Preparation method of methyl-terminated propenol polyether

A technology of terminal allyl alcohol polyether and allyl alcohol polyoxyethylene ether, which is applied in the field of preparation of methyl-capped allyl alcohol polyether, can solve the problem of low capping rate, reduce the probability of occurrence, and reduce the concentration distribution Uniformity improvement, the effect of ensuring uniformity

Inactive Publication Date: 2017-03-15
RUNHE ORGANICSILICONE NEW MATERIAL +1
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The sealing rate of the process is not high

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  • Preparation method of methyl-terminated propenol polyether

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Embodiment 1

[0033](1) In the external circulation spray reactor (the average diameter of the droplet Sauter is 10 μm), add allyl alcohol polyoxyethylene ether raw material (molecular weight: 150) 150kg, remove oxygen and nitrogen replacement protection, open the external circulation pump for high-speed Cycle the spray.

[0034] (2) Controlling reaction temperature is 0 ℃, and liquid caustic soda (10%NaOH solution) 404kg raw material is sprayed in the reactor, feeds 51kg of monochloromethane raw material slowly simultaneously, realizes the sufficient mixing reaction of the three, and the feeding spraying time is 36 hours. After the feeding was finished, the heat preservation cycle spray reaction was continued for 12 hours, and the reaction ended.

[0035] (3) After the reaction is finished, the crude product is neutralized with 50% phosphoric acid, and then undergoes a post-treatment process of vacuum distillation and filtration to prepare a methyl-terminated allyl alcohol polyether produ...

Embodiment 2

[0037] (1) In the external circulation spray reactor (the average diameter of the droplet Sauter is 300 μm), add allyl alcohol polyoxyethylene ether raw material (molecular weight: 6000) 600kg, remove oxygen and nitrogen replacement protection, open the external circulation pump for high-speed Cycle the spray.

[0038] (2) Control the temperature at 60°C, spray 22.5 kg of potassium hydroxide solution (50% KOH) into the reactor, and slowly add 10.1 kg of monochloromethane raw material at the same time to realize the full mixing reaction of the three. for 2 hours. After the feeding was finished, the heat preservation cycle spray reaction was continued for 2 hours, and the reaction ended.

[0039] (3) After the reaction is finished, the crude product is neutralized with 50% phosphoric acid, and then undergoes a post-treatment process of vacuum distillation and filtration to prepare a methyl-terminated allyl alcohol polyether product. The color of the methyl-capped allyl alcohol...

Embodiment 3

[0041] (1) In the external circulation spray reactor (the average diameter of the droplet Sauter is 50 μm), add allyl alcohol polyoxyethylene ether raw material (molecular weight is 525) 525kg, remove oxygen and nitrogen replacement protection, open the external circulation pump for high-speed Cycle the spray.

[0042] (2) Control the temperature at 10°C, spray 243 kg of potassium hydroxide solution (30% KOH solution) into the reactor, and slowly add 65.6 kg of monochloromethane raw material to realize the full mixing reaction of the three. for 24 hours. After the feeding was finished, the heat preservation cycle spray reaction was continued for 6 hours, and the reaction ended.

[0043] (3) After the reaction is finished, the crude product is neutralized with 50% phosphoric acid, and then undergoes a post-treatment process of vacuum distillation and filtration to prepare a methyl-terminated allyl alcohol polyether product. The color of the methyl-capped allyl alcohol polyeth...

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Abstract

The invention discloses a preparation method of methyl-terminated propenol polyether. The preparation method includes: adding a propenol polyoxyethylene ether raw material into an external-circulating spray-type reactor for deoxidizing, nitrogenizing, replacement and protection; starting an external circulating pump for high-speed circulating spraying, controlling reaction temperature to 0-60 DEG C, and spraying a liquid alkali raw material into the reactor; slowly adding a methane chloride raw material, and sufficiently mixing for reaction. The system belongs to dynamic control systems, side reaction is sufficiently inhibited, and a low-temperature method is further adopted to control dynamic reaction according to the characteristic that the side reaction is high in activation energy, so that hydrolysis reaction of methane chloride is inhibited, allyl isomerization reaction is further inhibited, the reaction system is higher in selectivity, and color of methyl-terminated propenol polyether which is finally obtained is lower than 30 while terminating rate is higher than 98%.

Description

technical field [0001] The invention relates to the technical field of chemical engineering, in particular to a method for preparing methyl-terminated allyl alcohol polyether. Background technique [0002] As a polyether with special structure and performance, alkyl-terminated polyether has been widely used in the fields of synthetic lubricating oil, daily chemical industry and chemical fiber oil. The alkyl-terminated polyether in which all the hydroxyl groups in the polyether molecular chain are substituted by alkyl groups has higher chemical stability than the polyether containing hydroxyl groups in the molecular chain. Utilizing the good heat resistance of alkyl-terminated polyether, it can be used as an excellent non-ionic surfactant in the oil agent for high-speed spinning of chemical fibers, and can also be used as an additive in high-temperature-resistant lubricating oil or heat-conducting oil. Utilizing its stability to strong alkali, it can be used in strong alkali...

Claims

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Application Information

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IPC IPC(8): C08G65/337C08G65/30
CPCC08G65/337C08G65/30
Inventor 朱建华张治国索艳格杨振施旭亮
Owner RUNHE ORGANICSILICONE NEW MATERIAL
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