2g allyl polyethenoxy ether vitriol and 2g Potassium Persulphate, be warming up to 50 ℃, reacted 0.1 hour, and dripped b then) mixed solution in the process 5 hours, continue reaction 3 hours.Be cooled to 25 ℃.Filter through 100 eye mesh screens, must be used for the emulsion of redispersable latex powder, solid content: 40.2wt%, median size 101.5nm (using Malven particle diameter instrument to record), pH=3.15 (using PHS-3C Accurate pH instrumentation to get).
3) preparation of strong cementability redispersable latex powder:
Protective colloid is modified polyvinyl alcohol A, and anti-caking agent is talcum powder and silicon-dioxide, and its component prescription is as follows:
| Form | Quality/g | |
| 1 | Strong cementability redispersable latex powder emulsion | 250 |
| 2 | Modified polyvinyl alcohol A | 6 |
| 3 | Talcum powder | 13 |
| 4 | Silicon-dioxide | 2 |
Step 1: the preparation of the emulsion of waiting to spray
Take by weighing the strong cementability redispersable latex powder of 250g emulsion, 6g modified polyvinyl alcohol A mixing, stirred 10 minutes, in said mixture, add 13g talcum powder and 2g silicon-dioxide anti-caking agent again, stirred 10～20 minutes, make emulsion to be sprayed.
Step 2: the spraying drying of emulsion
Adopt spray-drier to treat sprayable emulsion and carry out drying.The spraying drying inlet temperature that spray-drier is set is that 180 ℃, temperature out are that 75 ℃ of hot blast wind speed are 4m
3/ min, feeding speed are 50ml/min, atomizer rotating speed 300rpm, start heating system then, when treating that out temperature arrives set(ting)value, start the spraying drying that feeder system, atomization system and negative pressure system carry out emulsion.
The powder of dry back gained filters by 100 eye mesh screens, and sieving is prepared latex powder.
Embodiment 2
1) preparation of modified polyvinyl alcohol B:
With the 80g polyvinyl alcohol (molecular weight: 1000g/mol, alcoholysis degree: 99 moles of %), 400g deionized water, 20g vinyl methoxyl group diethoxy alkane mix, and is warming up to 95 ℃ of reactions 0.5 hour, reduces to 25 ℃, discharging, standby.
2) the redispersable latex powder emulsion is synthetic:
A) the 100g tertiary ethylene carbonate is standby.
B) the 100g tertiary ethylene carbonate is joined in the aqueous solution of 0.2g allyl polyethenoxy ether vitriol, 2g Sodium Persulfate and 33.6g deionized water high-speed stirring 30 minutes.Standby.
C) in the aqueous solution of 10g modified polyvinyl alcohol B, 0.1g allyl polyethenoxy ether vitriol, 0.1g Sodium Persulfate and 28g deionized water, be warming up to 90 ℃, reacted 1 hour, drip b then) mixed solution in the process 2 hours, continue reaction 0.5 hour.Be cooled to 25 ℃.Filter through 100 eye mesh screens, must be used for the emulsion of redispersable latex powder, solid content: 59.8wt%, median size 397.5nm (using Malven particle diameter instrument to record), pH=5.87 (using PHS-3C Accurate pH instrumentation to get).
3) preparation of strong cementability redispersable latex powder:
Protective colloid is modified polyvinyl alcohol B, and anti-caking agent is an attapulgite, and its component prescription is as follows:
| Form | Quality/g | |
| 1 | Strong cementability redispersable latex powder emulsion | 167 |
| 2 | Modified polyvinyl alcohol B | 50 |
| 3 | Attapulgite | 2 |
Step 1: the preparation of the emulsion of waiting to spray
Take by weighing the strong cementability redispersable latex powder of 167g emulsion, 50g modified polyvinyl alcohol B mixing, stirred 10 minutes, in said mixture, add 2g diatomite anti-caking agent again, stirred 10～20 minutes, make emulsion to be sprayed.
Step 2: the spraying drying of emulsion
Adopt spray-drier to treat sprayable emulsion and carry out drying.The spraying drying inlet temperature that spray-drier is set is that 180 ℃, temperature out are that 75 ℃ of hot blast wind speed are 4m
3/ min, feeding speed are 50ml/min, atomizer rotating speed 300rpm, start heating system then, when treating that out temperature arrives set(ting)value, start the spraying drying that feeder system, atomization system and negative pressure system carry out emulsion.
The powder of dry back gained filters by 100 eye mesh screens, and sieving is prepared latex powder.
