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Process for recovering distillation waste liquid generated by producing 1,4-butanediol

A technology of butanediol and waste liquid, applied in the preparation of organic compounds, organic chemistry, chemical instruments and methods, etc., can solve the problems of inability to deal with salt content, underutilization of residual liquid, waste of waste liquid resources, etc. Broad market and application prospects, good for environmental protection, and high product recovery

Inactive Publication Date: 2013-09-04
CHONGQING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main shortcoming of this method is: 1. this method can only handle 1, and the distillate raffinate that 4-butanediol content is high (more than 70%) and does not contain salt can directly carry out rectification recovery, can not handle comparatively common dark viscous Distillation raffinate with thick and high salt content has limited application range, poor applicability, and is not convenient for popularization and application
② Only one product, 1,4-butanediol in the distillation raffinate can be recovered, and the waste liquid resources for producing 1,4-butanediol are not fully utilized, and waste liquid is discharged, polluting the environment
③This method does not recycle the heavy oil discharged from the bottom of the rectification tower, which not only does not make full use of the raffinate, but also pollutes the environment
The main shortcoming of this method is: 1. this method can only handle the special waste liquid that water content is 50% and can directly carry out batch rectification, can't produce 1,4-butanediol relatively common viscous and Distillation waste liquid with high salt content is processed, which has poor applicability and is not convenient for popularization and application
② Only one product, 1,4-butanediol in the waste liquid can be recovered, and the waste liquid is not fully utilized, and the waste liquid is discharged, polluting the environment
③ The heavy oil discharged from the bottom of the rectification tower is not recycled, which not only pollutes the environment, but also wastes waste liquid resources

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] A kind of production 1, the concrete steps of the recovery process of the distillation waste liquid of 4-butanediol are as follows:

[0024] (1) Salting-out-extraction

[0025] The distillation waste liquid produced in the refining process of 1,4-butanediol produced by the Rapper method is used as raw material, the waste water discharged during the production of 1,4-butanediol is used as the extraction agent, and sodium sulfate is used as the salting-out agent. The salting-out-extraction is carried out in an acidic (sulfuric acid) environment. That is, according to raw material: extractant: salting-out agent: the mass ratio of sulfuric acid with a mass concentration of 98% is 1: 0.8: 0.08: 0.04, the extractant is first added to the raw material, stirred and mixed evenly, and mixed into a mixed solution. Add sulfuric acid dropwise to the mixed solution, stir evenly, then add the salting-out agent to the mixed solution after adding the sulfuric acid dropwise, heat and st...

Embodiment 2

[0031] A recovery process for distillation waste liquid producing 1,4-butanediol, same as implementation case 1, wherein:

[0032] In the (1) step, the mass ratio of raw material: extractant: salting-out agent: mass concentration of 98% sulfuric acid is 1: 1: 0.7: 0.15, the temperature of the mixed solution is 40° C., and the stratification is allowed to stand for 30 minutes.

[0033] In step (2), the lower water phase was cooled and crystallized at 0° C. for 3 h, and the upper oil phase was cooled and crystallized at 5° C. for 5 h. First collect butanol by-products under the condition of 0.08MPa vacuum in the kettle; then collect 1,4-butanediol product under the condition of 0.096MPa vacuum in the kettle; then collect 3 under the condition of 0.096MPa vacuum in the kettle -tetrahydrofuran methanol by-product; finally, the fusel alcohol is collected under the condition of 0.096MPa vacuum in the kettle.

[0034] In step (3), the mass ratio of substrate at the bottom of the ket...

Embodiment 3

[0036] A recovery process for distillation waste liquid producing 1,4-butanediol, same as implementation case 1, wherein:

[0037] In step (1), the mass ratio of raw materials: extractant: salting-out agent: sulfuric acid with a mass concentration of 98% is 1:2:1.5:0.1, the temperature of the mixed solution is 50° C., and the mixture is allowed to stand for 20 minutes.

[0038] In step (2), the lower water phase was cooled and crystallized at -5°C for 2 hours, and the upper oil phase was cooled and crystallized at 0°C for 4 hours. First collect butanol by-products under the condition of 0.07MPa vacuum in the kettle; then collect 1,4-butanediol product under the condition of 0.095MPa vacuum in the kettle; then collect 3 under the condition of 0.095MPa vacuum in the kettle -tetrahydrofuran methanol by-product; finally, the fusel alcohol is collected under the condition of 0.095MPa vacuum in the kettle.

[0039] In step (3), the mass ratio of substrate at the bottom of the kettl...

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PUM

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Abstract

The invention relates to a process for recovering distillation waste liquid generated by producing 1,4-butanediol and belongs to the technical field of recycling of organic waste liquid in the industrial production. According to the invention, the distillation waste liquid generated in the process of producing 1,4-butanediol by a Reppe method is used as a raw material; drained wastewater is used as an extracting agent; sodium sulfate is used as a salting-out agent; sulfuric acid is used as a catalyst for depolymerizing reaction; and by a circulating process of salting-out-extraction, reduced pressure batch distillation separation and depolymerizing reaction, various products in the distillation waste liquid, such as 1,4-butanediol, butanol and 3-tetrahydrofurfuryl alcohol are recovered. The process disclosed by the invention has the characteristics that various products can be recovered, the recovery rate of the products is high and the recovery economic benefits are good; the process sufficiently utilizes waste liquid resources and is beneficial to environment protection; the process is simple, reaction conditions are mild, equipment is conventional and recovery cost is low; and the process has a wide application range and is convenient to popularize and apply. The process can be widely applied to recycling of the organic waste liquid in the industrial production and is particularly suitable for recycling the waste liquid generated in the process of producing 1,4-butanediol by the Reppe method.

Description

technical field [0001] The invention belongs to the technical field of organic waste liquid recovery and utilization in industrial production, and in particular relates to a recovery process of distillation waste liquid for producing 1,4-butanediol. Background technique [0002] 1,4-Butanediol is an important organic chemical and fine chemical raw material with a wide range of uses, mainly used in the production of tetrahydrofuran, γ-butyrolactone, polyurethane, copolyester ether, polyester engineering plastics, elastic fibers, etc. . In addition, its derivatives are fine chemical products with high added value and are widely used in the synthesis of vitamin B 6 , pesticides, herbicides, solvents, wetting agents, chain extenders and adhesives. At present, most of the 1,4-butanediol production enterprises that have been built or are under construction in China use the Rapper process to produce 1,4-butanediol. 1,4-butanediol distillation waste liquid is produced. According...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/20C07C29/94
Inventor 朱文龙李牧青汪楠邵方元朱新万华龙魏顺安周小华
Owner CHONGQING UNIV
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