Preparation method of macromonomer methallyl alcohol polyoxyethylene ether of polycarboxylate water reducer

A technology of methallyl alcohol polyoxyethylene ether and methallyl alcohol, which is applied in the field of polyether synthesis in organic chemistry, can solve the problems of complex production process, overpressure of the reactor, easy gasification, etc. Simple process, reduced isomerization, and low PEG content

Active Publication Date: 2016-01-20
三江化工有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because methallyl alcohol, the raw material of methallyl alcohol polyoxyethylene ether, has double bonds, low boiling point, easy gasification, easy to cause rapid overpressure and overheating of the reactor, prone to production accidents, and the production process is relatively complicated

Method used

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  • Preparation method of macromonomer methallyl alcohol polyoxyethylene ether of polycarboxylate water reducer
  • Preparation method of macromonomer methallyl alcohol polyoxyethylene ether of polycarboxylate water reducer

Examples

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Embodiment 1

[0026] The preparation of embodiment 1 methallyl alcohol polyoxyethylene (60) ether

[0027] Add 0.75 mol (54 g) of methallyl alcohol and 1.92 g of boron trifluoride-diethyl ether into a 5 L pressure reactor, and connect the ethylene oxide metering tank to the pressure tank. Replace the air in the kettle with nitrogen for 3 times, and when the temperature of the kettle rises to 50-55° C., 7.5 mol (330 g) of ethylene oxide is passed through for 3.5 hours, and the reaction is continued for 0.5 hours. Then add an aqueous potassium hydroxide solution containing 30.51g of potassium hydroxide, dehydrate at 100°C for 1 hour, keep the temperature of the kettle at 100-105°C, feed 37.5mol (1650g) of ethylene oxide, and complete the process in 6.5 hours , continue to react for 0.5 hours. After the reaction is completed, cool down, release the pressure, add acetic acid for neutralization, and slice to obtain colorless flakes.

Embodiment 2

[0028] The preparation of embodiment 2 methallyl alcohol polyoxyethylene (50) ether

[0029] Add 0.5 mol (36 g) of methallyl alcohol and 0.07 g of boron trifluoride-diethyl ether into a 5 L pressure reactor, and connect the ethylene oxide metering tank to the pressure tank. The air in the kettle was replaced with nitrogen for 3 times, and when the temperature of the kettle rose to 30-35°C, 2.5 mol (110 g) of ethylene oxide was passed through for 2.5 hours, and the reaction was continued for 0.5 hours. Then add an aqueous sodium hydroxide solution containing 1.14g of sodium hydroxide, dehydrate at 100°C for 1 hour, wait for the temperature of the kettle to rise to 155-160°C, and feed 22.5mol (990g) of ethylene oxide for 2.5 hours After passing through, continue to react for 0.5 hour. After the reaction is completed, cool down, release the pressure, add acetic acid for neutralization, and slice to obtain colorless flakes.

Embodiment 3

[0030] Embodiment 3 Preparation of methallyl alcohol polyoxyethylene (55) ether

[0031] Add 1.0mol (72g) of methallyl alcohol and 1.21g of boron trifluoride-ether into a 5L pressure reactor, and connect the ethylene oxide metering tank to the pressure reactor. Replace the air in the kettle with nitrogen for 3 times. After the temperature of the kettle rises to 65-70° C., 7.5 mol (330 g) of ethylene oxide is passed through for 0.5 hours, and the reaction is continued for 0.5 hours. Then add sodium methoxide methanol solution containing 19.94g of sodium methoxide, demethanol at 100°C for 1 hour, wait for the temperature of the kettle to rise to 130-135°C, and feed 47.5mol (2090g) of ethylene oxide for 4.5 hours After passing through, continue to react for 0.5 hour. After the reaction is completed, cool down, release the pressure, add acetic acid for neutralization, and slice to obtain colorless flakes.

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Abstract

The invention relates to a preparation method of polycarboxylate water-reducing agent macromonomer methylallyl alcohol polyethenoxy ether, wherein the preparation method comprises the following process steps of: (1) adding oxirane in the presence of an acidic catalyst boron trifluoride-aether by taking methylallyl alcohol as an initial raw material for condensation reaction to obtain a methylallyl alcohol oligomer; (2) adding an alkali catalyst to the material, removing water or methanol under the condition of 100 DEG C for 1 hour, then adding the oxirane for condensation reaction, and then adding acetic acid for neutralization to obtain the methylallyl alcohol polyethenoxy ether. The preparation method disclosed by the invention is simple and safe in process, and the obtained product is high in relative molecular weight and high in iodine number.

Description

technical field [0001] The invention belongs to the technical field of polyether synthesis in organic chemistry, and in particular relates to a preparation method of macromonomer methallyl alcohol polyoxyethylene ether of a polycarboxylate water reducer. Background technique [0002] In recent years, my country's construction industry has developed rapidly, and the construction of major and key projects such as civil, railway, highway, bridge, tunnel, hydropower, seaport, wharf, airport, etc. cannot do without high-performance concrete, self-compacting concrete, high-strength concrete, high-strength concrete, fluid concrete. The demand for concrete is increasing, the quality requirements are getting higher and higher, and the performance requirements are becoming more and more comprehensive and diversified. Concrete that meets the above requirements cannot do without high-performance water reducing agents. [0003] At present, the high-performance water reducer is polycarbox...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/28C04B24/32C04B103/30
Inventor 潘晓宏
Owner 三江化工有限公司
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