CN111808240A - Plastic-retaining polycarboxylic acid water reducing agent and preparation method thereof - Google Patents
Plastic-retaining polycarboxylic acid water reducing agent and preparation method thereof Download PDFInfo
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- CN111808240A CN111808240A CN202010666313.6A CN202010666313A CN111808240A CN 111808240 A CN111808240 A CN 111808240A CN 202010666313 A CN202010666313 A CN 202010666313A CN 111808240 A CN111808240 A CN 111808240A
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- polycarboxylate superplasticizer
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/24—Macromolecular compounds
- C04B24/26—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B24/2688—Copolymers containing at least three different monomers
- C04B24/2694—Copolymers containing at least three different monomers containing polyether side chains
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/30—Water reducers, plasticisers, air-entrainers, flow improvers
- C04B2103/302—Water reducers
Abstract
The invention provides a plastic-retaining polycarboxylate superplasticizer and a preparation method thereof. The preparation method of the plastic-retaining polycarboxylate superplasticizer comprises the following steps: (1) adding 20-70 parts of prenyl alcohol polyoxyethylene ether macromonomer and 0.05-0.5 part of stabilizer into a four-neck flask, and uniformly stirring after the prenyl alcohol polyoxyethylene ether macromonomer is completely melted (2) weighing acrylic acid, hydroxyethyl acrylate and 2-acrylic acid 2-acrylamide and mixing to form a material A; (3) weighing 0.05-0.2 part of chain transfer agent and adding into a four-neck flask; (4) and (3) dropwise adding the material A and 0.3-0.6 part of initiator into a four-neck flask, and keeping the temperature for 0.5-1.5 h: (5) after the heat preservation is finished, 32% concentration liquid alkali is added for neutralization and stirring, and then the mixture is poured into a glass dish and cooled into a solid state.
Description
Technical Field
The invention relates to a water reducing agent and a preparation method thereof, in particular to a plastic-retaining polycarboxylate water reducing agent and a preparation method thereof, and belongs to the technical field of building material concrete admixtures.
Background
The polycarboxylate water reducing agent is a latest generation high-performance water reducing agent after common water reducing agents such as lignin, calcium lignosulfonate and the like, and sulfamate, aliphatic and melamine high-efficiency water reducing agents. The polycarboxylate superplasticizer has the advantages of high water reducing rate, low mixing amount, flexible molecular structure and the like, and can have different properties by adjusting the density of main chain carboxyl, the length of a side chain and grafting different functional groups.
Patent 1 (publication number: CN 106008847A) discloses a preparation method of a slump-retaining ether type polycarboxylic acid water reducer. Unsaturated ether macromonomer, unsaturated carboxylic acid small monomer, molecular weight regulator and initiator are used for polymerization reaction at the temperature of 50-70 ℃, and heat preservation is carried out for 1-2 hours, so as to obtain the slump-retaining polycarboxylic acid water reducing agent with the solid content of about 40%.
Patent 2 (publication number: CN 106008847A) discloses a preparation process of polycarboxylate superplasticizer powder. The solid polycarboxylate superplasticizer with the content of more than 95 percent is obtained by tape casting film forming, low-temperature vacuum evaporation, stripping and crushing. The water reducing agent has low mixing amount and high water reducing rate, and is suitable for long-distance transportation, packaging and storage.
The defects of the technology are as follows: the produced polycarboxylic acid products are mainly 30-50% in concentration, are not suitable for long-distance transportation and are inconvenient to apply in dry-mixed mortar. The special mortar such as grouting material, support mortar and the like has higher requirements on the fluidity of 30min and 60min, and the fluidity loss is adjusted mainly by adding organic matter retarders such as sodium gluconate, white sugar and the like or inorganic salt retarders such as sodium citrate, sodium tripolyphosphate and the like. However, such retarders tend to cause over-doping and have a large impact on the later strength. In addition, the cement has complex components, high-quality aggregate is reduced, and the content of soil and stone powder in the gravel aggregate is higher, so that the slump loss of the concrete is serious. Therefore, the plastic-retaining polycarboxylate superplasticizer is researched and developed and has a great application value when being applied to special mortar and concrete. At present, liquid polycarboxylic acid water reducing agent is prepared into polycarboxylic acid powder mainly by a high-temperature centrifugal spraying technology or a tape casting film forming technology. High-temperature centrifugal spraying or tape casting film forming equipment is expensive, the process is complex, and a large amount of energy is wasted in the production process.
Disclosure of Invention
The invention provides a plastic-retaining polycarboxylate superplasticizer and a preparation method thereof.
