CN111318228B - Preparation method of in-situ polymerization solid dispersant - Google Patents
Preparation method of in-situ polymerization solid dispersant Download PDFInfo
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Abstract
The invention discloses a preparation method of an in-situ polymerization solid dispersant, which comprises the following steps: premixing a (methyl) acrylate aqueous solution, maleic anhydride, an allyl polyether macromonomer and an initiator aqueous solution; spraying and adsorbing the carrier powder; aging for 2-4 hours; carrying out polymerization reaction; vacuumizing for 0.5-1 hour at 95-100 ℃; cooling to below 40 deg.C, detecting, pulverizing, sieving, and discharging. The preparation method of the invention adopts the process of pre-neutralization and in-situ polymerization, thus solving the problems of uniformity of physical mixing structure of the solid dispersant and difficult dissolution in use; the prepared solid dispersant is a novel solid aqueous dispersant, has the characteristics of environmental protection, safety, excellent dispersion performance, stable storage, convenient transportation and the like, perfects the variety of products in the domestic market, provides a novel dispersant variety for powder auxiliary agent products, and fills the blank of in-situ polymerization solid dispersants.
Description
Technical Field
The invention belongs to the field of fine chemical engineering, and particularly relates to a preparation method of an in-situ polymerization solid dispersing agent.
Background
Due to the development of science and technology and the change of various building materials, the trend of water-based and powder-based in recent years has led the mainstream of the market, and dry-mixed mortar, dry-mixed putty and commercial concrete mostly need a solid dispersant to disperse in the production and use processes. The varieties of the dispersing agents in the current market are more, and the solid dispersing agent is mainly an inorganic dispersing agent: such as sodium hexametaphosphate, sodium tripolyphosphate, and the like; the liquid dispersant has the advantages of high performance-to-cost ratio, stable performance and the like, but is inconvenient to use in the production process, and the conventional method is to synthesize the liquid dispersant first and then prepare the solid dispersant through processes of spray drying and the like, but the method has the disadvantages of complicated manufacturing process, large equipment investment and energy consumption and slow dissolving speed in use.
Due to the increasing aggravation of environmental protection problems, people have increasingly strengthened environmental protection awareness, and auxiliaries needed in the industries of textile, leather, packaging, coating, printing ink and the like are also increasingly water-based. At present, the varieties of dispersants in the market are more, but the varieties of the carboxylic acid dispersants modified by maleic anhydride are not more, and the maleic anhydride dispersants have stronger dispersing capacity and economic price, so that the dispersant is widely applied to the aspects of slurry dispersion and water treatment, the development of the carboxylic acid dispersants modified by the maleic anhydride can perfect market products, and a novel dispersant variety is provided for aqueous auxiliary agent products.
Disclosure of Invention
The invention aims to overcome the defects, and the technical problem to be solved is to provide a preparation method of a novel solid dispersing agent, which is simple in process, easy to implement and excellent in performance.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a preparation method of an in-situ polymerization solid dispersant comprises the following steps:
(1) premixing raw materials: accurately weighing a (methyl) acrylate aqueous solution, maleic anhydride, an allyl polyether macromonomer and an initiator aqueous solution, sequentially adding the weighed materials into a dropwise adding kettle, stirring the materials for 0.5 to 1 hour at the speed of 80 to 120rpm after the addition is finished, and fully mixing the materials to obtain a standby mixed solution A;
(2) and preparing carrier powder: weighing carrier powder, sequentially adding the carrier powder into a powder mixing device at 35-50 rpm
Stirring for 0.25-1 hour at the speed of (1), and fully mixing to obtain a standby material B;
(3) and spray adsorption: dropwise adding the standby mixed solution A prepared in the step (1) into the standby material B prepared by the powder mixing equipment in the step (2) at a speed of 0.3-1%/min under the stirring of 50-100 rpm, wherein the rotating speed of the powder mixing equipment is maintained at 35-50 rpm, and the dropwise addition is completed within 3-4 hours;
