CN101649017A - Polyacrylic ester thickener and preparation method thereof - Google Patents
Polyacrylic ester thickener and preparation method thereof Download PDFInfo
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- CN101649017A CN101649017A CN200910186072A CN200910186072A CN101649017A CN 101649017 A CN101649017 A CN 101649017A CN 200910186072 A CN200910186072 A CN 200910186072A CN 200910186072 A CN200910186072 A CN 200910186072A CN 101649017 A CN101649017 A CN 101649017A
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Abstract
The invention relates to a polyacrylic ester thickener and a preparation method thereof, in particular to a thickener used for the cloth edge coating adhesive of a loudspeaker chassis and a preparation method thereof. The polyacrylic ester thickener is prepared from the following raw materials in the proportion by weight through emulsion polymerization: 0.3-3.0 sodium dodecyl sulfate, 0.3-6.0 alkylphenol polyoxyethylene, 5.0-30.0 methacrylic acid, 5.0-30.0 ethyl acrylate, 0.5-5.0 N-methacrylamide, 0.5-5.0 synergistic agent, 0.1-5.0 ammonium persulfate and the balance of deionized water. The invention has the advantages that the thickener and the water-based polyacrylic ester fabric coating adhesive are matched in use for preparing the cloth edge of the loudspeaker chassis, thereby avoidingthe phenomenon of glue penetration of the cloth, beatifying the appearance of the product and improving the quality of the product.
Description
Technical field
The present invention relates to a kind of Polyacrylate thickeners and preparation method thereof.
Background technology
The application of esters of acrylic acid thickening material at present is more extensive, because its structure is various, wide in variety, can satisfy the requirement of various rheological properties, thereby development is very swift and violent.
The monomer that the acrylic acid synthesizing ester thickener is commonly used has: vinylformic acid, methacrylic acid, ethyl propenoate, butyl acrylate, acrylate long-chain ester, acrylamide, toxilic acid, maleic anhydride etc.Acid monomer with in the alkali and after can improve the viscosity of system, esters monomer is then given multipolymer with flexibility.Long-chain ester such as vinylformic acid 12, stearyl make to produce intermolecular association between macromolecular chain owing to the effect of hydrophobic grouping is assembled, and increase hydrodynamic volume, thereby increase the viscosity of system.
General letex polymerization and the reversed emulsion polymerization of adopting prepares, and the product that obtains is mobile emulsion or powder-product.Inverse emulsion polymerization needs to add a large amount of organic solvent and auxiliary agent in preparation process, and complex process has pollution to environment.With the thickening material product that traditional emulsion polymerisation process obtains under acidic conditions, the oneself viscosity of this series products is low, and thickening capabilities is still very strong, good stability, is difficult for characteristics such as mildew, can replace natural thickener.
The sound basin selvedge of loud speaker adopts polyacrylate dispersion as coating glue, in the coating process, acrylate textile adhesive coating is regulated viscosity to 25000mPaS with ammoniacal liquor, on base cloth, directly be coated with the scraper type coating machine, be coated with 4~6 layers by actual needs, the frictioning amount is 60~75g/m
2, dry naturally or 140 ℃ of oven dry.Adopt conventional acrylate thickening material, after coating is dried or is dried, the latex of coating can be penetrated into the back side of coating, form graniphyric glue stain, influenced on the one hand attractive in appearance as the product of loudspeaker cone selvedge, on the other hand, also may will influence the audio frequency resonant frequency of loud speaker, thereby can't obtain higher tonequality output.Study a kind of good thickening capabilities that has, simultaneously the thickening material that protects the glue ability is preferably arranged again, after drying after the coating or drying, the latex of coating can not be penetrated into the back side of coating, quality product, lifting product specification to improving sound basin selvedge have great importance.
Summary of the invention
The object of the present invention is to provide a kind of Polyacrylate thickeners and preparation method thereof, thickening material and water polyacrylic acid WP are used in this method, be used to prepare the loudspeaker cone selvedge, cloth the seep through phenomenon can not occur, and the back side that the latex of coating can not be penetrated into coating forms graniphyric glue stain.
