Preparation method of allyl alcohol polyether glycidyl ether

A technology of glycidyl ether and allyl alcohol polyether, which is applied in the chemical industry, can solve the problems of ring-opening addition side reactions of epoxy groups, many intermediate by-products, affecting product yield, etc., and achieves an improvement in the uniformity of concentration distribution. , the effect of reducing side reactions, improving selectivity and efficiency

Inactive Publication Date: 2017-03-15
RUNHE ORGANICSILICONE NEW MATERIAL +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the reported patents, there is almost no glycidyl ether for synthesizing long chains, and there are also problems such as the above-mentioned easy ring-opening addition of epoxy groups to produce side reactions, resulting in more intermediate by-products, which ultimately affect the yield of the product. Rate
[0006] Chinese patents CN104387576A, CN101928389A, CN102050943A and CN102060989A report several preparation methods of glycidyl ether group-terminated allyl alcohol polyether, using allyl alcohol polyether as raw material, through catalyst NaH, or raw material NaH, or solid base as Raw materials, glycidyl ether group-terminated allyl alcohol polyether has been prepared, but there are disadvantages such as high cost of raw materials and difficulty in popularization, too strong alkalinity of raw materials, deep color of products, and many by-products.

Method used

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  • Preparation method of allyl alcohol polyether glycidyl ether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (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.

[0031] (2) Control the temperature at 10° C., spray 93.5 kg of epichlorohydrin raw materials and 404 kg of liquid caustic soda (10% NaOH solution) into the reactor, realize the full mixing reaction of the three, and the feeding spray time is 24 hours. After the feeding was finished, the heat preservation cycle spray reaction was continued for 24 hours, and the reaction ended.

[0032] (3) After the reaction is completed, after neutralization with 50% phosphoric acid, the allyl alcohol polyether glycidyl ether is prepared through a post-treatment process of vacuum distillation and filtration. Allyl alcohol polyether glycidyl ether has a color of 20 and a capping rate of ...

Embodiment 2

[0034] (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.

[0035] (2) Control the temperature at 55° C., spray 13.9 kg of epichlorohydrin raw material and 12 kg of liquid caustic soda (50% NaOH solution) into the reactor, realize the full mixing reaction of the three, and the feeding spray time is 3 hours. After the feeding was finished, the heat preservation cycle spray reaction was continued for 3 hours, and the reaction ended.

[0036] (3) After the reaction is completed, after neutralization with 50% phosphoric acid, the allyl alcohol polyether glycidyl ether is prepared through a post-treatment process of vacuum distillation and filtration. Allyl alcohol polyether glycidyl ether has a color of 22 and a capping rate of 97...

Embodiment 3

[0038](1) In the external circulation spray reactor (the average diameter of the droplet is 50 μm), add allyl alcohol polyoxyethylene ether raw material (molecular weight: 500) 500kg, remove oxygen and nitrogen replacement protection, open the external circulation pump for high-speed Cycle the spray.

[0039] (2) Control the temperature at 15° C. Spray 120 kg of epichlorohydrin raw materials and 243 kg of potassium hydroxide solution (30% KOH solution) into the reactor to realize the sufficient mixing reaction of the three, and the feeding spray time is 12 hours. After the feeding was finished, the heat preservation cycle spray reaction was continued for 12 hours, and the reaction ended.

[0040] (3) After the reaction is completed, after neutralization with 50% phosphoric acid, the allyl alcohol polyether glycidyl ether is prepared through a post-treatment process of vacuum distillation and filtration. Allyl alcohol polyether glycidyl ether has a color of 18 and a capping ra...

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Abstract

The invention discloses a preparation method of allyl alcohol polyether glycidyl ether. The method comprises the following steps: in an external circulation spray reactor, adding allyl alcohol polyoxyethylene ether raw materials, carrying out deoxygenation-nitrogenization replacement protection, starting an outer circulating pump to carry out high-speed circulating spray; controlling the temperature at 10 to 55 DEG C, spraying epichlorohydrin raw materials and liquid caustic soda raw materials into the reactor to fully mix and make the allyl alcohol polyoxyethylene ether raw materials, the epichlorohydrin raw materials and the liquid caustic soda raw materials react and the like, the system belongs to a kinetic control system, and side effects are further sufficiently inhibited. In addition, according to the characteristic of high activation energy of the side effects, the preparation method of the allyl alcohol polyether glycidyl ether uses a low-temperature method to carry out kinetic reaction control, so that a reaction system is higher in selectivity. The color of the finally obtained product, namely the allyl alcohol polyether glycidyl ether is less than 40, and the capping rate of the allyl alcohol polyether glycidyl ether is greater than 96%.

Description

technical field [0001] The invention relates to the technical field of chemical engineering, in particular to a preparation method of allyl alcohol polyether glycidyl ether. 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. Alkyl-terminated polyethers in which all hydroxyl groups in the molecular chain are substituted by alkyl groups have higher chemical stability than polyethers 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 alkaline detergent formulat...

Claims

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Application Information

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IPC IPC(8): C08G65/337C07D303/27C07D301/28
CPCC08G65/337C07D301/28C07D303/27
Inventor 朱建华张治国索艳格杨振施旭亮
Owner RUNHE ORGANICSILICONE NEW MATERIAL
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