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High-solid-content ether slump-retaining polycarboxylate superplasticizer preparation method

A high-solid content, slump-preserving technology, applied in the field of concrete admixtures, can solve the problems of a large concentration range of high-concentration polycarboxylate superplasticizers, difficult installation of a stirring device, and difficult control of safety issues, etc. Good degree of retention performance, no formaldehyde content, the effect of reducing the price

Active Publication Date: 2018-08-17
ANHUI ZHONGTIE ENGINEER MATERIAL SCI & TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In the above method, high-concentration polycarboxylate water-reducers are prepared by means of high-pressure mercury lamp radiation initiation, ultraviolet light initiation, and microwave initiation. The device is not easy to install, and safety issues are not easy to control. At present, there is no source for the purchase of large-scale radiation equipment, ultraviolet light irradiation equipment, and microwave devices in China.
These methods are difficult to apply in industrial production

Method used

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Embodiment 1

[0034] A preparation method of high solid content ether type slump-retaining polycarboxylate water reducer, comprising the following steps:

[0035](1) Add 800g of isopentenol polyoxyethylene ether with a molecular weight of 2400 and 100g of distilled water into a 2000mL four-necked glass flask, turn on the mixer, stir at a speed of 240r / min, and heat it to 70°C with an electric heating mantle until the bottom material Dissolved into a homogeneous transparent solution;

[0036] (2) Take out the electric heating mantle, cool the material at the bottom of the kettle to 30°C with an ice-water bath, add 14.5g of chain transfer agent solution to the bottom of the kettle, a mixed solution prepared by 4.5g of sodium hypophosphite and 10g of water; Add 13.2g of initiator A solution to the bottom of the kettle, a mixed solution prepared from 3.2g of ammonium persulfate and 10g of water; after stirring for 5min, add dropwise monomer solution for 3h and initiator B solution for 3.5h; whe...

Embodiment 2

[0038] A preparation method of high solid content ether type slump-retaining polycarboxylate water reducer, comprising the following steps:

[0039] (1) Add 800g of isopentenol polyoxyethylene ether with a molecular weight of 3000 and 100g of distilled water into a 2000mL four-neck glass flask, turn on the mixer, stir at a speed of 260r / min, and heat to 65°C with an electric heating mantle until the bottom material Dissolved into a homogeneous transparent solution;

[0040] (2) Take out the electric heating mantle, cool the material at the bottom of the kettle to 25°C with an ice-water bath, add 35.8g of chain transfer agent solution to the bottom of the kettle, a mixed solution prepared by 15.8g of sodium methacrylate and 20g of water; after 10 minutes , add 18g initiator solution A to the bottom of the kettle, a mixed solution prepared by 8g ammonium persulfate and 10g water; after stirring for 5min, adopt single dropwise addition, and the dropping time is 3h; Ethyl ester, ...

Embodiment 3

[0042] A preparation method of high solid content ether type slump-retaining polycarboxylate water reducer, comprising the following steps:

[0043] (1) Add 800g of isopentenol polyoxyethylene ether with a molecular weight of 2900 and 100g of distilled water into a 2000mL four-necked glass flask, turn on the mixer, stir at a speed of 200r / min, and heat it to 80°C with an electric heating mantle until the bottom material Dissolved into a homogeneous transparent solution;

[0044] (2) Take out the electric heating mantle, cool the material at the bottom of the kettle to 20°C with an ice-water bath, add 4g of chain transfer agent solution to the bottom of the kettle, the chain transfer agent solution is 4g of mercaptoethanol; after 10min, add 7.8g of initiator to the bottom of the kettle A solution, the initiator A solution is hydrogen peroxide with a concentration of 50%; after stirring for 5 minutes, simultaneously drop the monomer solution for 3 hours, and the initiator B solu...

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Abstract

The invention discloses a high-solid-content ether slump-retaining polycarboxylate superplasticizer preparation method. The method includes steps: dissolving isopentenol polyoxyethylene ether into water, heating at 60-80 DEG C to melt, cooling to 20-30 DEG C, sequentially adding pre-prepared chain transfer agent solution and initiator A solution, adjusting stirring speed to 200-300r / min, dropwiseadding singly or doubly, wherein monomer-containing solution is subjected to dropwise adding for 2.5-3h, and initiator B solution is subjected to double dropwise adding for 3-3.5h, the first 1h reaction temperature rise in a reactor is controlled to be lower than 4 DEG C in a reaction process, and the whole reaction temperature does not exceed 40 DEG C; keeping the temperature for 1-2h after dropwise adding, and adopting caustic soda flakes to adjust product pH value to 7+ / -1 to obtain high-concentration ether slump-retaining polycarboxylate superplasticizer mother liquor in solid content of 80% and in state of thick liquid. Concrete mixed by adoption of the superplasticizer is great in slump retaining performance, and cost in production, transporting and storage processes is saved. In addition, products are green, environmentally friendly and free of formaldehyde, and discharging of waste gas, wastewater and industrial residues in the production process is avoided.

Description

technical field [0001] The invention relates to the technical field of concrete admixtures, in particular to a preparation method of a high-solid-content ether type slump-retaining polycarboxylate water reducer. Background technique [0002] The synthesis process of the traditional polycarboxylate superplasticizer is formed by free radical copolymerization in an aqueous solution under the action of an initiator, mainly with 20-50% liquid, which causes the problem of high cost for long-distance transportation and high development costs. Concentration polycarboxylate superplasticizer products are the primary condition for reducing transportation costs and promoting the widespread use of polycarboxylate superplasticizers in various places. At present, some progress has been made in the research on high-concentration / solid water-reducers in the industry. Among them, the relatively mature method of preparing powder polycarboxylate water-reducers is to use spray drying or vacuum d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F283/06C08F222/10C08F220/06C08F220/20C04B24/26C04B103/30
CPCC04B24/2605C04B2103/302C08F283/065C08F222/10C08F220/20
Inventor 汪志勇黄海林春红李双超温建峰陈娟许立李双
Owner ANHUI ZHONGTIE ENGINEER MATERIAL SCI & TECH CO LTD
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