Technology for post-treating cyanacetate

A cyanoacetate and process technology, which is applied in the post-treatment process field of industrial methyl cyanoacetate or ethyl cyanoacetate, can solve problems such as difficult rectification and separation of malonate diester impurities, and achieve high removal rate, The effect of simple equipment structure and simple process operation

Inactive Publication Date: 2012-02-15
常州市康瑞化工有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Water is involved in the whole process, and there are many opportunities for hydrolysis. At high temp...

Method used

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  • Technology for post-treating cyanacetate
  • Technology for post-treating cyanacetate

Examples

Experimental program
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Effect test

Embodiment 1

[0017] A treatment tower with a diameter of 200mm and a length of 2000mm. There is a PE sintered tube with a length of 300mm and a precision of 5μ in the tower body. After the filter medium, there is a ceramic membrane fine outlet filter. The treatment medium component is 50% Na 2 CO 3 , 20% CaO and 30% cation exchange resin; the components of methyl cyanoacetate liquid to be treated are 99.2% methyl cyanoacetate, 20ppm cyanide, 0.08% dimethyl malonate, 0.12% moisture, and 0.1% acidity ;The liquid to be treated enters the tower body from the inlet, passes through the treatment medium layer, filter medium layer and ceramic membrane fine outlet filter, and flows out from the outlet; the treatment flow rate is 1.0-1.5m 3 / h; the obtained finished product components are 99.4% of methyl cyanoacetate, cyanide<2ppm, 0.03% of dimethyl malonate, 0.01% of moisture, and 0.02% of acidity.

Embodiment 2

[0019] A treatment tower with a diameter of 100mm and a length of 1500mm. The filter medium layer is a microporous filter membrane, the precision of the filter medium is 0.142μ; the treatment medium component is 70% K 2 CO 3 , 10% CaO and 20% cation exchange resin; the components of methyl cyanoacetate liquid to be treated are 99.2% methyl cyanoacetate, 20ppm cyanide, 0.15% dimethyl malonate, 0.06% moisture, and 0.2% acidity ;The liquid to be treated enters the tower body from the inlet, passes through the treatment medium layer and the filter medium layer, and flows out from the outlet; the treatment flow rate is 0.150-0.200m 3 / h; the finished product components obtained after recycling treatment are 99.4% of methyl cyanoacetate, cyanide<2ppm, 0.05% of dimethyl malonate, 0.008% of moisture, and 0.02% of acidity.

Embodiment 3

[0021] A treatment tower with a diameter of 100mm and a length of 1500mm, the filter medium layer is a microporous filter membrane, the precision of the filter medium is 0.142μ; the treatment medium component is 70% K 2 CO 3 , 10% CaO and 20% cation exchange resin; the components of ethyl cyanoacetate liquid to be treated are 98.5% ethyl cyanoacetate, 20ppm cyanide, 0.80% diethyl malonate, 0.05% moisture, and 0.2% acidity ;The processing flow is 0.150-0.200m 3 / h; the liquid to be treated enters the tower body from the inlet, passes through the treatment medium layer and the filter medium layer, and flows out from the outlet; the finished product components obtained are ethyl cyanoacetate 98.7%, cyanide<2ppm, diethyl malonate 0.50 %, moisture 0.07%, acidity 0.02%.

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Abstract

The invention relates to the technical field of chemical engineering, and especially relates to a technology for post-treating cyanacetate. The technology for post-treating cyanacetate with an alkali neutralizer, an adsorbent and a drying agent is characterized in that: cyanacetate to be treated continuously goes through a tower filled with an excess solid treating medium, and a filtering medium, and a finished product is obtained in a one-step mode without separation, wherein the solid treating medium is a porous cylinder prepared from a material comprising, by mass, 5-30% of CaO, 30-80% of a carbonate and 5-60% of an ion exchange resin. The technology of the invention has the characteristics of simple equipment structure and simple flow operation; and the cyanacetate to be treated enters the tower from the inlet, goes through the treating medium and the filtering medium, and becomes the finished product after flowing out of the outlet, so the technology of the invention has the advantages of one-step continuous treating at normal temperature, no wastewater generation, no generation of dimalonate impurities, and high cyano removal rate, high acidity removal rate and high water removal rate when the water content is low.

Description

technical field [0001] The invention relates to the technical field of chemical engineering, in particular to a post-treatment process of industrial methyl cyanoacetate or ethyl cyanoacetate. Background technique [0002] Cyanoacetate, the main industrial product is methyl cyanoacetate or ethyl cyanoacetate, which are oily liquids slightly soluble in water, with a specific gravity slightly larger than water, a boiling point of 205-210°C, and a refractive index of about 1.412. It is easily hydrolyzed at high temperature, and is mainly used in dyes, adhesives, medicines, pesticides, fine chemical intermediates and organic solvents containing cyanide. The national standard GB / T26606-2011 stipulates the technical requirements for industrial methyl cyanoacetate, the main indicators are methyl cyanoacetate content, dimethyl malonate content, acidity and moisture. [0003] At present, the common process method of cyanoacetate post-treatment is: 1. In an intermittent glass-lined re...

Claims

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Application Information

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IPC IPC(8): C07C255/19C07C253/34
Inventor 李大忠张瑞宽袁根林周爱军
Owner 常州市康瑞化工有限公司
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