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Method for recovering acidic DMF in sucralose production

A technology of sucralose and a recovery method, which is applied to the preparation of sugar derivatives, sugar derivatives, and sugar derivatives, etc., can solve the problems of intractable solid salt residue, DMF loss, DMF decomposition, etc. The effect of cost reduction and fewer side reactions

Inactive Publication Date: 2020-09-01
ANHUI JINGHE IND
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The patent publication number is CN109503410A, which provides a treatment method of using dimethylamine and acidic DMF for neutralization reaction, and then rectifying. The disadvantage of this process is that DMF will be decomposed under strong alkaline conditions, resulting in the loss of DMF. After complex operations such as distillation, crystallization and filtration, a large amount of solid salt residue that is difficult to handle is produced at the same time

Method used

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  • Method for recovering acidic DMF in sucralose production

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Effect test

Embodiment 1

[0020] (1) Add 3000 L of acidic DMF (5wt% acetic acid, 80wt% DMF) into the reactor, add 300 L of ethanol to react, and the reaction temperature is 85°C, so that the pH value of the reaction mixture is 6.0;

[0021] (2) The reaction mixture is input into the rectification tower, and the operating conditions of the rectification tower are: feed amount 0.9m 3 / h, reflux ratio 1:3, kettle temperature 80°C, top temperature 50°C, negative pressure -0.08Mpa; a mixture containing DMF and ethyl acetate was obtained at the bottom of the tower, and a mixture containing ethanol, acetic acid and water was obtained at the top of the tower;

[0022] (3) The bottom mixture is sent to the light removal tower for rectification, and the bottom mixture (ethyl acetate, DMF) is subjected to rectification and separation operation. , the high-purity DMF obtained at the bottom of the rectification tower, and the ethyl acetate obtained by delighting are returned to the sucralose system to reuse the sep...

Embodiment 2

[0025] (1) Add 3,000 L of acidic DMF (12wt% acetic acid, 80wt% DMF) into the reactor, add 500 L of ethanol to react, and the reaction temperature is 85°C, so that the pH of the reaction mixture is 6.3;

[0026] (2) The reaction mixture is input into the rectification tower, and the operating conditions of the rectification tower are: feed amount 1m 3 / h, reflux ratio 1:3, kettle temperature 78°C, top temperature 48°C, negative pressure -0.07Mpa; a mixture containing DMF and ethyl acetate was obtained at the bottom of the tower, and a mixture containing ethanol, acetic acid and water was obtained at the top of the tower;

[0027] (3) The bottom mixture is sent to the light removal tower for rectification, and the bottom mixture (ethyl acetate, DMF) is subjected to rectification and separation operation. , the high-purity DMF obtained at the bottom of the rectification tower, and the ethyl acetate obtained by delighting are returned to the sucralose system to reuse the separated...

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Abstract

The invention relates to a method for recovering acidic DMF in sucralose production. The method is characterized by comprising the following steps: (1) introducing acidic DMF and ethanol into a reactor according to a flow ratio of 1:0.3, and reacting at 83-85 DEG C until the pH value is 6.0-6.4; (2) sending the obtained mixture into a primary separation tower, wherein the feeding amount is 0.8-1 m<3> / h, the reflux ratio is 1:3, the kettle temperature is 78-80 DEG C, the top temperature is 48-50 DEG C, and the negative pressure is -0.07 to -0.08 Mpa; (3) rectifying the mixture at the bottom ofthe primary separation tower at the kettle temperature of 90-95 DEG C and the top temperature of 78-80 DEG C under normal pressure according to the reflux ratio of 1:1 to obtain high-purity DMF at thebottom of the tower, and removing light components to obtain ethyl acetate for reuse; and (4) carrying out atmospheric distillation on the tower top liquid mixture of the primary separation tower atthe temperature of 73-75 DEG C, returning tower top ethanol to the reactor for reuse, and sending tower bottom acid-containing wastewater for treatment. The method has the following advantages: ethanol is adopted to replace dimethylamine for reaction, so the DMF product yield is high, side reactions are few, and rectification waste liquid and residues are few; and compared with dimethylamine, theethanol has the lower raw material cost, the cost can be saved by 1 million yuan every year, and the treatment cost is also reduced.

Description

technical field [0001] The invention belongs to the technical field of chemical industry and relates to a method for recovering acidic DMF in the production of sucralose. Background technique [0002] Sucralose is a fresh sweetener, its sweetness is 600-800 times that of sucrose, and its sweetness is similar to that of sucrose. Sucralose is not absorbed by the human body, has no bioaccumulation, and has high safety. The sucrose industry developed rapidly, the number of production enterprises gradually increased, and the output continued to increase. A large amount of DMF is used as acid in the production process of sucralose. As the production increases, the amount of DMF used also increases. [0003] The patent publication number is CN109503410A, which provides a treatment method of using dimethylamine and acidic DMF for neutralization reaction, and then rectifying. The disadvantage of this process is that DMF will be decomposed under strong alkaline conditions, resulting ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C233/03C07C231/24C07H5/02C07H1/00
CPCC07C231/24C07H1/00C07H5/02C07C233/03
Inventor 孙多龙王玉斌石剑刘学立
Owner ANHUI JINGHE IND
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