CN102875353B - Method for extracting acetic acid from carbon-soot-containing acetic acid water solution through dust removal/side-stream discharge/azeotropic rectification - Google Patents
Method for extracting acetic acid from carbon-soot-containing acetic acid water solution through dust removal/side-stream discharge/azeotropic rectification Download PDFInfo
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- CN102875353B CN102875353B CN201210392100.4A CN201210392100A CN102875353B CN 102875353 B CN102875353 B CN 102875353B CN 201210392100 A CN201210392100 A CN 201210392100A CN 102875353 B CN102875353 B CN 102875353B
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Abstract
The invention relates to a method for extracting acetic acid from a carbon-soot-containing acetic acid water solution through dust removal/side-stream discharge/azeotropic rectification, which comprises the following steps: pumping the carbon-soot-containing acetic acid water solution into a kettle of an azeotropic rectification tower, wherein the azeotropic rectification tower is provided with a side-stream discharge port, and the bottom of the kettle is connected with a dust settling chamber; when the liquid level reaches 1/3 of the volume of the kettle, turning on cooling water, heating until the temperatures at the tower top and the tower bottom of the azeotropic rectification tower are stable, and controlling the reflux ratio to be (4-5):1; continuing to add the carbon-soot-containing acetic acid water solution, and adding entrainer from the tower top; and after the temperatures at the tower top and the tower bottom of the azeotropic rectification tower are further stable, continuously feeding from the lower part of the azeotropic rectification tower, and continuously discharging from the tower top and the side stream. According to the method, the process is improved from two-step rectification and condensation to one-step azeotropic rectification and condensation, the content of the extracted acetic acid is up to 95.6% or above, the yield is 98.5%, the energy consumption is reduced, the cost is lowered, and the equipment investment and occupied space are reduced simultaneously.
Description
Technical field
The present invention relates to a kind of separating technology of acetic acid production, particularly a kind of de-dirt lateral line discharging azeotropic distillation extracts the separation method containing acetic acid in charcoal ash aqueous acetic acid.
Background technology
Acetic acid is one of important organic acid, is mainly used in synthesizing vinyl acetate, cellulose acetate, acetic anhydride, acetic ester, metal acetate salt and halogenated acetic acid etc., is also the important source material of pharmacy, dyestuff, agricultural chemicals and other organic syntheses.In addition at aspects such as photograph, medicine manufacture, cellulose acetate, fabric printing and rubber industries, also have been widely used.
Twice rectification method of domestic main employing is from extracting acetic acid containing the aqueous acetic acid of charcoal ash at present, first adopt azeotropic distillation to slough containing the water in charcoal ash aqueous acetic acid, then adopt rectificating method to take off charcoal ash, so just can obtain 95% above acetic acid, but because twice rectifying and condensation need to consume a large amount of energy, cause production cost too high.
Summary of the invention
The object of the invention is to overcome the defect of prior art, provide a kind of de-dirt lateral line discharging azeotropic distillation to extract the method containing acetic acid in the aqueous acetic acid of charcoal ash, on same rectifying tower, by an azeotropic distillation separation, obtain acetic acid, remove charcoal ash simultaneously, to save energy and reduce the cost, simplify production technique and the device of acetic acid.
The present invention adopts following technical scheme: a kind of de-dirt lateral line discharging azeotropic distillation extracts the method containing acetic acid in the aqueous acetic acid of charcoal ash, employing azeotropic distillation is separated, it is characterized in that, side line discharge is set on azeotropy rectification column, tower reactor bottom connects dust-settling compartment, described method comprises the steps, raw material is squeezed in azeotropy rectification column tower reactor containing the aqueous acetic acid of charcoal ash, when liquid level reach azeotropy rectification column tower reactor volume 1/3 time, open the water coolant of overhead condenser and side line condenser, start heating, when azeotropic distillation column overhead, when column bottom temperature is stablized, controlling azeotropy rectification column trim the top of column ratio is 4～5:1, continue to add the aqueous acetic acid containing charcoal ash, and add entrainer from azeotropic distillation column overhead, entrainer is the mixed solution of hexanaphthene and N-BUTYL ACETATE, until azeotropic distillation column overhead and column bottom temperature continue stable after, azeotropy rectification column underfeed mouth adds the aqueous acetic acid containing charcoal ash continuously, azeotropic distillation column overhead, side line starts continuous extraction, lateral line discharging is that mass content reaches more than 95.6% acetic acid.
In described method, control tower top drop temperature is that 80.5～81.5 ℃, lateral line discharging temperature are that 116.8～117.9 ℃ and tower reactor temperature are 121.5～123.6 ℃.
Contain the aqueous acetic acid of charcoal ash after separation, tower top discharging is water, and containing acetic acid 0.2-0.4% left and right, dust-laden raffinate enters dust-settling compartment, regular discharge after accumulation, and lateral line discharging acetic acid content reaches more than 95.6%, yield reaches 98.5%.
Described raw material consists of containing common its of aqueous acetic acid of charcoal ash, and comprising weight percent is 40～55% acetic acid and 1～4% charcoal ash, and all the other are water and trace impurity.
