CN112358221A - Formula and preparation method of water-reducing solid polycarboxylate superplasticizer - Google Patents
Formula and preparation method of water-reducing solid polycarboxylate superplasticizer Download PDFInfo
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- 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
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
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- 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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- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/30—Water reducers, plasticisers, air-entrainers, flow improvers
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Abstract
The invention discloses a water-reducing solid polycarboxylic acid water reducing agent formula which mainly comprises the following raw materials in parts by weight: 50-4000 parts of unsaturated polyoxyethylene ether 36, 390-410 parts of acrylic acid, 14-16 parts of mercaptopropionic acid, 21-23 parts of an oxidant, 10-14 parts of a reducing agent, 10-20 parts of an auxiliary agent, 80-100 parts of soft water, 10-12 parts of a thermal decomposition initiator, 14-18 parts of a neutralizing agent, 50-90 parts of unsaturated carboxylic acid small monomer, 9-12 parts of an organic reducing agent, 10-16 parts of a chain transfer agent, 22-26 parts of benzoyl peroxide, 20-22 parts of azodiisobutyronitrile, 100-200 parts of unsaturated amide small monomer, 14-16 parts of an anticorrosive bactericide and 13-17 parts of a thickening agent. The invention has the technical effects of product performance, good product performance and stability, long durability and strong adaptability, and realizes low mixing amount, high water reduction and high slump retaining.
Description
Technical Field
The invention relates to the technical field of water reducing agent formulas and processes, in particular to a formula of a water reducing type solid polycarboxylic acid water reducing agent and a preparation method thereof.
Background
At present, the polycarboxylate superplasticizer generally has a solid content of 40-60%, and then other auxiliary agents are added according to the actual conditions of each stirring station, so that 10-25% of the solid content is compounded and transported to the stirring station for use. This is only suitable for short distances, not for long distances and remote locations, which increases costs. Additive companies are really about to develop solid polycarboxylic acid plasticizers.
CN 106543382A is a solid sheet-like polycarboxylic acid water reducing agent and a polymerization preparation method thereof. Specifically, the method comprises the following steps: placing the polyether macromonomer in a reaction kettle, heating and stirring until the polyether macromonomer is completely melted, wherein the stable temperature is 65-75, adding weak chain transfer agents (sodium hypophosphite, sodium formate and sodium polyphosphate)), organic peroxy initiators, unsaturated dicarboxylic acids (itaconic acid and fumaric acid) and 1/3 acrylic acid at one time, then beginning to dropwise add 2/3 acrylic acid and strong chain transfer agents, adding the azo initiators twice in the dropwise adding process, curing for 1-2 hours after the dropwise adding is finished, adding a neutralizer, cooling and slicing to obtain a finished product.
CN 106749968A is a preparation method of an early-strength solid polycarboxylic acid water reducer. The method comprises the following specific steps: 1, adding an unsaturated polyether monomer into a reaction kettle to enable the unsaturated polyether monomer to be in a molten state, then adding a catalyst at one time, and uniformly stirring; 2, respectively dripping a first mixed solution (acrylic acid, a chloride ion-containing quaternary ammonium cationic monomer) and a second mixed solution (an initiator, a chain transfer agent and an organic solvent) into the material obtained in the step, and continuing to react after finishing dripping; and 3, after the reaction is finished, adopting a mechanical pump to pump odor and vacuum, removing the organic solvent in the material obtained in the step 2, and then adopting a condensation slicing machine to slice, thus obtaining the white flaky solid polycarboxylate superplasticizer.