Principle of the present invention is: acrylate and methacrylic acid are when copolyreaction, different at oil phase (being the monomer phase) with the partition ratio of aqueous phase, therefore, in emulsion polymerization systems, when methacrylic acid and acrylic ester copolymer, methacrylic acid is 2.34 at the partition ratio of monomer in mutually; When vinylformic acid and acrylic ester copolymer, partition ratio then is 1.10.That is to say, in the emulsion system of acrylic acid copolymer gained, there is more vinylformic acid homogeneous phase thing to stay in water, and the carboxyl in the copolymer emulsion particle is distributed on polymer particle and the aqueous phase interface morely, the emulsion of methacrylic acid is then opposite, carboxyl can enter in the emulsion copolymer grain morely, and the distribution in macromolecular chain is more even than acrylic acid.The water retention capacity of latex after to polymer beads suction in the infiltration situation of coating medium and the thickening material is relevant, promptly relevant with the character of water in polymer beads.The moisture content that general water-absorbing polymer absorbs can be divided into normal water and improper water, improper water combines with polymer beads and must compare firmly, but this part water-content is less, and normal water is under the wicking action of fabric, be easy to water-free part infiltration, thereby form the cloth phenomenon.The effective ways that reduce infiltration are to make the seepage water pressure of the water that contains in the polymer beads greater than the capillary force to fabric that water is oozed out from polymer beads.Analyze thus, add or do not add linking agent during polymerization less, or improve polymerization temperature, increase chain transfer, reduce polymericular weight, increase the content of soluble polymer in the polymer beads, all will improve the impermeabilisation ability of polymkeric substance.High temperature polymerization is more effective to the imperviousization ability that improves polymkeric substance, and this is that chain transfer increases because during high temperature polymerization, and the mole number of polymkeric substance increases, and joins the cause that slurry back seepage water pressure increases.Suitably reduce the consumption of cross-linking monomer, improve polymerization temperature, can polymer concentration and the relation curve of thickening viscosity become gently, help the raising of polymerisate permeability resistance.In addition, the monomer of some band sulfonic acid groups particularly with the vinyl monomer of sulfonic acid group, has good complexing, adsorptivity and surfactivity.
The present invention is achieved like this, and a kind of Polyacrylate thickeners is characterized in that, the material component weight percent is:
Sodium lauryl sulphate 0.3~3.0%
Alkylphenol polyoxyethylene 0.3~6.0%
Methacrylic acid 5.0~30.0%
Ethyl propenoate 5.0~30.0%
N methacrylamide 0.5~5.0%
Synergistic agent 0.5~5.0%
Ammonium persulphate 0.1~5.0%
The deionized water surplus.
Synergistic agent of the present invention is the monomer of band sulfonic acid group.
Synergistic agent of the present invention is the monomer of band vinyl.
Synergistic agent of the present invention is selected from one or more the mixture in sodium vinyl sulfonate, sodium allylsulfonate, sodium allyl sulfonate, the 2-acrylamide-2-methyl propane sulfonic acid monomer.
A kind of preparation method of Polyacrylate thickeners is characterized in that, concrete steps are:
(1) aqueous solution of adding compound emulsifying agent in reactor, its weight percentages: sodium lauryl sulphate 0.3~3.0%, alkylphenol polyoxyethylene 3.0~6.0%, deionized water 20~40% stirs;
(2) monomer mixture of adding 1/5, mixture is initiator+synergistic agent+N methacrylamide mixed aqueous solution, its weight percentages: methacrylic acid 5.0~30.0%, ethyl propenoate 5.0~30.0%, ammonium persulphate 0.1~5.0%, synergistic agent 0.5~5.0%, N methacrylamide 0.5~5.0%, deionized water 20~40 is warming up to 50~75 ℃, insulation 10~60min;
(3) be warmed up to 75~95 ℃, drip remaining initiator solution and monomer mixed solution simultaneously, and keep constant speed to drip, added in 0.5~2.5 hour, afterwards, 80~115 ℃ of insulation 0.5~2.5h cool to 35~45 ℃, filter, discharging promptly obtains Polyacrylate thickeners.