In order to achieve the purpose, the invention is realized by the following technical scheme:
the preparation method of the plastic-retaining polycarboxylate superplasticizer is characterized by comprising the following steps:
(1) adding 20-70 parts of prenyl alcohol polyoxyethylene ether macromonomer and 0.05-0.5 part of stabilizer into a four-neck flask, heating under the protection of nitrogen or other inert gases, uniformly stirring after the prenyl alcohol polyoxyethylene ether macromonomer is completely melted, and controlling the temperature at 70-85 ℃;
(2) weighing 5-20 parts of acrylic acid, 5-20 parts of hydroxyethyl acrylate and 5-20 parts of 2-acrylic acid 2-acrylamide, and mixing to form a material A;
(3) weighing 0.05-0.2 part of chain transfer agent and adding into a four-neck flask;
(4) and (3) dropwise adding the material A and 0.3-0.6 part of initiator into a four-neck flask, and keeping the temperature for 0.5-1.5 h:
(5) after the heat preservation is finished, adding 32% concentration liquid alkali for neutralization, controlling the pH value to be 6.5-7.5, stirring, pouring into a glass dish, and cooling to be solid;
(6) and (3) crushing the solid into a powdery plastic-retaining polycarboxylic acid water reducing agent by a low-temperature pulverizer.
The preferable scheme of the preparation method of the plastic-retaining polycarboxylate superplasticizer comprises the specific process of the step (3) of dropwise adding the material A, wherein the dropwise adding time is controlled to be 1.5-2.5h, and 1/3 initiator is added every 20-40min in the dropwise adding process and is added for three times.
According to the preferable scheme of the preparation method of the plastic-retaining polycarboxylate water reducer, the initiator is one or more of oil-soluble initiators such as dimethyl azobisisobutyrate, azobisisobutyronitrile and tert-butyl hydroperoxide.
According to the preferable scheme of the preparation method of the plastic-retaining polycarboxylate superplasticizer, the chain transfer agent is one or more of mercaptopropionic acid, mercaptoacetic acid and mercaptoethanol;
according to the preferable scheme of the preparation method of the plastic-retaining polycarboxylate superplasticizer, the stabilizer is p-styrene sulfonate.
The plastic-retaining polycarboxylate superplasticizer is prepared by adopting the methods of the schemes.
The specific working principle or reaction process of the invention is as follows:
the invention has the advantages that: by a bulk polymerization technology, a large monomer and an unsaturated small monomer are subjected to free radical polymerization reaction to directly synthesize the high-concentration plastic-retaining polycarboxylate superplasticizer in a reaction kettle, and the high-concentration plastic-retaining polycarboxylate superplasticizer can be diluted into polycarboxylate products with different concentrations or cooled into a blocky polycarboxylate superplasticizer at room temperature, and the blocky polycarboxylate superplasticizer is crushed into a specified powdery product by a low-temperature crusher. The plastic-retaining polycarboxylate superplasticizer powder can solve the problem of the loss of fluidity of dry-mixed mortar such as grouting materials and grouting materials produced by different varieties of cement over time and the slump loss of common concrete and high-performance concrete, does not need additional equipment in the preparation process, and has simple operation process. The reaction formula is as follows
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The preparation method of the plastic-retaining polycarboxylate superplasticizer comprises the following raw materials in parts by weight: prenol polyoxyethylene ether: 70; acrylic acid: 20; hydroxyethyl acrylate: 5; 2-acrylic acid 2-acrylamide: 5; initiator: 0.45 of; chain transfer agent: 0.07; a stabilizer: 0.2; alkali: 12; the preparation method comprises the following steps:
(1) assembling a four-mouth flask, a thermometer, a peristaltic pump, an adjustable temperature control electric heating jacket and a nitrogen protection device, and checking whether the equipment is intact;
(2) weighing 70 parts of 2400 molecular weight prenyl polyoxyethylene ether unsaturated macromonomer and 0.2 part of stabilizer, putting the monomers into a four-neck flask, starting a nitrogen protection device, starting heating, starting stirring when the monomers are completely melted, and controlling the temperature at 75 ℃;
(3) accurately weigh material A20 parts acrylic acid, 5 parts hydroxyethyl acrylate, 5 parts 2-propenoic acid 2-acrylamide into a conical flask.
