CN118388166A - Silica sol dispersion stabilizer for concrete and preparation method and application thereof - Google Patents

Silica sol dispersion stabilizer for concrete and preparation method and application thereof Download PDF

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Publication number
CN118388166A
CN118388166A CN202410773387.8A CN202410773387A CN118388166A CN 118388166 A CN118388166 A CN 118388166A CN 202410773387 A CN202410773387 A CN 202410773387A CN 118388166 A CN118388166 A CN 118388166A
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concrete
silica sol
parts
dispersion stabilizer
weight
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CN118388166B (en
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刘磊
吴伟
黄玉美
刘昭洋
方涛
罗鑫
王明焱
李茜茜
刘亚亮
刘江涛
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Sichuan Concrete Road Technology Co ltd
Shijiazhuang Chang'an Yucai Building Materials Co ltd
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Sichuan Concrete Road Technology Co ltd
Shijiazhuang Chang'an Yucai Building Materials Co ltd
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Abstract

The invention provides a silica sol dispersion stabilizer for concrete, and a preparation method and application thereof, and belongs to the technical field of concrete. The invention takes amino-trimethyl-phosphoric acid, diethanol monoisopropanolamine and dispersant solution as raw materials to prepare the silica sol dispersion stabilizer for concrete, wherein the amino-trimethyl-phosphoric acid can be tightly adsorbed around calcium and magnesium ions to form multi-ring chelate when being added into a concrete system and is dispersed in water in a loose form to prevent metal ions from affecting nano silicon dioxide; the diethanol monoisopropanolamine can reduce the surface energy of the nano silicon dioxide and weaken the characteristic of easy agglomeration; the dispersing agent solution can separate metal ions and nano silicon dioxide in a certain space, so that the influence of the metal ions on silica sol is reduced, the nano silicon dioxide can be uniformly distributed in a high-ion concentration system of concrete, the positive influence of the nano silicon dioxide on the performance of the concrete is exerted, and the performance improvement effect of the silica sol on the concrete is ensured.

Description

Silica sol dispersion stabilizer for concrete and preparation method and application thereof
Technical Field
The invention belongs to the technical field of concrete, and particularly relates to a silica sol dispersion stabilizer for concrete, and a preparation method and application thereof.
Background
Concrete is a material commonly used in construction engineering, and has been widely used because of its good mechanical properties and economy. However, in the long-term use process, the concrete is easy to crack, corrode and the like, so that the mechanical and durability of the concrete are reduced, and the service life of the building is influenced. In recent years, researchers introduce nano silica sol into concrete to improve the mechanical properties, the impermeability and the durability of the concrete, thereby solving the problems.
The silica sol is a dispersion of nano-scale silica particles in water or solvent, the silica in the silica sol is nano-scale, has small particle size and extremely high surface energy, and can be stably dispersed in the silica sol to form a stable colloidal solution. However, when the polymer is added into concrete, the polymer can be quickly agglomerated and automatically coalesced to form gel or precipitate under a high ion concentration system of the concrete. This causes the tiny silica particles to become large particles, severely affecting their activity and filling effect, and greatly compromising the silica sol's performance enhancement for concrete. The existing silica sol dispersing agent only can enable nano silicon dioxide to be stably dispersed in water or a solvent, cannot be uniformly dispersed in concrete pore liquid with high ion concentration, and can generate agglomeration in a concrete system, so that the nano silicon dioxide is densely filled and has limited reinforcing effect.
Therefore, how to provide a silica sol dispersion stabilizer capable of ensuring the performance improvement effect of silica sol on concrete is a technical problem to be solved by those skilled in the art.
Disclosure of Invention
In order to solve the technical problems, the invention provides a silica sol dispersion stabilizer for concrete, and a preparation method and application thereof.
In order to achieve the above purpose, the present invention provides the following technical solutions:
the silica sol dispersion stabilizer for the concrete comprises the following raw materials in parts by weight:
20-40 parts of aminotrimethylene phosphate, 10-20 parts of diethanol monoisopropanolamine and 40-70 parts of dispersant solution;
the preparation method of the dispersant solution comprises the following steps: adding water, maleic anhydride, dimethyl allyl ammonium chloride and sodium hypophosphite into a reactor, stirring and dissolving, then adding an acrylic acid solution and an ammonium persulfate solution for copolymerization, and cooling and regulating the pH value to obtain the dispersing agent solution.
