CN103497290A - Redispersible polymer latex powder and preparation method thereof - Google Patents
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Abstract
The invention relates to a redispersible polymer latex powder and a preparation method thereof. The redispersible polymer latex powder comprises the following raw materials in parts by weight: 45-55 parts of ethylene latex powder, 35-45 parts of amorphous starch, 5-10 parts of toughening agent, 1-4 parts of curing agent, 3-5 parts of crystallizing agent and 0.005-0.01 part of initiating agent. According to the preparation method of the redispersible polymer latex powder, the amorphous starch and the ethylene latex powder are subjected to graft copolymerization in a dry powder state through the mechanical force chemical action of a rod mill, so that the long-chain structure of ethylene latex powder is increased, the flexibility is increased, and the water retention is enhanced; the cross-linking cured toughening agent and active hydroxy of the amorphous starch grafted to the latex powder are in condensation reaction, so that the long-chain structure is further formed, the redispersible polymer latex powder with the long-chain structure and good water solubility is finally formed, and the water retention, the water resistance and the bonding strength are greatly enhanced. The redispersible polymer latex powder disclosed by the invention can be widely used in the field of building materials, such as dry-mixed mortar, ceramic tile adhesive, putty cream, waterproof slurry, and the like.
Description
Technical field
The present invention relates to the redispersable latex powder field, be specifically related to a kind of Redispersible Polymeric Emulsion Powder and preparation method.
Background technology
To 20 end of the centurys, this two large problems of shortage of resources and environmental pollution has become most important obstacle on society and national development road, relevant ministries and commissions of country have taked multinomial measure, and the serious building trade that consumes energy has been proposed to move towards environmental protection, energy-conservation demand for development.Country promotes Introduced From Abroad Advanced Idea and modern technique, and instructing building materials field to adopt to be dry mixed is main environmental protection, efficient building materials.With polymer emulsion, the inorganic coagulation material modifications such as cement have been used widely, the water mixed in rear emulsion due to both can also finally solidify with cement generation hydration reaction immediately, so be in most cases the form that adopts two-pack, at the construction field (site) each component is mixed in proportion, makes troubles to storage, transportation, construction etc.The appearance of redispersable latex powder, changed above-mentioned phenomenon.As being dry mixed building materials, dry-mix, dry powder paint, tile binding material, waterproof paint, building heat-insulating mortar, flexible mortar, gravity flowing levelling mortar etc. are developed rapidly.Not only reduce loss in process of construction and the harm in later stage, and save material, reduce cost, greatly reduced cement consumption, promoted structural quality.
Redispersable latex powder is as the additive that is dry mixed the building materials key, in recent years, and at dry-mixed mortar, dry powder paint, buildings waterproof, ceramic tile is bonding is widely used.Along with redispersable latex powder is also more and more wider in the application of China, consumption increases gradually, and at present the redispersable latex powder range of product of China is single, and quality product is poor, and therefore redispersable latex powder is from abroad, and expensive mostly.The domestic research to redispersable latex powder mainly concentrates on polymerization stage and drying stage, and to carry out modification more, but produce waywardly, and technique is unstable, causes production cost high, and the performance of product does not reach requirement.Especially exist poor water retention property, poor water resistance and bonding strength not to reach the defects such as requirement.
China Patent Publication No. CN100460427C discloses redispersable latex powder and the preparation method containing silane water-soluble polymers emulsion, the method is by vinyl polyfunctional group organo-siloxane function monomer and alkyl methacrylate, hydroxy alkyl ester, alkyl acrylate and carboxylic acid cross-linking monomer make emulsion by letex polymerization, obtain redispersable latex powder by drying, solved to a certain extent the latex powder water tolerance, but carry out modification in the letex polymerization stage, cost is high, production technique is wayward, the polymerized emulsion obtained after drying, performance loss is serious, and the water-retentivity of unresolved latex powder and cementability.
China Patent Publication No. CN100482743C discloses polymer powders redispersible Preparation Method And The Use in a kind of water that improves water-fast adhesiveproperties, this synthetic resin powder obtains by a kind of dispersion emulsion composition of drying, water tolerance and cementability have been solved to a certain extent, but after drying, performance has been subject to serious loss.
Above-mentioned redispersable latex powder carries out modification in letex polymerization stage and drying stage, production technique is difficult to control, production cost is high, the redispersable latex powder performance loss is serious after drying, therefore, the problem that the redispersable latex powder ubiquity is on the high side and water tolerance is poor at present, compare and have a certain distance with the parent emulsion.