CN 106749970A is a solid-tablet polycarboxylic slump retaining agent and a preparation method thereof. Specifically, the method comprises the following steps: placing a polyether macromonomer in a reaction kettle, heating and stirring until the polyether macromonomer is completely dissolved, wherein the stable temperature is 65-75, adding a weak chain transfer agent (sodium hypophosphite, sodium formate and sodium polyphosphate)), an organic peroxy initiator, unsaturated dicarboxylic acid (itaconic acid and fumaric acid) and an unsaturated sulfonic acid small monomer at one time, then adding concentrated sulfuric acid, and adjusting the pH value of a base solution to 5.0; and (3) starting to dropwise add acrylic acid, hydroxyalkyl acrylate and a strong chain transfer agent, adding the azo initiator twice in the dropwise adding process, curing for 1-2 hours after dropwise adding is finished, adding a neutralizing agent, cooling and slicing to obtain a finished product.
None of the above-identified patents relate to the effect of system viscosity on product properties during synthesis. In fact, in the polymerization process, the increase of the system concentration can cause slow permeation or poor compatibility among an oxidant, a reducing agent, a polyether macromonomer and an acrylic acid small monomer in the reaction process, thereby causing the produced product to be poor.
Disclosure of Invention
The invention aims to provide a formula of a water-reducing solid polycarboxylic acid water reducing agent and a preparation method thereof, and aims to solve the problems in the background art.
In order to realize the purpose, the invention provides the following technical scheme: the formula of the water-reducing solid polycarboxylate superplasticizer mainly comprises the following raw materials in parts by weight: 50-4000 parts of unsaturated polyoxyethylene ether 36, 390-410 parts of acrylic acid, 14-16 parts of mercaptopropionic acid, 21-23 parts of an oxidant, 10-14 parts of a reducing agent, 10-20 parts of an auxiliary agent, 80-100 parts of soft water, 10-12 parts of a thermal decomposition initiator, 14-18 parts of a neutralizing agent, 50-90 parts of unsaturated carboxylic acid small monomer, 9-12 parts of an organic reducing agent, 10-16 parts of a chain transfer agent, 22-26 parts of benzoyl peroxide, 20-22 parts of azodiisobutyronitrile, 100-200 parts of unsaturated amide small monomer, 14-16 parts of an anticorrosive bactericide and 13-17 parts of a thickening agent.
Preferably, the oxidant is hydrogen peroxide and ammonium persulfate.
Preferably, the reducing agent is sodium hypophosphite.
Preferably, the auxiliary agent is sodium polyether phosphate and sodium polyether sulfate.
Preferably, the thermal decomposition initiator is one or more of azodiisobutyronitrile, azodiisoheptonitrile, azodiisobutyronitrile dimethyl ester, ammonium persulfate and potassium persulfate.
Preferably, the neutralizing agent is one or more of potassium hydroxide aqueous solution, sodium hydroxide aqueous solution, ethanolamine, diethanolamine and triethanolamine.
Preferably, the unsaturated carboxylic small monomer is one or more of methacrylic acid, maleic anhydride, itaconic acid and fumaric acid.
Preferably, the organic reducing agent is one or more of L-ascorbic acid, N-methylaniline, N-ethylaniline, N-dimethylaniline and N, N-diethylaniline.
Preferably, the unsaturated polyoxyethylene ether is one or more of isobutylene polyoxyethylene ether, allyl alcohol polyoxyethylene ether, isopentenol polyoxyethylene ether and methyl allyl polyoxyethylene ether, and the average molecular weight is 2400-4000.