(4) aging: after the dropwise adding is finished, maintaining the powder mixing equipment at the rotating speed of 15-30 rpm for 2-4 hours; and simultaneously detecting, wherein the following standards are qualified: 1. the surface of the powder equipment is not adhered; 2. all particles are uniform and have no obvious large particles; 3. the surface is not obviously wet;
(5) and (3) polymerization reaction: the powder equipment starts to heat while maintaining the rotating speed of 15-30 rpm, and when the temperature reaches 70 DEG C
Keeping the temperature for 0.5 hour, continuously raising the temperature to 75 ℃, keeping the temperature for 0.5 hour, continuously raising the temperature to 80 ℃, keeping the temperature for 0.5 hour, continuously raising the temperature to 85 ℃, keeping the temperature for 0.5 hour, raising the temperature to 90 ℃, keeping the temperature for 0.5-1.5 hours, raising the temperature to 95 ℃;
(6) and vacuumizing: vacuumizing for 0.5-1 hour at 95-100 ℃; the aim is to remove residual monomers and water which are not completely reacted;
(7) cooling to below 40 ℃, and crushing, screening and discharging after the detection is qualified to obtain the in-situ polymerization solid dispersant; the qualified indexes of the detection are as follows: the appearance is faint yellow powder, the solid content is 85% -95%, and the PH = 6.0-7.0;
wherein the weight ratio of the standby material B in the step (2) to the standby mixed liquid A in the step (1) is 30-90: 10-70 parts of;
wherein the mass ratio of the (methyl) acrylate aqueous solution to the maleic anhydride to the allyl polyether macromonomer to the initiator aqueous solution is as follows: 120-160: 15-30: 20-60: 50-100.
Wherein, the (methyl) acrylate is one or more of sodium salt, potassium salt and ammonium salt.
Further, the (meth) acrylate aqueous solution is one or two of acrylate or methacrylate aqueous solution.
Furthermore, when the (meth) acrylate aqueous solution is a mixture of acrylate and methacrylate aqueous solutions, the mass ratio is as follows: (20-90)% (10-80)%.
Still further, the mass concentration range of the (meth) acrylate aqueous solution is 60% to 70%.
Wherein the allyl polyether macromonomer is PEG series, namely methyl allyl alcohol polyoxyethylene ether, and the molecular weight of the allyl polyether macromonomer is one or more of 600-3000.
Wherein, the initiator is one or two of ammonium persulfate, potassium persulfate and sodium persulfate.
Further, when the initiator is a mixture of two kinds, the mass ratio of the two kinds is as follows: (40-90)% (10-60)%.
Furthermore, the mass concentration range of the initiator aqueous solution is 20-30%.
Wherein, the carrier is one or more of white carbon black, bentonite, calcium carbonate and wollastonite.
The polymerization reaction in the invention is an irregular copolymerization reaction, and because the product is an auxiliary product and the dosage of the product in an application formula is very small, the polymerization process of the product must have good uniformity; the reactivity of different monomers is different, particularly the polymerization activity of allyl polyether macromonomer is poor, so that the problem of reactivity ratio exists, and in order to ensure that the high molecular structure of the product has better uniformity in carrier particles, a slow dripping and double-screw mixing process is adopted, namely the dripping speed of a liquid material is controlled to be less than or equal to the adsorption speed of the liquid material and the proper rotating speed, so that the added liquid can be uniformly distributed in the particles.
Has the advantages that: the preparation method of the in-situ polymerization solid dispersant adopts the pre-neutralization and in-situ polymerization process, so that the problems of the uniformity of the physical mixing structure of the solid dispersant and the difficulty in dissolution in use are solved; the maleic anhydride- (methyl) acrylate-polyether dispersant prepared by the preparation method of the in-situ polymerization solid dispersant is a novel solid aqueous dispersant, has the characteristics of environmental protection, safety, excellent dispersing performance, stable storage, convenient transportation and the like, improves the types of products in domestic markets, provides novel dispersant varieties for powder auxiliary products, and fills the blank of the in-situ polymerization solid dispersant; the in-situ polymerization solid dispersant has the advantages of economic price, wide application range and good application prospect; the preparation method provided by the invention is simple in process and easy to realize large-scale production.
