Alkyl polyoxyether and preparation method thereof, and polycarboxylate superplasticizer prepared from alkyl polyoxyether and preparation method thereof

A technology of polyoxyalkyl ether and polycarboxylic acid, applied in the fields of polyoxyalkylene water reducing agent and preparation, polyoxyalkylene ether and preparation thereof, can solve the problem of concrete bleeding and segregation, high production cost and low water reduction rate and other problems, to achieve a good slow-release effect, delay the hydrolysis rate, and improve the water reduction rate.

Active Publication Date: 2017-07-04
JIANGSU OXIRANCHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The traditional high-performance polycarboxylate water-reducing agent has a high water-reducing rate, but its slump-retaining performance is poor, and its single use will cause the slump loss of concrete to be too fast, which will bring great difficulties to the construction, and even cause concrete failure. Therefore, it must be compounded with the high-retention slump water reducer mother liquor in a certain proportion during use, resulting in difficult control of product quality, complicated production process and high production cost
In the application process of the compound product, one of them may be insufficient or excessive, which will bring more difficulties to the construction. For example, the amount of high slump-retaining water-reducing agent in the compound product is insufficient, which will cause the loss of concrete slump If it is too fast, the amount of high-performance polycarboxylate superplasticizer is insufficient, which will cause the initial expansion of the concrete to be small and the fluidity will be poor. However, if any of the two is added too much, it will cause bleeding and segregation of the concrete, scratching the bottom, etc. occurrence of phenomenon
[0004] Chinese patent CN 103275280A reports a synthesis method and characteristics of a high-slump water-reducing agent. The product synthesized by this method needs to be used in combination with a high-performance water-reducing agent, which increases the complexity of the process and the production cost.
Chinese patent CN 103387349A reports a slump-retaining naphthalene-based high-efficiency water reducer. Compared with polycarboxylic acid products, the production process of this product is more polluting, consumes more energy, and has a lower water-reducing rate.

Method used

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  • Alkyl polyoxyether and preparation method thereof, and polycarboxylate superplasticizer prepared from alkyl polyoxyether and preparation method thereof
  • Alkyl polyoxyether and preparation method thereof, and polycarboxylate superplasticizer prepared from alkyl polyoxyether and preparation method thereof
  • Alkyl polyoxyether and preparation method thereof, and polycarboxylate superplasticizer prepared from alkyl polyoxyether and preparation method thereof

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Embodiment 1

[0041] The synthesis of embodiment 1 monomer A

[0042] Add 26.8g of cinnamyl alcohol and 0.35g of sodium methoxide into the high pressure reactor, seal the equipment, pass nitrogen to replace the air in the high pressure reactor, raise the temperature to 100-120°C, and feed 290g of ethylene oxide raw material, when the temperature rises the pressure drops Initiate the reaction, and then feed 30g of propylene oxide to control the reaction temperature at 110-130°C and the pressure in the kettle at 0.3-0.5MPa.

[0043] After the reaction is completed, the pressure in the kettle gradually drops until it stops falling for 30 minutes, and the material is aged and cooled to obtain the monomer A. NMR of A monomer 1 H spectrum as figure 1 Shown (400MHz, D 2 O).

Embodiment 2

[0044] The synthesis of embodiment 2 monomer B

[0045] Add 20.5g 4-hydroxystyrene and 0.36g sodium methylate in the high-pressure reactor, seal the equipment, pass nitrogen to replace the air in the high-pressure reactor, heat up, to 100-120°C, feed 300g ethylene oxide raw material, when The rise in temperature and the drop in pressure indicate that the reaction is initiated, and then 45g of propylene oxide is introduced to control the reaction temperature at 110-130° C. and the pressure in the kettle at 0.3-0.5 MPa.

[0046] After the reaction is completed, the pressure in the kettle gradually drops until it stops falling for 30 minutes, and then the material is aged and cooled to obtain the B monomer. NMR of B monomer 1 H spectrum as figure 2 Shown (400MHz, deuterated dimethyl sulfoxide).

Embodiment 3

[0047] The preparation of embodiment 3 polycarboxylate superplasticizer

[0048] Add 295g of monomer A, 275g of deionized water, and 3.5g of cyclohexyl acrylate into a 1000ml round-bottomed three-necked flask, stir and dissolve evenly, add 1.8g of hydrogen peroxide with a mass concentration of 30%, and the reaction temperature is 40°C. and B solution, the dropping time is 1h, after the dropwise addition, continue to react for 1h, and then get clear and bright polycarboxylate superplasticizer mother liquor.

[0049] Wherein A solution is formed from 28g of acrylic acid, 20g of deionized water and 0.5g of ascorbic acid; B solution is formed of 1.2g of thioglycolic acid and 30g of deionized water.

[0050] The weight average molecular weight of the obtained polycarboxylate water reducer is about 35700 through gel chromatography test.

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Abstract

The invention provides alkyl polyoxyether with a structure as shown in a formula (I) or formula (II) which is described in the specification. The invention also provides a preparation method for the alkyl polyoxyether, a polycarboxylate superplasticizer prepared with the alkyl polyoxyether as a polymerization monomer and a preparation method for the polycarboxylate superplasticizer. The alkyl polyoxyether provided by the invention contains a phenyl ring which exerts great steric hindrance effect in a polymer molecule in preparation of the polycarboxylate superplasticizer, so the prepared polycarboxylate superplasticizer is endowed with better slump loss resistance. The polycarboxylate superplasticizer provided by the invention uses the alkyl polyoxyether as the monomer, has the both advantages of high water-reducing rate and high slump loss resistance, and is convenient to use and obviously reduced in the doping rate in concrete; so cost for production and construction is reduced, requirements of environmental protection are better met, and immense economic and social benefits can be produced.

Description

technical field [0001] The invention relates to the field of high molecular polymers, in particular to a polyoxyalkyl ether and a preparation method thereof, a polycarboxylate water reducer obtained therefrom and a preparation method thereof. Background technique [0002] With the implementation of the "One Belt, One Road" strategy, a round of infrastructure construction climax has emerged along the Belt and Road and surrounding areas, and the demand for commercial concrete has increased sharply. However, as an indispensable component of commercial concrete, the demand for water reducers The volume has also increased, but its market competition has become more intense, so it is increasingly important to increase research and development of new products. [0003] The traditional high-performance polycarboxylate water-reducing agent has a high water-reducing rate, but its slump-retaining performance is poor, and its single use will cause the slump loss of concrete to be too fa...

Claims

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Application Information

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IPC IPC(8): C08G65/28C08F283/06C08F220/06C08F220/18C08F222/06C04B24/26C04B103/30
CPCC04B24/2694C08F283/065C08G65/2609C08G65/2612C04B2103/30C08F220/1806C08F220/1818C08F220/1804
Inventor 朱建民刘兆滨董振鹏顾晓华韩海峰
Owner JIANGSU OXIRANCHEM CO LTD
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