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Preparation method and application of unsaturated polyether

A technology of unsaturated polyether, applied in unsaturated polyether and its application in the synthesis of polycarboxylate water reducer, the field of preparation of unsaturated polyether, to achieve high water reducing rate, small slump, water reducing The effect of reducing the amount of liquid agent used

Inactive Publication Date: 2015-01-21
HONGBAOLI GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, most of the research is to use different unsaturated alcohols and ethylene oxide to react to prepare polyethers with different molecular weights, such as: Chinese patents CN102206335B, CN102504239A, CN102134313A, and the research on the molecular structure of polycarboxylate superplasticizers is still in progress. rarely reported

Method used

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  • Preparation method and application of unsaturated polyether

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Add 116.1g of methallyl alcohol and 1.5g of sodium methoxide into the 1L first reactor, replace nitrogen twice, raise the temperature to 90-105°C, add propylene oxide continuously, control the reaction pressure at 0.1-0.35MPa, and add 118.6 g propylene oxide, slaking and degassing, after the pressure is reduced to 0, the discharge obtains 233.0 grams of intermediate product A; 116.0 g of intermediate product A and 4.0 g of sodium methylate are added in the 5L second reactor, and nitrogen replacement is performed twice, Raise the temperature to 105-135°C, add ethylene oxide continuously, control the reaction pressure at 0.10-0.40MPa, add 2669.0g ethylene oxide in total, mature and degas, and reduce the pressure to 0 to obtain polyether B; The temperature of the polyether B is lowered to 90-100°C, and 4.5 g of acetic acid is added to the polyether B so that the pH value is between 5-7, and the unsaturated polyether 1 is obtained by discharging.

Embodiment 2

[0030] Add 144.2g of methallyl alcohol and 1.0g of potassium metal into 1L reactor 1, replace with nitrogen twice, raise the temperature to 100-105°C, add 1,2-epoxybutane continuously, and control the reaction pressure to 0.1-0.2MPa , add 145.5g of 1,2-epoxybutane in total, ripen and degas, after reducing the pressure to 0, discharge to obtain 279.7 grams of intermediate product A; add 140.0g of intermediate product A and 4.0g of metal to 5L reactor 2 Potassium, nitrogen replacement twice, heating up to 115-155°C, adding ethylene oxide continuously, controlling the reaction pressure at 0.10-0.30MPa, adding 3850.5g ethylene oxide in total, aging and degassing, and reducing the pressure to 0 , to obtain polyether B; lower the temperature of polyether B to 85-95° C., add 6.8 g of citric acid to polyether B so that the pH value is between 5-7, and unsaturated polyether 2 is obtained by discharging.

Embodiment 3

[0032] Add 86.3g of prenyl alcohol and 2.3g of sodium prenolate to 1L reactor 1, replace with nitrogen twice, raise the temperature to 100-110°C, add propylene oxide continuously, control the reaction pressure at 0.15-0.3MPa, a total of 120.0 g propylene oxide, ripening and degassing, after the pressure is reduced to 0, the discharge obtains 205.0 grams of intermediate product A; 80.0 g of intermediate product A and 1.5 g of sodium metal are added to 3L reactor 2, nitrogen replacement is performed twice, and the temperature is raised To 120-130°C, continuously add ethylene oxide, control the reaction pressure to 0.10-0.40MPa, a total of 1985.0g ethylene oxide, ripen and degas, reduce the pressure to 0, and discharge to obtain polyether B; The temperature of polyether B is lowered to 85-90° C., and 5.0 g of phosphoric acid is added to polyether B so that the pH value is between 5-7, and unsaturated polyether 3 is obtained by discharging.

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Abstract

The invention relates to a preparation method and application of unsaturated polyether. The preparation method comprises the following steps: (1) adding unsaturated alcohol and a catalyst into a first reactor, replacing with nitrogen, continuously adding epoxide with short branches and reacting to obtain an intermediate product A, wherein the unsaturated alcohol is one or a mixture of more than two of methyl allyl alcohol and isoamyl alcohol at any proportion and the mass ratio of the unsaturated alcohol to epoxide is 1.0:(0.1-5.0); and (2) putting the intermediate product A obtained in the step (1) and the catalyst into a second reactor, replacing with nitrogen, continuously introducing ethylene oxide and reacting to obtain polyether B, and neutralizing the pH value of the polyether B product to be 5-7 with a neutralizing reagent, wherein the mass ratio of the intermediate product A to ethylene oxide is 1.0:(15.0-51.0). The invention also provides the unsaturated polyether prepared by the preparation method, which is disclosed by the invention and application of unsaturated polyether in synthesis of polycarboxylic water reducer and the water reducer prepared from the unsaturated polyether synthesized by the method has the advantages of low doping amount, high water reduction rate, good slump-retaining agent and like.

Description

technical field [0001] The invention belongs to the technical field of polyether synthesis, specifically a preparation method of unsaturated polyether, and the unsaturated polyether prepared by the method of the invention and its application in synthesizing polycarboxylate water reducer. Background technique [0002] Unsaturated polyether is used as the main raw material in polycarboxylate cement water reducing agent. The commonly used ones are allyl alcohol, methallyl alcohol and prenyl alcohol as raw materials to directly react with ethylene oxide anion polymerization to obtain a certain molecular weight. Polyether monomer, this type of polyether has good water solubility, will not be hydrolyzed and deteriorated, and the water reducing rate of the synthesized water reducer is generally high. At present, most of the research is to use different unsaturated alcohols and ethylene oxide to react to prepare polyethers with different molecular weights, such as: Chinese patents C...

Claims

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Application Information

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IPC IPC(8): C08G65/28C04B24/16C08F283/06C04B103/30
Inventor 黄东平邢益辉芮益华梁余东魏斌
Owner HONGBAOLI GRP CO LTD
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