A preparation method of a water-reducing solid polycarboxylate superplasticizer specifically comprises the following steps:
the method comprises the following steps: placing two unsaturated carboxylic acid small monomers and unsaturated amide small monomers with different molecular weights in a thermocouple reaction kettle, heating and melting, adding a thermal decomposition initiator and an organic reducing agent, and mixing and stirring for 30-50 min;
step two: then, beginning to dropwise add a mixed solution of a chain transfer agent, benzoyl peroxide and azobisisobutyronitrile 2 into the mixture obtained in the step one, wherein the dropwise adding time is 2-8 hours;
step three: after the dropwise addition is finished, preserving heat for 1.5-3 h at the melting temperature, and after the free radical bulk polymerization reaction is finished, adjusting the pH value to 5-6 by using a neutralizer to prepare an additive;
step four: placing the acrylic acid and the mercaptopropionic acid into a four-neck flask provided with a thermometer, a speed-regulating stirrer, a reflux condenser tube and a dropping device, starting stirring, keeping the rotating speed at 120r/min, and mixing and stirring for 30-50 min to prepare a material A;
step five: placing sodium phosphate and polyether sodium phosphate into a four-neck flask provided with a thermometer, a speed-regulating stirrer, a reflux condenser tube and a dropping device, starting stirring and keeping the rotating speed at 120r/min, adding soft water, mixing and stirring for 40-50 min, and preparing a material B;
step six: adding methallyl polyoxyethylene ether 2400 into a heat-insulating four-neck flask provided with a thermometer, a speed-regulating stirrer, a reflux condenser pipe and a dropping device under stirring, and heating to 60-65 ℃;
step seven: adding hydrogen peroxide, ammonium sulfate and soft water mixed solution, and then simultaneously dripping the material A and the material B, wherein the material A is uniformly dripped after 2-4 hours, and the material B is uniformly dripped after 3-4 hours;
step seven: and after the material B is dripped, adding the additive, the antiseptic bactericide and the thickening agent prepared in the third step, mixing and stirring for 1-2 hours, curing for 1.5 hours, and then cooling and slicing.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention discloses a formula and a preparation method of a water-reducing solid polycarboxylic acid water reducing agent, aiming at overcoming the defect that the performance of a product is reduced due to the fact that an oxidant and a reducing agent are difficult to permeate in a polyether macromonomer and a small monomer because the viscosity of a system is large in the reaction process, and the compatibility of the oxidant and the reducing agent with the polyether macromonomer and an inorganic structure is improved by introducing an auxiliary agent with the polyether structure and the inorganic structure by utilizing the principle of similar intermiscibility, so that the improvement of the performance of the product is facilitated.
2. According to the formula and the preparation method of the water-reducing solid polycarboxylic acid water reducing agent, the performance of the water-reducing solid polycarboxylic acid water reducing agent provided by the invention is unchanged after dissolution, the neat paste dispersing performance, the water-reducing dispersing performance, the fluidity and the slump retaining capacity are excellent, and the product performance with low dosage, high water reduction and high slump retaining performance is realized.
3. The water-reducing solid polycarboxylate superplasticizer provided by the invention can be prepared into a sheet shape according to application requirements, has good stability, long durability and strong adaptability, can greatly reduce the transportation cost and the packaging cost, and is suitable for long-distance transportation and export.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the 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.
The invention provides a technical scheme that: the formula of the water-reducing solid polycarboxylate superplasticizer mainly comprises the following raw materials in parts by weight: 50-4000 parts of unsaturated polyoxyethylene ether 36, 390-410 parts of acrylic acid, 14-16 parts of mercaptopropionic acid, 21-23 parts of an oxidant, 10-14 parts of a reducing agent, 10-20 parts of an auxiliary agent, 80-100 parts of soft water, 10-12 parts of a thermal decomposition initiator, 14-18 parts of a neutralizing agent, 50-90 parts of unsaturated carboxylic acid small monomer, 9-12 parts of an organic reducing agent, 10-16 parts of a chain transfer agent, 22-26 parts of benzoyl peroxide, 20-22 parts of azodiisobutyronitrile, 100-200 parts of unsaturated amide small monomer, 14-16 parts of an anticorrosive bactericide and 13-17 parts of a thickening agent.
Preferably, the oxidant is hydrogen peroxide and ammonium persulfate.
Preferably, the reducing agent is sodium hypophosphite.
Preferably, the auxiliary agent is sodium polyether phosphate and sodium polyether sulfate.
Preferably, the thermal decomposition initiator is one or more of azodiisobutyronitrile, azodiisoheptonitrile, azodiisobutyronitrile dimethyl ester, ammonium persulfate and potassium persulfate.
Preferably, the neutralizing agent is one or more of potassium hydroxide aqueous solution, sodium hydroxide aqueous solution, ethanolamine, diethanolamine and triethanolamine.