Summary of the invention
The present invention is directed to the defect of heavy losses of water-retentivity, water tolerance and the cementability of the redispersable latex powder made at present after the emulsion drying, a kind of low-cost Redispersible Polymeric Emulsion Powder by ethene rubber powder and amorphous starch graft copolymer is provided, and this Redispersible Polymeric Emulsion Powder has excellent water-retentivity, water tolerance and bonding strength.
Further aim of the present invention is to provide a kind of preparation method who prepares Redispersible Polymeric Emulsion Powder under dry powder, and the method is to react by mechanical force and chemical, under the dry powder condition, graft copolymerization occurs.
A kind of Redispersible Polymeric Emulsion Powder of the present invention is characterized in that parts by weight of raw materials is composed as follows:
45～55 parts of ethene rubber powders,
35～45 parts of amorphous starch,
5～10 parts of toughner,
1～4 part of ripening agent,
3～5 parts of crystallizing agents,
0.005～0.01 part of initiator,
Wherein, described ethene rubber powder is the powdery, water-soluble rubber powder, and commonly used have at least one in ethylene-vinyl acetate copolymerization rubber powder, vinyl acetate copolymerized rubber powder; Described amorphous starch is 100～200 purpose amorphous structure granular starchs, and, there are a large amount of living radicals in degree of crystallinity≤5% on starch chain, and internal structure is loose, has good reactive behavior, preferably the amorphous yam starch; Described toughner is acid amides and derivative thereof; Described ripening agent is at least one in sodium sulfate, zinc sulfate, ammonium sulfate, potassium alum; Described crystallizing agent is at least one in sodium methyl silicate, Starso, potassium silicate, has good water-soluble, perviousness, film-forming properties, cementability, can in water, form free silicate; Described initiator is the BPO peroxy initiator, can decomposite free radical at 75～100 ℃, as the interface initiator of powder ethene rubber powder.
Acid amides described above and derivative thereof are at least one in urea, acrylamide, 2-acrylamide-2-methylpro panesulfonic acid.
The preparation method of a kind of Redispersible Polymeric Emulsion Powder provided by the invention, be under the dry powder condition, to pass through to prepare by graft copolymerization, and concrete preparation process is as follows:
1) 45～55 parts by weight of ethylene rubber powders, 35～45 weight part amorphous starch, 0.005～0.01 part of weight initiator are poured in ribbon mixer and mixed 3～5min, send into rod mill after mixing, the rotating speed of rod mill is controlled at 150～250r/min, the rod milling time is controlled at 15～25min, ethene rubber powder active group under the strong shearing action of rod mill is caused by initiator, with the active group generation graft copolymerization of amorphous starch, forms backbone;
2) 5～10 weight part toughner, 1～4 weight part ripening agent are added in step 1), rod milling again, the rotating speed of rod mill is controlled at 100～200r/min, the rod milling time is controlled at 10～20min, under the mechanical force and chemical effect, in toughner, contained amide group is ripened the agent cross-linking curing, and with the activity hydroxy generation condensation reaction of amorphous starch, further form backbone, significantly improve the bonding strength after film forming;
3) by step 2) the rod milling material that obtains puts into high mixer, and obtains a kind of Redispersible Polymeric Emulsion Powder after 3～5 weight part crystallizing agents mix in high mixer.
Graft copolymerization, by adopting amorphous starch, occurs with the ethene rubber powder in the present invention under the powdery condition, has increased ethene rubber powder backbone, and its snappiness is increased, and water-retentivity improves; The toughner of cross-linking curing and the activity hydroxy generation condensation reaction that is grafted to the amorphous starch on rubber powder, further form backbone, the final water-soluble good Redispersible Polymeric Emulsion Powder that forms a kind of backbone, increased substantially water-retentivity, water tolerance and bonding strength.
The present invention has further adopted crystallizing agent, when Redispersible Polymeric Emulsion Powder is applied in sand-cement slurry, putty, the calcium ion, the magnesium ion generation crystallization reaction that in crystallizing agent, in free silicate and sand-cement slurry, putty, exist, form fine and close structure, improved film-forming properties, cementability, the water-repellancy of redispersable latex powder.
Ribbon mixer described in above-mentioned preparation process, by U-shaped container, double-deck ribbon agitating vane, formed, the long body tube structure of U-shaped, guaranteed the slight drag campaign in cylindrical shell of mixed material, under the effect of double-deck ribbon agitating vane, make material form more eddy current in flowing, make to mix more even.
Rod mill described in above-mentioned preparation process is the stirring-type rod mill, comprises cylindrical shell and stirring rod, and its technical characteristics is to be provided with 6 groups of rotatable stirring rod in cylindrical shell, and stirring rod is fixed on cylindrical shell two end axles end surface, and during rotation, stirring rod is ground with the cylinder face.
