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Process for recovering 1,4-butanediol

A technology of butanediol and process, which is applied in the field of recycling of distillation waste, can solve the problems of underutilization, increase production cost of enterprises, increase production cost, etc., and achieve easy availability, prolong service life, and save costs. Effect

Inactive Publication Date: 2013-06-19
CHONGQING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main disadvantages of this incineration treatment of distillation waste are: ① serious pollution to the environment
②Waste of resources
Since the distillation waste contains a large amount of alcohol ether oligomers, if they are directly burned, these organic substances will not be fully utilized, resulting in a serious waste of resources
③Increase the production cost of the enterprise
For the direct combustion of distillation waste, enterprises need to invest in incinerators and ancillary equipment to deal with these wastes, thus increasing the production cost of enterprises

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] A kind of reclaiming 1, the concrete steps of the technique of 4-butanediol are as follows:

[0024] (1) Depolymerization reaction

[0025] The distillation waste in the process of producing 1,4-butanediol with the Rapper method is a raw material, and the dilute sulfuric acid with a mass concentration of 15% is a catalyst, and the mass ratio of the dilute sulfuric acid catalyst according to the distillation waste raw material: dilute sulfuric acid catalyst is 1: 1.3 The proportion of dilute sulfuric acid catalyst is added to the distillation waste raw material, stirred and mixed evenly to prepare a mixture. Then pump the mixture into an autoclave, heat and pressurize, and depolymerize the mixture for 7 hours at a temperature of 150°C and a pressure of 0.5 MPa. After the reaction, let it cool down naturally and release the pressure to normal temperature and pressure. The depolymerization reaction liquid in the autoclave is collected for further processing.

[0026] (2)...

Embodiment 2

[0031] A kind of technique that reclaims 1,4-butanediol, with implementation case 1, wherein:

[0032] In the 1st (1) step, the mass concentration of catalyzer is 5% dilute sulfuric acid, distillation waste raw material: the mass ratio of dilute sulfuric acid catalyst is 1: 1.0, and the temperature of autoclave is 120 ℃, pressure is 0.2MPa, depolymerization reaction 3h.

[0033] In the (2) step, stand for stratification for 30 minutes, the cooling temperature of the cooler is 5° C., cooling and crystallization for 40 minutes, the pH value of the centrifugal supernatant is adjusted to 6.8, the rotating speed of the centrifuge is 1000 r / min, and centrifugation is performed for 20 minutes.

[0034] In step (3), the pressure of the wiped film evaporator is 10kPa, the temperature is 180°C, and the temperature of the cooler is 60°C.

Embodiment 3

[0036] A kind of technique that reclaims 1,4-butanediol, with implementation case 1, wherein:

[0037] In the 1st (1) step, the mass concentration of catalyzer is 30% dilute sulfuric acid, distillation waste raw material: the mass ratio of dilute sulfuric acid catalyst is 1: 1.5, and the temperature of autoclave is 180 ℃, pressure is 1.0MPa, depolymerization reaction 13h.

[0038] In the (2) step, stand for stratification for 120 minutes, the cooling temperature of the cooler is 10° C., cooling and crystallization for 80 minutes, the pH value of the centrifuged liquid is adjusted to 7.3, the rotating speed of the centrifuge is 3000 r / min, and centrifuged for 10 minutes.

[0039] In step (3), the pressure of the wiped film evaporator is 50kPa, the temperature is 220°C, and the temperature of the cooler is 80°C.

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Abstract

The invention discloses a process for recovering 1,4-butanediol, and belongs to the technical field of the recycling of organic waste in the industrial production. A 1,4-butanediol product in distillation waste is circularly recovered by taking the distillation waste generated in the process of producing the 1,4-butanediol by a Reppe process as a raw material and dilute sulfuric acid as a catalyst through the simple process of depolymerization reaction, separation, distillation and condensation. The process has the characteristics that: the process is simple, and easy to operate; equipment issimple and has high performance-price ratio; secondary pollution is avoided, the process is favorable for environmental protection, and energy sources are saved; and resources can be circularly utilized, production cost can be reduced, the process is convenient for promotion and application and the like. The process can be widely applied to the recycling of the organic waste in the industrial production, and is particularly suitable for recycling the distillation waste generated in the process of producing the 1,4-butanediol by the Reppe process.

Description

technical field [0001] The invention belongs to the technical field of organic waste recovery and utilization in industrial production, and in particular relates to the recovery of 1,4-butanediol from the distillation waste produced in the process of producing 1,4-butanediol by using dilute sulfuric acid as a catalyst craft. Background technique [0002] 1,4-Butanediol is an important fine chemical raw material, which can be used to produce important chemical products such as tetrahydrofuran, γ-butyrolactone, polybutylene terephthalate and polyurethane, and can also be used as a solvent, enhancer, etc. Wet agent, plasticizer and chain extender and crosslinking agent in polyurethane synthesis, etc. In recent years, due to the wide application of 1,4-butanediol and its derivatives, the demand for 1,4-butanediol and its derivatives has continued to grow, and the market prospect is quite broad. [0003] At present, large-scale 1,4-butanediol production enterprises at home and ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C31/20C07C29/10C07C29/80
Inventor 魏顺安谭世语董立春张红晶吕利平杨楠尤新强王攀
Owner CHONGQING UNIV
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