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A kind of preparation method of (2-phosphonic acid-propylene) malonic acid

A malonic acid and phosphonic acid technology, applied in the field of fine chemicals, can solve the problems of adaptability limitation, reduce the effective carboxyl group and phosphorus content of polycarboxylate superplasticizers, and reduce the performance of superplasticizers, so as to reduce the unit dosage. , Outstanding retarding effect, high slump retention effect

Active Publication Date: 2022-04-08
SHANDONG TAIHE WATER TREATMENT TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] For the modification of the above-mentioned polycarboxylate water reducer, the monomers provided before polymerization are all olefins containing phosphonic acid groups or phosphoric acid ester groups. Without carboxyl groups, the synthesis of water reducers needs to be copolymerized with other carboxyl group-containing olefin monomers To introduce carboxyl groups, this method reduces the effective carboxyl group and phosphorus content of polycarboxylate water reducers, thereby reducing the performance of the water reducer and limiting its adaptability in concrete

Method used

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  • A kind of preparation method of (2-phosphonic acid-propylene) malonic acid
  • A kind of preparation method of (2-phosphonic acid-propylene) malonic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Step 1: Add 180g of absolute ethanol, 122g of isopropenephosphonic acid, 104g of malonic acid and 0.61g of sodium ethoxide into a 500ml round bottom glass flask in sequence, start stirring and reflux condensed water, heat to reflux state, and keep reflux state Reaction 4.06 After h, cool down and filter to obtain 403.1 g of filtrate.

[0024] Step 2: Transfer the filtrate into a 1L three-necked round-bottomed glass flask, add 1.22g red phosphorus as a catalyst, check the airtightness of the reaction system and after the test is qualified, start the stirring and tail gas absorption device, heat to reflux, and 85.2g chlorine gas According to the flow rate of 21.2g / h, it is slowly passed under the liquid surface. After 4.02h, the chlorine gas is passed through, and after the reflux reaction is continued for 30min, the temperature is lowered to 35°C.

[0025] Step 3: Slowly add a mixture of 204g sodium hydroxide and 280g calcium oxide under stirring, start stirring, heat up...

Embodiment 2

[0027] Step 1: Add 162g of absolute ethanol, 122g of isopropene phosphonic acid, 109g of malonic acid and 0.61g of sodium ethoxide into a 500ml round bottom glass flask in sequence, start stirring and reflux condensed water, heat to reflux state, and keep reflux state Reaction 4.04 After h, cool down and filter to obtain 388.7 g of filtrate.

[0028] Step 2: Transfer the filtrate into a 1L three-necked round-bottomed glass flask, add 2.44g red phosphorus as a catalyst, check the airtightness of the reaction system and after the debugging is qualified, start the stirring and tail gas absorption device, heat to reflux, and 106.5g chlorine gas According to the flow rate of 21.3g / h, it is slowly passed under the liquid surface. After 5.0h, the chlorine gas is passed through, and after the reflux reaction is continued for 30min, the temperature is lowered to 37°C.

[0029] Step 3: Slowly add 220g of sodium hydroxide and 280g of calcium oxide mixture under stirring, start stirring, ...

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Abstract

The invention discloses a method for preparing a water reducer monomer (2-phosphonic acid-propylene) malonic acid, specifically using isopropenephosphonic acid and malonic acid through Michael addition, chlorination, dehydrochlorination and other reactions The first step is to synthesize (2-phosphonic acid-propylene) malonic acid, which realizes the coexistence of phosphonic acid group and carboxyl group in the unit, and (2-phosphonic acid-propylene) malonic acid continues to combine with alkenyl polyoxyethylene ether The polycarboxylate superplasticizer prepared by macromonomer polymerization not only has high dispersibility, high slump retention, but also has outstanding retarding effect. The unit dosage of the agent.

Description

technical field [0001] The patent of the present invention relates to the technical field of fine chemicals, in particular to a method for preparing a water reducer monomer (2-phosphonic acid-propylene) malonic acid. Background technique [0002] With the continuous improvement of my country's construction technology level and the upgrading of building facilities, the requirements for the performance of infrastructure material concrete are getting higher and higher. Concrete with high strength, high fluidity and high durability is favored. Commonly referred to as concrete refers to the cement concrete that is obtained by mixing cement as the cementitious material, sand, stone, etc. as aggregates and water in a certain proportion, after mixing, molding and curing. Concrete is often used together with concrete additives. Commonly used admixtures mainly include water reducers, retarders, air-entraining agents, early strength agents, antifreeze agents, expansion agents, etc., an...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/38C08F283/06C08F230/02
CPCC07F9/3826C08F283/065C08F230/02
Inventor 周响程终发王燕平陆久田刘全华王宁宁齐晓婧
Owner SHANDONG TAIHE WATER TREATMENT TECH CO LTD
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