Preferably, the unsaturated carboxylic small monomer is one or more of methacrylic acid, maleic anhydride, itaconic acid and fumaric acid.
Preferably, the organic reducing agent is one or more of L-ascorbic acid, N-methylaniline, N-ethylaniline, N-dimethylaniline and N, N-diethylaniline.
Preferably, the unsaturated polyoxyethylene ether is one or more of isobutylene polyoxyethylene ether, allyl alcohol polyoxyethylene ether, isopentenol polyoxyethylene ether and methyl allyl polyoxyethylene ether, and the average molecular weight is 2400-4000.
A preparation method of a water-reducing solid polycarboxylate superplasticizer specifically comprises the following steps:
the method comprises the following steps: placing two unsaturated carboxylic acid small monomers and unsaturated amide small monomers with different molecular weights in a thermocouple reaction kettle, heating and melting, adding a thermal decomposition initiator and an organic reducing agent, and mixing and stirring for 30-50 min;
step two: then, beginning to dropwise add a mixed solution of a chain transfer agent, benzoyl peroxide and azobisisobutyronitrile 2 into the mixture obtained in the step one, wherein the dropwise adding time is 2-8 hours;
step three: after the dropwise addition is finished, preserving heat for 1.5-3 h at the melting temperature, and after the free radical bulk polymerization reaction is finished, adjusting the pH value to 5-6 by using a neutralizer to prepare an additive;
step four: placing the acrylic acid and the mercaptopropionic acid into a four-neck flask provided with a thermometer, a speed-regulating stirrer, a reflux condenser tube and a dropping device, starting stirring, keeping the rotating speed at 120r/min, and mixing and stirring for 30-50 min to prepare a material A;
step five: placing sodium phosphate and polyether sodium phosphate into a four-neck flask provided with a thermometer, a speed-regulating stirrer, a reflux condenser tube and a dropping device, starting stirring and keeping the rotating speed at 120r/min, adding soft water, mixing and stirring for 40-50 min, and preparing a material B;
step six: adding methallyl polyoxyethylene ether 2400 into a heat-insulating four-neck flask provided with a thermometer, a speed-regulating stirrer, a reflux condenser pipe and a dropping device under stirring, and heating to 60-65 ℃;
step seven: adding hydrogen peroxide, ammonium sulfate and soft water mixed solution, and then simultaneously dripping the material A and the material B, wherein the material A is uniformly dripped after 2-4 hours, and the material B is uniformly dripped after 3-4 hours;
step seven: and after the material B is dripped, adding the additive, the antiseptic bactericide and the thickening agent prepared in the third step, mixing and stirring for 1-2 hours, curing for 1.5 hours, and then cooling and slicing.
Under the condition of ensuring that the preparation methods of the first step, the second step, the third step, the fourth step, the fifth step and the seventh step are not changed, the water-reducing solid polycarboxylic acid water reducing agent is prepared according to the following examples.
Example one
3650 g of methyl allyl polyoxyethylene ether 2400 is added into a heat-preservation four-neck flask provided with a thermometer, a speed-regulating stirrer, a reflux condenser and a dropping device under stirring, the temperature is raised to 60-65 ℃, then 21 g of hydrogen peroxide (3.6 g of ammonium persulfate +8 g of water) mixed solution is added, then a material A (390 g of acrylic acid, 14 g of mercaptopropionic acid) and a material B (10 g of sodium hypophosphite and 82 g of water) are simultaneously dropped, the material A is uniformly dropped for 3 hours, the material B is uniformly dropped for 3.5 hours, after the material B is dropped, the material B is cured for 1.5 hours, and then the slices are cooled.