Advantage of the present invention is: the present invention utilizes this thickening material and water polyacrylic acid WP to be used, when this polyacrylate polymers adds the alkali thickening, the rapid swelling of its molecule, negatively charged ion along the multipolymer macromolecular chain produces the Coulomb repulsion effect, make the rapid expansion of multipolymer macromolecular chain and extend, self molecular volume increases manyfold rapidly, the sterically hindered increase of molecular motion, molecule free movement space and amplitude reduce greatly, and its macroscopical physical phenomenon is exactly that viscosity increases rapidly.Simultaneously,, make it have high viscosity constraint, free water molecule is reduced greatly owing to have a certain amount of sulfonic acid group, particularly vinyl sulfonic acid group.On application performance, show as its protect viscosity can with the raising of water retention property, have very high structural viscosity as the acrylic polymer of thickening material, thereby make it have good thickening capabilities and viscosity constraint ability.
Thickening material of the present invention and water polyacrylic acid WP are used, be used to prepare the loudspeaker cone selvedge, cloth the seep through phenomenon can not occur, the back side that the latex of coating can not be penetrated into coating forms graniphyric glue stain, improved on the one hand product attractive in appearance of loudspeaker cone selvedge, on the other hand, also will reduce disadvantageous effect, thereby obtain higher tonequality output the audio frequency resonant frequency of loud speaker.
Embodiment
The embodiment of a kind of Polyacrylate thickeners of the present invention and preparation method thereof below is provided.
Embodiment 1
(1) weight proportion of material component is: %
Sodium lauryl sulphate 0.3
Alkylphenol polyoxyethylene 0.5
Methacrylic acid 12
Ethyl propenoate 18
N methacrylamide 0.5
Synergistic agent 0.5
Ammonium persulphate 0.6
Deionized water 67.6
Synergy wherein is sodium vinyl sulfonate.
(2) preparation method is:
(1) in reactor by weight formula ratio add the aqueous solution of compound emulsifying agent: sodium lauryl sulphate 0.3, alkylphenol polyoxyethylene 0.6, deionized water 30 stirs;
(2) monomer mixture of adding 1/5: methacrylic acid 12, ethyl propenoate 18,1/5 (initiator+synergistic agent+N methacrylamide) mixed aqueous solution: ammonium persulphate 0.6, synergistic agent 0.5, N methacrylamide 0.5, deionized water surplus, be warming up to 65 ℃, insulation 20min;
(3) be warmed up to 85 ℃, drip remaining initiator solution and monomer mixed solution simultaneously, and keep constant speed to drip, added in 0.5 hour, afterwards, 95 ℃ of insulation 0.5h cool to 45 ℃, filter discharging.
Embodiment 2
(1) weight proportion of material component is: %
Sodium lauryl sulphate 0.3
Alkylphenol polyoxyethylene 0.5
Methacrylic acid 8
Ethyl propenoate 22
N methacrylamide 0.8
Synergistic agent 2.5
Ammonium persulphate 0.5
Deionized water 65.4
Synergy wherein is the propenyl sodium sulfonate.
(2) preparation method is:
(1) in reactor by weight formula ratio add the aqueous solution of compound emulsifying agent: sodium lauryl sulphate 0.3, alkylphenol polyoxyethylene 0.5, deionized water 30 stirs;
(2) monomer mixture of adding 1/5: methacrylic acid 8, ethyl propenoate 22,1/5 (initiator+synergistic agent+N methacrylamide) mixed aqueous solution: ammonium persulphate 0.5, synergistic agent 2.5, N methacrylamide 0.8, deionized water surplus, be warming up to 75 ℃, insulation 40min;
(3) be warmed up to 80 ℃, drip remaining initiator solution and monomer mixed solution simultaneously, and keep constant speed to drip, added in 1 hour, afterwards, 95 ℃ of insulation 1h cool to 40 ℃, filter discharging.
Embodiment 3
(1) weight proportion of material component is: %
Sodium lauryl sulphate 0.3
Alkylphenol polyoxyethylene 0.5
Methacrylic acid 10
Ethyl propenoate 20
N methacrylamide 2.8
Synergistic agent 4.5
Ammonium persulphate 0.5
Deionized water 61.4
Synergy wherein is 2-acrylamide-2-methyl propane sulfonic acid.
