Process and device for preparing orthoformate by using byproduct hydrocyanic acid from acrylonitrile production

An orthoformate and hydrocyanic acid technology, applied in ether preparation, organic chemistry and other directions, can solve the problems of low added value and waste of resources, and achieve the effects of reducing reaction by-products, improving product quality and stable reaction temperature

Active Publication Date: 2009-02-04
YINGKOU YINGXIN CHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

These products have low add

Method used

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  • Process and device for preparing orthoformate by using byproduct hydrocyanic acid from acrylonitrile production
  • Process and device for preparing orthoformate by using byproduct hydrocyanic acid from acrylonitrile production
  • Process and device for preparing orthoformate by using byproduct hydrocyanic acid from acrylonitrile production

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Embodiment 1: the molar ratio of reaction material is hydrocyanic acid: ethanol: hydrogen bromide=1: 3.5: 1.30.

[0020] Add 231.82kg of hydrocyanic acid (content 99%, pure 229.50kg, 8.5kmol), the first ethanol 432.26kg (content 99.5%, pure 430kg, 9.35kmol), inert solvent 2000kg, into the built-in plastic tube bundle coil In the halogenation reaction kettle of the heat exchanger, the temperature is lowered to -20°C, and 894.0kg of hydrogen bromide is uniformly introduced, and the reaction temperature is maintained at -20 to 10°C. , add the second portion of ethanol 943.12kg (content 99.5%, pure 938.4kg, 20.40kmol), adjust the pH of the reaction solution=3-4.0, keep the temperature at 50-60°C, and the total reaction time is 24 hours. After the alcoholysis, the ammonium bromide was removed by filtration, and after the solvent was evaporated, 1072.90 kg of triethyl orthoformate was obtained by rectification, with a content of 99.8%, 1070.75 kg of pure, and a yield of 85%. ...

Embodiment 2

[0021] Embodiment 2: the molar ratio of reaction material is hydrocyanic acid: ethanol: hydrogen chloride=1: 4.0: 1.20.

[0022] Add 231.82kg of hydrocyanic acid (content 99%, pure 229.50kg, 8.5kmol), the first ethanol 510.85kg (content 99.5%, pure 508.3kg, 11.05kmol), inert solvent 2000kg, into the built-in metal coil In the halogenation reaction kettle of the heat exchanger, the temperature was lowered to -15°C, and 372.3kg of hydrogen chloride was evenly introduced, and the reaction temperature was maintained at -18 to 10°C. After completion, the temperature was maintained at 10-50°C to form a salt. The second part of ethanol is 1061.0kg (content 99.5%, pure 1055.7kg, 22.95kmol), adjust the pH of the reaction solution to 2-2.5, keep the temperature at 50-60°C, and the total reaction time is 15 hours. After the alcoholysis, the ammonium chloride was removed by filtration, and after the solvent was evaporated, 1049.75 kg of triethyl orthoformate was obtained by rectification,...

Embodiment 3

[0023] Embodiment 3: the molar ratio of reaction material is hydrocyanic acid: methanol: hydrogen bromide=1: 3.5: 1.10.

[0024] Add 230.19kg of hydrocyanic acid (99.7% content, 229.50kg pure, 8.5kmol), the first methanol 300.70kg (99.5%, 299.2kg pure, 9.35kmol), and 2000kg inert solvent into the built-in plastic tube bundle In the halogenation reaction kettle of the tube heat exchanger, cool down to -18°C, evenly feed 756.4kg of hydrogen bromide, maintain the reaction temperature at -18 to 10°C, and keep the temperature at 10-40°C to form a salt, and the imide salt is precipitated Finally, add the second portion of methanol 656.08kg (content 99.5%, pure 652.8kg, 20.40kmol), adjust the pH of the reaction solution=1-2.0, keep the temperature at 50-60°C, and the total reaction time is 10 hours. After the alcoholysis, the ammonium bromide was removed by filtration, and after the solvent was evaporated, 768.34kg of trimethyl orthoformate was obtained by rectification, with a conte...

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Abstract

The present invention relates to a process for preparing orthoformate by taking advantage of hydrocyanic acid, as by-product in production of acrylic nitrile, and apparatus therefore. The hydrocyanic acid, as by-product in production of acrylic nitrile, is adopted as a starting raw material and, together with alkyl alcohol and halogen hydride, is dissolved in an indifferent solvent; then after halogenation, salt forming and alcoholysis reactions, crystal separation and distillation rectification, the orthoformate is obtained. By adopting a reactor equipped with stirring, built-in plastics bundled tubes or metal dish tube heat interchanger to resolve the heat exchange problem existing in the aggregation exothermic halogenation and salt forming reactions, the present invention prevents blasting boiling and exploding accident states from appearing during the course of reaction, facilitates placidity and controllability of the reaction temperature, and achieves the requirement for safe reactions.

Description

technical field [0001] The present invention relates to the field of organic chemistry, in particular, the present invention relates to a method and a device for preparing orthoformate by utilizing hydrocyanic acid, a by-product of acrylonitrile production. Background technique [0002] Orthoformate is a general term for products such as trimethyl orthoformate, triethyl orthoformate, tripropyl orthoformate, and tributyl orthoformate. These products are mainly used as pharmaceutical intermediates, and also as intermediates for pesticides, chemicals, and spices. In recent years, developed countries have begun to apply it to the production of high-grade paints and coatings to eliminate the adverse effects of formaldehyde on the environment. Paint factories and paint factories in China have also begun to apply it. According to the forecast of experts, the use and market demand of orthoformate still have a rapid growth trend. [0003] At present, the domestic production of ort...

Claims

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Application Information

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IPC IPC(8): C07C41/01C07C43/32
Inventor 高庆昌
Owner YINGKOU YINGXIN CHEM TECH CO LTD
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