Example two
3650 g of methyl allyl polyoxyethylene ether 2400 and 5 g of polyether sodium sulfate are added into a heat-insulating four-neck flask provided with a thermometer, a speed-regulating stirrer, a reflux condenser and a dropping device under stirring, the mixture is heated to 60-65 ℃, then 21 g of hydrogen peroxide and (3.6 g of ammonium persulfate and 8 g of water) are added, then a material A (390 g of acrylic acid and 14 g of mercaptopropionic acid) and a material B (10 g of sodium hypophosphite, 5 g of polyether sodium phosphate and 82 g of water) are simultaneously dropped, the material A is uniformly dropped for 3 hours, the material B is uniformly dropped for 3.5 hours, after the material B is dropped, the material B is cured for 1.5 hours and then is cooled and sliced.
EXAMPLE III
3650 g of methyl allyl polyoxyethylene ether 2400 and 5 g of polyether sodium sulfate are added into a heat-insulating four-neck flask provided with a thermometer, a speed-regulating stirrer, a reflux condenser and a dropping device under stirring, the mixture is heated to 60-65 ℃, then 21 g of hydrogen peroxide and a mixed solution of 3.6 g of ammonium persulfate and 8 g of water are added, then a material A (390 g of acrylic acid and 14 g of mercaptopropionic acid) and a material B (10 g of sodium hypophosphite and 82 g of water) are simultaneously dropped, the material A is uniformly dropped for 3 hours, the material B is uniformly dropped for 3.5 hours, after the material B is dropped, the material B is cured for 1.5 hours, and then the slices are cooled.
Example four
3650 g of methyl allyl polyoxyethylene ether 2400 is added into a heat-preservation four-neck flask provided with a thermometer, a speed-regulating stirrer, a reflux condenser and a dropping device under stirring, the temperature is raised to 60-65 ℃, then 21 g of hydrogen peroxide (3.6 g of ammonium persulfate +8 g of water) mixed solution is added, then a material A (390 g of acrylic acid, 14 g of mercaptopropionic acid) and a material B (10 g of sodium hypophosphite, 5 g of polyether sodium phosphate and 82 g of water) are simultaneously dropped, the material A is uniformly dropped for 3 hours, the material B is uniformly dropped for 3.5 hours, after the material B is dropped, the material B is cured for 1.5 hours, and then the slices are cooled.
Experiment one: after the water reducing agents prepared in the first embodiment, the second embodiment, the third embodiment, the fourth embodiment and the fifth embodiment are applied to the same concrete, gel permeation chromatography instrument tests are respectively carried out, and the test conditions are as follows: the column temperature is 40 ℃, the flow rate is 0.6 ml/min, the sample injection amount is 1%, and the data of a test spectrogram are shown in the following table:
the experimental results are as follows: from the analysis of the spectrogram data, the main peak content of the embodiment I without adding the sodium polyether sulfate and the sodium polyether phosphate is the minimum, and the main peak content of the embodiment II with adding the sodium polyether sulfate and the sodium polyether phosphate is the maximum. Sodium polyether phosphate alone has a greater main peak content than sodium polyether sulfate alone.
Experiment two: the water reducing agents prepared in the first embodiment, the second embodiment, the third embodiment, the fourth embodiment and the fifth embodiment are applied to the same concrete and then are subjected to slump tests and slump tests, and the test data are shown in the following table:
the experimental results are as follows: from the concrete evaluation, the concrete performance is the worst in the first embodiment in which neither sodium polyether sulfate nor sodium polyether phosphate is added, and the concrete performance is the best in the second embodiment in which both sodium polyether sulfate and sodium polyether phosphate are added. The performance of the concrete is better when only sodium polyether phosphate is added than when only sodium polyether sulfate is added.
According to the comprehensive gel permeation chromatography table and concrete evaluation, the invention is effective, namely, the auxiliary agent with a polyether structure and an inorganic catalyst structure is introduced by utilizing the similar intermiscibility principle, so that the compatibility and permeability of the oxidant and the reducing agent in small monomers such as polyether macromonomer, acrylic acid and the like are facilitated, and the product performance is improved.