The outstanding characteristics of the present invention are:
1, under dry powder, by ethene rubber powder and amorphous starch, toughner, graft copolymerization, condensation reaction occurring under the mechanical force and chemical effect forms a kind of Redispersible Polymeric Emulsion Powder with backbone, without drying, water-retentivity, water tolerance and bonding strength have been increased substantially;
2, the present invention is by adopting crystallizing agent, while making redispersable latex powder be applied to sand-cement slurry, putty can with free calcium ion, magnesium ion generation crystallization reaction, form fine and close structure, improved film-forming properties, cementability, the water-repellancy of redispersable latex powder;
3, the present invention adopts natural polymer amorphous starch material, and raw material is easy to get, and cost is low, and product performance are good;
4, the present invention adopts totally-enclosed continuous cleaning type production, and technique is brief, the product environmental protection, can be widely used in the building materials fields such as dry-mixed mortar, ceramic tile are bonding, putty paste, waterproofing slurry.
Embodiment
Below by embodiment, the present invention is described in further detail, but this should be interpreted as to scope of the present invention only limits to following example.In the situation that do not break away from aforesaid method thought of the present invention, various replacements or the change according to ordinary skill knowledge and customary means, made, all should be within the scope of the present invention.
embodiment 1
1) 50 parts of ethylene-vinyl acetate copolymerization rubber powders, 40 parts of amorphous yam starchs, 0.005 part of BPO peroxy initiator are poured in ribbon mixer and mixed 4min, send into rod mill after mixing, the rotating speed of rod mill is controlled 160r/min, rod milling time 18min, ethene rubber powder active group under the strong shearing action of rod mill is caused by initiator, with the active group generation graft copolymerization of amorphous starch, forms backbone;
2) 5 parts of acrylamides, 1 part of sodium sulfate, 2 parts of zinc sulfate are added to step 1), rod milling again, the rotating speed of rod mill is controlled at 110r/min, the rod milling time is controlled at 10min, under mechanical force, in toughner, contained amide group is ripened the agent cross-linking curing, and with the activity hydroxy generation condensation reaction of amorphous starch, further form backbone;
3) by step 2) the rod milling material that obtains puts into high mixer, and obtains a kind of water-soluble good Redispersible Polymeric Emulsion Powder after 3 parts of Starsos mix in high mixer.
The Redispersible Polymeric Emulsion Powder obtained, for the ceramic wall and floor bricks tackiness agent, has good bonding energy, water tolerance.Get the redispersable latex powder 7kg of gained, with the general silicate cement of 400kg PO42.5,593kg fineness, be that 50～100 purpose quartz sands mix, according to water cement ratio, about 1:4 stirs modulation, establishing criteria JC/T547-2005 " ceramic wall and floor bricks tackiness agent " is for the bonding test of ceramic tile, and its performance reaches the strong index.Concrete detected result is as follows:
| Interventions Requested | Unit | Standard-required (strong C2) | The present embodiment test result |
| Gluing former intensity stretches | Mpa | ≥1.0 | 4.5 |
| Stretching adhesive strength after immersion | Mpa | ≥1.0 | 4.4 |
| Tensile strength after thermal ageing | Mpa | ≥1.0 | 4.2 |
| Stretching adhesive strength after freeze-thaw cycle | Mpa | ≥1.0 | 4.1 |
embodiment 2
1) 50 parts of ethylene-vinyl acetate copolymerization rubber powders, 45 parts of amorphous yam starchs, 0.007 part of BPO peroxy initiator are poured in ribbon mixer and mixed 5min, send into rod mill after stirring, the rotating speed of rod mill is controlled 200r/min, rod milling time 20min, ethene rubber powder active group under the strong shearing action of rod mill is caused by initiator, with the active group generation graft copolymerization of amorphous starch, forms backbone;
2) 5 parts of urea, 3 parts of acrylamides, 1 part of sodium sulfate, 1 part of zinc sulfate are added to step 1), rod milling again, the rotating speed of rod mill is controlled at 150r/min, the rod milling time is controlled at 15min, under mechanical force, in toughner, contained amide group is ripened the agent cross-linking curing, and with the activity hydroxy generation condensation reaction of amorphous starch, further form backbone;
3) by step 2) the rod milling material that obtains puts into high mixer, with 1 part of sodium methyl silicate, 2 parts of potassium silicates, obtains a kind of water-soluble good Redispersible Polymeric Emulsion Powder after mixing in high mixer.
