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Process for separating acetic acid from DMAC azeotrope

A technology of azeotrope and acetic acid, which is applied in the field of solvent purification and recovery process, can solve the problems of increased refining difficulty, high processing cost, and high difficulty, and achieve the effect of simple control, low requirements, large equipment processing capacity, and reduced recovery cost

Active Publication Date: 2010-09-22
绍兴海纳膜技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The treatment of these wastes has always been a difficult point, because the existing distillation and refining equipment cannot be used for separation, and usually these wastes can only be discharged and discarded as fuel
There are also some manufacturers who add a large amount of water to the waste to dilute it to 60-80% of the water content, add sodium hydroxide to neutralize the pH, and then enter the vacuum evaporator with stirring to evaporate and recover the water-containing DMAC. At the same time, it will produce DMAC containing more The gray-black anhydrous sodium acetate powder of impurities; however, these sodium acetates cannot be recycled and must be paid for by a professional environmental protection company; and during neutralization, it is difficult to control the acid content of 0.2-1.0% at the end point, and the partial acid removal effect is not good. Good (acid removal is not complete, only 95-70%), alkaline DMAC decomposes more, increasing the difficulty of refining; in addition, the equipment processing capacity is low; steam consumption is large, and the processing cost is high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Embodiment 1: 38 milliliters of weak base resin A enters the ion-exchange column of diameter 10 millimeters

[0027] 1) Adsorption treatment

[0028] Contain 60 milliliters of DMAC diluents of DMAC60%, acetic acid 6% and go into the column, enter and wash with 70 milliliters of water again after entering the flat resin liquid level, every 10 milliliters of column solutions are used as a sample measurement, and the concentration that records is shown in the following table:

[0029] Acetic acid %

[0030] In the table: in 1-2 samples, it is basically the water before the DMAC dilution material enters the column, so there is basically no acetic acid and DMAC components; in 3-4 samples, acetic acid is low and DMAC is high, which can be refined and recovered; in 5-9 samples Acetic acid and DMAC are relatively high, and the acetic acid needs to be adsorbed by the resin column again, and can only be refined and recovered after passing through; 10-13 samples show tha...

Embodiment 2

[0035] Embodiment 2: 38 milliliters weak base resin B enters the ion-exchange column of diameter 10 millimeters

[0036] 1) Adsorption treatment

[0037] Contain DMAC60%, 60 milliliters of DMAC dilute material of acetic acid 6% enter column, enter 70 milliliters of water washes after leveling resin liquid level, go out column solution every 10 milliliters and measure as a sample, concentration sees the following table:

[0038] Acetic acid %

[0039] In the table: 1-2 samples are basically the water before the DMAC dilution material enters the column, so there is basically no acetic acid and DMAC components; 3-4 samples have low acetic acid and high DMAC, which can be refined and recovered; 5-9 samples The acetic acid and DMAC in the sample are relatively high, and the acetic acid needs to be adsorbed by the resin column again, and it can be refined and recovered after passing through; 10-13 samples contain DMAC and acetic acid remaining in the adsorption resin, whic...

Embodiment 3

[0044] Embodiment 3: 37 milliliters weak base resin C enters the ion-exchange column of diameter 10 millimeters

[0045] Adsorption treatment

[0046] Contain DMAC60%, 50 milliliters of DMAC dilution material of acetic acid 4.2% enters column, enters 90 milliliters of water washes after leveling the resin liquid level, every 10 milliliters of column solutions are measured as a sample; Concentration sees the following table:

[0047] Acetic acid %

0

0

0.29

1.4

2.5

3.4

3.5

2.5

1.9

1.3

1.0

0.8

0.8

0.6

DMAC%

0

0

27

52

59

59

54

35

14

0

0

0

0

0

[0048]In the table: 1-2 samples are basically the water before the DMAC dilution material enters the column, so there is basically no acetic acid and DMAC components; 3 samples have low acetic acid and DMAC is high, which can be refined and recovered; 4-7 samples Acetic acid and DM...

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PUM

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Abstract

The invention relates to a purification and recovery process of a dimethylacetamide (DMAC), and aims to provide a process which is characterized by simple process, lower treatment cost and effectively usable recovered substances. The technical scheme is as follows: the process for separating acetic acid from DMAC azeotrope comprises the following steps that: (1) weak alkaline resin is adopted to absorb the acetic acid; absorbent resin DMAC eluting water is added into the DMAC azeotrope material to be diluted to the material which contains 5 to 90 percent of water, and then injected into a columnar container filled with weak alkaline resin to absorb the acetic acid therein; (2) the content of the acetic acid of the water containing DMAC, and if the acid is removed by more than 95 percent relative to the DMAC azeotrope material, the material is conveyed to a distillation tower to be refined and recovered and the other material is absorbed again to remove the acetic acid until 95 percentof acid is removed, and the material is conveyed to the distillation tower to be refined and recovered; and (3) according to different groups contained in the weak alkaline resin, different regeneration methods are adopted; and the resin after regeneration is used for absorbing acetic acid again in step (1).

Description

technical field [0001] The invention relates to a process for purifying and recovering solvents, in particular to a process for purifying and recovering dimethylacetamide (DMAC). Background technique [0002] DMAC (dimethylacetamide) is recycled as a solvent in the production of spandex (the production process uses a distillation tower to recover), and its decomposition product, acetic acid, will slowly accumulate until it becomes the highest azeotrope (about 15% of acetic acid, dimethylacetamide DMAC waste in the state of amide about 85%). The treatment of these wastes has always been a difficult point, because the existing distillation and refining equipment cannot be used for separation, and usually these wastes can only be discharged and discarded as fuel. There are also some manufacturers who add a large amount of water to the waste to dilute it to 60-80% of the water content, add sodium hydroxide to neutralize the pH, and then enter the vacuum evaporator with stirring...

Claims

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Application Information

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IPC IPC(8): C07C233/05C07C231/24B01D15/08
Inventor 刘伟斌
Owner 绍兴海纳膜技术有限公司
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