Synthesis method of phenyl containing polycarboxylic acid water reducer and product thereof

A synthesis method and technology of polycarboxylic acid, applied in the field of admixtures of concrete, can solve problems such as unfavorable free radical copolymerization reaction, unfavorable product quality control, increase of influencing factors, etc., and achieves suitable for large-scale industrial production and excellent initial water reduction. rate, water solubility enhancement effect

Inactive Publication Date: 2018-09-11
SHANGHAI TAIJIE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the prior art, the method for introducing phenyl functional groups is mainly to utilize organic compounds containing phenyl and unsaturated double bonds such as styrene and propylene to participate in copolymerization; however, there are two main problems in this method. First, benzene Compounds such as ethylene and styrene-propylene have low solubility in water, which is unfavorable for free radical copolymerization of water as a solvent system; the second, directly using organic compounds containing phenyl and unsaturated double bonds to participate in copolymerization will make the already containing unsaturated The reaction system of carboxylic acid and unsaturated modified polyether is more complicated, which increases the influencing factors and is not conducive to the quality control of products

Method used

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preparation example Construction

[0020] According to the synthetic method described in the first aspect, it comprises the following steps:

[0021] S1: Add phenyl-containing polyethylene glycol compounds, acrylic acid or methacrylic acid, p-toluenesulfonic acid as a catalyst, and a polymerization inhibitor to the first reaction vessel, and perform esterification at 75°C to 95°C for 30 minutes to 150min, generate unsaturated intermediate;

[0022] S2: Add the unsaturated intermediate, unsaturated carboxylic acid and persulfuric acid initiator into the second reaction vessel, and thermally initiate free radical copolymerization reaction at 55°C-80°C, and react after 2.5h-6.5h Complete, post-treatment, that is, the phenyl-containing polycarboxylate water reducer.

[0023] In a preferred embodiment, the weight average molecular weight of the phenyl-containing polyethylene glycol compound is 600-3000.

[0024] In a preferred embodiment, the polymerization inhibitor is hydroquinone or p-quinone; and the mass of t...

Embodiment 1

[0034] S1: Add 1500g of phenyl-containing polyethylene glycol compound with a weight average molecular weight of 1500, 120g of methacrylic acid, 35g of p-toluenesulfonic acid and 2.0g of hydroquinone into the first reaction vessel, heat up to 85°C and reflux React for 90min, and then use a rotary evaporator to remove unreacted methacrylic acid to obtain an unsaturated intermediate;

[0035] S2: Add 1500g of the unsaturated intermediate, 200g of acrylic acid and 20g of sodium persulfate to the second reaction vessel, mechanically stir, perform free radical copolymerization at 70°C for 4.5h, and finally add 35wt% sodium hydroxide aqueous solution to adjust the pH value to 5.5 to obtain the phenyl-containing polycarboxylate superplasticizer ①.

Embodiment 2

[0037] S1: Add 2000g of phenyl-containing polyethylene glycol compound with a weight average molecular weight of 2000, 100g of acrylic acid, 30g of p-toluenesulfonic acid and 1.5g of p-benzoquinone into the first reaction vessel, heat up to 80°C and reflux for 120min , and then use a rotary evaporator to remove unreacted acrylic acid to obtain an unsaturated intermediate;

[0038] S2: Add 2000g of the unsaturated intermediate, 220g of methacrylic acid and 25g of ammonium persulfate to the second reaction vessel, mechanically stir, perform free radical copolymerization at 60°C for 5.5h, and finally add 35wt% sodium hydroxide aqueous solution to adjust When the pH value reaches 6.0, the phenyl-containing polycarboxylate superplasticizer ② is obtained.

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Abstract

The invention provides a synthesis method of a phenyl containing polycarboxylic acid water reducer. The synthesis method comprises following steps: step one, adding phenyl containing polyethylene glycol compounds, acrylic acid (or methacrylic acid), p-toluene sulfonic acid, and a polymerization inhibitor into a first reactor, and carrying out esterification reactions at a temperature of 75-95 DEGC to generate an unsaturated intermediate; and step two, adding the unsaturated intermediate, an unsaturated carboxylic acid, and a persulfuric acid into a second reactor, carrying out free radical copolymerization reactions at a temperature of 55-80 DEG C, and performing a post treatment to obtain the phenyl containing polycarboxylic acid water reducer. The operation of the synthesis method is simple, the cost is low, and the synthesis method is suitable for massive industrial production. The synthesized phenyl containing polycarboxylic acid water reducer has a high primary water-reducing rate, a high cement slurry expansion degree and a wide application prospect.

Description

technical field [0001] The invention belongs to the field of concrete admixtures, and in particular relates to a synthesis method of a phenyl-containing polycarboxylate water reducer and a product prepared according to the synthesis method. Background technique [0002] Polycarboxylate concrete admixture is the third generation of concrete admixture after lignosulfonate water reducer and naphthalene water reducer. It is widely used in various industrial buildings, civil buildings, roads and bridges at home and abroad. , has become the most widely used and used construction admixture; especially, polycarboxylate concrete admixtures are used in some engineering fields, such as nuclear power projects, high-strength concrete (C60 and above), ultra-high-strength concrete (C80 and Above), high-speed railway engineering, high-rise / super high-rise pumping and other concrete application fields play an irreplaceable role. [0003] In the prior art, the synthesis process of polycarbox...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F283/06C08F220/06C08F222/06C04B24/26C04B103/30
CPCC04B24/2605C04B24/2694C04B2103/302C08F283/065C08F220/06C08F222/06
Inventor 朱伟亮王少峰
Owner SHANGHAI TAIJIE CHEM
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