Embodiment 3
1) preparation of modified polyvinyl alcohol C:
With the 60g polyvinyl alcohol (molecular weight: 10000g/mol, alcoholysis degree: 88 moles of %), 300g deionized water, 40g vinyltriethoxysilane mix, and is warming up to 90 ℃ of reactions 3 hours, reduces to 25 ℃, discharging, standby.
2) the redispersable latex powder emulsion is synthetic:
A) 50g methyl methacrylate, 49g n-butyl acrylate, 1g mercaptoethanol are mixed and made into mix monomer, standby.
B) the 90g mix monomer is joined in the aqueous solution of 1g allyl polyethenoxy ether, 1g ammonium persulphate and 50g deionized water high-speed stirring 30 minutes.Standby.
C) the 10g mix monomer is added in the aqueous solution of using 44g deionized water dissolving 20g modified polyvinyl alcohol C, 1g allyl polyethenoxy ether vitriol and 1g ammonium persulphate, be warming up to 70 ℃, reacted 0.5 hour, and dripped b then) mixed solution in the process 3 hours, continue reaction 2 hours.Be cooled to 25 ℃.Filter through 100 eye mesh screens, must be used for the emulsion of redispersable latex powder, solid content: 49.8wt%, median size 261nm (using Malven particle diameter instrument to record), pH=4.25 (using PHS-3C Accurate pH instrumentation to get).
3) preparation of strong cementability redispersable latex powder:
Protective colloid is modified polyvinyl alcohol C, and anti-caking agent is kaolin and pure aluminium silicate, and its component prescription is as follows:
| Form | Quality/g | |
| 1 | Strong cementability redispersable latex powder emulsion | 200 |
| 2 | Modified polyvinyl alcohol C | 20 |
| 3 | Kaolin | 5 |
| 4 | Pure aluminium silicate | 3 |
Step 1: the preparation of the emulsion of waiting to spray
Take by weighing the strong cementability redispersable latex powder of 200g emulsion, 20g modified polyvinyl alcohol C mixing, stirred 10 minutes, in said mixture, add 5g kaolin and 3g pure aluminium silicate anti-caking agent again, stirred 10～20 minutes, make emulsion to be sprayed.
Step 2: the spraying drying of emulsion
Adopt spray-drier to treat sprayable emulsion and carry out drying.The spraying drying inlet temperature that spray-drier is set is that 180 ℃, temperature out are that 75 ℃ of hot blast wind speed are 4m
3/ min, feeding speed are 50ml/min, atomizer rotating speed 300rpm, start heating system then, when treating that out temperature arrives set(ting)value, start the spraying drying that feeder system, atomization system and negative pressure system carry out emulsion.
The powder of dry back gained filters by 100 eye mesh screens, and sieving is prepared latex powder.
Embodiment 4
1) preparation of modified polyvinyl alcohol D:
With the 50g polyvinyl alcohol (molecular weight: 5000g/mol, alcoholysis degree: 95 moles of %), 150g deionized water, 50g vinyl oxyethyl group diisopropoxy silane mixture, be warming up to 85 ℃ of reactions 2 hours, reduce to 25 ℃, discharging, standby.
2) the redispersable latex powder emulsion is synthetic:
A) 80g vinylbenzene, 20g vinyl toluene are mixed and made into mix monomer, standby.
B) the 85g mix monomer is joined in the aqueous solution of 0.5g vinyl Soxylat A 25-7,1.5g ammonium persulphate and 40g deionized water high-speed stirring 30 minutes.Standby.
C) the 15g mix monomer is added in the aqueous solution of using 39.95g deionized water dissolving 18.75g modified polyvinyl alcohol D, 1.5g vinyl Soxylat A 25-7 and 0.5g Potassium Persulphate, be warming up to 80 ℃, reacted 15 minutes, and dripped b then) mixed solution in the process 4 hours, continue reaction 1.5 hours.Be cooled to 25 ℃.Filter through 100 eye mesh screens, must be used for the emulsion of redispersable latex powder, solid content: 54.89wt%, median size 319nm (using Malven particle diameter instrument to record), pH=4.48 (using PHS-3C Accurate pH instrumentation to get).