The technical effects are as follows: the invention discloses a formula and a preparation method of a water-reducing solid polycarboxylic acid water reducing agent, aiming at overcoming the defect that the performance of a product is reduced due to the fact that an oxidant and a reducing agent are difficult to permeate in a polyether macromonomer and a small monomer because the viscosity of a system is large in the reaction process, and the compatibility of the oxidant and the reducing agent with the polyether macromonomer and an inorganic structure is improved by introducing an auxiliary agent with the polyether structure and the inorganic structure by utilizing the principle of similar intermiscibility, so that the improvement of the performance of the product is facilitated. According to the formula and the preparation method of the water-reducing solid polycarboxylic acid water reducing agent, the performance of the water-reducing solid polycarboxylic acid water reducing agent provided by the invention is unchanged after dissolution, the neat paste dispersing performance, the water-reducing dispersing performance, the fluidity and the slump retaining capacity are excellent, and the product performance with low dosage, high water reduction and high slump retaining performance is realized. The water-reducing solid polycarboxylate superplasticizer provided by the invention can be prepared into a sheet shape according to application requirements, has good stability, long durability and strong adaptability, can greatly reduce the transportation cost and the packaging cost, and is suitable for long-distance transportation and export.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (10)
1. The formula of the water-reducing solid polycarboxylate superplasticizer is characterized in that: the raw material components mainly comprise the following components in parts by weight: 50-4000 parts of unsaturated polyoxyethylene ether 36, 390-410 parts of acrylic acid, 14-16 parts of mercaptopropionic acid, 21-23 parts of an oxidant, 10-14 parts of a reducing agent, 10-20 parts of an auxiliary agent, 80-100 parts of soft water, 10-12 parts of a thermal decomposition initiator, 14-18 parts of a neutralizing agent, 50-90 parts of unsaturated carboxylic acid small monomer, 9-12 parts of an organic reducing agent, 10-16 parts of a chain transfer agent, 22-26 parts of benzoyl peroxide, 20-22 parts of azodiisobutyronitrile, 100-200 parts of unsaturated amide small monomer, 14-16 parts of an anticorrosive bactericide and 13-17 parts of a thickening agent.
2. The water-reducing solid polycarboxylate water reducer formulation according to claim 1, characterized in that: the oxidant is hydrogen peroxide and ammonium persulfate.
3. The water-reducing solid polycarboxylate water reducer formulation according to claim 1, characterized in that: the reducing agent is sodium hypophosphite.
4. The water-reducing solid polycarboxylate water reducer formulation according to claim 1, characterized in that: the auxiliary agent is sodium polyether phosphate and sodium polyether sulfate.
5. The water-reducing solid polycarboxylate water reducer formulation according to claim 1, characterized in that: the thermal decomposition initiator is one or a mixture of azodiisobutyronitrile, azodiisoheptonitrile, dimethyl azodiisobutyrate, ammonium persulfate and potassium persulfate.
6. The water-reducing solid polycarboxylate water reducer formulation according to claim 1, characterized in that: the neutralizing agent is one or more of potassium hydroxide aqueous solution, sodium hydroxide aqueous solution, ethanolamine, diethanolamine and triethanolamine.
7. The water-reducing solid polycarboxylate water reducer formulation according to claim 1, characterized in that: the unsaturated carboxylic acid small monomer is one or a mixture of methacrylic acid, maleic anhydride, itaconic acid and fumaric acid.
8. The water-reducing solid polycarboxylate water reducer formulation according to claim 1, characterized in that: the organic reducing agent is one or a mixture of L-ascorbic acid, N-methylaniline, N-ethylaniline, N-dimethylaniline and N, N-diethylaniline.
9. The water-reducing solid polycarboxylate water reducer formulation according to claim 1, characterized in that: the unsaturated polyoxyethylene ether is one or more of isobutylene polyoxyethylene ether, allyl alcohol polyoxyethylene ether, isoamylol polyoxyethylene ether and methyl allyl polyoxyethylene ether, and the average molecular weight is 2400-4000.