(4) Accurately weighing 0.07 part of mercaptopropionic acid serving as a chain transfer agent, and adding the chain transfer agent into a four-neck flask;
(5) and (5) beginning to dropwise add the material A, and controlling the dropwise adding time to be about 2 hours. Weighing 0.45 part of azobisisobutyronitrile as an initiator, adding 1/3 initiator every half hour in the process of dropwise adding, and finishing the addition for three times;
(6) after the material A is dripped, preserving heat for 1h, adding 12 parts of alkali for neutralization after the heat preservation is finished, controlling the pH value to be about 7, stirring for 5min, and pouring the obtained plastic-retaining polycarboxylic acid water reducing agent into a glass dish for cooling;
(7) and when the plastic-retaining polycarboxylate water reducer is cooled to be solid, the powder of the low-temperature pulverizer is changed into powdery plastic-retaining polycarboxylate water reducer.
Example 2
The preparation method of the plastic-retaining polycarboxylate superplasticizer comprises the following raw materials in parts by weight: prenol polyoxyethylene ether: 20; acrylic acid: 10; hydroxyethyl acrylate: 10; 2-acrylic acid 2-acrylamide: 10; initiator: 0.3; chain transfer agent: 0.05; a stabilizer: 0.05; alkali: 10; the preparation method comprises the following steps:
(1) assembling a four-mouth flask, a thermometer, a peristaltic pump, an adjustable temperature control electric heating jacket and a nitrogen protection device, and checking whether the equipment is intact;
(2) weighing 20 parts of 2400 molecular weight prenyl polyoxyethylene ether unsaturated macromonomer and 0.05 part of stabilizer, putting the monomers into a four-neck flask, starting a nitrogen protection device, starting heating, starting stirring when the monomers are completely melted, and controlling the temperature at 75 ℃;
(3) accurately weighing 10 parts of acrylic acid, 10 parts of hydroxyethyl acrylate and 10 parts of 2-acrylic acid 2-acrylamide in a conical flask;
(4) accurately weighing 0.05 part of chain transfer agent (thioglycollic acid) and adding the chain transfer agent into a four-neck flask;
(5) and (5) beginning to dropwise add the material A, and controlling the dropwise adding time to be about 2 hours. Weighing 0.3 part of initiator (dimethyl azodiisobutyrate), adding 1/3 initiator every half hour in the process of dropwise adding, and finishing adding for three times;
(6) after the material A is dripped, preserving heat for 1h, adding 10 parts of alkali for neutralization after the heat preservation is finished, controlling the pH value to be about 7, stirring for 5min, and pouring the plastic-retaining polycarboxylic acid water reducing agent into a glass dish for cooling;
(7) and when the plastic-retaining polycarboxylate water reducer is cooled to be solid, the powder of the low-temperature pulverizer is changed into powdery plastic-retaining polycarboxylate water reducer.
Example 3
The preparation method of the plastic-retaining polycarboxylate superplasticizer comprises the following raw materials in parts by weight: prenol polyoxyethylene ether: 45, a first step of; acrylic acid: 10; hydroxyethyl acrylate: 20; 2-acrylic acid 2-acrylamide: 20; initiator: 0.6; chain transfer agent: 0.2; a stabilizer: 0.5; alkali: 50; the preparation method comprises the following steps:
(1) assembling a four-mouth flask, a thermometer, a peristaltic pump, an adjustable temperature control electric heating jacket and a nitrogen protection device, and checking whether the equipment is intact;
(2) weighing 45 parts of 2400 molecular weight prenyl polyoxyethylene ether unsaturated macromonomer and 0.2 part of stabilizer, putting the monomers into a four-neck flask, starting a nitrogen protection device, starting heating, starting stirring when the monomers are completely melted, and controlling the temperature at 85 ℃.
(3) Material a was accurately weighed into a erlenmeyer flask, 10 parts acrylic acid, 20 parts hydroxyethyl acrylate, 20 parts 2-propenoic acid 2-acrylamide.
(4) Accurately weighing 0.6 part of chain transfer agent (thioglycollic acid) and adding the chain transfer agent into a four-neck flask;
(5) and (5) beginning to dropwise add the material A, and controlling the dropwise adding time to be about 2 hours. Weighing 0.6 part of initiator (tert-butyl hydroperoxide), adding 1/3 initiator every half hour in the process of dropwise adding, and finishing adding for three times;
(6) after the material A is dripped, preserving heat for 1h, adding 5 parts of alkali for neutralization after the heat preservation is finished, controlling the pH value to be about 7, stirring for 5min, pouring the high-concentration plastic-retaining polycarboxylate superplasticizer into a glass dish, and cooling;
(7) and when the plastic-retaining polycarboxylate water reducer is cooled to be solid, the powder of the low-temperature pulverizer is changed into powdery plastic-retaining polycarboxylate water reducer.
