CN111087551A - Method for continuously preparing polycarboxylate water reducing agent - Google Patents
Method for continuously preparing polycarboxylate water reducing agent Download PDFInfo
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- CN111087551A CN111087551A CN201911330107.1A CN201911330107A CN111087551A CN 111087551 A CN111087551 A CN 111087551A CN 201911330107 A CN201911330107 A CN 201911330107A CN 111087551 A CN111087551 A CN 111087551A
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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
- C04B24/2605—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing polyether side chains
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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
- C08F4/00—Polymerisation catalysts
- C08F4/40—Redox systems
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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
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- Curing Cements, Concrete, And Artificial Stone (AREA)
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Abstract
The invention discloses a method for continuously preparing a polycarboxylate water reducer, which comprises the steps of continuously introducing a macromonomer water solution into a pipeline reactor, simultaneously introducing an oxidant water solution, a small monomer water solution and a reducing agent water solution into the pipeline reactor in a three-section continuous mode, carrying out copolymerization reaction on a reaction liquid obtained by mixing the macromonomer water solution in the pipeline reactor, continuously introducing an alkaline solution for neutralization reaction after the copolymerization reaction is finished, adjusting the pH value, and continuously allowing the neutralized reaction liquid to move into a finished product storage tank in the pipeline reactor to obtain the polycarboxylate water reducer. The invention has the advantages that the production process is continuous, the production efficiency is improved, the process flow is simple, the water reducing rate of the polycarboxylate water reducing agent can reach more than 30 percent, and the polycarboxylate water reducing agent does not contain substances which influence the environment, such as formaldehyde, aromatic hydrocarbon and the like, so the polycarboxylate water reducing agent is also an environment-friendly water reducing agent.
Description
Technical Field
The invention relates to the technical field of concrete admixtures, in particular to a method for continuously preparing a polycarboxylate water reducing agent.
Background
With the rapid advance of national infrastructure, the vigorous development of concrete industry is driven, and people pay more and more attention to the improvement of concrete performance by using concrete admixtures. The polycarboxylate water reducing agent has many unique advantages as a concrete admixture, and is valued by people, for example, the water reducing agent has the advantages of relatively good compatibility with different cements, good fluidity of concrete when the mixing amount is low, low viscosity and relatively good slump retentivity when the water-cement ratio is low, environmental friendliness and the like.
At present, large-scale engineering is increasingly constructed, so that the requirement on the polycarboxylate water reducing agent is increasingly high, but in the prior art, the synthesis method of the polycarboxylate water reducing agent is complex in process and high in energy consumption, the production process has certain influence on the environment, and continuous production cannot be realized, so that the polycarboxylate water reducing agent with excellent performance and stable quality is developed, the requirement of economic construction is met, and the method has practical significance.
Disclosure of Invention
The invention aims to solve the problems and designs a method for continuously preparing a polycarboxylate water reducing agent.
The technical scheme of the invention is that the method for continuously preparing the polycarboxylate water reducing agent comprises the following steps:
s1, continuously introducing a macromonomer aqueous solution into a pipeline reactor, simultaneously introducing an oxidant aqueous solution, a small monomer aqueous solution and a reducing agent aqueous solution into the pipeline reactor in a three-section continuous mode, and carrying out copolymerization reaction on a reaction solution obtained by mixing the macromonomer aqueous solution in the pipeline reactor, wherein the introducing amount of the oxidant aqueous solution, the small monomer aqueous solution and the reducing agent aqueous solution in a first section in the three-section continuous mode is respectively 50%, and the introducing amount of the oxidant aqueous solution, the small monomer aqueous solution and the reducing agent aqueous solution in a second section and a third section is respectively 25%.
S2, after the copolymerization reaction is finished, continuously introducing an alkaline solution for neutralization reaction, adjusting the pH value, and continuously allowing the neutralized reaction liquid to move to a finished product storage tank in the pipeline reactor to obtain the polycarboxylate water reducing agent.
As a further description of the present invention, the first-stage inlet of the three-stage continuous process in S1 is preferably disposed at an inlet of the pipeline reactor into which the aqueous solution of the macromonomer is introduced, the second-stage inlet is preferably disposed at a position at which the reaction solution advances in the pipeline reactor for 0.5 hour, the third-stage inlet is preferably disposed at a position at which the reaction solution advances in the pipeline reactor for 1 hour, the alkaline solution in S2 is preferably a sodium hydroxide solution, and the inlet of the alkaline solution is preferably disposed at a position which is a distance from the third-stage inlet and a distance from the finished product storage tank.