10. A preparation method of a water-reducing solid polycarboxylate superplasticizer is characterized by comprising the following steps: the method specifically comprises the following steps:
the method comprises the following steps: placing two unsaturated carboxylic acid small monomers and unsaturated amide small monomers with different molecular weights in a thermocouple reaction kettle, heating and melting, adding a thermal decomposition initiator and an organic reducing agent, and mixing and stirring for 30-50 min;
step two: then, beginning to dropwise add a mixed solution of a chain transfer agent, benzoyl peroxide and azobisisobutyronitrile 2 into the mixture obtained in the step one, wherein the dropwise adding time is 2-8 hours;
step three: after the dropwise addition is finished, preserving heat for 1.5-3 h at the melting temperature, and after the free radical bulk polymerization reaction is finished, adjusting the pH value to 5-6 by using a neutralizer to prepare an additive;
step four: placing the acrylic acid and the mercaptopropionic acid into a four-neck flask provided with a thermometer, a speed-regulating stirrer, a reflux condenser tube and a dropping device, starting stirring, keeping the rotating speed at 120r/min, and mixing and stirring for 30-50 min to prepare a material A;
step five: placing sodium phosphate and polyether sodium phosphate into a four-neck flask provided with a thermometer, a speed-regulating stirrer, a reflux condenser tube and a dropping device, starting stirring and keeping the rotating speed at 120r/min, adding soft water, mixing and stirring for 40-50 min, and preparing a material B;
step six: adding methallyl polyoxyethylene ether 2400 into a heat-insulating four-neck flask provided with a thermometer, a speed-regulating stirrer, a reflux condenser pipe and a dropping device under stirring, and heating to 60-65 ℃;
step seven: adding hydrogen peroxide, ammonium sulfate and soft water mixed solution, and then simultaneously dripping the material A and the material B, wherein the material A is uniformly dripped after 2-4 hours, and the material B is uniformly dripped after 3-4 hours;
step seven: and after the material B is dripped, adding the additive, the antiseptic bactericide and the thickening agent prepared in the third step, mixing and stirring for 1-2 hours, curing for 1.5 hours, and then cooling and slicing.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114479970A (en) * | 2022-03-01 | 2022-05-13 | 北京时代思动科技有限公司 | Low-doping water coal slurry additive and preparation method thereof |
| CN114634602A (en) * | 2022-05-19 | 2022-06-17 | 济南城建集团有限公司 | Hyperbranched solid polycarboxylic acid water reducing agent and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107163197A (en) * | 2017-04-28 | 2017-09-15 | 江苏尼高科技有限公司 | High-performance solid polycarboxylate water-reducer and preparation method thereof |
| CN108821633A (en) * | 2018-07-09 | 2018-11-16 | 山西佳维新材料股份有限公司 | A kind of water reducing type solid polycarboxylic acid water reducing agent and preparation method thereof |
-
2020
- 2020-09-04 CN CN202010922052.XA patent/CN112358221A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107163197A (en) * | 2017-04-28 | 2017-09-15 | 江苏尼高科技有限公司 | High-performance solid polycarboxylate water-reducer and preparation method thereof |
| CN108821633A (en) * | 2018-07-09 | 2018-11-16 | 山西佳维新材料股份有限公司 | A kind of water reducing type solid polycarboxylic acid water reducing agent and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 李东来等: "一种早强型聚羧酸减水剂的合成及性能研究", 《四川建材》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114479970A (en) * | 2022-03-01 | 2022-05-13 | 北京时代思动科技有限公司 | Low-doping water coal slurry additive and preparation method thereof |
| CN114479970B (en) * | 2022-03-01 | 2023-10-27 | 北京时代思动科技有限公司 | Preparation method of low-doping coal water slurry additive |
| CN114634602A (en) * | 2022-05-19 | 2022-06-17 | 济南城建集团有限公司 | Hyperbranched solid polycarboxylic acid water reducing agent and preparation method thereof |
| CN114634602B (en) * | 2022-05-19 | 2022-07-29 | 济南城建集团有限公司 | Preparation method of hyperbranched solid polycarboxylate superplasticizer |
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