Preferably, the weight ratio of the maleic anhydride to the dimethylallyl ammonium chloride to the sodium hypophosphite to the acrylic acid solution to the ammonium persulfate solution is (10-15) to (6-8) to (5-6) to (50-55) to (31.5-32).
Preferably, the acrylic acid solution is composed of 30 to 35 parts by weight of acrylic acid and 20 parts by weight of water, and the ammonium persulfate solution is composed of 1.5 to 2 parts by weight of ammonium persulfate and 30 parts by weight of water.
Preferably, the temperature of the copolymerization is 80-85 ℃, the atmosphere is nitrogen, and the time is 4-5h.
The invention also provides a preparation method of the silica sol dispersion stabilizer, which comprises the following steps: weighing the raw materials according to the parts by weight, mixing the aminotrimethylene phosphate, the diethanol monoisopropanolamine and the dispersing agent solution, and uniformly stirring to obtain the silica sol dispersion stabilizer.
The invention also provides the silica sol dispersion stabilizer for the concrete or the application of the silica sol dispersion stabilizer for the concrete prepared by the preparation method in the concrete.
Preferably, the mixing amount of the silica sol dispersion stabilizer for the concrete is 2-5% of the mass of the silica sol.
Compared with the prior art, the invention has the following advantages and technical effects:
The invention takes amino-trimethyl-phosphoric acid, diethanol monoisopropanolamine and dispersant solution as raw materials to prepare the silica sol dispersion stabilizer for concrete, wherein the amino-trimethyl-phosphoric acid can be tightly adsorbed around calcium and magnesium ions when being added into a concrete system, forms multi-ring chelate with metal ions such as calcium and magnesium and the like, and is dispersed in water in a loose form to prevent the metal ions from affecting nano silicon dioxide; the diethanol monoisopropanolamine can reduce the surface energy of the nano silicon dioxide and weaken the characteristic of easy agglomeration; the dispersing agent solution prepared by copolymerizing water, maleic anhydride, dimethyl allyl ammonium chloride, sodium hypophosphite, acrylic acid solution and ammonium persulfate solution is an amphoteric dispersing agent, one end of the dispersing agent can act through cationic groups and nano silicon dioxide, the other end of the dispersing agent can act through anionic groups and metal ions, and the metal ions and the nano silicon dioxide can be separated in a certain space by combining electrostatic repulsive force and steric hindrance of the dispersing agent, so that the influence of metal ions such as calcium, magnesium and the like on silica sol is reduced, the nano silicon dioxide can be uniformly distributed in a high-ion concentration system of concrete, the positive influence of the nano silicon dioxide on the performance of the concrete is exerted, and the effect of the silica sol on improving the performance of the concrete is ensured.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In order that the above-recited objects, features and advantages of the present invention will become more apparent, a more particular description of the invention will be rendered by reference to specific embodiments thereof.
The embodiment of the invention provides a silica sol dispersion stabilizer for concrete, which comprises the following raw materials in parts by weight:
20-40 parts of aminotrimethylene phosphate, 10-20 parts of diethanol monoisopropanolamine and 40-70 parts of dispersant solution;
the preparation method of the dispersant solution comprises the following steps: adding water, maleic anhydride, dimethyl allyl ammonium chloride and sodium hypophosphite into a reactor, stirring and dissolving, then adding an acrylic acid solution and an ammonium persulfate solution for copolymerization, and cooling and regulating the pH value to obtain the dispersing agent solution.
In a preferred embodiment, the silica sol dispersion stabilizer for concrete comprises 20 to 40 parts by weight, preferably 25 to 30 parts by weight of aminotrimethylene phosphate.
In a preferred embodiment, the silica sol dispersion stabilizer for concrete comprises 10-20 parts by weight, preferably 15-20 parts by weight of diethanol monoisopropanolamine.