As a further illustration of the present invention, the distance from the inlet of the alkaline solution to the inlet of the third section is preferably a distance of 1 to 4 hours for the reactants to travel in the pipeline reactor, and the distance from the finished product storage tank is preferably a distance of 0.5 hours for the reaction solution to travel in the pipeline reactor.
As a further illustration of the invention, the macromonomer in S1 is preferably one or two of prenyl polyoxyethylene ether or isobutenyl polyoxyethylene ether; the oxidant is preferably one or two of sodium persulfate, ammonium persulfate, potassium persulfate and hydrogen peroxide; the small monomer is preferably one or a mixture of methacrylic acid or acrylic acid; the reducing agent is preferably one or two of sodium sulfite, sodium bisulfite and vitamin C.
As a further illustration of the present invention, the molecular weight of the macromonomer in S1 is preferably 2000-3000, the molar ratio of the macromonomer to the small monomer is preferably 1:2-1:10, the amount of the oxidant is preferably 0.01-5% of the total mass of the macromonomer and the small monomer, and the amount of the reductant is preferably 0.01-2% of the total mass of the macromonomer and the small monomer.
As a further illustration of the present invention, the reaction temperature of the copolymerization reaction in S1 is preferably room temperature, and the reaction time is preferably 2.5 to 6 hours.
As a further illustration of the invention, the pH of S2 is preferably adjusted to 7-9 by the addition of the sodium hydroxide solution.
As a further illustration of the invention, the water reducing rate of the polycarboxylate water reducing agent reaches more than 30%.
The method has the beneficial effects that the initiation mode adopted by the copolymerization reaction in the preparation method is redox initiation, the oxidant and the reducing agent form the initiator, the pipeline reactor and the three-section continuous mode are adopted, the production process is continuous, the production efficiency is improved, meanwhile, the setting of the distance of the inlet of the alkaline solution ensures the time of the copolymerization reaction, the interval distance is too short, the reaction is incomplete, the interval distance is too long, and the production efficiency is reduced, so the polycarboxylate water reducing agent with excellent performance and stable quality is obtained by the selection of process control and a formula, the process flow is simple, and the resource waste caused by multi-step reaction can be avoided; the polycarboxylate water reducing agent has higher water reducing effect, and the water reducing rate can reach more than 30%; the polycarboxylate water reducing agent does not contain substances which affect the environment, such as formaldehyde, aromatic hydrocarbon and the like, so the polycarboxylate water reducing agent is also an environment-friendly water reducing agent.
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FIG. 1 is a schematic diagram of the working principle of the present invention;
fig. 2 is a schematic cross-sectional view of the segments of the present invention.
Detailed Description
Firstly, the research of the invention is designed for the purpose that the polycarboxylate water reducing agent has relatively good compatibility with different cements, can enable concrete to have good fluidity when the mixing amount is low, has the superior characteristics of low viscosity and relatively good slump retentivity when the water-cement ratio is low, is environment-friendly and the like, so that the requirement on the polycarboxylate water reducing agent is higher and higher, but the synthesis method of the polycarboxylate water reducing agent in the prior art has complex process and high energy consumption, has certain influence on the environment in the production process, and cannot be continuously produced, so that the invention researches the polycarboxylate water reducing agent with excellent performance and stable quality.
The invention will be further described with reference to the accompanying drawings in which:
for the sake of simplicity, MAA means "methacrylic acid", AA means "acrylic acid", TPEG means "prenyl polyoxyethylene ether", and HPEG means "isobutenyl polyoxyethylene ether".
Example 1 (a) starting material:
aqueous solution of macromonomer: 2200g of TPEG-2200 (molecular weight 2200) and 2200ml of water;
aqueous solution of small monomers: 86gMAA, 216gAA and 300ml water;
aqueous solution of oxidizing agent: 51g ammonium persulfate and 400ml water;
aqueous solution of reducing agent: 12.5g of sodium sulfite, 5g of vitamin C and 400ml of water.