Detailed Description
Example 1:
raw materials: methacrylic acid sodium salt aqueous solution (aqueous solution having a mass concentration of 63.5%): 200g of the total weight of the mixture;
maleic anhydride: 37.5 g;
HPEG (molecular weight 2200, available from Huangma technologies, Inc., Zhejiang): 56g of the total weight of the mixture;
ammonium persulfate aqueous solution (25% by mass aqueous solution): 120g of a mixture;
white carbon black 622s (purchased from winning industry group): 412g
The process comprises the following steps:
1. premixing raw materials: accurately weighing 200g of a methacrylic acid sodium salt aqueous solution with the mass concentration of 63.5%, 37.5g of maleic anhydride, 56g of HPEG and 120g of an ammonium persulfate aqueous solution with the mass concentration of 25%, sequentially adding the weighed materials into a dropwise adding kettle, stirring the materials at the speed of 100rpm for 1 hour after the addition is finished, and fully mixing the materials to obtain a standby mixed solution A;
2. preparing carrier powder: 412g of white carbon black 622S is weighed and then added into a powder mixing device, and the mixture is stirred for 0.8 hour at the speed of 45rpm and is fully mixed to form a spare material B;
3. spray adsorption: dropwise adding the standby mixed liquor A prepared in the step (1) into the standby material B prepared by the powder mixing equipment in the step (2) at the speed of 0.3%/min under the stirring of 50rpm, keeping the rotating speed of the powder mixing equipment at 45rpm, and completing the dropwise addition, wherein the required time is about 4 hours;
4. aging: after the dropwise addition is completed, the powder mixing equipment is maintained at the rotating speed of 30rpm for about 2 hours, and meanwhile, the detection is in accordance with the qualified standard: (1) the surface of the powder equipment is not adhered; (2) all the particles are uniform and have no obvious large particles; (3) no obvious moisture on the surface;
5. polymerization reaction: the powder equipment maintains the rotating speed of 15rpm and starts to heat at the same time, when the temperature reaches 70 ℃, the temperature is kept for 0.5 hour, the temperature is continuously increased to 75 ℃, the temperature is kept for 0.5 hour, the temperature is continuously increased to 80 ℃, the temperature is kept for 0.5 hour, the temperature is continuously increased to 85 ℃, the temperature is kept for 0.5 hour, the temperature is increased to 90 ℃, and the temperature is kept for 1.5 hours when the temperature is increased to 95 ℃;
6. vacuumizing: vacuum is applied at 100 ℃ for 0.5 hour in order to remove residual monomers and water which have not reacted completely;
7. cooling to below 40 ℃, detecting to be qualified (the appearance is faint yellow powder, the solid content is 89.5%, and the PH = 6.6; is qualified), and then crushing, screening and discharging to obtain the in-situ polymerization solid dispersing agent.