In a preferred embodiment, the silica sol dispersion stabilizer for concrete comprises 40 to 70 parts, preferably 55 to 60 parts, of a dispersant solution in parts by weight.
In a preferred embodiment, the method of preparing the dispersant solution comprises: adding water, maleic anhydride, dimethyl allyl ammonium chloride and sodium hypophosphite into a reactor, stirring and dissolving, then adding an acrylic acid solution and an ammonium persulfate solution for copolymerization, and cooling and regulating the pH value to obtain the dispersing agent solution. The invention takes maleic anhydride, dimethyl allyl ammonium chloride and acrylic acid as monomers, takes sodium hypophosphite and ammonium persulfate as initiators, prepares the amphoteric dispersant solution through copolymerization, cooling and pH adjustment, and can reduce the influence of metal ions such as calcium, magnesium and the like on silica sol.
In a preferred embodiment, the water is used in an amount of 100 parts by weight.
In a preferred embodiment, the weight ratio of maleic anhydride, dimethylallyl ammonium chloride, sodium hypophosphite, acrylic acid solution and ammonium persulfate solution is (10-15) to (6-8) to (5-6) to (50-55) to (31.5-32), more preferably (12-14) to (6-7) to (5.5-5.8) to (52-53) to (31.7-31.8).
In a preferred embodiment, the acrylic acid solution is composed of 30 to 35 parts by weight of acrylic acid and 20 parts by weight of water; the ammonium persulfate solution consists of 1.5-2 parts by weight of ammonium persulfate and 30 parts by weight of water.
In a preferred embodiment, the reactor is equipped with a stirrer, a dripping device and a heating device.
In a preferred embodiment, the temperature of the copolymerization is 80-85 ℃, the atmosphere is nitrogen, and the time is 4-5 hours.
In a preferred embodiment, the acrylic acid solution and the ammonium persulfate solution are completely dripped within 1 hour, and the reaction is continued for 4 hours after the dripping is completed.
In a preferred embodiment, the temperature reduction is to within 40 ℃.
In a preferred embodiment, the pH adjustment is to a pH of 7-8 with a 30% strength by mass NaOH solution.
The embodiment of the invention also provides a preparation method of the silica sol dispersion stabilizer for concrete, which comprises the following steps: weighing the raw materials according to the parts by weight, mixing the aminotrimethylene phosphoric acid, the diethanol monoisopropanolamine and the dispersing agent solution, and uniformly stirring to obtain the silica sol dispersion stabilizer for the concrete.
The invention also provides the silica sol dispersion stabilizer for the concrete or the application of the silica sol dispersion stabilizer for the concrete prepared by the preparation method in the concrete.
In a preferred embodiment, the silica sol dispersion stabilizer for concrete is incorporated in an amount of 2 to 5% by mass of the silica sol.
Unless otherwise specified, the parts in the embodiment of the invention represent "parts by weight".
Unless otherwise specified, the starting materials in the examples of the present invention were all obtained by commercial purchase.
Example 1
The silica sol dispersion stabilizer for the concrete is prepared from the following raw materials in parts by weight: 20 parts of aminotrimethylene phosphate, 10 parts of diethanol monoisopropanolamine and 70 parts of dispersant solution;
The preparation method of the dispersant solution comprises the following steps: adding 100 parts by weight of water, 10 parts by weight of maleic anhydride, 8 parts by weight of dimethyl allyl ammonium chloride and 5.8 parts by weight of sodium hypophosphite into a reactor provided with a stirrer, a dripping device and a heating device, stirring and dissolving, introducing nitrogen, heating to 80 ℃, dripping 53 parts by weight of acrylic acid solution (consisting of 33 parts by weight of acrylic acid and 20 parts by weight of deionized water) and 31.5 parts by weight of ammonium persulfate solution (consisting of 1.5 parts by weight of ammonium persulfate and 30 parts by weight of deionized water) into the reactor, dripping the mixture within 1h, continuing to react for 4h after dripping, reducing the temperature of the system to within 40 ℃ after finishing the dripping, and regulating the pH to 7-8 by using a NaOH solution with the mass concentration of 30%;
the preparation method of the silica sol dispersion stabilizer for the concrete comprises the following steps: weighing the raw materials according to the parts by weight, mixing the aminotrimethylene phosphate, the diethanol monoisopropanolamine and the dispersing agent solution, and uniformly stirring to obtain the silica sol dispersion stabilizer.