(II) the process steps:
s1, continuously introducing a macromonomer aqueous solution into a pipeline reactor, simultaneously introducing an oxidant aqueous solution, a small monomer aqueous solution and a reducing agent aqueous solution from a first section of inlet arranged at an inlet of the macromonomer aqueous solution into the pipeline reactor, wherein the introduction amount of the first section is 50% respectively, introducing the oxidant aqueous solution, the small monomer aqueous solution and the reducing agent aqueous solution from a second section of inlet arranged at a position where a reaction solution reaches in the pipeline reactor after 0.5 hour of advancing, wherein the introduction amount of the second section is 25% respectively, introducing the oxidant aqueous solution, the small monomer aqueous solution and the reducing agent aqueous solution from a third section of inlet arranged at a position where the reaction solution reaches in the pipeline reactor after 1 hour of advancing, wherein the introduction amount of the third section is 25% respectively, and continuously carrying out copolymerization reaction on the mixed reaction solution in the pipeline reactor at room temperature.
S2, after the copolymerization reaction is finished, introducing a sodium hydroxide solution into an alkaline solution inlet which is arranged at a distance from a third section inlet and is a distance that a reactant travels in the pipeline reactor for 1.5 hours and a distance from a finished product storage tank is a distance that a reaction solution travels in the pipeline reactor for 0.5 hour for neutralization reaction, adjusting the pH value to 7-9, and continuously moving the neutralized reaction solution into a finished product storage tank in the pipeline reactor to obtain the polycarboxylate water reducer.
Example 2 (a) starting material:
aqueous solution of macromonomer: 1200g of TPEG-2400, 1200g of HPEG-2400 (molecular weight 2400), and 2400ml of water;
aqueous solution of small monomers: 360gAA and 300ml water;
aqueous solution of oxidizing agent: 27.6g of ammonium persulfate, 13.8g of hydrogen peroxide and 400ml of water are mixed;
aqueous solution of reducing agent: 8.3g vitamin C was mixed with 400ml water.
(II) the process steps:
s1, continuously introducing a macromonomer aqueous solution into a pipeline reactor, simultaneously introducing an oxidant aqueous solution, a small monomer aqueous solution and a reducing agent aqueous solution from a first section of inlet arranged at an inlet of the macromonomer aqueous solution into the pipeline reactor, wherein the introduction amount of the first section is 50% respectively, introducing the oxidant aqueous solution, the small monomer aqueous solution and the reducing agent aqueous solution from a second section of inlet arranged at a position where a reaction solution reaches in the pipeline reactor after 0.5 hour of advancing, wherein the introduction amount of the second section is 25% respectively, introducing the oxidant aqueous solution, the small monomer aqueous solution and the reducing agent aqueous solution from a third section of inlet arranged at a position where the reaction solution reaches in the pipeline reactor after 1 hour of advancing, wherein the introduction amount of the third section is 25% respectively, and continuously carrying out copolymerization reaction on the mixed reaction solution in the pipeline reactor at room temperature.
S2, after the copolymerization reaction is finished, introducing a sodium hydroxide solution into an alkaline solution inlet which is arranged at a distance from a third section of inlet opening and is a distance that a reactant travels in the pipeline reactor for 2 hours and a distance from a finished product storage tank is a distance that a reaction solution travels in the pipeline reactor for 0.5 hour for neutralization reaction, adjusting the pH value to 7-9, and continuously moving the neutralized reaction solution in the pipeline reactor to the finished product storage tank to obtain the polycarboxylate water reducer.
Example 3 (a) starting material:
aqueous solution of macromonomer: 2500g of HPEG-2500 is mixed with 2500ml of water;
aqueous solution of small monomers: 86gMAA, 288gAA and 300ml water;
aqueous solution of oxidizing agent: mixing 21g of hydrogen peroxide, 14g of potassium persulfate and 400ml of water;
aqueous solution of reducing agent: 35g of sodium bisulfite were mixed with 400ml of water.
(II) the process steps:
s1, continuously introducing a macromonomer aqueous solution into a pipeline reactor, simultaneously introducing an oxidant aqueous solution, a small monomer aqueous solution and a reducing agent aqueous solution from a first section of inlet arranged at an inlet of the macromonomer aqueous solution into the pipeline reactor, wherein the introduction amount of the first section is 50% respectively, introducing the oxidant aqueous solution, the small monomer aqueous solution and the reducing agent aqueous solution from a second section of inlet arranged at a position where a reaction solution reaches in the pipeline reactor after 0.5 hour of advancing, wherein the introduction amount of the second section is 25% respectively, introducing the oxidant aqueous solution, the small monomer aqueous solution and the reducing agent aqueous solution from a third section of inlet arranged at a position where the reaction solution reaches in the pipeline reactor after 1 hour of advancing, wherein the introduction amount of the third section is 25% respectively, and continuously carrying out copolymerization reaction on the mixed reaction solution in the pipeline reactor at room temperature.
