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Recycle method of hydrocyanation catalyst for butadiene-based synthesis of adiponitrile

A cyclic application and hydrocyanation technology, applied in the field of chemical product production, can solve the problems of increasing the amount of secondary hydrocyanation, the need, and affecting the effect of the secondary hydrocyanation reaction, and achieve the effect of eliminating the influence and reducing the process cost.

Inactive Publication Date: 2015-11-04
CHONGQING ZHONGPING ZIGUANG SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because the ligand requirement of zero-valent nickel is lower than primary hydrocyanation when catalyzing secondary hydrocyanation, therefore, the remaining solution after the primary hydrocyanation reaction solution is separated out product and unreacted reactant as described above is used as The catalyst is directly used in secondary hydrocyanation, which is equivalent to increasing the amount of zero-valent nickel ligands used in secondary hydrocyanation, thereby increasing the raw material cost of the process; in addition, the change in the material ratio of zero-valent nickel to ligands will also affect Reaction effect of secondary hydrocyanation
Separating and recovering the catalyst from the reaction liquid of the secondary hydrocyanation by rectification and extraction requires equipment such as extraction agent and separation tower, which also increases the cost of raw materials and equipment of the process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Embodiment 1, secondary hydrocyanation

[0025] In a four-neck flask equipped with mechanical stirring, nitrogen blanketing device, thermometer and condenser tube, add 44.4g of catalyst consisting of zero-valent nickel and tri-m-cresyl phosphite (the moles of zero-valent nickel and three-m-cresyl phosphite ratio of 1:10), 1.02g of zinc chloride and 37.5g of 3-pentenenitrile, start stirring, raise the temperature to 50°C, and feed 15ml of hydrocyanic acid at a certain flow rate under the condition of nitrogen protection, and the feeding time is 2 hours , The reaction ends when hydrocyanic acid is passed through. The gas chromatographic detection results of the obtained reaction solution showed that the reaction conversion rate was 76%, and the selectivity of adiponitrile was 86%.

[0026] Distill the resulting reaction solution under reduced pressure at 180°C and 0.5kPa (distill out the products adiponitrile and methylglutaronitrile, as well as the unreacted reactants 3...

Embodiment 2

[0027] Embodiment 2, secondary hydrocyanation

[0028] In a four-neck flask equipped with mechanical stirring, nitrogen blanketing device, thermometer and condenser tube, add 66.6g of catalyst consisting of zero-valent nickel and tri-p-cresyl phosphite (mole of zero-valent nickel and tri-p-cresyl phosphite The ratio is 1:25), 1.53g aluminum trichloride and 56.3g 3-pentenenitrile, start stirring, raise the temperature to 100°C, and feed 22.5ml of hydrocyanic acid at a certain flow rate under the condition of nitrogen protection, and the feeding time is After 3 hours, hydrocyanic acid was passed through and the reaction was completed. The gas chromatographic detection results of the obtained reaction solution showed that the reaction conversion rate was 80%, and the selectivity of adiponitrile was 85%.

[0029] Distill the resulting reaction solution under reduced pressure at 160°C and 0.2kPa (distill out the products adiponitrile and methylglutaronitrile, as well as the unreac...

Embodiment 3

[0030] Embodiment 3, secondary hydrocyanation

[0031] In a four-neck flask equipped with mechanical stirring, nitrogen blanketing device, thermometer and condenser tube, add 33.3g of a catalyst consisting of zero-valent nickel and tri-o-cresyl phosphite (the moles of zero-valent nickel and tri-o-cresyl phosphite The ratio is 1:50), 0.765g tin dichloride and 28.15g 3-pentenenitrile, start stirring, raise the temperature to 150°C, and feed 11.3ml hydrocyanic acid at a certain flow rate under the condition of nitrogen protection, and the feeding time is After 1 hour, the hydrogen cyanide was introduced and the reaction was completed. The gas chromatographic detection results of the obtained reaction solution showed that the reaction conversion rate was 85%, and the selectivity of adiponitrile was 86%.

[0032] The resulting reaction solution was distilled under reduced pressure at 200°C and 1kPa to remove the products adiponitrile and methylglutaronitrile, as well as the unreac...

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Abstract

The invention discloses a recycle method of a hydrocyanation catalyst for butadiene-based synthesis of adiponitrile. The method comprises that a primary hydrocyanation reaction residual solution separated from products and unreacted reactants is directly used as a catalyst and is recycled in primary hydrocyanation reaction, and / or a part of a secondary hydrocyanation reaction residual solution separated from products and unreacted reactants is replaced by a fresh catalyst and an assistant every time, wherein the replaced amount of the fresh catalyst and the assistant is 5-50wt% the amount of the used fresh catalyst and the assistant, and the treated residual solution is used for secondary hydrocyanation reaction. The recycle method is simple and easy, the primary and secondary hydrocyanation catalysts respectively realize self-circulation, the primary hydrocyanation catalyst can be recycled 10 times or more, the secondary hydrocyanation catalyst can be recycled 30 times or more, and in the process, a reaction transformation rate and product selectivity are basically stable so that a technical cost is reduced and catalyst material ratio change-caused influence on secondary hydrocyanation reaction is eliminated.

Description

technical field [0001] The invention belongs to the technical field of chemical product production, and relates to a method for recycling catalysts in the chemical product production process. Background technique [0002] Adiponitrile is one of the main raw materials for the production of the new material nylon 66. In addition, it is also widely used in electronics, light industry and other organic synthesis fields. The production process of adiponitrile is currently mainly butadiene method and acrylonitrile electrolytic dimerization method. Among them, the synthesis of adiponitrile by the butadiene method is mainly divided into three steps: primary hydrocyanation, isomerization, and secondary hydrocyanation: the primary hydrocyanation is to react butadiene and hydrocyanic acid in the presence of a catalyst to generate 3 -Pentenenitrile (3PN) and 2-methyl-3-butenenitrile (2M3BN); isomerization is the 2-methyl-3-butenenitrile produced by primary hydrocyanation in the presenc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C255/04C07C253/10
CPCY02P20/584
Inventor 杜彩霞李世民颜英杰孙洪飞庞金强李俊锋黄常勇付红旗龙晓钦
Owner CHONGQING ZHONGPING ZIGUANG SCI & TECH
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