3) preparation of strong cementability redispersable latex powder:
Protective colloid is modified polyvinyl alcohol D, and anti-caking agent is diatomite and pure aluminium silicate, and its component prescription is as follows:
| Form | Quality/g | |
| 1 | Strong cementability redispersable latex powder emulsion | 182 |
| 2 | Modified polyvinyl alcohol D | 20 |
| 3 | Diatomite | 7 |
| 4 | Pure aluminium silicate | 1 |
Step 1: the preparation of the emulsion of waiting to spray
Take by weighing the strong cementability redispersable latex powder of 182g emulsion, 20g modified polyvinyl alcohol D mixing, stirred 10 minutes, in said mixture, add 7g diatomite and 1g pure aluminium silicate anti-caking agent again, stirred 10～20 minutes, make emulsion to be sprayed.
Step 2: the spraying drying of emulsion
Adopt spray-drier to treat sprayable emulsion and carry out drying.The spraying drying inlet temperature that spray-drier is set is that 180 ℃, temperature out are that 75 ℃ of hot blast wind speed are 4m
3/ min, feeding speed are 50ml/min, atomizer rotating speed 300rpm, start heating system then, when treating that out temperature arrives set(ting)value, start the spraying drying that feeder system, atomization system and negative pressure system carry out emulsion.
The powder of dry back gained filters by 100 eye mesh screens, and sieving is prepared latex powder.
Embodiment 5
1) preparation of modified polyvinyl alcohol E:
With 70g polyvinyl alcohol (molecular weight: 2500g/mol, 92 moles of %), 200g deionized water, 10g vinyl oxyethyl group diisopropoxy silane, 20g vinyltriethoxysilane mix, and is warming up to 82 ℃ of reactions 3.5 hours, reduces to 25 ℃ alcoholysis degree:, discharging, standby.
2) the redispersable latex powder emulsion is synthetic:
A) 50g vinyl-acetic ester, 30g ethyl acrylate, 19g vinylbenzene and 1g2-mercaptoethanol are mixed and made into mix monomer, standby.
B) 95 parts of mix monomers are joined in the aqueous solution of 1g allyl polyethenoxy ether vitriol, 1g allyl polyethenoxy ether, 0.8g Sodium Persulfate and 61.8g deionized water high-speed stirring 30 minutes.Standby.
C) 5 parts of mix monomers are added in the aqueous solution of using 64g deionized water dissolving 12g modified polyvinyl alcohol E, 2g allyl polyethenoxy ether vitriol and 0.7g Sodium Persulfate, be warming up to 65 ℃, reacted 25 minutes, and dripped b then) mixed solution in the process 3.5 hours, continue reaction 1.5 hours.Be cooled to 25 ℃.Filter through 100 eye mesh screens, must be used for the emulsion of redispersable latex powder, solid content: 45.13wt%, median size 135nm (using Malven particle diameter instrument to record), pH=3.74 (using PHS-3C Accurate pH instrumentation to get).
3) preparation of strong cementability redispersable latex powder:
Protective colloid is modified polyvinyl alcohol E, and anti-caking agent is kaolin and silicon-dioxide, and its component prescription is as follows:
| Form | Quality/g | |
| 1 | Strong cementability redispersable latex powder emulsion | 222 |
| 2 | Modified polyvinyl alcohol E | 12 |
| 3 | Kaolin | 3 |
| 4 | Silicon-dioxide | 1 |
Step 1: the preparation of the emulsion of waiting to spray
Take by weighing the strong cementability redispersable latex powder of 222g emulsion, 12g modified polyvinyl alcohol E mixing, stirred 10 minutes, in said mixture, add 3g kaolin and 1g silicon-dioxide anti-caking agent again, stirred 10～20 minutes, make emulsion to be sprayed.
Step 2: the spraying drying of emulsion
Adopt spray-drier to treat sprayable emulsion and carry out drying.The spraying drying inlet temperature that spray-drier is set is that 180 ℃, temperature out are that 75 ℃ of hot blast wind speed are 4m
3/ min, feeding speed are 50ml/min, atomizer rotating speed 300rpm, start heating system then, when treating that out temperature arrives set(ting)value, start the spraying drying that feeder system, atomization system and negative pressure system carry out emulsion.
The powder of dry back gained filters by 100 eye mesh screens, and sieving is prepared latex powder.
Embodiment 6
1) preparation of modified polyvinyl alcohol F:
With 65g polyvinyl alcohol (molecular weight: 7500g/mol, 85 moles of %), 300g deionized water, 25g vinyl oxyethyl group diisopropoxy silane, 10g vinyl methoxyl group diethoxy alkane mix, and is warming up to 88 ℃ of reactions 2.5 hours, reduces to 25 ℃ alcoholysis degree:, discharging, standby.