(2) preparation method is:
(1) in reactor by weight formula ratio add the aqueous solution of compound emulsifying agent: sodium lauryl sulphate 0.3, alkylphenol polyoxyethylene 0.5, deionized water 30 stirs;
(2) monomer mixture of adding 1/5: methacrylic acid 10, ethyl propenoate 20,1/5 (initiator+synergistic agent+N methacrylamide) mixed aqueous solution: ammonium persulphate 0.5, synergistic agent 4.5, N methacrylamide 2.8, deionized water surplus, be warming up to 80 ℃, insulation 30min;
(3) be warmed up to 85 ℃, drip remaining initiator solution and monomer mixed solution simultaneously, and keep constant speed to drip, added in 1.5 hours, afterwards, 95 ℃ of insulation 1.5h cool to 40 ℃, filter discharging.
Embodiment 4
(1) weight proportion of material component is: %
Sodium lauryl sulphate 0.3
Alkylphenol polyoxyethylene 0.5
Methacrylic acid 10
Ethyl propenoate 20
N methacrylamide 2.8
Synergistic agent 4.5
Ammonium persulphate 0.5
Deionized water 61.4
Synergy wherein is sodium vinyl sulfonate 1.5 and 2-acrylamide-2-methyl propane sulfonic acid 3.0.
(2) preparation method is:
With embodiment 3.
Performance test
The present invention is by following performance comparison test: get acrylate textile adhesive coating, add 5% acrylate thickening material, the ammoniacal liquor with 25% is regulated viscosity to 25000mPaS, directly is coated with the scraper type coating machine on base cloth, be coated with 6 layers by actual needs, the frictioning amount is 60~75g/m
2, dry naturally.Select one group of domestic like product thickening material that generally uses else, select the cloth of same material for use, and adopt identical impregnation prescription,, prepare sound basin selvedge raw material, dry naturally by same frictioning amount and frictioning mode.
The result shows, utilizes the loudspeaker cone selvedge of the synthetic WP preparation of acrylate thickening material of the present invention, does not have the strike-through phenomenon.
The above only is a preferred implementation of the present invention; should be pointed out that for those skilled in the art, without departing from the inventive concept of the premise; can also make some improvements and modifications, these improvements and modifications also should be considered within the scope of protection of the present invention.
The embodiment of a kind of Polyacrylate thickeners of the present invention and preparation method thereof below is provided.
Embodiment 1
(1) weight proportion of material component is: %
Sodium lauryl sulphate 0.3
Alkylphenol polyoxyethylene 0.5
Methacrylic acid 12
Ethyl propenoate 18
N methacrylamide 0.5
Synergistic agent 0.5
Ammonium persulphate 0.6
Deionized water 67.6
Synergy wherein is sodium vinyl sulfonate.
(2) preparation method is:
(1) in reactor by weight formula ratio add the aqueous solution of compound emulsifying agent: sodium lauryl sulphate 0.3, alkylphenol polyoxyethylene 0.6, deionized water 30 stirs;
(2) monomer mixture of adding 1/5: methacrylic acid 12, ethyl propenoate 18,1/5 (initiator+synergistic agent+N methacrylamide) mixed aqueous solution: ammonium persulphate 0.6, synergistic agent 0.5, N methacrylamide 0.5, deionized water surplus, be warming up to 65 ℃, insulation 20min;
(3) be warmed up to 85 ℃, drip remaining initiator solution and monomer mixed solution simultaneously, and keep constant speed to drip, added in 0.5 hour, afterwards, 95 ℃ of insulation 0.5h cool to 45 ℃, filter discharging.
Embodiment 2
(1) weight proportion of material component is: %
Sodium lauryl sulphate 0.3
Alkylphenol polyoxyethylene 0.5
Methacrylic acid 8
Ethyl propenoate 22
N methacrylamide 0.8
Synergistic agent 2.5
Ammonium persulphate 0.5
Deionized water 65.4
Synergy wherein is the propenyl sodium sulfonate.