Example 2:
raw materials: sodium acrylate salt aqueous solution (62.1% aqueous solution by mass): 196 g;
maleic anhydride: 48g of the total weight of the mixture;
HPEG (molecular weight 2800, available from Huangma technologies, Inc., Zhejiang): 60g of the total weight of the mixture;
sodium persulfate aqueous solution (30% by mass aqueous solution): 55g of the total weight of the mixture;
aqueous potassium persulfate solution (30% by mass aqueous solution): 65g of the total weight of the mixture;
white carbon black 517 (available from shin brightness chemical company limited, Jiangxi): 350g, calcium carbonate (1250 mesh): 102g
The process comprises the following steps:
1. premixing raw materials: accurately weighing 196g of 62.1 mass percent acrylic acid sodium salt aqueous solution, 48g of maleic anhydride, 60g of HPEG, 55g of 30 mass percent sodium persulfate aqueous solution and 65g of 30 mass percent potassium persulfate aqueous solution, sequentially adding into a dropwise adding kettle, stirring at the speed of 80rpm for 0.8 hour after the addition is finished, and fully mixing to obtain a standby mixed solution A;
2. preparing carrier powder: weighing 350g of white carbon black 517 and 102g of calcium carbonate (1250 meshes), adding the weighed materials into a powder mixing device, stirring the materials at a speed of 50rpm for 0.5 hour, and fully mixing the materials to obtain a spare material B;
3. spray adsorption: dropwise adding the standby mixed liquor A prepared in the step (1) into the standby material B prepared by the powder mixing equipment in the step (2) at a speed of 1%/min under the stirring of 100rpm, wherein the rotating speed of the powder mixing equipment is maintained at 38rpm, and the dropwise addition is completed, and the required time is about 3 hours;
4. aging: after the dripping is finished, the powder equipment maintains the rotating speed of 15rpm for about 4 hours, and meanwhile, the detection meets the qualified standard: (1) the surface of the powder equipment is not adhered; (2) all the particles are uniform and have no obvious large particles; (3) no obvious moisture on the surface;
5. polymerization reaction: the powder equipment maintains the rotating speed of 30rpm and starts to heat at the same time, when the temperature reaches 70 ℃, the temperature is kept for 0.5 hour, the temperature is continuously increased to 75 ℃, the temperature is kept for 0.5 hour, the temperature is continuously increased to 80 ℃, the temperature is kept for 0.5 hour, the temperature is continuously increased to 85 ℃, the temperature is kept for 0.5 hour, the temperature is increased to 90 ℃, and the temperature is kept for 1.5 hours when the temperature is increased to 95 ℃;
6. vacuumizing: vacuumizing for 1 hour at 95 ℃; the aim is to remove residual monomers and water which are not completely reacted;
7. cooling to below 40 ℃, detecting to be qualified (the appearance is faint yellow powder, the solid content is 91.7%, and the PH = 6.4; is qualified), and then crushing, screening and discharging to obtain the in-situ polymerization solid dispersing agent.
Example 3:
raw materials: ammonium methacrylate salt aqueous solution (aqueous solution with a mass concentration of 68.4%): 100g of the total weight of the mixture;
ammonium acrylate salt aqueous solution (aqueous solution with a mass concentration of 68.4%): 110g
Maleic anhydride: 50g of the total weight of the mixture;
HPEG (molecular weight 1100, available from Huangjiang Royal, Zhejiang Royal, Inc.: 75g of the total weight of the mixture;
ammonium persulfate aqueous solution (25% by mass aqueous solution): 150g of the total weight of the mixture;
fumed silica A200 (purchased from winning industry group): 320g, calcium carbonate (1500 mesh): 102g
The process comprises the following steps:
1. premixing raw materials: accurately weighing 100g of 68.4% methacrylic acid ammonium salt aqueous solution, 110g of 68.4% acrylic acid ammonium salt aqueous solution, 50g of maleic anhydride, 75g of HPEG and 150g of 25% ammonium persulfate aqueous solution, then sequentially adding the materials into a dropwise adding kettle, stirring the materials at the speed of 120rpm for 0.5 hour after the materials are added, and fully mixing the materials to obtain a standby mixed solution A;
2. preparing carrier powder: weighing 320g of fumed silica A200 and 102g of calcium carbonate (1500 meshes), adding the weighed materials into a powder mixing device, stirring the materials at the speed of 35rpm for 1 hour, and fully mixing the materials to obtain a spare material B;
3. spray adsorption: dropwise adding the standby mixed liquor A prepared in the step (1) into the standby material B prepared by the powder mixing equipment in the step (2) at the speed of 0.5%/min under the stirring of 80rpm, wherein the rotating speed of the powder mixing equipment is maintained at 35rpm, and the required time is about 3.75 hours;
4. aging: after the dripping is finished, the powder equipment maintains the rotating speed of 25rpm for about 2.8 hours, and meanwhile, the detection meets the qualified standard: (1) the surface of the powder equipment is not adhered; (2) all the particles are uniform and have no obvious large particles; (3) no obvious moisture on the surface;
5. polymerization reaction: the powder equipment maintains the rotating speed of 28rpm and starts heating at the same time, when the temperature reaches 70 ℃, the temperature is kept for 0.5 hour, the temperature is continuously increased to 75 ℃, the temperature is kept for 0.5 hour, the temperature is continuously increased to 80 ℃, the temperature is kept for 0.5 hour, the temperature is continuously increased to 85 ℃, the temperature is kept for 0.5 hour, the temperature is increased to 90 ℃, and the temperature is kept for 1.5 hours when the temperature is increased to 95 ℃;
6. vacuumizing: vacuumizing at 100 deg.C for 0.5 hr; the aim is to remove residual monomers and water which are not completely reacted;
7. cooling to below 40 ℃, detecting to be qualified (the appearance is faint yellow powder, the solid content is 87.6%, and the PH =6.3 is qualified), and then crushing, screening and discharging to obtain the in-situ polymerization solid dispersing agent.