2) the redispersable latex powder emulsion is synthetic:
A) 70g vinyl-acetic ester, 26g methacrylic acid-2-hydroxypropyl acrylate, 2.5g vinylformic acid and 1.5g Thiovanic acid butyl ester are mixed and made into mix monomer, standby.
B) the 88g mix monomer is joined in the aqueous solution of 0.6g allyl polyethenoxy ether vitriol, 0.4g vinyl Soxylat A 25-7,1.2g ammonium persulphate and 61.5g deionized water high-speed stirring 30 minutes.Standby.
C) the 12g mix monomer is added in the aqueous solution of using 40g deionized water dissolving 24g modified polyvinyl alcohol F, 1.5g allyl polyethenoxy ether vitriol and 0.6g Sodium Persulfate, be warming up to 55 ℃, reacted 40 minutes, and dripped b then) mixed solution in the process 2.5 hours, continue reaction 1.8 hours.Be cooled to 25 ℃.Filter through 100 eye mesh screens, must be used for the emulsion of redispersable latex powder, solid content: 47.92wt%, median size 225nm (using Malven particle diameter instrument to record), pH=3.94 (using PHS-3C Accurate pH instrumentation to get).
3) preparation of strong cementability redispersable latex powder:
Protective colloid is modified polyvinyl alcohol F, and anti-caking agent is a talcum powder, and its component prescription is as follows:
| Form | Quality/g | |
| 1 | Strong cementability redispersable latex powder emulsion | 208.3 |
| 2 | Modified polyvinyl alcohol F | 16 |
| 3 | Talcum powder | 11 |
Step 1: the preparation of the emulsion of waiting to spray
Take by weighing the strong cementability redispersable latex powder of 208.3g emulsion, 16g modified polyvinyl alcohol F mixing, stirred 10 minutes, in said mixture, add 11g talcum powder anti-caking agent again, stirred 10～20 minutes, make emulsion to be sprayed.
Step 2: the spraying drying of emulsion
Adopt spray-drier to treat sprayable emulsion and carry out drying.The spraying drying inlet temperature that spray-drier is set is that 180 ℃, temperature out are that 75 ℃ of hot blast wind speed are 4m
3/ min, feeding speed are 50ml/min, atomizer rotating speed 300rpm, start heating system then, when treating that out temperature arrives set(ting)value, start the spraying drying that feeder system, atomization system and negative pressure system carry out emulsion.
The powder of dry back gained filters by 100 eye mesh screens, and sieving is prepared latex powder.
Embodiment 7
1) preparation of modified polyvinyl alcohol G:
With the 55g polyvinyl alcohol (molecular weight: 8000g/mol, alcoholysis degree: 90 moles of %), 350g deionized water, 45g vinyl oxyethyl group diisopropoxy silane mixture, be warming up to 92 ℃ of reactions 4 hours, reduce to 25 ℃, discharging, standby.
2) the redispersable latex powder emulsion is synthetic:
A) 60g vinylbenzene, 39.5g methacrylic acid-2-ethylhexyl and 0.5g tert-dodecyl mercaptan are mixed and made into mix monomer, standby.
B) 88 parts of mix monomers are joined in the aqueous solution of 1.2g allyl polyethenoxy ether vitriol, 1.8g Potassium Persulphate and 70g deionized water high-speed stirring 30 minutes.Standby.
C) the 12g mix monomer is added in the aqueous solution of using 55.4g deionized water dissolving 40.5g modified polyvinyl alcohol G, 0.8g allyl polyethenoxy ether vitriol and 0.8g Sodium Persulfate, be warming up to 55 ℃, reacted 15 minutes, and dripped b then) mixed solution in the process 4 hours, continue reaction 2.5 hours.Be cooled to 25 ℃.Filter through 100 eye mesh screens, must be used for the emulsion of redispersable latex powder, solid content: 42.05wt%, median size 293nm (using Malven particle diameter instrument to record), pH=4.28 (using PHS-3C Accurate pH instrumentation to get).
3) preparation of strong cementability redispersable latex powder:
Protective colloid is modified polyvinyl alcohol G, and anti-caking agent is talcum powder and kaolin, and its component prescription is as follows:
| Form | Quality/g | |
| 1 | Strong cementability redispersable latex powder emulsion | 238.1 |
| 2 | Modified polyvinyl alcohol G | 27 |
| 3 | Talcum powder | 4 |
| 4 | Kaolin | 5 |
Step 1: the preparation of the emulsion of waiting to spray
Take by weighing the strong cementability redispersable latex powder of 238.1g emulsion, 27g modified polyvinyl alcohol G mixing, stirred 10 minutes, in said mixture, add 4g talcum powder and 5g kaolin anti-caking agent again, stirred 10～20 minutes, make emulsion to be sprayed.