Example 2
The silica sol dispersion stabilizer for the concrete is prepared from the following raw materials in parts by weight: 25 parts of aminotrimethylene phosphate, 15 parts of diethanol monoisopropanolamine and 60 parts of dispersing agent solution;
the preparation method of the dispersant solution comprises the following steps: adding 100 parts by weight of water, 12 parts by weight of maleic anhydride, 8 parts by weight of dimethyl allyl ammonium chloride and 6 parts of sodium hypophosphite into a reactor provided with a stirrer, a dripping device and a heating device, stirring and dissolving, introducing nitrogen, heating to 82 ℃, dripping 55 parts by weight of acrylic acid solution (consisting of 35 parts by weight of acrylic acid and 20 parts by weight of deionized water) and 31.7 parts by weight of ammonium persulfate solution (consisting of 1.7 parts by weight of ammonium persulfate and 30 parts by weight of deionized water), dripping over 1 hour, continuing to react for 4 hours after dripping, reducing the temperature of the system to be within 40 ℃ after finishing the dripping, and regulating the pH to 7-8 by using a NaOH solution with the mass concentration of 30%;
The preparation method of the silica sol dispersion stabilizer for concrete is the same as in example 1.
Example 3
The silica sol dispersion stabilizer for the concrete is prepared from the following raw materials in parts by weight: 30 parts of aminotrimethylene phosphate, 15 parts of diethanol monoisopropanolamine and 55 parts of dispersant solution;
The preparation method of the dispersant solution comprises the following steps: adding 100 parts by weight of water, 14 parts by weight of maleic anhydride, 7 parts by weight of dimethyl allyl ammonium chloride and 5.5 parts by weight of sodium hypophosphite into a reactor provided with a stirrer, a dripping device and a heating device, stirring and dissolving, introducing nitrogen, heating to 83 ℃, dripping 52 parts by weight of acrylic acid solution (consisting of 32 parts by weight of acrylic acid and 20 parts by weight of deionized water) and 31.8 parts by weight of ammonium persulfate solution (consisting of 1.8 parts by weight of ammonium persulfate and 30 parts by weight of deionized water), dripping over 1h, continuing to react for 4h after dripping over, reducing the temperature of the system to within 40 ℃ after finishing the dripping, and regulating the pH to 7-8 by using a NaOH solution with the mass concentration of 30%;
The preparation method of the silica sol dispersion stabilizer for concrete is the same as in example 1.
Example 4
The silica sol dispersion stabilizer for the concrete is prepared from the following raw materials in parts by weight: 40 parts of aminotrimethylene phosphate, 20 parts of diethanol monoisopropanolamine and 40 parts of dispersant solution;
The preparation method of the dispersant solution comprises the following steps: adding 100 parts by weight of water, 15 parts by weight of maleic anhydride, 6 parts by weight of dimethyl allyl ammonium chloride and 5 parts by weight of sodium hypophosphite into a reactor provided with a stirrer, a dripping device and a heating device, stirring and dissolving, introducing nitrogen, heating to 85 ℃, dripping 50 parts by weight of acrylic acid solution (consisting of 30 parts by weight of acrylic acid and 20 parts by weight of deionized water) and 32 parts by weight of ammonium persulfate solution (consisting of 2 parts by weight of ammonium persulfate and 30 parts by weight of deionized water), dripping over 1h, continuing to react for 4h, reducing the temperature of the system to be within 40 ℃ after the dripping is finished, and regulating the pH value to 7-8 by using a NaOH solution with the mass concentration of 30%;
The preparation method of the silica sol dispersion stabilizer for concrete is the same as in example 1.
Comparative example 1
The silica sol dispersion stabilizer for concrete is different from example 1 in that aminotrimethylene phosphoric acid is omitted, and the silica sol dispersion stabilizer is composed of the following raw materials in parts by weight: 12.5 parts of diethanol monoisopropanolamine and 87.5 parts of dispersant solution.