The redispersable latex powder obtained, for exterior coating, have good water tolerance, film-forming properties, cementability.According to GB/T9755-2001 " exterior wall coating material of synthetic resin emulsion " requirement, test its specific targets as follows:
| Project | Standard-required | Originally execute the example test result |
| Application property | Brush accessible | Brush accessible |
| Appearance of film | Normally | Normally |
| Low-temperature stability | Never degenerate | Never degenerate |
| Time of drying (surface drying)/h | ≤2 | 1.0 |
| Water tolerance | 96 hours without abnormal | 240 hours without abnormal |
| Alkali resistance (48h) | Without abnormal | Without abnormal |
| Artificial ageing resistance | 600h is non-foaming, do not peel off, flawless | 1000h is non-foaming, do not peel off, flawless |
embodiment 3
1) 25 parts of ethylene-vinyl acetate copolymerization rubber powders, 25 parts of vinyl acetate copolymerized rubber powders, 40 parts of amorphous yam starchs, 0.008 part of BPO peroxy initiator are poured in ribbon mixer and mixed 4min, send into rod mill after mixing, the rotating speed of rod mill is controlled 160r/min, rod milling time 18min, ethene rubber powder active group under the strong shearing action of rod mill is caused by initiator, with the active group generation graft copolymerization of amorphous starch, forms backbone;
2) 2 parts of urea, 3 parts of 2-acrylamide-2-methylpro panesulfonic acids, 2 parts of sodium sulfate, 1 part of ammonium sulfate are added to step 1), rod milling again, the rotating speed of rod mill is controlled at 180r/min, the rod milling time is controlled at 13min, under mechanical force, in toughner, contained amide group is ripened the agent cross-linking curing, and with the activity hydroxy generation condensation reaction of amorphous starch, form backbone;
3) by step 2) the rod milling material that obtains puts into high mixer, with 2 parts of sodium methyl silicates, 3 parts of potassium silicates, obtains a kind of water-soluble good Redispersible Polymeric Emulsion Powder after high mixer mixes.
The Redispersible Polymeric Emulsion Powder obtained can significantly promote water-retentivity, workability, the plasticity of mortar, and 1% addition water-reducing rate surpasses 25%, and its fundamental property detected result is as follows:
| Interventions Requested | Unit | The present embodiment test result |
| Outward appearance | -- | But white free flowing powder |
| Solid content | % | 98.5 |
| PH value | ? | 6-8 |
| Minimum film-forming temperature | ℃ | -5 |
embodiment 4
1) 22 parts of ethylene-vinyl acetate copolymerization rubber powders, 23 parts of vinyl acetate copolymerized rubber powders, 45 parts of amorphous yam starchs, 0.01 part of BPO peroxy initiator are poured in ribbon mixer and mixed 4min, send into rod mill after mixing, the rotating speed of rod mill is controlled 190r/min, rod milling time 20min, ethene rubber powder active group under the strong shearing action of rod mill is caused by initiator, with the active group generation graft copolymerization of amorphous starch, forms backbone;
2) 3 parts of acrylamides, 2 parts of 2-acrylamide-2-methylpro panesulfonic acids, 1 part of sodium sulfate, 1 part of ammonium sulfate are added to step 1), rod milling again, the rotating speed of rod mill is controlled at 130r/min, the rod milling time is controlled at 17min, under mechanical force, in toughner, contained amide group is ripened the agent cross-linking curing, and with the activity hydroxy generation condensation reaction of amorphous starch, further form backbone;
3) by step 2) the rod milling material that obtains puts into high mixer, with 2 parts of sodium methyl silicates, 2 parts of potassium silicates, obtains a kind of water-soluble good Redispersible Polymeric Emulsion Powder after mixing in high mixer.
The redispersable latex powder obtained, for interior wall coating, has excellent over-all properties.According to the interior wall primer requirement of GB/T9756-2009 " resin latex dope ", test its specific targets as following table:
| Project | Standard-required | Originally execute the example test result |
| Application property | Brush accessible | Brush accessible |
| Appearance of film | Normally | Normally |
| Low-temperature stability (3 circulations) | Never degenerate | Never degenerate |
| Time of drying (surface drying)/h | ≤2 | 1.1 |
| Alkali burnout resistance (48h) | Without abnormal | Without abnormal |
| Alkali resistance (24h) | Without abnormal | Without abnormal |
Claims (7)
1. a Redispersible Polymeric Emulsion Powder is characterized in that parts by weight of raw materials is composed as follows:
45～55 parts of ethene rubber powders,
35～45 parts of amorphous starch,
5～10 parts of toughner,
1～4 part of ripening agent,
3～5 parts of crystallizing agents,
0.005～0.01 part of initiator,
Wherein, described ethene rubber powder is the powdery, water-soluble rubber powder, and commonly used have at least one in ethylene-vinyl acetate copolymerization rubber powder, vinyl acetate copolymerized rubber powder; Described amorphous starch is 100～200 purpose amorphous structure granular starchs; Described toughner is acid amides and derivative thereof; Described ripening agent is at least one in sodium sulfate, zinc sulfate, ammonium sulfate, potassium alum; Described crystallizing agent is the salt that contains the free silica acid group; Described initiator is the BPO peroxy initiator.
