Preparation method and application of block polymer

A block polymer and compound technology, applied in the field of block polymer preparation, can solve the problems of complex operation process, harsh polymerization conditions, low polymerization conversion rate, etc., to achieve controllable reaction process, simple operation process, and raw material conversion high rate effect

Active Publication Date: 2016-03-09
JIANGSU SOBUTE NEW MATERIALS +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, because living radical polymerization is very sensitive to impurities such as water and oxygen in the polymerization environment, the purity of the polymerization reagent is high, and it needs to be carried out in a solvent. The polymerization conditions are very harsh, the polymerization conversion rate is low, and the operation process is complicated. The amount of solvent used is large, so it is difficult for industrialization, and the use of expensive initiators and chain transfer agents causes a substantial increase in cost, and it is currently difficult to achieve industrialization

Method used

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  • Preparation method and application of block polymer
  • Preparation method and application of block polymer
  • Preparation method and application of block polymer

Examples

Experimental program
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Effect test

preparation example Construction

[0041] Preparation of Compound C:

[0042] Add 0.5 mol of epichlorohydrin, 0.2 mol of sodium hydroxide, 0.005 mol of phase transfer catalyst tetra-n-butylammonium bisulfate, 0.05 mol of monoalkyl polyethylene glycol in a three-necked flask with stirring, and keep the temperature at 60 ℃, stirred rapidly for 5h, filtered, and the filtrate was distilled under reduced pressure to remove excess epichlorohydrin, and the product was tested by HPLC. The conversion rate of monoalkyl polyethylene glycol was 85% to 90%. Ethyl acetate is the eluent) for separation and purification to obtain epoxy-terminated alkyl polyethylene glycol with a purity greater than 99% (see Table 1 for specific parameters).

[0043] Summary of epoxy-terminated alkyl polyethylene glycol prepared in table 1

[0044] the code

Embodiment 1

[0046] The mole number of compound A is 4% of the total mole number of compound B and compound C, and the molar ratio of compound B to compound C is 0.505:1.

[0047] In a dry 2L reactor with stirring, add 12.12g of ethylene glycol monomethyl ether and 1.61g of sodium metal, stir until the sodium metal is completely dissolved, and seal the reactor. Repeat the following operation twice: after vacuuming, replace with nitrogen to a pressure of 0.01MPa. Then start stirring and raise the temperature to 80-100°C, keep the reaction pressure at 0-0.05MPa, and continuously and slowly add 136.5g of methyl glycidic acid dropwise into the reactor at a uniform speed for 4 hours while maintaining the reaction temperature at 80-100°C. 100°C; after the feeding is completed, continue to maintain the constant temperature for 0.5h, and then continuously and dropwise add 1457.5g of compound C-1 to the reactor at a uniform speed for 5h, while maintaining the reaction temperature at 80-100°C; after...

Embodiment 2

[0049] The mole number of compound A is 2.1% of the total mole number of compound B and compound C, and the molar ratio of compound B to compound C is 0.806:1.

[0050] In a dry 2L reactor with stirring, add 7.45g of ethylene glycol monoethyl ether and 3.99g of sodium methoxide, stir until the sodium methoxide is completely dissolved, and seal the reactor. Repeat the following operation twice: after vacuuming, replace with nitrogen to a pressure of 0.02MPa. Then start stirring and heat up to 100-120°C, keep the reaction pressure at 0-0.05MPa, and continuously and dropwise add 211.49g of ethyl glycidate to the reactor at a uniform speed for 6 hours while keeping the reaction temperature at 100- 120°C; after the feeding is completed, continue to maintain the constant temperature for 1 hour, and then continuously and dropwise add 1378.5g of compound C-2 to the reactor at a uniform speed for 8 hours, while maintaining the reaction temperature at 100-120°C; after the end of the fee...

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Abstract

The invention provides a preparation method of a block polymer and application thereof as a cement dispersing agent. The method is simple in operation process and high in raw material conversion rate; the molecular structure of a target product is controllable and adjustable; the industrialization is easy to realize; the prepared block polymer used as the cement dispersing agent is good in dispersion effect, and the gradual loss of concrete slump is small. The method comprises the following steps: (1), performing ring-opening polymerization reaction on a specific alkyl alcohol as a compound A and a specific ester-containing epoxide as a compound B, as well as a specific polyether-containing epoxide as a compound C in sequence, wherein the mole ratio of the compound B to the compound C is (0.5 to 3) to 1; (2), performing hydrolysis on an ester group, so as to obtain the block polymer with the weight-average molecular weight of 10000 to 30000. The prepared block polymer used as the cement dispersing agent is good in dispersion effect, and the gradual loss of concrete slump is small.

Description

technical field [0001] The invention relates to a preparation method and application of a block polymer, belonging to the technical field of concrete admixtures. Background technique [0002] Cement dispersant, also known as water reducing agent, can reduce the mixing water consumption of concrete without affecting the fluidity of cement-based materials, or increase the fluidity of cement-based material mixtures without affecting the water consumption , or both, is an admixture with water-reducing and strengthening effects. The main purpose of using cement dispersants in engineering is to reduce the water consumption of cement-based materials, reduce the water-cement ratio, save the amount of cement, improve the strength of cement-based materials, improve their workability, and improve construction efficiency and quality. [0003] There are many kinds of substances used for cement dispersion, including lignin sulfonic acid (salt), naphthalene sulfonate / formaldehyde polycond...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/28C04B24/32C04B103/30
Inventor 杨勇刘加平冉千平曹攀攀黄振翟树英
Owner JIANGSU SOBUTE NEW MATERIALS
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