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CN-121991298-A - High-performance super-early-strength polycarboxylate superplasticizer and preparation method thereof

CN121991298ACN 121991298 ACN121991298 ACN 121991298ACN-121991298-A

Abstract

The invention discloses a high-performance super-early-strength polycarboxylate water reducer and a preparation method thereof, relating to the technical field of concrete additives, wherein the high-performance super-early-strength polycarboxylate water reducer is prepared by reacting monomers s, and then the polyethylene glycol divinyl ether, acrylic acid, a monomer s and methacrylic acid-2-hydroxyethyl phosphate are polymerized to obtain the modified polyethylene glycol divinyl ether. The invention combines the raw materials such as acrylic acid, monomer s, methacrylic acid-2-hydroxyethyl phosphate and the like, and can endow the polycarboxylate water reducer with good early strength performance and mud resistance.

Inventors

  • LI SHUGANG
  • YAN GANG
  • ZHANG XIAOLI
  • WANG YAN

Assignees

  • 五家渠格辉新材料有限责任公司

Dates

Publication Date
20260508
Application Date
20260210

Claims (10)

  1. 1. The preparation method of the high-performance super early-strength polycarboxylate superplasticizer is characterized by comprising the following steps of: A1, mixing and stirring an aqueous solution containing nitroimidazole and ethanol, adding a reducing agent, and heating and stirring to obtain a product A1; a2, mixing and stirring a product a1, ethyl acetate and epichlorohydrin, adding tetrabutylammonium bromide, starting reflux, heating and stirring, cooling to room temperature, adding alkali liquor, and continuing stirring to obtain a product A2; Step A3, mixing and stirring the product a2, sodium naphthalene sulfonate containing amino and ethanol, adding triethylamine, heating and stirring to obtain a product A3; Step A4, mixing and stirring terminal alkenyl carboxylic acid and acetonitrile, placing the mixture in an ice-water bath, adding HOAt, stirring, adding EDC, continuously stirring, adding a catalyst and a product a3, heating to room temperature, and stirring to obtain a product A4; Step A5, mixing and stirring polyethylene glycol divinyl ether and deionized water to obtain a mixture 1, mixing and stirring acrylic acid, a monomer s, methacrylic acid-2-hydroxyethyl phosphate and deionized water to obtain a mixture 2, mixing and stirring ascorbic acid, thioglycollic acid and deionized water to obtain a mixture 3, mixing and stirring the mixture 1 and a hydrogen peroxide solution, sequentially adding the mixture 2 and the mixture 3 under stirring, continuing stirring, cooling, and regulating pH to obtain the high-performance super-early-strength polycarboxylate water reducer.
  2. 2. The preparation method of the high-performance super early-strength polycarboxylate superplasticizer is characterized in that in the step A1, the dosage ratio of nitroimidazole to ethanol aqueous solution to reducing agent is 7.5-8.5g:35-45mL:9.5-10.5g, and the nitroimidazole is 1, 2-dimethyl-5-nitroimidazole.
  3. 3. The preparation method of the high-performance super early strength polycarboxylate superplasticizer as claimed in claim 1, wherein in the step A1, the ethanol aqueous solution is prepared by mixing ethanol and water according to a volume ratio of 1-2:1, and adding sodium bicarbonate to adjust pH to 8-9.
  4. 4. The preparation method of the high-performance super early-strength polycarboxylate superplasticizer is characterized in that in the step A2, the dosage ratio of the product a1 to ethyl acetate to epichlorohydrin to tetrabutylammonium bromide to alkali liquor is 7-8 g/40-50 mL/10-11 g/0.7-0.9 g/13-15 mL.
  5. 5. The preparation method of the high-performance super early-strength polycarboxylate superplasticizer is characterized in that in the step A3, the dosage ratio of the product a2 to sodium naphthalene sulfonate, ethanol and triethylamine is 18-20g to 25-27g to 105-115mL to 8-8.5g, and the sodium naphthalene sulfonate is 4-amino-1-naphthalene sulfonate sodium salt.
  6. 6. The preparation method of the high-performance super early strength polycarboxylate superplasticizer, as set forth in claim 1, is characterized in that in the step A4, the dosage ratio of the product a3, the terminal alkenyl carboxylic acid, acetonitrile, HOAt, the catalyst and EDC is 21-22g:10-11g:105-115mL:6.5-7.5g:1-1.2g:9-9.5g.
  7. 7. The preparation method of the high-performance super early-strength polycarboxylate superplasticizer, as set forth in claim 1, is characterized in that in the step A4, the dosage ratio of the product A4, haloalkoxysilane and absolute ethanol is 32-34g:12-14g:90-100mL.
  8. 8. The preparation method of the high-performance super early-strength polycarboxylate superplasticizer is characterized in that in the step A5, the dosage ratio of polyethylene glycol divinyl ether to deionized water in the mixture 1 is 19-21g:115-125mL, and the dosage ratio of acrylic acid, monomer s, methacrylic acid-2-hydroxyethyl phosphate to deionized water in the mixture 2 is 32-34g:82-84g:5-7g:240-250mL.
  9. 9. The preparation method of the high-performance super early-strength polycarboxylate superplasticizer, as set forth in claim 1, is characterized in that in the step A5, the dosage ratio of ascorbic acid, thioglycollic acid and deionized water in the mixture 3 is 5.5-6g:1.6-1.8g:38-42mL, and the dosage ratio of the mixture 1, hydrogen peroxide solution, the mixture 2 and the mixture 3 is 140-145mL:34-36mL:360-37 mL:45-50mL.
  10. 10. A high-performance super early strength polycarboxylate water reducer prepared by the preparation method of the high-performance super early strength polycarboxylate water reducer according to any one of claims 1 to 9.

