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Method and device for recovering DMAC (dimethylacetamide) and isoquinoline from solution

A technology of isoquinoline and solution, which is applied in the field of recycling DMAC and isoquinoline, can solve the problems of difficult handling of reaction solids, greenhouse gas emissions, complicated separation process, etc., and achieves the effects of easy industrial application, reduced emissions, and simple method flow

Pending Publication Date: 2022-05-20
RAYITEK HI TECH FILM CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, there are problems such as greenhouse gas emissions, resource waste, raw material consumption, complicated separation process, and difficult handling of reaction solids in the prior art methods. Therefore, it is necessary to explore a new method with simple process, energy saving and environmental protection, so as to achieve The purpose of refining and recovering DMAC and isoquinoline

Method used

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  • Method and device for recovering DMAC (dimethylacetamide) and isoquinoline from solution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] (1) Pump the mixed solution raw materials into the middle part of the first-effect dehydration tower (1), the total feed amount is 3093.93kg / h, including DMAC857.66kg / h, isoquinoline 53.59kg / h, water 1903.75kg / h, heavy components 4.51kg / h, tower top pressure 13kpa(A), operating temperature 51.2°C, gas phase water under reduced pressure is obtained at the top of the tower, and liquid phase water is obtained by condensation with a condenser and refrigerant, and the water is divided into two parts, 33%wt pump reflux To the top of the tower, 67% wt is extracted and recovered outside the system, and the output flow rate is 1906.29kg / h; the concentrated mixed solution of isoquinoline, acetic acid, DMAC, water, and heavy components is obtained from the tower reactor, which is pumped into the second-effect dehydration tower (2);

[0043] (2) The mixed liquid from the tank of the first-effect dehydration tower (1) enters the top of the second-effect dehydration tower (2), the pr...

Embodiment 2

[0050] In the step (4), the isoquinoline refining tower (4) tower top pressure 1.5kpa (A), 104 ℃ of operating temperatures; In the step (5), the acetic acid tower (5) operating temperature 158 ℃; In the step (6), the DMAC tower ( 6) The operating temperature is 82° C., and the other steps are the same as in Example 1.

[0051] The obtained isoquinoline product mass fraction is 99.89%, and the DMAC product mass fraction is 99.93%.

Embodiment 3

[0053] Isoquinoline refining tower (4) tower top pressure 1.9kpa (A) in step (4), 107 ℃ of operating temperatures; 160 ℃ of acetic acid tower (5) operating temperatures in step (5); DMAC tower ( 6) The operating temperature is 87° C., and the other steps are the same as in Example 1.

[0054] The obtained isoquinoline product mass fraction is 99.66%, and the DMAC product mass fraction is 99.81%.

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Abstract

The invention relates to a method and a device for refining and recovering DMAC (dimethylacetamide) and isoquinoline from a solution, and the method comprises the following steps: removing moisture from a raw material solution by a multi-effect rectification technology, and feeding the dehydrated material into an isoquinoline-DMAC acetic acid azeotrope separation tower; the isoquinoline kettle liquid of the separation tower kettle is refined by a refining tower to obtain isoquinoline with the mass fraction of more than or equal to 99.6% at the tower top, and a small amount of heavy kettle liquid obtained in the tower kettle is treated additionally; a DMAC acetic acid azeotrope is obtained at the top of the separation tower, part of the DMAC acetic acid azeotrope is refluxed, the other part of the DMAC acetic acid azeotrope enters an azeotrope separation system, and DMAC-acetic acid separation is achieved through a rectification technology under special operation conditions; high-concentration acetic acid liquid obtained at the top of the acetic acid tower is treated additionally, and DMAC with the mass fraction larger than or equal to 99.8% is obtained at the top of the DMAC The method has the advantages of high DMAC and isoquinoline product yield, high purity, no introduction of other media, no generation of solid wastes, energy saving and environmental protection, and can realize continuous operation.

Description

technical field [0001] The invention belongs to the technical field of chemical product purification, and relates to a method and a device for recovering DMAC and isoquinoline from a solution. Background technique [0002] As a high-performance fiber material, polyimide has good development prospects in various application fields. During the preparation and production of polyimide materials, a mixed tail gas containing N, N dimethylacetamide (DMAC), isoquinoline, and acetic acid will be produced. Since DMAC and acetic acid will form the highest azeotrope, conventional distillation It is difficult to separate the two by means, so the existing technology is difficult to recover the economically beneficial N,N dimethylacetamide component from the tail gas. The mainstream treatment technology for this tail gas in the world is the combustion method. The production cost of this technology is high, and the large amount of greenhouse gases produced has an irreversible negative impa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/24C07C233/05C07D217/02B01D3/14B01D3/32B01D3/42
CPCC07C231/24C07D217/02B01D3/146B01D3/322B01D3/42C07C233/05Y02P20/10
Inventor 林占山覃立森何志斌袁舜齐汤昌丹
Owner RAYITEK HI TECH FILM CO LTD
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