(2) preparation method is:
(1) in reactor by weight formula ratio add the aqueous solution of compound emulsifying agent: sodium lauryl sulphate 0.3, alkylphenol polyoxyethylene 0.5, deionized water 30 stirs;
(2) monomer mixture of adding 1/5: methacrylic acid 8, ethyl propenoate 22,1/5 (initiator+synergistic agent+N methacrylamide) mixed aqueous solution: ammonium persulphate 0.5, synergistic agent 2.5, N methacrylamide 0.8, deionized water surplus, be warming up to 75 ℃, insulation 40min;
(3) be warmed up to 80 ℃, drip remaining initiator solution and monomer mixed solution simultaneously, and keep constant speed to drip, added in 1 hour, afterwards, 95 ℃ of insulation 1h cool to 40 ℃, filter discharging.
Embodiment 3
(1) weight proportion of material component is: %
Sodium lauryl sulphate 0.3
Alkylphenol polyoxyethylene 0.5
Methacrylic acid 10
Ethyl propenoate 20
N methacrylamide 2.8
Synergistic agent 4.5
Ammonium persulphate 0.5
Deionized water 61.4
Synergy wherein is 2-acrylamide-2-methyl propane sulfonic acid.
(2) preparation method is:
(1) in reactor by weight formula ratio add the aqueous solution of compound emulsifying agent: sodium lauryl sulphate 0.3, alkylphenol polyoxyethylene 0.5, deionized water 30 stirs;
(2) monomer mixture of adding 1/5: methacrylic acid 10, ethyl propenoate 20,1/5 (initiator+synergistic agent+N methacrylamide) mixed aqueous solution: ammonium persulphate 0.5, synergistic agent 4.5, N methacrylamide 2.8, deionized water surplus, be warming up to 80 ℃, insulation 30min;
(3) be warmed up to 85 ℃, drip remaining initiator solution and monomer mixed solution simultaneously, and keep constant speed to drip, added in 1.5 hours, afterwards, 95 ℃ of insulation 1.5h cool to 40 ℃, filter discharging.
Embodiment 4
(1) weight proportion of material component is: %
Sodium lauryl sulphate 0.3
Alkylphenol polyoxyethylene 0.5
Methacrylic acid 10
Ethyl propenoate 20
N methacrylamide 2.8
Synergistic agent 4.5
Ammonium persulphate 0.5
Deionized water 61.4
Synergy wherein is sodium vinyl sulfonate 1.5 and 2-acrylamide-2-methyl propane sulfonic acid 3.0.
(2) preparation method is:
With embodiment 3.
Performance test
The present invention is by following performance comparison test: get acrylate textile adhesive coating, add 5% acrylate thickening material, the ammoniacal liquor with 25% is regulated viscosity to 25000mPaS, directly is coated with the scraper type coating machine on base cloth, be coated with 6 layers by actual needs, the frictioning amount is 60~75g/m
2, dry naturally.Select one group of domestic like product thickening material that generally uses else, select the cloth of same material for use, and adopt identical impregnation prescription,, prepare sound basin selvedge raw material, dry naturally by same frictioning amount and frictioning mode.
The result shows, utilizes the loudspeaker cone selvedge of the synthetic WP preparation of acrylate thickening material of the present invention, does not have the strike-through phenomenon.
The above only is a preferred implementation of the present invention; should be pointed out that for those skilled in the art, without departing from the inventive concept of the premise; can also make some improvements and modifications, these improvements and modifications also should be considered within the scope of protection of the present invention.
Claims (5)
1, a kind of Polyacrylate thickeners is characterized in that, the material component weight percent is:
Sodium lauryl sulphate 0.3~3.0%
Alkylphenol polyoxyethylene 0.3~6.0%
Methacrylic acid 5.0~30.0%
Ethyl propenoate 5.0~30.0%
N methacrylamide 0.5~5.0%
Synergistic agent 0.5~5.0%
Ammonium persulphate 0.1~5.0%
The deionized water surplus.
2. a kind of Polyacrylate thickeners as claimed in claim 1 is characterized in that, described synergistic agent is the monomer of band sulfonic acid group.