S2, after the copolymerization reaction is finished, introducing a sodium hydroxide solution into an alkaline solution inlet which is arranged at a distance from a third section of inlet opening and is a distance that a reactant travels in the pipeline reactor for 3 hours and a distance from a finished product storage tank is a distance that a reaction solution travels in the pipeline reactor for 0.5 hour for neutralization reaction, adjusting the pH value to 7-9, and continuously moving the neutralized reaction solution in the pipeline reactor to the finished product storage tank to obtain the polycarboxylate water reducer.
Example 4 (a) starting material:
aqueous solution of macromonomer: 2400g of TPEG-3000, 400g of HPEG-2000 and 2800ml of water;
aqueous solution of small monomers: 172g MAA, 360gAA and 300ml water;
aqueous solution of oxidizing agent: 21g of hydrogen peroxide and 400ml of water are mixed;
aqueous solution of reducing agent: 10g of sodium bisulfite, 16g of vitamin C and 400ml of water.
(II) the process steps:
s1, continuously introducing a macromonomer aqueous solution into a pipeline reactor, simultaneously introducing an oxidant aqueous solution, a small monomer aqueous solution and a reducing agent aqueous solution from a first section of inlet arranged at an inlet of the macromonomer aqueous solution into the pipeline reactor, wherein the introduction amount of the first section is 50% respectively, introducing the oxidant aqueous solution, the small monomer aqueous solution and the reducing agent aqueous solution from a second section of inlet arranged at a position where a reaction solution reaches in the pipeline reactor after 0.5 hour of advancing, wherein the introduction amount of the second section is 25% respectively, introducing the oxidant aqueous solution, the small monomer aqueous solution and the reducing agent aqueous solution from a third section of inlet arranged at a position where the reaction solution reaches in the pipeline reactor after 1 hour of advancing, wherein the introduction amount of the third section is 25% respectively, and continuously carrying out copolymerization reaction on the mixed reaction solution in the pipeline reactor at room temperature.
S2, after the copolymerization reaction is finished, introducing a sodium hydroxide solution into an alkaline solution inlet which is arranged at a distance from a third section of inlet opening and is a distance that a reactant travels in the pipeline reactor for 3.5 hours and a distance from a finished product storage tank is a distance that a reaction liquid travels in the pipeline reactor for 0.5 hour for neutralization reaction, adjusting the pH value to 7-9, and continuously moving the neutralized reaction liquid into a finished product storage tank in the pipeline reactor to obtain the polycarboxylate water reducer.
The polycarboxylate water reducing agents obtained in the above examples were measured according to the standard of GB8076 to obtain table 1.
Example 1 | Example 2 | Example 3 | Example 4 | |
Water reduction rate% | 31 | 34 | 35 | 32 |
As can be seen from Table 1, the water-reducing rates of the polycarboxylate water-reducing agents are all greater than 30%.
The technical solutions described above only represent the preferred technical solutions of the present invention, and some possible modifications to some parts of the technical solutions by those skilled in the art all represent the principles of the present invention, and fall within the protection scope of the present invention.
Claims (8)
1. A method for continuously preparing a polycarboxylate water reducing agent is characterized by comprising the following steps:
s1, continuously introducing a macromonomer aqueous solution into a pipeline reactor, simultaneously introducing an oxidant aqueous solution, a small monomer aqueous solution and a reducing agent aqueous solution into the pipeline reactor in a three-section continuous mode, and carrying out copolymerization reaction on a reaction solution obtained by mixing the macromonomer aqueous solution in the pipeline reactor, wherein the introducing amount of the oxidant aqueous solution, the small monomer aqueous solution and the reducing agent aqueous solution in a first section in the three-section continuous mode is respectively 50%, and the introducing amount of the oxidant aqueous solution, the small monomer aqueous solution and the reducing agent aqueous solution in a second section and a third section is respectively 25%;
s2, after the copolymerization reaction is finished, continuously introducing an alkaline solution for neutralization reaction, adjusting the pH value, and continuously allowing the neutralized reaction liquid to move to a finished product storage tank in the pipeline reactor to obtain the polycarboxylate water reducing agent.
