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Method and apparatus for synthesizing of chloromethylether of ethylamine intermediate product

A technology of chloromethyl ethyl ether and synthesis method, which is applied in the directions of ether preparation, organic part exchange to prepare ether, organic chemistry, etc., can solve the problems of high consumption of formaldehyde and ethanol, large amount of outsourcing, environmental pollution, etc., and achieves production cost Low, low consumption, environmental improvement effect

Inactive Publication Date: 2008-11-12
CNPC JILIN CHEM GROUP CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the aforementioned process, the COD content in the sewage exceeds the standard, up to 12000mg / L, and a large amount of money needs to be invested in wastewater treatment; hydrochloric acid gas causes corrosion and leakage of equipment pipelines, which seriously pollutes the environment
At the same time, the utilization rate of hydrogen chloride is only about 60%, the consumption of formaldehyde and ethanol is high, and a large amount of supplementary chloromethyl ethyl ether needs to be purchased, resulting in high production costs of acetochlor

Method used

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  • Method and apparatus for synthesizing of chloromethylether of ethylamine intermediate product
  • Method and apparatus for synthesizing of chloromethylether of ethylamine intermediate product

Examples

Experimental program
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Embodiment 1

[0029] Embodiment 1 (device required for the synthetic method of acetochlor intermediate chloromethyl ethyl ether)

[0030] As can be seen from Fig. 1, realize the required device of the synthetic method of acetochlor intermediate chloromethyl ethyl ether, this device mainly contains hydrochloric acid gas buffer tank 3, condenser 4, absorption tank 4, A still 1 and B still 2 , the tops of the A kettle 1 and the B kettle 2 are respectively equipped with an injector A1-2 and an injector B 2-2, and the described injector A 1-2 and the injector B 2-2 are respectively connected to the respective kettles through pipelines The top is connected, and the circulating pump C 1-1 of A kettle 1 and the circulating pump D 2-1 of B kettle 2 are connected to the bottom of the respective reaction kettles through pipelines to form a closed-circuit circulation system of A kettle 1 and B kettle 2; hydrochloric acid gas buffer Tank 3 is connected to the bottom pipes of A kettle 1 and B kettle 2 re...

example example 2

[0031] Example example 2: (the synthetic method of acetochlor intermediate chloromethyl ethyl ether of the present invention)

[0032] As can be seen from Fig. 1, according to the molar ratio of paraformaldehyde: ethanol: HCl=1: 1.1: 2, the paraformaldehyde 600kg of 94% by weight is dissolved in the ethanol 1200L (about 950kg) of 95% percentage respectively. The obtained formaldehyde / ethanol solution is pumped into A kettle 1 and B kettle 2 to carry out etherification reaction.

[0033]Open the K1 valve on the pipeline connecting the bottom pipe of A kettle 1 and the HCl gas buffer tank 3, the K3 valve on the pipeline connecting injector A 1-2 on the top of A kettle 1, and connect the injector B 2-2 and A on the B kettle 2 The K5 valve on the pipeline of kettle 1, the K8 valve on the pipeline connecting the top of kettle 2 of B and the top of condenser 4, the valve on the pipeline connecting the bottom of condenser 4 and the top of kettle 2 of B; at the same time, close the in...

example 3

[0040] Example 3: (the synthetic method of acetochlor intermediate chloromethyl ethyl ether of the present invention)

[0041] As can be seen from Fig. 1, according to the molar ratio of paraformaldehyde: ethanol: HCl=1: 1.2: 2.3, the paraformaldehyde 600kg of 94% by weight percentage is dissolved in 95% by weight ethanol 1375L (about 1100kg) respectively, will obtain The formaldehyde / ethanol solution pumped into A kettle 1 and B kettle 2.

[0042] Open the K1 valve on the pipeline connecting the bottom pipe of A kettle 1 and the HCl gas buffer tank 3, the K3 valve on the pipeline connecting injector A 1-2 on the top of A kettle 1, and connect the injector B 2-2 and A on the B kettle 2 The K5 valve on the pipeline of kettle 1, the K8 valve on the pipeline connecting the top of kettle 2 of B and the top of condenser 4, the valve on the pipeline connecting the bottom of condenser 4 and the top of kettle 2 of B; at the same time, close the injector A 1- 2 and the K2 valve on the...

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Abstract

The invention discloses a method and a device for synthesizing chloromethyl ethyl ether, an immediate of acetochlor. Polyformaldehyde and alcohol with the needed amount are added into an A kettle and a B kettle; through circulating ejection systems of the A kettle and the B kettle, hydrochloric acid gas enters the A kettle to react, escaped hydrochloric acid gas continues to be etherified in an ejector of the A kettle and the A kettle, and the unreacted hydrochloric acid gas enters an ejector of the B kettle and the B kettle and continues to react; and uncondensed gas enters a condenser and an absorbing tank. When a product in the A kettle is qualified, the product is discharged; the operation is switched to feed fillings into the A kettle; the hydrochloric acid gas enters the B kettle for etherification, the escaped hydrochloric acid gas continues to be etherified in the B kettle and the ejector of the B kettle, the unreacted hydrochloric acid gas enters the A kettle and the ejector of the A kettle and continues to react, and unreacted light component gas enters the condenser and the absorbing tank; when a product in the B kettle is qualified, the product is discharged, and one-time switching operation of the A kettle and the B kettle is finished. The utilization rate of the hydrochloric acid gas is improved by 30 percent or so, no waste water exists during the etherification, and the cost of the product is apparently reduced.

Description

technical field [0001] The invention relates to the improvement of the etherification process in the preparation of acetochlor, in particular to the synthesis method and device of the acetochlor intermediate chloromethyl ethyl ether. Background technique [0002] As we all know, acetochlor is an excellent herbicide, which is widely used in corn, cotton, peanut and soybean fields for pre-emergent weeding. [0003] At present, the production of acetochlor mainly includes two steps of acylation and etherification. Etherification adopts double-pot switching operation, and hydrochloric acid gas reacts with polyoxymethylene and ethanol to produce chloromethyl ethyl ether. The HCl gas from the HCl gas buffer tank is introduced into the reaction kettle through the bottom tube, and the etherification reaction is carried out under stirring to generate chloromethyl ethyl ether, and the unreacted hydrochloric acid gas enters the 2 kettles in series to continue the reaction. Unload whe...

Claims

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Application Information

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IPC IPC(8): C07C43/17C07C41/14
Inventor 王传林田晓军霍凤华李子辉历秀萍
Owner CNPC JILIN CHEM GROUP CORP
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