Example 4:
carrying out performance test on the in-situ polymerization solid dispersant prepared in the embodiment 1-3, and meanwhile, comparing the in-situ polymerization solid dispersant with a blank sample;
200g of water were placed in 4 1000ml stainless steel tanks, of which 1 tank was a blank control (comparative),
and 3, starting stirring, respectively and sequentially adding 0.6% of the in-situ polymerization solid dispersant prepared in the examples 1-3, 200g of rutile titanium dioxide and 100g of calcium carbonate (800 meshes), stirring at the speed of 1000rpm for 1.0 hour after the addition is finished, standing for 0.5 hour, and measuring the viscosity, wherein the dispersing effect of the dispersant can be represented, and the results are as follows:
| comparative example | Example 1 | Example 2 | Example 3 | |
| Addition amount (wt%) | 0 | 0.6 | 0.6 | 0.6 |
| Viscosity (25 ℃, centipoise (cP)) | Semi-solid state, no measurement | 1090 | 620 | 750 |
The results show that the dispersant prepared by the preparation method of the in-situ polymerization solid dispersant has good dispersion effect.
Claims (9)
1. The preparation method of the in-situ polymerization solid dispersant is characterized by comprising the following steps:
(1) premixing raw materials: accurately weighing a (methyl) acrylate aqueous solution, maleic anhydride, an allyl polyether macromonomer and an initiator aqueous solution, sequentially adding the weighed materials into a dropwise adding kettle, stirring the materials for 0.5 to 1 hour at the speed of 80 to 120rpm after the addition is finished, and fully mixing the materials to obtain a standby mixed solution A;
(2) and preparing carrier powder: weighing carrier powder, sequentially adding the carrier powder into a powder mixing device at 35-50 rpm
Stirring for 0.25-1 hour at the speed of (1), and fully mixing to obtain a standby material B; the carrier is one or more of white carbon black, bentonite, calcium carbonate and wollastonite; the powder mixing equipment is double-screw mixing equipment;
(3) and spray adsorption: dropwise adding the standby mixed solution A prepared in the step (1) into the standby material B prepared by the powder mixing equipment in the step (2) at a speed of 0.3-1%/min under the stirring of 50-100 rpm, maintaining the rotating speed of the powder mixing equipment at 35-50 rpm, and completing the dropwise addition; in the dropping process, the dropping speed of the standby mixed liquid A is controlled to be less than or equal to the adsorption speed of the standby mixed liquid A;
(4) aging: after the dropwise adding is finished, maintaining the powder mixing equipment at the rotating speed of 15-30 rpm for 2-4 hours;
(5) and (3) polymerization reaction: the powder mixing equipment starts to heat while maintaining the rotating speed of 15-30 rpm, and when the temperature reaches 70 DEG C
Keeping the temperature for 0.5 hour, continuously raising the temperature to 75 ℃, keeping the temperature for 0.5 hour, continuously raising the temperature to 80 ℃, keeping the temperature for 0.5 hour, continuously raising the temperature to 85 ℃, keeping the temperature for 0.5 hour, raising the temperature to 90 ℃, keeping the temperature for 0.5-1.5 hours, raising the temperature to 95 ℃;
(6) and vacuumizing: vacuumizing for 0.5-1 hour at 95-100 ℃;
(7) cooling to below 40 ℃, and crushing, screening and discharging after the detection is qualified to obtain the in-situ polymerization solid dispersant;
wherein the weight ratio of the standby material B in the step (2) to the standby mixed liquid A in the step (1) is 30-90: 10-70;
wherein the mass ratio of the (methyl) acrylate aqueous solution to the maleic anhydride to the allyl polyether macromonomer to the initiator aqueous solution is as follows: 120-160: 15-30: 20-60: 50-100.