Comparative example 1
The preparation method of the plastic-retaining polycarboxylate superplasticizer comprises the following raw materials in parts by weight: prenol polyoxyethylene ether: 60, adding a solvent to the mixture; acrylic acid: 20; hydroxyethyl acrylate: 5; 2-acrylic acid 2-acrylamide: 5; initiator: 0.45 of; chain transfer agent: 0.07; alkali: 12; the preparation method comprises the following steps:
(1) assembling a four-mouth flask, a thermometer, a peristaltic pump, an adjustable temperature control electric heating jacket and a nitrogen protection device, and checking whether the equipment is intact;
(2) weighing 60 parts of 2400 molecular weight prenyl polyoxyethylene ether unsaturated macromonomer, putting the monomer into a four-neck flask, starting a nitrogen protection device, starting heating, starting stirring when the monomer is completely melted, and controlling the temperature at 75 ℃;
(3) accurately weigh material A20 parts acrylic acid, 5 parts hydroxyethyl acrylate, 5 parts 2-propenoic acid 2-acrylamide into a conical flask.
(4) Accurately weighing 0.07 part of mercaptopropionic acid serving as a chain transfer agent, and adding the chain transfer agent into a four-neck flask;
(5) and (5) beginning to dropwise add the material A, and controlling the dropwise adding time to be about 2 hours. Weighing 0.45 part of azobisisobutyronitrile as an initiator, adding 1/3 initiator every half hour in the process of dropwise adding, and finishing the addition for three times;
(6) after the material A is dripped, preserving heat for 1h, adding 12 parts of alkali for neutralization after the heat preservation is finished, controlling the pH value to be about 7, stirring for 5min, and pouring the obtained plastic-retaining polycarboxylic acid water reducing agent into a glass dish for cooling;
(7) and when the plastic-retaining polycarboxylate water reducer is cooled to be solid, the powder of the low-temperature pulverizer is changed into powdery plastic-retaining polycarboxylate water reducer.
Comparative example 2
The preparation method of the plastic-retaining polycarboxylate superplasticizer comprises the following raw materials in parts by weight: prenol polyoxyethylene ether: 60, adding a solvent to the mixture; acrylic acid: 20; hydroxyethyl acrylate: 5; 2-acrylic acid 2-acrylamide: 5; initiator: 0.45 of; chain transfer agent: 0.07; a stabilizer: 0.2; alkali: 12; the preparation method comprises the following steps:
(1) assembling a four-mouth flask, a thermometer, a peristaltic pump, an adjustable temperature control electric heating jacket and a nitrogen protection device, and checking whether the equipment is intact;
(2) weighing 60 parts of 2400-molecular-weight prenyl polyoxyethylene ether unsaturated macromonomer and 0.2 part of stabilizer, putting the monomers into a four-neck flask, starting a nitrogen protection device, starting heating, starting stirring when the monomers are completely melted, and controlling the temperature to be 95 ℃;
(3) accurately weigh material A20 parts acrylic acid, 5 parts hydroxyethyl acrylate, 5 parts 2-propenoic acid 2-acrylamide into a conical flask.
(4) Accurately weighing 0.07 part of mercaptopropionic acid serving as a chain transfer agent, and adding the chain transfer agent into a four-neck flask;
(5) and (5) beginning to dropwise add the material A, and controlling the dropwise adding time to be about 2 hours. Weighing 0.45 part of azobisisobutyronitrile as an initiator, adding 1/3 initiator every half hour in the process of dropwise adding, and finishing the addition for three times;
(6) after the material A is dripped, preserving heat for 1h, adding 12 parts of alkali for neutralization after the heat preservation is finished, controlling the pH value to be about 7, stirring for 5min, and pouring the obtained plastic-retaining polycarboxylic acid water reducing agent into a glass dish for cooling;
(7) and when the plastic-retaining polycarboxylate water reducer is cooled to be solid, the powder of the low-temperature pulverizer is changed into powdery plastic-retaining polycarboxylate water reducer.
