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Preparation and pre-use treatment method for glycolonitrile with cyanide-containing tail gas as raw material

A technology of hydroxyacetonitrile and tail gas, which is applied in the preparation of carboxylic acid nitriles, chemical instruments and methods, and the preparation of organic compounds, etc., can solve the problems of industrial waste water, waste gas, environmental pollution, etc., and achieve the effect of avoiding direct discharge into the atmosphere

Inactive Publication Date: 2016-04-06
ZHEJIANG QIANJIANG BIOCHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] The cyanation reaction is a very important step reaction in the synthesis process of mainstream steroid drug intermediates. This type of reaction uses potassium cyanide, sodium cyanide, acetone cyanohydrin, etc. Industrial wastewater and waste gas containing HCN are easy to pollute the environment

Method used

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  • Preparation and pre-use treatment method for glycolonitrile with cyanide-containing tail gas as raw material
  • Preparation and pre-use treatment method for glycolonitrile with cyanide-containing tail gas as raw material
  • Preparation and pre-use treatment method for glycolonitrile with cyanide-containing tail gas as raw material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Embodiment 1: the screening of catalyst.

[0017] Basic process such as figure 1 As shown, the reaction device is as figure 2 , Weigh 130g NaCN into the reaction bottle A1, and add 81g of formaldehyde (configured into an aqueous solution with a mass concentration of 37%) into the 500ml reaction bottle B2 and the 500ml reaction bottle C3, and add different catalysts, stir for 10min, and connect Tail gas absorption device 4, use the dropping funnel to slowly add acetic acid to the reaction bottle A1, control the dropping speed and control the temperature of the reaction bottle B2 to 15°C with a water bath, and take a sample to detect the product concentration in the reaction bottle B2 after 1 hour of reaction. Experimental results show that various bases can play a catalytic role, sodium sulfite is relatively ideal, but the amount of catalyst directly affects the pH of the reaction system, so the input amount of reaction catalyst base must be strictly controlled. If th...

Embodiment 2

[0020] Example 2: Screening of catalyst addition.

[0021] Basic process such as figure 1 As shown, the reaction device is as figure 2 , Weigh 130g NaCN into reaction bottle A1, and add 81g formaldehyde (configured into an aqueous solution with a mass concentration of 37%) into 500ml reaction bottle B2 and 500ml reaction bottle C3, and add different amounts of catalyst NaCN 2 SO 3 , stirred for 10 minutes, connected the tail gas absorbing device 4, slowly added acetic acid dropwise to the reaction bottle A1 with a dropping funnel, controlled the dropping speed and controlled the temperature of the reaction bottle B2 to 15°C with a water bath, and took samples at intervals to detect the remaining formaldehyde in the reaction bottle B2 When the concentration of formaldehyde in the reaction solution is ≤0.5%, the reaction is considered to be over. After the end, sulfuric acid is used as a stabilizer to adjust the pH to 2.0, and the reaction end time is recorded. The concentra...

Embodiment 3

[0024] Embodiment 3: determination of reaction temperature.

[0025] Basic process such as figure 1 As shown, the reaction device is as figure 2 As shown, in combination with the above experiments, 130g of NaCN was weighed into the reaction bottle A1, and 81g of formaldehyde (configured into an aqueous solution with a mass concentration of 37%) was added to the 500ml reaction bottle B2 and 500ml reaction bottle C3, and NaCN was added. 2 SO 3 , stirred for 10 minutes, connected the tail gas absorption device 4, slowly added acetic acid dropwise to the reaction bottle A1 with a dropping funnel, added dropwise at a certain speed and controlled different reaction temperatures with a water bath, and took samples at intervals to detect the remaining amount of formaldehyde in the reaction bottle B2 , when the concentration of formaldehyde in the reaction solution is ≤0.5%, the reaction is considered to be over, and after the end, sulfuric acid is used as a stabilizer to adjust the...

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Abstract

The invention relates to a preparation and pre-use treatment method for glycolonitrile with cyanide-containing tail gas as the raw material. According to the method, the cyanide-containing tail gas is introduced into multiple stages of reaction stills containing formaldehyde and a catalyst to be directly subjected to an addition reaction, and a glycolonitrile product with a certain concentration is obtained; after material transferring, the glycolonitrile product is stored under the effect of a stabilizer for use, and before use, the pH is regulated with base or weak base till the glycolonitrile product is neutral. The catalyst is one of basic compounds including Na2SO3, Na2CO3, NaHCO3 and NaOH, the mass concentration of formaldehyde is 35%-37%, the mol ratio of formaldehyde to the catalyst is 1:(0.001-0.05), and the reaction temperature is 5-20 DEG C. According to the method, HCN in industrial waste gas of a steroid drug is chemically absorbed through formaldehyde, the catalyst and the stabilizer, glycolonitrile is generated through the reaction and serves as a raw material for biological preparation of glycollic acid, and therefore the cyanide-containing tail gas is fully absorbed and utilized and prevented from being directly exhausted to the atmosphere and polluting the environment.

Description

technical field [0001] The invention belongs to the technical field of waste gas recovery and utilization, and in particular relates to a method for the preparation and pre-use treatment of hydroxyacetonitrile using cyanide-containing tail gas as a raw material. Background technique [0002] The cyanation reaction is a very important step reaction in the synthesis process of mainstream steroid drug intermediates. This type of reaction uses potassium cyanide, sodium cyanide, acetone cyanohydrin, etc. Industrial wastewater and waste gas containing HCN are easy to pollute the environment. Recycling of waste water and waste gas not only reduces pollution, is beneficial to environmental protection, but also achieves the purpose of fully utilizing resources. How to recycle and turn waste into wealth is a very important topic in this field. Contents of the invention [0003] The purpose of the present invention is to provide a method for preparing hydroxyacetonitrile by using c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C255/12C07C253/00
CPCC07C253/00C07C255/12Y02A50/20
Inventor 薛建萍祝金山徐玉华唐璐敏傅业件
Owner ZHEJIANG QIANJIANG BIOCHEMICAL CO LTD
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