Continuous desalination technology before steaming for resource utilization of BDO device waste liquid

A resource recovery and waste liquid technology, which is applied in the field of continuous desalination before steaming, can solve the problems of difficult product specification stability, insufficient use of waste liquid, inconvenient promotion and application, etc., and achieves reduced recycling costs, is conducive to environmental protection, The effect of high added value of the product

Inactive Publication Date: 2019-02-15
CHONGQING UNIV
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AI Technical Summary

Problems solved by technology

The main disadvantages of this method are: ①The intermittent operation is labor-intensive, suitable for small production scale, and the product specifications are difficult to stabilize
The main shortcoming of this method is: 1. this method can only handle the special raffinate that water content is 50% and can directly carry out intermittent 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 other waste liquids are discharged, polluting the environment
③ The heavy oil discharged from the bottom of the distillation tower is not recycled, which not only pollutes the environment, but also wastes waste liquid resources

Method used

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  • Continuous desalination technology before steaming for resource utilization of BDO device waste liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] The specific steps of a continuous desalination process before steaming for resource utilization of BDO device waste liquid are as follows:

[0031] (1) Neutralization and replacement

[0032] The waste liquid of the BDO unit, together with the return washing brine and the alcohol phase of the salting device, enters the normal temperature neutralization tank, keeps the water content in the mixed liquid at 30%, and adds 98% concentrated sulfuric acid according to a certain proportion to oxidize the hydrogen in the substrate Most of the sodium and sodium formate are replaced by sodium sulfate and volatile formic acid. The temperature of the neutralization tank is controlled at 10°C, and the pH of the solution is 3.0. At this time, some sodium sulfate crystals will be produced in the solution. After continuous centrifugal filtration, the filtrate enters the low-temperature neutralization tank, and a certain proportion of 98% concentrated sulfuric acid is added to strictly ...

Embodiment 2

[0042] A continuous desalination process before steaming for resource utilization of BDO device waste liquid, same as implementation case 1, wherein:

[0043] In step (1), keep the water content in the mixed solution as 35%, control the temperature of the neutralization tank at 15° C., and the pH of the solution to be 3.2; after adding sulfuric acid, the pH of the solution is 2.3, and the temperature is replaced at -7° C.

[0044] In the (2) step, the temperature of the salt-dissolving kettle is dissolved at 60°C; the temperature of the lower floor water phase crystallizer is -2°C, and the temperature of the second wash filtrate crystallizer is -2°C to complete the sodium sulfate crystallization; the second wash filter salt crystallizer The temperature was controlled at 90°C.

[0045] In the (3) step, in the atmospheric distillation concentrator, control the outlet temperature of 115°C; in the vacuum wiped film evaporator I, the operating pressure is 7kPa, and the liquid phase...

Embodiment 3

[0049] A continuous desalination process before steaming for resource utilization of BDO device waste liquid, same as implementation case 1, wherein:

[0050] In step (1), keep the water content in the mixed solution as 40%, control the temperature of the neutralization tank at 20° C., and the pH of the solution to be 3.5; the pH of the solution after adding sulfuric acid is 2.4, and the temperature is replaced at -5° C.

[0051] In the (2) step, the temperature of the salt-dissolving kettle is dissolved at 65°C; the lower floor water phase crystallizer temperature is 0°C, and the second washing filtrate crystallizer temperature is 0°C to complete the sodium sulfate crystallization; the second washing filter salt crystallizer is at temperature Controlled at 105°C.

[0052] In the (3) step, in the atmospheric distillation concentrator, control the outlet liquid temperature to 120°C; in the vacuum wiped film evaporator I, the operating pressure is 10kPa, and the liquid phase out...

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Abstract

The invention discloses a continuous desalination technology before steaming for resource utilization of BDO device waste liquid, and belongs to the technical field of organic waste liquid recycling in industrial production. According to the technology, the BDO device waste liquid is mixed with return salt-leaching water, and sodium formate in the mixed liquid is completely displaced with sodium sulfate through neutralization and displacement of sulfuric acid; a displacement solution is frozen and filtered, and filter salt is washed and concentrated twice to obtain anhydrous sodium sulfate; filter liquor is subjected to atmospheric concentration and first-stage reduced pressure membrane scraping distillation, light components in the filter liquor is steamed out, and low boiling alcohol, water and a formic acid water solution are separated from the light components through third-stage rectification; a remaining solution after the first-stage reduced pressure membrane scraping distillation is subjected to second-stage reduced pressure membrane scarping distillation, a BDO product with the content of 99.5% or more than 99.5% is obtained after rectification of the distilled coarse BDO,and a distillation substrate is salt-free tar which can be used for oil burning boiler byproduct steam. The technology has the advantages that various products can be recycled, the product recycle rate is high, waste liquid resources are utilized sufficiently, the environmental protection is facilitated, the recycle cost is low, the applicable range of the technology is wide, the technology is convenient for popularization and application and the like.

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 continuous desalination process before steaming for resource utilization of waste liquid from a BDO device. Background technique [0002] 1,4-Butanediol (hereinafter referred to as BDO) is an important organic chemical and fine chemical raw material with a wide range of uses, mainly used in the production of polybutylene terephthalate (PBT) engineering plastics and fibers, tetrahydrofuran , γ-butyrolactone, polyurethane artificial leather, polyurethane elastomer and polyurethane sole glue, etc. In addition, its derivatives vinylpyrrolidone, polyvinylpyrrolidone, etc. are fine chemical products with high added value, widely used in medicine, cosmetics, pesticides, herbicides, solvents, moisturizers, chain extenders and adhesives, etc. . In recent years, the total domestic BDO production capacity has con...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/74C07C29/80C07C29/88C07C29/76C07C31/20C07C51/02C07C51/42C07C51/44C07C53/02C01D5/00C01D5/16
CPCC01D5/00C01D5/16C07C29/74C07C29/76C07C29/80C07C29/88C07C51/02C07C51/42C07C51/44C07C31/207C07C53/02
Inventor 周杰张婷孙诗瑞严诚磊魏顺安
Owner CHONGQING UNIV
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