The specific results of the above embodiments can be referred to the following table
The examples 1-2 can obviously improve the fluidity loss of various special mortars and the slump loss of concrete by adjusting different ester group densities and amide group densities, the example 3 can increase the fluidity loss of the mortars by continuously optimizing the test temperature and adding a proper amount of stabilizer, and can change the fluidity or the slump retention time by adjusting the mixing amount, and the performance of the example 3 is superior to that of the examples 1-2. The comparative examples 1-2 adjust the stabilizing agent and the synthesis temperature, the activation energy is increased in the synthesis process, the polycarboxylic acid water reducing agent is easy to implode in the free radical synthesis process, and the polycarboxylic acid powder with stable performance cannot be synthesized, and the experimental effect of the comparative examples 1-2 is obviously poorer than that of the examples 1-3.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (5)
1. The preparation method of the plastic-retaining polycarboxylate superplasticizer is characterized by comprising the following steps:
(1) adding 20-70 parts of prenyl polyoxyethylene ether macromonomer (TPEG) and 0.05-0.5 part of stabilizer into a four-neck flask, heating under the protection of nitrogen or other inert gases, uniformly stirring after the prenyl polyoxyethylene ether macromonomer is completely melted, and controlling the temperature at 70-85 ℃;
(2) weighing 5-20 parts of acrylic acid, 5-20 parts of hydroxyethyl acrylate and 5-20 parts of 2-acrylic acid 2-acrylamide, and mixing to form a material A;
(3) weighing 0.05-0.2 part of chain transfer agent and adding into a four-neck flask;
(4) and (3) dropwise adding the material A and 0.3-0.6 part of initiator into a four-neck flask, and keeping the temperature for 0.5-1.5 h:
(5) after the heat preservation is finished, adding 32% concentration liquid alkali for neutralization, controlling the pH value to be 6.5-7.5, stirring, pouring into a glass dish, and cooling to be solid;
(6) and (3) crushing the solid into a powdery plastic-retaining polycarboxylic acid water reducing agent by a low-temperature pulverizer.
2. The preparation method of the plastic-retaining polycarboxylate superplasticizer according to claim 1, which is characterized by comprising the following steps: and the step (3) comprises the specific process of dropwise adding the material A, wherein the dropwise adding time is controlled to be 1.5-2h, and 1/3 initiator is added every 20-40min in the dropwise adding process, and the addition is completed in three times.
3. The preparation method of the plastic-retaining polycarboxylate superplasticizer according to claim 1, which is characterized by comprising the following steps: the initiator is one or more of dimethyl azodiisobutyrate, azodiisobutyronitrile and tert-butyl hydroperoxide.
4. The preparation method of the plastic-retaining polycarboxylate superplasticizer according to claim 1, which is characterized by comprising the following steps: the chain transfer agent is one or more of mercaptopropionic acid, mercaptoacetic acid and mercaptoethanol;
the preparation method of the plastic-retaining polycarboxylate superplasticizer according to claim 1, which is characterized by comprising the following steps: the stabilizer is a mixture of end-capped amide phosphate and p-styrene sulfonate, and the specific proportion is 1-2: 1-2.
5. The plastic-retaining polycarboxylate superplasticizer is characterized by comprising the following components in parts by weight: prepared by the process of any one of claims 1 to 4.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20130231415A1 (en) * | 2012-03-05 | 2013-09-05 | Ruetgers Polymers Ltd. | Slump Retaining and Dispersing Agent for Hydraulic Compositions |
| CN106543382A (en) * | 2016-12-07 | 2017-03-29 | 湖北工业大学 | A kind of solid lamellar polycarboxylate water-reducer and its polymerization process for preparing |
| CN107759748A (en) * | 2017-11-07 | 2018-03-06 | 上海三瑞高分子材料股份有限公司 | A kind of solid high early strength poly-carboxylic water reducer and preparation method thereof |
| CN111019064A (en) * | 2019-12-26 | 2020-04-17 | 河北铁园科技发展有限公司 | Polycarboxylate superplasticizer and preparation method thereof |
| CN111170671A (en) * | 2018-11-13 | 2020-05-19 | 北京市建筑工程研究院有限责任公司 | Preparation method of slump-retaining solid polycarboxylate superplasticizer |
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2020
- 2020-07-13 CN CN202010666313.6A patent/CN111808240A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20130231415A1 (en) * | 2012-03-05 | 2013-09-05 | Ruetgers Polymers Ltd. | Slump Retaining and Dispersing Agent for Hydraulic Compositions |
| CN106543382A (en) * | 2016-12-07 | 2017-03-29 | 湖北工业大学 | A kind of solid lamellar polycarboxylate water-reducer and its polymerization process for preparing |
| CN107759748A (en) * | 2017-11-07 | 2018-03-06 | 上海三瑞高分子材料股份有限公司 | A kind of solid high early strength poly-carboxylic water reducer and preparation method thereof |
| CN111170671A (en) * | 2018-11-13 | 2020-05-19 | 北京市建筑工程研究院有限责任公司 | Preparation method of slump-retaining solid polycarboxylate superplasticizer |
| CN111019064A (en) * | 2019-12-26 | 2020-04-17 | 河北铁园科技发展有限公司 | Polycarboxylate superplasticizer and preparation method thereof |
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Application publication date: 20201023 |