Preparation method of polyester type pure solid polycarboxylic acid high-performance water reducing agent

A pure solid, polycarboxylic acid technology, applied in the field of polycarboxylate high-performance water reducers, can solve the problems of inability to fully realize solid polyester type water reducers, enrich the preparation methods of synthetic polycarboxylates, etc., and achieve good market competition force and application prospects, avoiding the reduction of separation and concentration efficiency, and reducing the effect of transportation costs

Active Publication Date: 2013-04-03
BEIJING UNIV OF TECH
5 Cites 33 Cited by

AI-Extracted Technical Summary

Problems solved by technology

The polymerization step in this method adopts the bulk polymerization method, and the whole process does not use water as a solvent or medium, which effectively improves the problem that in the past, the aqueous solution system was us...
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Abstract

The invention discloses a preparation method of a polyester type pure solid polycarboxylic acid high-performance water reducing agent, belonging to the field of water reducing agents. According to the invention, by taking a (methyl) acrylic acid monomer and a polyethylene glycol compound as reactants, a polymerizable macromonomer is prepared through esterification reaction under the effect of a catalyst, and the polymerizable macromonomer conducts a free radical bulk polymerization reaction with an unsaturated carboxylic acid monomer and a chain transfer agent under the effect of an initiator in an environment without any solvent to obtain the polyester type pure solid polycarboxylic acid high-performance water reducing agent. The method disclosed by the invention has strong process controllability, high degree of polymerization and low cost and prevents environmental pollution; a completely anhydrous polyester type pure solid polycarboxylic acid high-performance water reducing agent is prepared through esterification reaction and bulk polymerization, which has neat cement paste liquidity and holding ability, cement adaptability and concrete application performance similar to a traditional solution method; meanwhile, since the polymer product is an anhydrous pure solid, a solution with any concentration can be prepared according to actual needs; and without the after-treatment processes such as heating and drying, solvent separation and the like, the transportation is more convenient, and good market competitiveness and application prospects are realized.

Technology Topic

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  • Preparation method of polyester type pure solid polycarboxylic acid high-performance water reducing agent
  • Preparation method of polyester type pure solid polycarboxylic acid high-performance water reducing agent
  • Preparation method of polyester type pure solid polycarboxylic acid high-performance water reducing agent

Examples

  • Experimental program(12)
  • Effect test(1)

Example Embodiment

[0022] Example 1
[0023] First, 100 g of methoxy polyethylene glycol (molecular weight 2500) was added to the reactor, and the temperature was raised to 50 °C. When the methoxy polyethylene glycol was in a liquid state, 0.07 g of hydroquinone, 0.07 g of hydroquinone, 14.41g acrylic acid, 1.5g p-toluenesulfonic acid, and stirring time for 20 minutes at each feeding interval, add 17.16g cyclohexane when the temperature rises to 80°C, continue to heat up to 105°C to carry out esterification reaction, while reacting The water obtained from the reaction was separated, and after 6 hours of reaction, the cyclohexane was removed by vacuuming to obtain the esterification reaction product; the esterification reaction product was added to the reactor, the temperature was raised to 50 ° C, and 2.76g of mercapto groups were sequentially added to the reactor. Acetic acid, 4.32g of acrylic acid, 0.48g of dibenzoyl peroxide, and the stirring time of each feeding interval is 20 minutes, continue to heat up to 95 ° C to carry out bulk polymerization, react for 4 hours, stop the reaction, and cool to 40 ° C to obtain 122.85g of the reaction product of polyester type pure solid, and finally adding 228.15g of water to dilute to obtain a polycarboxylate superplasticizer with a concentration of 35%.

Example Embodiment

[0024] Example 2
[0025] After the cement dispersant with a mass fraction of 35% obtained in Example 1 was stored at 6°C for 30 days, its implementation effect was measured.

Example Embodiment

[0026] Example 3
[0027] First, 50g polyethylene glycol (molecular weight 500) was added to the reactor, and the temperature was raised to 70°C. When the polyethylene glycol was in a liquid state, 0.65g phenothiazine, 12.91g methacrylic acid, 5g phenothiazine, 5g Phosphoric acid, and the stirring time is 5 minutes at each feeding interval. When the temperature is raised to 100 ° C, 18.87 g of toluene are added, and the temperature is continued to be raised to 110 ° C to carry out the esterification reaction. The toluene was removed by vacuuming to obtain the esterification reaction product; the esterification reaction product was added to the reactor, the temperature was raised to 70 ° C, and 0.53 g of mercaptopropionic acid, 4.8 g of acrylic acid, 32.67 g of maleic anhydride, 1.64g of azobisisobutyronitrile, and the stirring time was 5 minutes at each feeding interval, the temperature was continued to be raised to 75°C for bulk polymerization, the reaction was carried out for 8 hours, the reaction was stopped, and 106.66g of polyester pure was obtained by cooling to 25°C. The solid reaction product was finally diluted with 130.36 g of water to obtain a polycarboxylate superplasticizer with a concentration of 45%.
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Description & Claims & Application Information

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the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
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Owner:NANJING RUIDI HIGH TECH
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