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Synthesis method for triethyl orthoformate

A technology of triethyl orthoformate and ethanol, which is applied in the field of synthesis of triethyl orthoformate, can solve the problems of product damage, reduced output of triethyl orthoformate, and imperfect dehydration efficiency, etc., and achieves reduced loss and simple synthesis method Feasible effect

Active Publication Date: 2014-03-26
临沭县华盛化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition to some moisture in the raw materials, in the production process, equipment (cooling coils, tower kettle reboilers, etc.) often inevitably have slight water leakage and water seepage, and the high water content in the system will also make orthoformic acid The production of triethyl ester decreased
[0006] In the synthesis reaction of triethyl orthoformate, the mass fraction of water in the reaction synthesis liquid is usually more than 1%. Even if the moisture can be reduced to about 0.5% after proper drying, more than 15% of the product will be hydrolyzed and destroyed. Therefore, whether the trace moisture in the synthetic liquid can be completely removed is the key to further improving the yield of triethyl orthoformate
The literature (removal of trace moisture in triethyl orthoformate synthesis liquid, Wang Xiangrong, etc., Shanxi Chemical Industry 2008) has studied the dehydrating agent and dehydration conditions for removing trace moisture in the one-step synthetic reaction of triethyl orthoformate, and found that glycerol It can be used as a dehydrating agent in one-step synthesis, in which the amount of glycerol is relatively large, which is 7% of the quality of the synthetic liquid, and the minimum water quality in the synthetic liquid is about 0.2%, and the maximum of triethyl orthoformate is The productive rate is 98%; it can be seen that glycerol is used as a dehydrating agent in a relatively large amount, and the dehydration efficiency is not perfect yet

Method used

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  • Synthesis method for triethyl orthoformate
  • Synthesis method for triethyl orthoformate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] A kind of synthetic method of triethyl orthoformate, it comprises the steps:

[0022] First add 60% solvent to the neutralization crystallization kettle, cool down to about 0°C, add ethanol, continue to cool down to minus 5°C, add dehydrating agent, the amount of dehydrating agent added is 1% of the solvent mass, and then pass HCl gas , continue to cool down to minus 7°C, add imine, and then slowly add another 40% solvent, after 1 hour, the neutralization and crystallization is completed, discharge the material into the alcoholysis kettle, heat up to about 20°C, add ethanol for alcoholysis, and keep warm After reacting for 10 hours, carry out centrifugation to obtain the mixed solution, and then distill to obtain the finished triethyl orthoformate, and the solid obtained by centrifugation is ammonium chloride, which is then sold as a by-product.

[0023] The above-mentioned dehydrating agent is composed of glycerol, activated clay and 4A molecular sieve, and the mass ra...

Embodiment 2

[0028] A kind of synthetic method of triethyl orthoformate, it comprises the steps:

[0029] First add 60% solvent to the neutralization crystallization kettle, cool down to about 0°C, add ethanol, continue to cool down to minus 5°C, add dehydrating agent, the amount of dehydrating agent added is 2% of the solvent mass, and then pass HCl gas , continue to cool down to minus 7°C, add imine, and then slowly add another 40% solvent, after 1 hour, the neutralization and crystallization is completed, discharge the material into the alcoholysis kettle, heat up to about 20°C, add ethanol for alcoholysis, and keep warm After reacting for 10 hours, carry out centrifugation to obtain the mixed solution, and then distill to obtain the finished triethyl orthoformate, and the solid obtained by centrifugation is ammonium chloride, which is then sold as a by-product.

[0030] The above-mentioned dehydrating agent is composed of glycerol, activated clay and 4A molecular sieve, and the mass ra...

Embodiment 3

[0036] The dehydration effect comparison of dehydrating agent of the present invention:

[0037] Groups: divided into four groups, wherein, control group 1: without adding any dehydrating agent; control group 2: glycerol; control group 3: glycerol+4A molecular sieve (mass ratio is 5: 1); the present invention: Glycerol + activated clay + 4A molecular sieve (mass ratio is 5:1:1). The added amount of the above-mentioned dehydrating agent is 2% of the solvent mass. Moisture and triethyl orthoformate product yield in the mixed solution after detecting alcoholysis, specifically refer to table 3:

[0038] table 3

[0039] group

[0040] Conclusion: the dehydrating agent of the present invention is obviously better than the glycerol dehydrating agent and the molecular sieve dehydrating agent in the prior art, and the dosage is small, so that the moisture is greatly reduced and the yield of triethyl orthoformate is greatly improved.

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Abstract

The invention discloses a synthesis method for triethyl orthoformate. In the synthesis method, a dehydrating agent is used and comprises glycerin, active argil and 4A molecular sieve at the mass ratio of 10:(2-1):(2-1). Through the dehydrating agent, moisture in the synthesis process of triethyl orthoformate can be greatly decreased, the loss amount of the triethyl orthoformate product in the separation stage can be reduced, the raw material waste and industrial energy consumption can be reduced, and the synthesis method is applicable to large-scale industrial production.

Description

technical field [0001] The invention belongs to the technical field of triethyl orthoformate production, and relates to a synthesis method of triethyl orthoformate. Background technique [0002] Triethyl orthoformate, also known as triethoxymethane, is a colorless transparent liquid widely used as an intermediate in the synthesis of chloroquine, quinoline, dichloroquinoline, norfloxacin, ciprofloxacin, and fluperquine It is also used in the synthesis of acrylic acid and other fibers and methine dyes and cyanine dyes; as an anti-halation material, it is widely used in photosensitive materials such as photographic medicines and color film films. [0003] There are many synthetic methods for triethyl orthoformate, including one-step method, two-step method, phase transfer method, etc. according to foreign literature reports. At present, most of the domestic pesticide factories and pharmaceutical factories adopt the two-step method. The two-step method is to use solid alkali an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/32C07C41/60C01C1/16
CPCC01C1/16C07C41/60C07C43/32
Inventor 赵一凡赵志刚孙承权王亮亮
Owner 临沭县华盛化工有限公司
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