2. The method for continuously preparing the polycarboxylate water reducing agent according to the name of claim 1, wherein the first section of the inlet of the aqueous solution of the macromonomer into the pipeline reactor in the three-section continuous mode in the S1 is preferably arranged at a position where the reaction liquid reaches in the pipeline reactor after 0.5 hour of traveling, the third section of the inlet is preferably arranged at a position where the reaction liquid reaches in the pipeline reactor after 1 hour of traveling, the alkaline solution in the S2 is preferably sodium hydroxide solution, and the inlet of the alkaline solution is preferably arranged at a position which is at a certain distance from the third section of the inlet and at a certain distance from the finished product storage tank.
3. The method for continuously preparing the polycarboxylate water reducer according to claim 2, characterized in that the distance between the inlet of the alkaline solution and the inlet of the third section is preferably 1-4 hours for the reactants to travel in the pipeline reactor, and the distance between the inlet of the alkaline solution and the finished product storage tank is preferably 0.5 hours for the reaction liquid to travel in the pipeline reactor.
4. The method for continuously preparing the polycarboxylate water reducer according to claim 1, wherein the macromonomer in S1 is preferably one or two of prenyl polyoxyethylene ether and isobutenyl polyoxyethylene ether; the oxidant is preferably one or two of sodium persulfate, ammonium persulfate, potassium persulfate and hydrogen peroxide; the small monomer is preferably one or a mixture of methacrylic acid or acrylic acid; the reducing agent is preferably one or two of sodium sulfite, sodium bisulfite and vitamin C.
5. The method for continuously preparing the polycarboxylate water reducer as claimed in claim 1, wherein the molecular weight of the macromonomer in the S1 is preferably 2000-3000, the molar ratio of the macromonomer to the small monomer is preferably 1:2-1:10, the amount of the oxidant is preferably 0.01-5% of the total mass of the macromonomer and the small monomer, and the amount of the reducing agent is preferably 0.01-2% of the total mass of the macromonomer and the small monomer.
6. The method for continuously preparing the polycarboxylate water reducer according to the claim 1, wherein the reaction temperature of the copolymerization reaction in the S1 is preferably room temperature, and the reaction time is preferably 2.5-6 hours.
7. The method for continuously preparing the polycarboxylate water reducer according to the claim 1, wherein the pH value is preferably adjusted to 7-9 by adding the sodium hydroxide solution into the S2.
8. The method for continuously preparing the polycarboxylate water reducer according to claim 1, characterized in that the water reduction rate of the polycarboxylate water reducer is more than 30%.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN112999993A (en) * | 2021-02-08 | 2021-06-22 | 乌兰浩特市圣益商砼有限公司 | Vortex-spraying two-stage strengthening reactor for preparing polycarboxylate superplasticizer and preparation method |
CN114870785A (en) * | 2021-12-17 | 2022-08-09 | 广东科隆智谷新材料股份有限公司 | Continuous reaction equipment for preparing polycarboxylate superplasticizer |
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CN103537241A (en) * | 2013-10-16 | 2014-01-29 | 北京新奥混凝土集团有限公司 | Single-channel tubular reaction device for producing polycarboxylate superplasticizer |
CN207694770U (en) * | 2017-12-14 | 2018-08-07 | 山西康特尔精细化工有限责任公司 | The efficient production layout structure of polycarboxylate water-reducer |
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Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN103537241A (en) * | 2013-10-16 | 2014-01-29 | 北京新奥混凝土集团有限公司 | Single-channel tubular reaction device for producing polycarboxylate superplasticizer |
CN207694770U (en) * | 2017-12-14 | 2018-08-07 | 山西康特尔精细化工有限责任公司 | The efficient production layout structure of polycarboxylate water-reducer |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN112999993A (en) * | 2021-02-08 | 2021-06-22 | 乌兰浩特市圣益商砼有限公司 | Vortex-spraying two-stage strengthening reactor for preparing polycarboxylate superplasticizer and preparation method |
CN112999993B (en) * | 2021-02-08 | 2023-04-07 | 乌兰浩特市圣益商砼有限公司 | Vortex-spraying two-stage strengthening reactor for preparing polycarboxylate superplasticizer and preparation method |
CN114870785A (en) * | 2021-12-17 | 2022-08-09 | 广东科隆智谷新材料股份有限公司 | Continuous reaction equipment for preparing polycarboxylate superplasticizer |
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Application publication date: 20200501 |