2. a kind of Redispersible Polymeric Emulsion Powder according to claim 1, it is characterized in that described amorphous starch crystals degree≤5%, have a large amount of living radicals on starch chain, and internal structure is loose, there is good reactive behavior, preferably the amorphous yam starch.
3. a kind of Redispersible Polymeric Emulsion Powder according to claim 1, is characterized in that described toughner is at least one in urea, acrylamide, 2-acrylamide-2-methylpro panesulfonic acid.
4. a kind of Redispersible Polymeric Emulsion Powder according to claim 1, is characterized in that described crystallizing agent is at least one in sodium methyl silicate, Starso, potassium silicate.
5. according to the described a kind of Redispersible Polymeric Emulsion Powder of claim 1～4, it is characterized in that the preparation method is reaction preparation under the dry powder condition, concrete preparation process is as follows:
1) 45～55 parts by weight of ethylene rubber powders, 35～45 weight part amorphous starch, 0.005～0.01 part of weight initiator are poured in ribbon mixer and mixed 3～5min, send into rod mill after mixing, the rotating speed of rod mill is controlled at 150～250r/min, the rod milling time is controlled at 15～25min, ethene rubber powder active group under the strong shearing action of rod mill is caused by initiator, with the active group generation graft copolymerization of amorphous starch, forms backbone;
2) 5～10 weight part toughner, 1～4 weight part ripening agent are added in step 1), rod milling again, the rotating speed of rod mill is controlled at 100～200r/min, the rod milling time is controlled at 10～20min, under the mechanical force and chemical effect, in toughner, contained amide group is ripened the agent cross-linking curing, and with the activity hydroxy generation condensation reaction of amorphous starch, further form backbone, significantly improve the bonding strength after film forming;
3) by step 2) the rod milling material that obtains puts into high mixer, and obtains a kind of Redispersible Polymeric Emulsion Powder after 3～5 weight part crystallizing agents mix in high mixer.
6. as the preparation method of claim 5 Redispersible Polymeric Emulsion Powder, it is characterized in that the described ribbon mixer of step 1), by U-shaped container, double-deck ribbon agitating vane, formed, the long body tube structure of U-shaped, guaranteed the slight drag campaign in cylindrical shell of mixed material, under the effect of double-deck ribbon agitating vane, make material form more eddy current in flowing, make to mix more even.
7. as the preparation method of claim 5 Redispersible Polymeric Emulsion Powder, it is characterized in that the described rod mill of step 1) is the stirring-type rod mill, comprise cylindrical shell and stirring rod, its technical characteristics is to be provided with 6 groups of rotatable stirring rod in cylindrical shell, stirring rod is fixed on cylindrical shell two end axles end surface, and during rotation, stirring rod is ground with the cylinder face.
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| CN107603521A (en) * | 2017-10-27 | 2018-01-19 | 桂林市漓江机电制造有限公司 | A kind of non-cement-based tile adhesives of anti-formaldehyde |
| CN108395809A (en) * | 2018-03-21 | 2018-08-14 | 合肥广民建材有限公司 | A kind of indoor wall environment-friendly waterproof paint and preparation method thereof |
| WO2021239234A1 (en) * | 2020-05-28 | 2021-12-02 | Wacker Chemie Ag | Process for preparing water-redispersible polymer powders for dry formulations of construction materials |
| CN114045083A (en) * | 2021-11-29 | 2022-02-15 | 山东贝壳防水科技有限公司 | Method for manufacturing waterproof and moistureproof material for underground space |
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Effective date of registration: 20201109 Address after: Room 509, building 2, No.96, banhe Road, Huangpu District, Guangzhou City, Guangdong Province Patentee after: Guangzhou jiantubao building materials Co.,Ltd. Address before: 313000, No. 2599, weaving Avenue, Wuxing District, Zhejiang, Huzhou Patentee before: ZHEJIANG DADONGWU GROUP CONSTRUCTION OF THE NEW MATERIAL Ltd. |
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