The preparation method of the dispersant solution and the preparation method of the silica sol dispersion stabilizer for concrete are the same as in example 1.
Comparative example 2
The silica sol dispersion stabilizer for concrete is different from example 1 in that the diethanol monoisopropanolamine is omitted, and the silica sol dispersion stabilizer is composed of the following raw materials in parts by weight: 22.2 parts of aminotrimethylene phosphate and 77.8 parts of dispersant solution.
The preparation method of the dispersant solution and the preparation method of the silica sol dispersion stabilizer for concrete are the same as in example 1.
Comparative example 3
The silica sol dispersion stabilizer for concrete is different from example 1 in that the dispersant solution is omitted, and specifically consists of the following raw materials in parts by weight: 66.7 parts of amino trimethophosphoric acid and 33.3 parts of diethanol monoisopropanolamine.
The preparation method of the silica sol dispersion stabilizer for concrete is the same as in example 1.
Performance testing
The silica sol dispersion stabilizer for concrete prepared in examples 1 to 4 and comparative examples 1 to 3 was subjected to performance test, and concrete with a mass mixing ratio of single concrete of cement to fly ash to sand to stone to water to admixture of 432:48:688:1122:155:4.8 was used as a test object, cement was Etsheng PO 42.5 cement, fly ash was first-grade fly ash, sand was medium sand with a fineness modulus of 3.1, stone was crushed stone with a continuous gradation of 5mm to 20mm, and the admixture was a polycarboxylic acid high-performance admixture. And adding silica sol into the concrete to prepare silica sol concrete, wherein the concentration of the silica sol is 30%, the mixing amount is 3% of the mass of the cementing material in the concrete, and water in the silica sol is subtracted from the mixing water. The silica sol dispersion stabilizer for concrete, the aminotrimethylene phosphoric acid, the diethanol monoisopropanolamine and the dispersant solution prepared in example 1, which are prepared in examples 1-3 and comparative examples 1-3, are respectively added into the silica sol concrete, the mixing amount is 3.5% of the mass of the silica sol, the stability of the silica sol in the high-ion concentration concrete pore liquid is observed through a concrete pore liquid sedimentation test, and the 7d compressive strength and the 28d compressive strength of the concrete are tested according to GB/T50081-2002 general concrete mechanical property test method, and the results are shown in Table 1.
TABLE 1 comparison of Properties of silica sol dispersion stabilizers for concrete
Settling condition of adding silica sol into concrete pore liquid 7D compressive Strength (MPa) 28D compressive Strength (MPa)
Pore liquid / Concrete 43.6 60.2
Pore liquid + silica sol A large amount of sedimentation Concrete + silica sol 45.3 62.4
Interstitial fluid + silica sol + example 1 No sedimentation Concrete + silica sol + example 1 56.2 71.9
Interstitial fluid + silica sol + example 2 No sedimentation Concrete + silica sol + example 2 58.5 73.6
Interstitial fluid + silica sol + example 3 No sedimentation Concrete + silica sol + example 3 57.2 72.9
Interstitial fluid + silica sol + example 4 No sedimentation Concrete + silica sol + example 4 57.3 70.8
Pore liquid, silica sol and aminotrimethylene phosphate With precipitation Concrete, silica sol and amino-trimethylene phosphate 46.1 64.5
Pore liquid, silica sol and diethanol monoisopropanolamine With precipitation Concrete, silica sol and diethanol monoisopropanolamine 48.2 65.1
Pore liquid + silica sol + dispersant solution With precipitation Concrete + silica sol + dispersant solution 47.6 64.8
Pore fluid + silica sol + comparative example 1 Microprecipitation of Concrete + silica sol + comparative example 1 50.1 67.7
Pore fluid + silica sol + comparative example 2 Microprecipitation of Concrete + silica sol + comparative example 2 49.3 66.2
Pore fluid + silica sol + comparative example 3 Small amount of precipitate Concrete + silica sol + comparative example 3 51.6 68.4
From the above data, it can be seen that the silica sol dispersion stabilizer for concrete is not added, sedimentation and aggregation occur quickly when the silica sol dispersion stabilizer is added into the pore liquid of concrete, and the agglomerated particles become large and are difficult to exert nano characteristics, so that the effect of increasing the strength of concrete is greatly reduced, and the silica sol can still maintain a good dispersion state in the pore liquid of concrete after the silica sol dispersion stabilizer for concrete is added, so that the strength of concrete can be effectively improved. And compared with the method without adding the silica sol dispersion stabilizer, the silica sol dispersion stabilizer for the concrete provided by the invention is added into a concrete system, so that the 7d compressive strength and the 28d compressive strength of the concrete are improved by about 12 MPa.
