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Method for treating kettle residues in industrial preparation of butyryl chloride

A treatment method, the technology of butyryl chloride kettle, which is applied in the field of organic synthesis and chemical "three wastes" treatment, can solve environmental pollution and other problems, achieve the effect of improving economic benefits and eliminating odor pollution sources

Pending Publication Date: 2020-09-29
阜新达得利化工股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method of the invention not only solves the problem of environmental pollution caused by the sour smell of the kettle residue, but also brings higher economic value

Method used

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  • Method for treating kettle residues in industrial preparation of butyryl chloride

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Embodiment 1 (laboratory scale)

[0031] Put 196g of the still residue from the industrial preparation method of butyryl chloride synthesis by the reaction of butyric acid and phosphorus trichloride into a 500ml reaction bottle, slowly add 150g (3.22mol) of absolute ethanol dropwise for about 2 hours, dropwise In the initial stage, the heat is exothermic violently, and white smoke is released. Control the reaction temperature between 25 and 50°C, stop the dropwise addition when the dropwise addition is no longer exothermic, stir for 1 hour, and distill the reaction liquid under reduced pressure. The pressure is -0.06MPa, 41°C Take out the distillate, steam to 90°C and no distillate flows out, and end the distillation. During the distillation process, there is a fruity aroma.

[0032] After testing, a total of 224.0 g of the organic phase was evaporated, which was colorless and transparent, with a fruity aroma, and was identified as ethyl butyrate. GC detection purity: ...

Embodiment 2

[0033] Embodiment 2 (laboratory scale)

[0034]Put 196g of the still residue from the industrial preparation method of butyryl chloride synthesis by the reaction of butyric acid and phosphorus trichloride into a 500ml reaction bottle, and slowly add 110g (3.44mol) of anhydrous methanol dropwise for about 2 hours. In the initial stage, the heat is exothermic violently, and white smoke is released. Control the reaction temperature between 25 and 50°C, stop the dropwise addition when the dropwise addition is no longer exothermic, stir for 1 hour, distill the reaction solution under reduced pressure, the pressure is -0.06MPa, and exit at 38°C. Distillate fractions, steamed to 85 ° C, no fractions flow out, the distillation is over, and there is a fruity aroma during the distillation process.

[0035] After testing, a total of 192.0 g of the organic phase was evaporated, which was colorless and transparent, with a fruity aroma. After identification, the organic phase was methyl but...

Embodiment 3

[0036] Embodiment 3 (industrial scale)

[0037] Put 800kg of still residue from the industrial preparation method of synthesizing butyryl chloride with butyric acid and phosphorus trichloride into a 2000L enamel reaction kettle, and slowly add 593kg (12.9kmol) of absolute ethanol dropwise for about 3 hours. At the beginning of the dropwise addition, there is a violent exotherm, and white smoke is emitted. Control the reaction temperature between 25 and 50°C. Stop the dropwise addition when the dropwise addition is no longer exothermic, stir for 2 hours, and distill the reaction solution under reduced pressure. The pressure is -0.06MPa, 40°C Take out the distillate, steam to 90°C and no distillate flows out, and end the distillation. During the distillation process, there is a fruity aroma.

[0038] After testing, a total of 958.0 kg of organic phase was evaporated, which was colorless and transparent, with a fruity aroma, and was identified as ethyl butyrate. GC detection pur...

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Abstract

The invention discloses a method for treating butyryl chloride kettle residues in synthesis of butyryl chloride prepared from butyric acid and phosphorus trichloride. The method is simple, convenientand feasible in industry, and treats butyryl chloride residues in a distillation kettle, the conversion rate is high, and a byproduct namely spice-grade butyrate is produced at the same time.

Description

technical field [0001] The invention relates to the field of organic synthesis and chemical "three wastes" treatment, in particular to a method for treating the residue in the industrial preparation of butyryl chloride. Background technique [0002] Butyryl chloride is an important intermediate in organic synthesis, mainly used in the preparation of butylbenzene and drugs such as diuretic acid, trachodin, and clevidipine butyrate. It is known that butyryl chloride is also known as butyryl chloride and n-butyryl chloride. It is a colorless and transparent liquid with a pungent smell and a sour odor. It has a boiling point of 102 ° C. It is miscible with ether and decomposes in water or alcohol. , flammable and corrosive. [0003] At present, the common method for preparing butyryl chloride in industry is to react butyric acid with a chlorination reagent. Commonly used chlorination reagents include: thionyl chloride, phosphorus trichloride and phosphorus pentachloride. The s...

Claims

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Application Information

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IPC IPC(8): C07C67/14C07C67/08C07C67/54C07C69/24B01J27/10C11B9/00
CPCC07C67/14C07C67/08C07C67/54B01J27/10C11B9/0015
Inventor 聂强赵庆瑞
Owner 阜新达得利化工股份有限公司
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