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Preparation method of ether ester copolymer water reducer

A preparation process and technology of water reducing agent, which are applied in the field of preparation technology of ether ester type polymer water reducing agent, can solve the problem of restricting the application and development of polycarboxylic acid series water reducing agent, difficult to popularize water reducing agent in a large range, and stable in quality. problems such as poor performance, to achieve the effects of easy control of the process, stable product performance and mild reaction conditions

Active Publication Date: 2012-07-11
中轻日化科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the research on polycarboxylate water reducers is still in the laboratory stage, and there are few varieties of practical products. There are two main reasons for this: on the one hand, although polycarboxylate water reducers have many excellent properties, There is also the problem of adaptability to cement. my country has a vast territory and a wide variety of cement. It is difficult to popularize a single type of water reducer on a large scale, which limits the application and development of polycarboxylate water reducers. On the other hand, it is The synthesis process of most water reducers is generally cumbersome and has poor quality stability. Therefore, it is imperative to develop a preparation process for polycarboxylate water reducers with simple operation process, adjustable molecular structure and excellent performance.

Method used

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  • Preparation method of ether ester copolymer water reducer

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] A) Mix 68.4g of MgO and 28g of diatomaceous earth evenly, add it to 400ml of aqueous solution containing 23g of aluminum chloride, stir for 1hr, wash, dry, calcinate at 500℃ for 1hr, grind and sieving to obtain a Mg-Al composite catalyst. The catalyst powder contains 65% magnesium oxide, 8.4% alumina, and 26.2% diatomaceous earth.

[0022] B) Put 120g of petroleum ether and 60g of dodecanethiol into the reactor, add a mixture of 200g of methyl acrylate and 20g of azobisisobutyronitrile by dripping, dripping for 30min, and react at 70℃ for 5h, Then the heating was stopped, and the reaction mixture was poured into 1 times the mass of the reaction mixture to purify the polymer in deionized water to obtain a polymethyl acrylate with a viscosity average molecular weight of 5000.

[0023] C) Add the product obtained in B) to the above catalyst (the amount is 0.2wt% of the amount of polymethyl acrylate), the ethoxylation temperature is 150°C, and add ethylene oxide (the amount of ...

Embodiment 2

[0025] A) 300ml of an aqueous solution containing 85g of aluminum nitrate and 27g of diatomaceous earth was added dropwise to 150ml of a dispersion containing 58g of CaO, and stirred at room temperature for 1 hour to obtain a mixed catalyst slurry, which was passed through a strong basic anion exchange resin Remove NO 3 - After the ion exchange is completed, the catalyst is separated from the ion resin, dried, calcined at 500° C. for 1 hr, ground and sieved to obtain a Ca-Al composite catalyst. The catalyst powder contains 60% calcium oxide, 12% alumina, and 28% diatomaceous earth.

[0026] B) Add 155g of cyclohexane and 80g of sodium bisulfite into the reactor, add a mixture of 150g of methyl acrylate and 15g of dibenzoyl peroxide by dripping, dripping time 40min, and react at 30℃ for 8h , Then stop heating, pour the reaction mixture system into deionized water twice the mass of the mixture to purify the polymer to obtain polymethyl acrylate with a viscosity average molecular we...

Embodiment 3

[0029] A) Mix 20g MgO with 9g4A zeolite, add it to 500ml of 1.9% gallium nitrate aqueous solution, stir vigorously for 1hr, dry at 110℃ for 2hr, calcinate at 500℃ for 1hr, grind and sieving to obtain a gallium ion-containing MgO Composite catalyst. The catalyst powder contains 61.6% of magnesium oxide, 10.7% of gallium oxide, and 27.7% of 4A zeolite.

[0030] B) Add 320g of tetrahydrofuran and 38g of dithioester into the reactor, add a mixture of 40g of methyl acrylate and 2g of azobisisobutyronitrile by dripping, dripping for 60min, react at 80℃ for 7h, then stop Heating, pour the reaction mixture system into deionized water 5 times the mass of the mixture to purify the polymer to obtain polymethyl acrylate with a viscosity average molecular weight of 90,000.

[0031] C) Add the product obtained in A) to the above catalyst (the amount is 2wt% of the amount of polymethyl acrylate), the ethoxylation temperature is 220°C, and add ethylene oxide (the amount of ethylene oxide and the ...

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Abstract

The invention relates to a preparation method of an ether ester copolymer water reducer, which is characterized in that a solvent and a chain transfer agent are added to a reactor, a mixture of methyl acrylate and an initiator are added to the reactor by a dropping mode, wherein the dropping time is 30-80 minutes, the mixture is reacted at the temperature of 30-100 DEG C for 5-10h, the deionized water with weight which accounts for 100-500wt% of weight of the reacted mixture is added in the reacted mixture for purifying to obtain viscous liquid polymethyl acrylate. Polymethyl acrylate and an alkaline ester catalyst are put into the reactor, nitrogen is used for displacing air in the system, heating is carried out to the ethoxylation temperature, ethylene oxide is introduced for an addition reaction, wherein the mass ratio of ethylene oxide to polymethyl acrylate is 1:0.11-99, an aging process is carried out for 0.5-1h, the temperature is cooled to 70-100 DEG C, the material is discharged to obtain the ether ester polymer water reducer. The water reducer of the invention has the advantages of simple process step, strong operability, flexible adjustment of product molecular structure, and stable performance.

Description

Technical field [0001] The invention belongs to a preparation process of a water reducing agent, and specifically relates to a preparation process of an ether ester type polymer water reducing agent. Background technique [0002] With the development of water-reducing agent technology, polycarboxylic acid-based water-reducing agents have become a new generation of concrete admixtures that have been studied in China after the traditional naphthalene-based, sulfamic acid-based, and melamine-based water-reducing agents. It has the characteristics of low dosage, high water reduction rate, no segregation, no bleeding, good retention of concrete slump performance, and good compatibility with cement. In addition, this type of water reducing agent has a large degree of freedom in molecular design during the synthesis process , Its molecular structure design is to introduce strong polar groups carboxyl, sulfonic acid, polyoxyethylene, etc. on the main chain or side chain of the molecule, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F120/14C08F8/00C08F2/38C08G65/26C04B24/28C04B24/32
Inventor 孙永强史修启张勇康保安罗毅
Owner 中轻日化科技有限公司
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