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Process for preparing orthoformate from hydrocyanic acid as waste gas of acrylonitrile plant

A technology for waste gas hydrocyanic acid and acrylonitrile plant, which is applied in the preparation of organic compounds, chemical instruments and methods, organic chemistry, etc. Good, low-cost, high-yield effects

Inactive Publication Date: 2004-08-25
山东未名天源生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] High cost, low yield and quality, unable to compete with hydrocyanic acid method

Method used

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  • Process for preparing orthoformate from hydrocyanic acid as waste gas of acrylonitrile plant
  • Process for preparing orthoformate from hydrocyanic acid as waste gas of acrylonitrile plant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Example 1 The molar ratio of the reaction materials is hydrocyanic acid: ethanol: hydrobromic acid = 1: 3.5: 1.1.

[0024] Feed HCN 218.18kg (content 99%, pure 216kg, 8kmol), the first part of absolute ethanol 443.8kg (content 99.5%, pure 441.6kg, 9.6kmol) and 2000L solvent oil, add to the reaction kettle and stir well, cool down To -10°C, evenly feed 712.8kg of hydrogen bromide gas, the reaction process maintains a temperature of -10~-20°C, after passing through, maintain this temperature, after the imide salt is completely precipitated, add a second portion of absolute ethanol 850.6kg ( content of 99.5%, converted to pure 846.4kg, 18.4kmol), adjust the pH of the reaction solution to 0.5-3.0, keep the temperature at 50-60°C, react for 48 hours, remove ammonium bromide after alcoholysis, evaporate the solvent and then rectify to obtain orthoformic acid tris The ethyl ester finished product is 984.67kg, the content determined by chromatography is 99.20%, the pure 976.8kg...

Embodiment 2

[0025] Example 2 The molar ratio of the reaction materials is hydrocyanic acid: ethanol: hydrobromic acid=1: 3.8: 1.2.

[0026] Feed HCN 218.18kg (content 99%, pure 216kg, 8kmol), the first portion of absolute ethanol 517.7kg (content 99.5%, pure 515.2kg, 11.2kmol), cool to -5 ° C, pass hydrogen bromide gas 777.6 kg, the reaction temperature is -5~-10°C, after passing through, maintain this temperature, after the imide salt is completely precipitated, add the second portion of absolute ethanol 887.6kg (content 99.5%, pure 883.2kg, 19.2kmol), and maintain the temperature After reacting for 24 hours at 40-50°C, 964.84kg of triethyl orthoformate was obtained, the content determined by chromatography was 99.03%, and the pure product was 955.5kg, with a yield of 80.7%. The rest are the same as Example 1.

Embodiment 3

[0027] Example 3 The molar ratio of the reaction materials is hydrocyanic acid: ethanol: hydrobromic acid=1: 3.75: 1.25.

[0028] Feed intake HCN 218.18kg (content 99%, pure 216kg, 8kmol), the first part of absolute ethanol 499.2kg (content 99.5%, pure 496.8kg, 10.8kmol), inert solvent cyclohexane, cooled to 5 ℃, Pass 810kg of hydrogen bromide gas, the reaction temperature is 5-10°C, after passing through, maintain this temperature, after the imide salt is completely precipitated, add the second part of absolute ethanol 887.6kg (content 99.5%, pure 883.2kg, 19.2kmol) , keeping the temperature at 30-40° C., and reacting for 36 hours, 919.24 kg of triethyl orthoformate was obtained, with a content of 98.92%, 909.3 kg of pure product, and a yield of 76.8%. The rest are the same as Example 1.

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Abstract

A process for preparing orthoformate from the hydrocyanic acid as the waste gas of acrylonitrile plant includes such steps as reaction of hydrocyanic acid as initial raw material on corresponding alcohol and halogen acid in inertial solvent through forming salt, alcoholysis, crystallizing, separation and rectifying to obtain trimethyl orthoformate with methanol or triethyl orthoformate with ethanol. Its advantages include low cost, high output rate and quality, and use of waste as raw material.

Description

technical field [0001] The invention belongs to the category of environmental protection technology, and relates to a process for preparing orthoformate by using hydrogen cyanide, the waste gas discharged from an acrylonitrile factory. Background technique [0002] The production process of acrylonitrile discharges a large amount of waste gas containing hydrocyanic acid (the content of hydrocyanic acid is about 70-95%, the rest is nitrogen 2.0-28%, ammonia 1.0-1.5%, propylene 1.0-1.5%), acrylonitrile plant of Qilu Petrochemical Company The current annual discharge is about 4,800 tons. The traditional treatment method is to use it as a by-product of sodium cyanide. The disadvantage of the traditional treatment method is that the added value of by-products is low and resources are wasted. [0003] US 3,641,164 proposed HCN and C 1 ~C 4 Alkyl alcohol and HCl can prepare orthoformate, but this is the U.S. patent application in the early 1970s, which is a small amount of test ...

Claims

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Application Information

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IPC IPC(8): C07C41/60C07C43/32
Inventor 高庆昌
Owner 山东未名天源生物科技有限公司