The present application is not limited to the above-mentioned embodiments, and any changes or substitutions that can be easily understood by those skilled in the art within the technical scope of the present application are intended to be included in the scope of the present application. Therefore, the protection scope of the present application should be subject to the protection scope of the claims.

Claims (7)

1. The silica sol dispersion stabilizer for the concrete is characterized by comprising the following raw materials in parts by weight:
20-40 parts of aminotrimethylene phosphate, 10-20 parts of diethanol monoisopropanolamine and 40-70 parts of dispersant solution;
the preparation method of the dispersant solution comprises the following steps: adding water, maleic anhydride, dimethyl allyl ammonium chloride and sodium hypophosphite into a reactor, stirring and dissolving, then adding an acrylic acid solution and an ammonium persulfate solution for copolymerization, and cooling and regulating the pH value to obtain the dispersing agent solution.
2. The silica sol dispersion stabilizer for concrete according to claim 1, wherein the weight ratio of maleic anhydride, dimethylallyl ammonium chloride, sodium hypophosphite, acrylic acid solution and ammonium persulfate solution is (10-15): (6-8): (5-6): (50-55): (31.5-32).
3. The silica sol dispersion stabilizer for concrete according to claim 2, wherein the acrylic acid solution is composed of 30 to 35 parts by weight of acrylic acid and 20 parts by weight of water, and the ammonium persulfate solution is composed of 1.5 to 2 parts by weight of ammonium persulfate and 30 parts by weight of water.
4. The silica sol dispersion stabilizer for concrete according to claim 1, wherein the copolymerization temperature is 80 to 85 ℃, the atmosphere is nitrogen, and the time is 4 to 5 hours.
5. The method for preparing the silica sol dispersion stabilizer for concrete according to any one of claims 1 to 4, comprising the steps of: weighing the raw materials according to the parts by weight, mixing the aminotrimethylene phosphoric acid, the diethanol monoisopropanolamine and the dispersing agent solution, and uniformly stirring to obtain the silica sol dispersion stabilizer for the concrete.
6. The silica sol dispersion stabilizer for concrete according to any one of claims 1 to 4 or the silica sol dispersion stabilizer for concrete prepared by the preparation method according to claim 5, for use in concrete.
7. The use of the silica sol dispersion stabilizer for concrete according to claim 6, wherein the mixing amount of the silica sol dispersion stabilizer for concrete is 2-5% of the mass of the silica sol.
CN202410773387.8A 2024-06-17 2024-06-17 Silica sol dispersion stabilizer for concrete and preparation method and application thereof Active CN118388166B (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113264703A (en) * 2021-06-30 2021-08-17 河南砼道中人新材料技术有限公司 High-performance concrete glue reducing agent and preparation method thereof
CN115872654A (en) * 2021-09-27 2023-03-31 中国石油化工股份有限公司 Oil well cement settlement stabilizer, preparation method thereof and cement paste
CN115947560A (en) * 2023-03-13 2023-04-11 石家庄市长安育才建材有限公司 Additive for improving concrete workability and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113264703A (en) * 2021-06-30 2021-08-17 河南砼道中人新材料技术有限公司 High-performance concrete glue reducing agent and preparation method thereof
CN115872654A (en) * 2021-09-27 2023-03-31 中国石油化工股份有限公司 Oil well cement settlement stabilizer, preparation method thereof and cement paste
CN115947560A (en) * 2023-03-13 2023-04-11 石家庄市长安育才建材有限公司 Additive for improving concrete workability and preparation method thereof

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