Step 2: the spraying drying of emulsion
Adopt spray-drier to treat sprayable emulsion and carry out drying.The spraying drying inlet temperature that spray-drier is set is that 180 ℃, temperature out are that 75 ℃ of hot blast wind speed are 4m
3/ min, feeding speed are 50ml/min, atomizer rotating speed 300rpm, start heating system then, when treating that out temperature arrives set(ting)value, start the spraying drying that feeder system, atomization system and negative pressure system carry out emulsion.
The powder of dry back gained filters by 100 eye mesh screens, and sieving is prepared latex powder.
Embodiment 8
1) preparation of modified polyvinyl alcohol C:
With the 60g polyvinyl alcohol (molecular weight: 10000g/mol, alcoholysis degree: 88 moles of %), 300g deionized water, 40g vinyltriethoxysilane mix, and is warming up to 90 ℃ of reactions 3 hours, reduces to 25 ℃, discharging, standby.
2) the redispersable latex powder emulsion is synthetic:
D) 50g methyl methacrylate, 50g ethyl propenoate are mixed and made into mix monomer, standby.
E) the 90g mix monomer is joined in the aqueous solution of 1g allyl polyethenoxy ether, 1g ammonium persulphate and 50g deionized water high-speed stirring 30 minutes.Standby.
F) the 10g mix monomer is added in the aqueous solution of using 44g deionized water dissolving 20g modified polyvinyl alcohol C, 1g allyl polyethenoxy ether vitriol and 1g ammonium persulphate, be warming up to 70 ℃, reacted 20 minutes, and dripped b then) mixed solution in the process 3 hours, continue reaction 2 hours.Be cooled to 25 ℃.Filter through 100 eye mesh screens, must be used for the emulsion of redispersable latex powder, solid content: 49.8wt%, median size 261nm (using Malven particle diameter instrument to record), pH=4.25 (using PHS-3C Accurate pH instrumentation to get).
3) preparation of strong cementability redispersable latex powder:
Protective colloid is modified polyvinyl alcohol C, and anti-caking agent is kaolin and pure aluminium silicate, and its component prescription is as follows:
| Form | Quality/g | |
| 1 | Strong cementability redispersable latex powder emulsion | 200 |
| 2 | Modified polyvinyl alcohol C | 20 |
| 3 | Kaolin | 5 |
| 4 | Pure aluminium silicate | 3 |
Step 1: the preparation of the emulsion of waiting to spray
Take by weighing the strong cementability redispersable latex powder of 200g emulsion, 20g modified polyvinyl alcohol C mixing, stirred 10 minutes, in said mixture, add 5g kaolin and 3g pure aluminium silicate anti-caking agent again, stirred 10～20 minutes, make emulsion to be sprayed.
Step 2: the spraying drying of emulsion
Adopt spray-drier to treat sprayable emulsion and carry out drying.The spraying drying inlet temperature that spray-drier is set is that 180 ℃, temperature out are that 75 ℃ of hot blast wind speed are 4m
3/ min, feeding speed are 50ml/min, atomizer rotating speed 300rpm, start heating system then, when treating that out temperature arrives set(ting)value, start the spraying drying that feeder system, atomization system and negative pressure system carry out emulsion.
The powder of dry back gained filters by 100 eye mesh screens, and sieving is prepared latex powder.
Embodiment 9
Comparative Examples 1: the latex powder of pressing the method preparation of CN1139944A
Comparative Examples 2: the latex powder of pressing the method preparation of CN1903898A
Embodiment 1～8 and Comparative Examples 1～2 prepared latex powder are used for following finishing mucilage composition:
The finishing mucilage composition:
300.0 part cement 325
600.0 part quartz sand (0.1-0.4mm)
40.0 part latex powder
2.0 part ether of cellulose
0.8 part starch ethers
0.5 part fiber
150 parts of dicalcium powders
The every 1000g dry mixture of water 200g
The method of pressing JC/T993-2006 detects tensile bond strength
Said sample maintenance 14 days (normal curing: temperature (23 ± 2) ℃, relative humidity 60%)
Finishing mucilage on the polystyrene sheet material is measured
| Sample | Tensile bond strength, MPa |
| Comparative Examples 1 | 0.11 |
| Comparative Examples 2 | 0.10 |
| Embodiment 1 | 0.12 |
| Embodiment 2 | 0.14 |
| Embodiment 3 | 0.13 |
| Embodiment 4 | 0.13 |
| Embodiment 5 | 0.12 |
| Embodiment 6 | 0.13 |
| Embodiment 7 | 0.14 |
| Embodiment 8 | 0.15 |
From above-mentioned application experiment: use the finishing mucilage of the redispersable latex powder preparation of embodiments of the invention 1～8 preparation to compare with Comparative Examples 1～2, tensile bond strength is good, has better cohesiveness.