2. The method for preparing the in-situ polymerization solid dispersant according to claim 1, characterized in that: the (methyl) acrylate is one or more of sodium salt, potassium salt and ammonium salt.
3. The method for preparing an in-situ polymerized solid dispersant according to claim 1, wherein: the (methyl) acrylate aqueous solution is one or two of acrylate or methacrylate aqueous solution.
4. The method for preparing an in-situ polymerized solid dispersant according to claim 3, wherein: when the (meth) acrylate aqueous solution is a mixture of acrylate and methacrylate aqueous solutions, the mass ratio is as follows: (20-90)% (10-80)%.
5. The method for preparing the in-situ polymerization solid dispersant according to claim 1, characterized in that: the mass concentration range of the (methyl) acrylate aqueous solution is 60-70%.
6. The method for preparing an in-situ polymerized solid dispersant according to claim 1, wherein: the allyl polyether macromonomer is PEG series, namely methyl allyl alcohol polyoxyethylene ether, and the molecular weight of the allyl polyether macromonomer is one or more of 600-3000.
7. The method for preparing an in-situ polymerized solid dispersant according to claim 1, wherein: the initiator is one or two of ammonium persulfate, potassium persulfate and sodium persulfate.
8. The method for preparing an in-situ polymerized solid dispersant according to claim 7, wherein: when the initiator is a mixture of two types, the mass ratio of the two types is as follows: (40-90)% (10-60)%.
9. The method for preparing the in-situ polymerization solid dispersant according to claim 1, characterized in that: the mass concentration range of the initiator aqueous solution is 20-30%.
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| CN102120792A (en) * | 2010-11-19 | 2011-07-13 | 苏州博纳化学科技有限公司 | Preparation method of maleic anhydride-(meth)acrylic acid dispersant |
| WO2016118146A1 (en) * | 2015-01-22 | 2016-07-28 | Halliburton Energy Services, Inc. | Compatibilized cement composition for treatment of a subterranean formation |
| CN107344822A (en) * | 2017-06-05 | 2017-11-14 | 南宁科恺混凝土外加剂有限公司 | One kind is containing bentonitic premixing mortar water-keeping thickening material and preparation method thereof |
| CN108359062A (en) * | 2018-03-23 | 2018-08-03 | 刘翠芬 | High-adaptability type solid polycarboxylic acid water reducing agent and its bulk polymerization preparation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US20020099115A1 (en) * | 2000-11-28 | 2002-07-25 | Daisuke Shibai | Powder dispersant for hydraulic compositions |
| CN106957394A (en) * | 2017-04-18 | 2017-07-18 | 芜湖弘马新材料有限公司 | A kind of polycarboxylic-acid hyper-dispersant and its preparation method and application |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102120792A (en) * | 2010-11-19 | 2011-07-13 | 苏州博纳化学科技有限公司 | Preparation method of maleic anhydride-(meth)acrylic acid dispersant |
| WO2016118146A1 (en) * | 2015-01-22 | 2016-07-28 | Halliburton Energy Services, Inc. | Compatibilized cement composition for treatment of a subterranean formation |
| CN107344822A (en) * | 2017-06-05 | 2017-11-14 | 南宁科恺混凝土外加剂有限公司 | One kind is containing bentonitic premixing mortar water-keeping thickening material and preparation method thereof |
| CN108359062A (en) * | 2018-03-23 | 2018-08-03 | 刘翠芬 | High-adaptability type solid polycarboxylic acid water reducing agent and its bulk polymerization preparation method |
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