Method of preparing poly carboxylic acid series water reducer using maleic anhydride

A technology based on maleic anhydride and polycarboxylic acid, applied in the field of concrete water reducer, can solve the problems of complex process, long reaction time, difficult separation and purification, etc., and achieve the effect of simple process, short reaction time and cost reduction

Inactive Publication Date: 2007-04-18
HENAN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

"From the above, it can be seen that the method of preparing concrete water reducer with maleic anhydride needs to add polymerization inhibitor and solvent in the esterification reaction. After the reaction, it is difficult to separate and purify, the process is more complicated and the reaction time is longer.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 60.0 g of polyethylene glycol with a molecular weight of 1000, 18.0 g of maleic anhydride, and solid acid SO 4 2- / ZrO 2 Put 6.3g into the reaction container, heat and stir evenly to dissolve the reactant completely, vacuumize 0.2 atmospheres, keep the temperature at 85±5°C, and react for 4 hours to generate polyethylene glycol maleic anhydride ester (PEM) and A mixture of maleic anhydride remains. Put 40.0g of the obtained mixture and 18.0g of sodium methacrylsulfonate into a reaction vessel, add 80.0g of water, heat, stir evenly to completely dissolve the reactants, and dropwise add 13.0g of acrylic acid while adding 8% by mass 82.8g of ammonium persulfate solution, control the dropping rate, finish dropping in about 100 minutes, keep the temperature at 85±5°C, react for 4 hours, add sodium hydroxide to neutralize after cooling, adjust PH=7~8, and finally get The polycarboxylate high-performance concrete water reducer of the present invention.

Embodiment 2

[0026] 60.0 g of polyethylene glycol with a molecular weight of 1000, 24.0 g of maleic anhydride, and solid acid SO 4 2- / ZrO 2 6.3g is put into the reaction container, heats, stirs and makes reactant dissolve completely, vacuumizes 0.2 atmospheric pressure, keeps temperature at 85 ± 5 ℃, reacts for 4 hours, obtains polyethylene glycol maleic anhydride ester compound (PEM) and A mixture of maleic anhydride remains. Put 40.0g of the obtained mixture and 18.0g of sodium methacrylsulfonate into a reaction vessel, add 80.0g of water, heat, stir evenly to completely dissolve the reactants, and dropwise add 13.0g of acrylic acid while adding 8% by mass 82.8g of ammonium persulfate solution, control the dropping rate, finish dropping in about 100 minutes, keep the temperature at 85±5°C, react for 4 hours, add sodium hydroxide to neutralize after cooling, adjust PH=7~8, and finally get The polycarboxylate high-performance concrete water reducer of the present invention.

Embodiment 3

[0028] 60.0 g of polyethylene glycol with a molecular weight of 1000, 18.0 g of maleic anhydride, and solid acid SO 4 2- / ZrO 2 Put 4.7g into the reaction vessel, heat and stir evenly to dissolve the reactant completely, vacuumize 0.3 atmospheres, keep the temperature at 85±5°C, and react for 4 hours to generate polyethylene glycol maleic anhydride ester (PEM) and A mixture of maleic anhydride remains. Put 40.0g of the obtained mixture and 18.0g of sodium methacrylsulfonate into a reaction vessel, add 80.0g of water, heat, stir evenly to completely dissolve the reactants, and dropwise add 13.0g of acrylic acid while adding 8% by mass 82.8g of ammonium persulfate solution, control the dropping rate, finish dropping in about 100 minutes, keep the temperature at 85±5°C, react for 4 hours, add sodium hydroxide to neutralize after cooling, adjust PH=7~8, and finally get The polycarboxylate high-performance concrete water reducer of the present invention.

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Abstract

The present invention relates to a method for preparing polycarboxylate water-reducing agent by utilizing maleic anhydride. Said method includes the following steps: (1), using solid acid SO42- / ZrO2 as catalyst, as catalyst, utilizing esterification reaction of polyethylene glycol and maleic anhydride at 80 deg.C-90 deg.C under the condition of reduced pressure to obtain the mixture of polyethylene glycol maleic anhydride esterified product (PEM) and residual maleic anhydride, the relative molecular weight of the described polyethylene glycol is 1000; and (2), using ammonium persulfate as initiator, making the above-mentioned mixture, acrylic acid and sodium methylpropenyl sulfonate undergo the process of copolymerization reaction for 3-5h at 85 deg.C so as to obtain the invented product.

Description

(1) Technical field [0001] The invention relates to a concrete water reducer, in particular to a method for preparing a polycarboxylate water reducer by using maleic anhydride as a raw material. (2) Background technology [0002] At present, concrete water reducers at home and abroad are usually divided into three series, one is lignosulfonate water reducer; the other is sulfonated aromatic polymer water reducer; the third is polycarboxylate water reducer. But there are also a small amount of other types, such as melamine and sulfamate. [0003] The slow setting phenomenon of lignosulfonate water reducer is relatively serious, and its raw material comes from industrial waste liquid. The performance of lignin and the influence of toxic and harmful chemicals are difficult to control, and its water reduction rate is only about 8%-13%. At present, the domestic use is not large, but it is still used because of its low price. [0004] Naphthalene-based water reducers have the ch...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B24/24C04B24/04
Inventor 管学茂张海波王明丽
Owner HENAN POLYTECHNIC UNIV
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