Description

High-performance super-early-strength polycarboxylate superplasticizer and preparation method thereof Technical Field The invention relates to the technical field of concrete additives, in particular to a high-performance super-early-strength polycarboxylate superplasticizer and a preparation method thereof. Background With the development of concrete preparation technology, various aspects of concrete performance are required to be higher, and accordingly, research and production of concrete additives are also developed towards the direction of environmental protection and high performance. The water reducer is a concrete admixture with the widest application range and the largest usage amount, and the water reducer is mixed into fresh concrete, so that the flocculation structure of cement particles can be destroyed, the effect of dispersing the cement particles and hydrating the cement particles is achieved, free water in the flocculation structure is released, the flowing dispersibility of concrete mixture is increased, and the research of the polycarboxylic acid water reducer has become a hotspot for research and development of the concrete admixture at home and abroad. However, in the actual use process, the common polycarboxylate water reducer can obviously delay the hydration of cement, especially in cold environment (such as 0-5 ℃), the hydration reaction rate is reduced, the compactness of the water reducer adsorption layer is increased, the stability is enhanced, the nucleation of C-S-H (hydrated calcium silicate) gel is further inhibited, the early strength development of concrete is slow, and the application is limited in the concrete with higher requirement on early strength. At present, the common early strength agents for concrete mainly comprise chloride salt systems, sulfate systems, carbonate systems, organic systems, minerals and composite early strength agents, but the conventional early strength agents are easy to introduce chloride ions or alkali metals into the concrete, and can cause damage to the concrete structure no matter the reinforcing steel bar corrosion caused by the chloride ions or the aggregate reaction caused by excessive alkali metals. Therefore, how to develop early strength monomers with high-efficiency dispersing and hydration promoting functions, so that the prepared polycarboxylate water reducer can still effectively improve the early strength of concrete in a cold environment, and further research is needed. Disclosure of Invention In order to solve the technical problems, the invention provides a high-performance super-early-strength polycarboxylate superplasticizer and a preparation method thereof. The aim of the invention can be achieved by the following technical scheme: a preparation method of a high-performance super-early-strength polycarboxylate superplasticizer comprises the following steps: A1, mixing and stirring an aqueous solution containing nitroimidazole and ethanol, adding a reducing agent, and heating and stirring to obtain a product A1; a2, mixing and stirring a product a1, ethyl acetate and epichlorohydrin, adding tetrabutylammonium bromide, starting reflux, heating and stirring, cooling to room temperature, adding alkali liquor, and continuing stirring to obtain a product A2; Step A3, mixing and stirring the product a2, sodium naphthalene sulfonate containing amino and ethanol, adding triethylamine, heating and stirring to obtain a product A3; Step A4, mixing and stirring terminal alkenyl carboxylic acid and acetonitrile, placing the mixture in an ice-water bath, adding HOAt, stirring, adding EDC, continuously stirring, adding a catalyst and a product a3, heating to room temperature, and stirring to obtain a product A4; Step A5, mixing and stirring polyethylene glycol divinyl ether and deionized water to obtain a mixture 1, mixing and stirring acrylic acid, a monomer s, methacrylic acid-2-hydroxyethyl phosphate and deionized water to obtain a mixture 2, mixing and stirring ascorbic acid, thioglycollic acid and deionized water to obtain a mixture 3, mixing and stirring the mixture 1 and a hydrogen peroxide solution, sequentially adding the mixture 2 and the mixture 3 under stirring, continuing stirring, cooling, and regulating pH to obtain the high-performance super-early-strength polycarboxylate water reducer. Further, the preparation method of the high-performance super-early-strength polycarboxylate superplasticizer comprises the following specific steps of: A1, mixing and stirring an aqueous solution containing nitroimidazole and ethanol for 25-30min, adding a reducing agent, heating to 50-60 ℃, stirring and reacting for 3-4h, adjusting the pH to 4.5-5 with a hydrochloric acid solution, extracting with ethyl acetate, adjusting the pH of an aqueous phase to 9-10, extracting with ethyl acetate, collecting an organic phase, washing with a saturated sodium chloride solution, drying with anhydrous sodium sulfate, filtering, and steaming to obtain