3. a kind of Polyacrylate thickeners as claimed in claim 1 is characterized in that, described synergistic agent is the monomer of band vinyl.
4. a kind of Polyacrylate thickeners as claimed in claim 1, it is characterized in that described synergistic agent is selected from one or more the mixture in sodium vinyl sulfonate, sodium allylsulfonate, sodium allyl sulfonate, the 2-acrylamide-2-methyl propane sulfonic acid monomer.
5. the preparation method of the described a kind of Polyacrylate thickeners of claim 1 is characterized in that, concrete steps are:
(1) aqueous solution of adding compound emulsifying agent in reactor, its weight percentages: sodium lauryl sulphate 0.3~3.0%, alkylphenol polyoxyethylene 3.0~6.0%, deionized water 20~40% stirs;
(2) monomer mixture of adding 1/5, mixture is initiator+synergistic agent+N methacrylamide mixed aqueous solution, its weight percentages: methacrylic acid 5.0~30.0%, ethyl propenoate 5.0~30.0%, ammonium persulphate 0.1~5.0%, synergistic agent 0.5~5.0%, N methacrylamide 0.5~5.0%, deionized water 20~40 is warming up to 50~75 ℃, insulation 10~60min;
(3) be warmed up to 75~95 ℃, drip remaining initiator solution and monomer mixed solution simultaneously, and keep constant speed to drip, added in 0.5~2.5 hour, afterwards, 80~115 ℃ of insulation 0.5~2.5h cool to 35~45 ℃, filter, discharging promptly obtains Polyacrylate thickeners.
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Cited By (9)
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CN102399351A (en) * | 2010-11-19 | 2012-04-04 | 苏州博纳化学科技有限公司 | Preparation method of emulsion-type thickening agent |
CN102504089A (en) * | 2011-09-28 | 2012-06-20 | 贵州大学 | Preparation method of water-resistant acrylic ester core-shell emulsion |
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2009
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CN102399351A (en) * | 2010-11-19 | 2012-04-04 | 苏州博纳化学科技有限公司 | Preparation method of emulsion-type thickening agent |
CN102504089A (en) * | 2011-09-28 | 2012-06-20 | 贵州大学 | Preparation method of water-resistant acrylic ester core-shell emulsion |
CN102504089B (en) * | 2011-09-28 | 2013-12-25 | 贵州大学 | Preparation method of water-resistant acrylic ester core-shell emulsion |
CN102504078A (en) * | 2011-10-16 | 2012-06-20 | 浙江精业生化有限公司 | Method for preparing electrolyte-resisting thickening agent |
CN102504078B (en) * | 2011-10-16 | 2013-12-18 | 绍兴县震东化工有限公司 | Method for preparing electrolyte-resisting thickening agent |
CN102533176A (en) * | 2011-12-26 | 2012-07-04 | 北京高盟新材料股份有限公司 | Waterborne gravure paper-plastic composite adhesive and preparation method thereof |
CN103788283A (en) * | 2014-01-17 | 2014-05-14 | 广州市东雄化工有限公司 | Hydrophobic modified associative thickener and preparation method thereof |
CN103788283B (en) * | 2014-01-17 | 2016-01-20 | 广州市东雄化工有限公司 | A kind of hydrophobically modified associative thickener and preparation method thereof |
CN104877455A (en) * | 2014-02-27 | 2015-09-02 | 真彩文具股份有限公司 | A low-viscosity antibacterial gel-ink thickening agent and a preparing method thereof |
CN108221459A (en) * | 2017-12-30 | 2018-06-29 | 常州思宇环保材料科技有限公司 | A kind of preparation method of glassine paper |
CN109797576A (en) * | 2019-01-08 | 2019-05-24 | 青岛明月海藻集团有限公司 | A kind of penetration printing thickener and preparation method thereof |
CN109797576B (en) * | 2019-01-08 | 2021-07-30 | 青岛明月海藻集团有限公司 | Penetrating printing paste and preparation method thereof |
CN111961212A (en) * | 2020-08-28 | 2020-11-20 | 浙江九本环保技术有限公司 | Novel rheological thickening water-retaining agent for papermaking, preparation method and application |
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