Claims (10)
1. a redispersable latex powder emulsion is characterized in that the preparation method comprises the steps:
A) 0～100 parts by weight of ethylene base ester, 0～100 weight part (methyl) acrylate, 0～100 weight part (methyl) vinylbenzene and 0～2 weight part molecular weight regulator are mixed and made into mix monomer, total amount is 100 weight parts;
B) mix monomer with 80～100 weight part step a) mixes with 0.2～2 weight part reactive emulsifier, 0.2～2 weight part initiator and 35～100 weight parts waters, is made into mixing solutions;
C) mix monomer with 0～20 weight part step a) adds in the organic siloxane modified polyvinyl alcohol of 2-10 weight part, 0.1～2 weight part reactive emulsifier, 0.1～2 weight part initiator and 32～62 weight parts waters, reacted 0.1～1.0 hour under 50 ℃～90 ℃ conditions, drip b then) mixing solutions of step, the dropping time is 2～5 hours, reacted 0.5～3 hour, and obtained the redispersable latex powder emulsion.
2. redispersable latex powder emulsion according to claim 1 is characterized in that, the weight solid content is 40%～60%, and median size is 100nm～400nm, pH value 3～6.
3. redispersable latex powder emulsion according to claim 1 is characterized in that, said vinyl ester is selected from the vinyl acetate or the tertiary ethylene carbonate of 1 to 10 carbon atom, non-branch or branching type alkyl carboxylic acid.
4. redispersable latex powder emulsion according to claim 1, it is characterized in that said (methyl) acrylate is selected from vinyl cyanide, methyl acrylate, ethyl propenoate, n-butyl acrylate, isobutyl acrylate, ethyl acrylate, vinylformic acid-2-hydroxyl ethyl ester, vinylformic acid-2-hydroxypropyl acrylate, methyl methacrylate, Jia Jibingxisuanyizhi, n-BMA, methacrylic acid-2-ethylhexyl, 2-hydroxyethyl methacrylate, methacrylic acid-2-hydroxypropyl acrylate, acrylic or methacrylic acid C
8～C
16Alkyl ester.
5. redispersable latex powder emulsion according to claim 1 is characterized in that, said molecular weight regulator is at least a in ethyl thioglycolate, Thiovanic acid butyl ester, mercaptoethanol, 2 mercapto ethanol or the tert-dodecyl mercaptan.
6. redispersable latex powder emulsion according to claim 1 is characterized in that, said initiator is selected from least a in Potassium Persulphate, Sodium Persulfate or the ammonium persulphate.
7. redispersable latex powder emulsion according to claim 1 is characterized in that, said reactive emulsifier is selected from least a in allyl polyethenoxy ether ammonium sulfate, allyl polyethenoxy ether or the vinyl Soxylat A 25-7.
8. according to each described redispersable latex powder emulsion of claim 1～7, it is characterized in that said organic siloxane modified polyvinyl alcohol prepares by the following method:
40～80 weight account polyethylene alcohol, 100～400 weight parts waters and 20～60 weight part organo-siloxanes are mixed, 80～95 ℃ of reactions 0.5～5 hour, can obtain modified polyvinyl alcohol, 83～99 moles of % of organic siloxane modified polyvinyl alcohol alcoholysis degree of gained, molecular weight 500～10000g/mol;
Said organo-siloxane is selected from least a in vinyl three TMOSs, vinyl methoxyl group diethoxy alkane, vinyltriethoxysilane, the vinyl oxyethyl group diisopropoxy silane.
9. a redispersable latex powder is characterized in that, comprises the component of following parts by weight:
100 parts of each described redispersable latex powder emulsions (over dry) of claim 1～8,3～10 parts of modified polyvinyl alcohols (over dry), 2～15 parts of anti-caking agents, above-mentioned parts by weight are benchmark with the butt component.
10. redispersable latex powder according to claim 9 is characterized in that, said anti-caking agent is at least a in diatomite, pure aluminium silicate, talcum powder, attapulgite, kaolin or the silicon-dioxide.
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