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Refining method for reducing content and smell of benzyl halide in benzyl ether

A refining method and technology of benzyl ether, applied in ether preparation, chemical instruments and methods, ether separation/purification, etc., can solve the problems of benzyl ether with strong odor, increased safety hazards, high equipment requirements, etc., to eliminate odor and simplify Refined operation, low energy consumption effect

Active Publication Date: 2022-04-22
ZHEJIANG HUANGMA TECH +3
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to achieve a higher yield and end-capping rate, benzyl ethers are generally prepared with excess alkali and benzyl halides, so that more benzyl halides remain in the product benzyl ethers, resulting in the use of benzyl-type halogenated hydrocarbons. The obtained benzyl ether has a strong odor
At present, the refining method of benzyl ether is generally to remove the benzyl halide by vacuumizing at a high temperature of 130-150 ° C, but for unreacted benzyl chloride (boiling point is 175 ° C), benzyl bromide (boiling point is 198 ℃) and other benzyl halides with higher boiling points, it needs relatively harsh high temperature and extremely low pressure conditions to remove, which requires high equipment, which not only increases safety hazards, but also takes a long time and consumes high energy.

Method used

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  • Refining method for reducing content and smell of benzyl halide in benzyl ether
  • Refining method for reducing content and smell of benzyl halide in benzyl ether

Examples

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Effect test

Embodiment 1

[0035] A refining method for reducing benzyl halide content and odor in benzyl ether, comprising the following steps:

[0036] S1. Add 97 g of triethylamine (0.48 mol) solution with a mass concentration of 50% to 1410 g of the crude benzyl ether product after the etherification reaction (the capping rate is calculated as 90%, containing 0.4 mol of benzyl chloride), and start stirring , reflux reaction at 60°C for 2 hours;

[0037] S2, after the heat preservation is finished, let it stand for stratification, the upper layer liquid is the crude product, and the lower layer water phase is separated from the system and recovered to obtain an aqueous solution containing the phase transfer catalyst benzyltriethylammonium chloride;

[0038] S3, add 3.26g neutralizing agent phosphoric acid aqueous solution (mass percentage concentration 50%) to make pH=4 in upper layer liquid, then add adsorbent magnesium silicate 14g, filter aid diatomite 7g, refine under 100 ℃, 10mbar After filtrat...

Embodiment 2

[0041] A refining method for reducing benzyl halide content and odor in benzyl ether, comprising the following steps:

[0042] S1. Add 95 g of triethylamine (0.42 mol) solution with a mass concentration of 45% to 1280 g of crude benzyl ether after the etherification reaction (the capping rate is calculated as 90%, containing 0.3 mol of benzyl bromide), and start stirring , reflux reaction at 70°C for 1.5h;

[0043] S2, after the heat preservation is finished, let it stand for stratification, the upper layer liquid is the crude product, and the lower layer water phase is separated from the system and recovered to obtain an aqueous solution containing the phase transfer catalyst benzyltriethylammonium bromide;

[0044] S3, add 2.72g neutralizing agent phosphoric acid aqueous solution (mass percentage concentration 50%) to make pH=3.8 to upper layer liquid, then add adsorbent magnesium silicate 12g, filter aid diatomite 6g, refine under 100 ℃, 10mbar After filtration, the refine...

Embodiment 3

[0047] A refining method for reducing benzyl halide content and odor in benzyl ether, comprising the following steps:

[0048] S1. Add 48 g of triethylamine (0.28 mol) solution with a mass concentration of 60% to 1670 g of crude benzyl ether after the etherification reaction (the capping rate is calculated as 90%, containing 0.2 mol of benzyl chloride), and start stirring , reflux reaction at 65°C for 3 hours;

[0049] S2, after the heat preservation is finished, let it stand for stratification, the upper layer liquid is the crude product, and the lower layer water phase is separated from the system and recovered to obtain an aqueous solution containing the phase transfer catalyst benzyltriethylammonium chloride;

[0050] S3, add 3.08g neutralizing agent phosphoric acid aqueous solution (mass percentage concentration 50%) to make pH=4.2 in upper layer liquid, then add adsorbent magnesium silicate 16g, filter aid diatomite 8g, refine under 100 ℃, 10mbar After filtration, the r...

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Abstract

The invention discloses a refining method for reducing the content and smell of benzyl halide in benzyl ether, and belongs to the technical field of chemical engineering. According to the refining method, a triethylamine solution is added before conventional refining post-treatment to consume benzyl halide which is not completely reacted, a phase transfer catalyst which is easily dissolved in water is generated, and the phase transfer catalyst is easily separated from benzyl ether after layering, so that the prepared benzyl ether is free of benzyl halide residues and odorless; compared with the prior art, the method has the advantages of mild reaction conditions, low energy consumption and high refining efficiency.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a refining method for reducing the benzyl halide content and odor in benzyl ether. Background technique [0002] At present, benzyl-terminated polyoxyethylene polyoxypropylene block polyether is usually obtained by shortening the ether chain of a general polyether defoamer and using benzyl-termination. The resulting product has excellent stability on the surface of solid caustic It is non-toxic, low foaming at low temperature, and easy to biodegrade. It is especially suitable for use as a special dishwashing agent, so it is included in the "List of Food Detergent Raw Materials (Ingredient) (First Batch)". The reaction that obtains benzyl ether by fatty alcohol polyoxyethylene polyoxypropylene ether through Williamson ether-forming reaction is as follows: [0003] ROH+NaOH→RONa+H 2 o [0004] [0005] The halogenated hydrocarbon used in the above reaction is benzyl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/44C07C41/36C07C41/34C07C43/164B01J31/02
CPCC07C41/44C07C41/36C07C41/34B01J31/0239C07C43/164
Inventor 张静金一丰张美军王马济世陈荧杰
Owner ZHEJIANG HUANGMA TECH
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