The mixed solution that the preferred hexanaphthene of described entrainer and N-BUTYL ACETATE mass ratio are 1:1.
Beneficial effect of the present invention is:
The present invention proposes to adopt de-dirt lateral line discharging azeotropic distillation to extract the method containing acetic acid in the aqueous acetic acid of charcoal ash de-dirt, on same de-dirt lateral line discharging azeotropy rectification column, realize acetic acid extraction and remove charcoal ash, so not only twice rectifying and condensation are improved to an azeotropic distillation and a condensation, reduced energy expenditure, processed 1 ton of raw material and can save 31% energy consumption; Simplified the technology and equipment of acetic acid production simultaneously, reduced investment and the occupied ground of equipment, reduced processing cost, energy-saving effect is remarkable.
Below in conjunction with specific embodiment, describe the present invention, specific embodiment is not construed as limiting the invention.Protection scope of the present invention is defined by the claims.
Accompanying drawing explanation
Fig. 1 is the process flow diagram that the present invention extracts the de-dirt lateral line discharging azeotropic distillation adopting containing acetic acid in the aqueous acetic acid of charcoal ash.
Fig. 2 is the process flow diagram that acetic acid is extracted in twice rectifying of available technology adopting.
Embodiment
Embodiment 1
De-dirt lateral line discharging azeotropic distillation of the present invention extracts containing the technical process of acetic acid in the aqueous acetic acid of charcoal ash as shown in Figure 1, the stage number N=62 piece of azeotropy rectification column 3, at stage number N=50 place, side line discharge 4 is set, tower reactor bottom connects dust-settling compartment 1, and miscellaneous equipment is mainly reboiler 6, surge tank 11 and side line condenser 8 and overhead condenser 14.
Described de-dirt lateral line discharging azeotropic distillation extracts the method containing acetic acid in the aqueous acetic acid of charcoal ash, comprise the steps, aqueous acetic acid containing charcoal ash is squeezed in azeotropy rectification column 3 tower reactors, and the aqueous acetic acid that contains charcoal ash is the solution containing (wt%) 51.05% acetic acid, 47.71% water and 1.24% charcoal ash, when liquid level reach azeotropy rectification column 3 tower reactor volumes 1/3 time, open the water coolant of side line condenser 8 and overhead condenser 14, start heating, when azeotropy rectification column 3 tower tops, when column bottom temperature is stablized, control azeotropy rectification column 3 trim the top of column than being 5:1, continue to add the aqueous acetic acid containing charcoal ash, and add entrainer from azeotropy rectification column 3 tower top surge tanks 11, be that hexanaphthene and N-BUTYL ACETATE ratio are 1:1(quality meter) mixed solution, until azeotropy rectification column 3 tower tops and column bottom temperature continue stable after, stock liquid is from opening for feed 2 continuously feedings of azeotropy rectification column 3 bottoms, from azeotropy rectification column 3 tower tops and side line discharge 4, start continuous extraction, controlling azeotropy rectification column 3 tower top temperatures is 80.5～81.5 ℃, lateral line discharging temperature is 121.5～123.6 ℃ of 116.8～117.9 ℃ and tower reactor temperature.After separation, tower top discharging is water, and containing acetic acid 0.2-0.4% left and right, lateral line discharging acetic acid content reaches more than 95.6%, yield reaches 98.5%, regularly discharges dust-laden solution at the bottom of tower.
De-dirt lateral line discharging azeotropic distillation de-dirt result are as shown in table 1.
The de-dirt result of the de-dirt lateral line discharging azeotropic distillation of table 1
Adopting aforesaid method to process 1 ton of raw material consumption heat is 1376000KJ/h.Adopt de-dirt lateral line discharging azeotropic distillation to compare with twice rectification process, not only saved 31% energy consumption, simplified production technique simultaneously.
Control Example 1
Existing separation mainly adopts rectification method twice containing the aqueous acetic acid of charcoal ash, first adopt azeotropic distillation to slough containing the water in charcoal ash aqueous acetic acid, then adopt rectificating method to take off charcoal ash, obtain 95% above acetic acid, its production process as shown in Figure 2, mainly comprises azeotropy rectification column T-1 21 in the device adopting, the first condenser 22, layering return tank 23, the second condensers 24, rectifying tower T-2 25 and vaporizer 26.Adopt aforesaid method to extract containing acetic acid in charcoal ash aqueous acetic acid, acetic acid content reaches more than 95%, and one time yield reaches 98.1%, but because twice rectifying and condensation need to consume a large amount of energy, causes production cost too high.
According to the technological process shown in Fig. 2, under the condition of table 2, process 1 ton containing the solution of 51.05% acetic acid, 47.71% water and 1.24% charcoal ash, obtain the result shown in table 3.As seen from Table 3, when feed throughput is 1000K/h, consumption of calorie is 2016000KJ/h.
The processing condition of twice rectifying of table 2
Twice rectifying of table 3 and twice condenser heat consumption table
Claims (1)
1. a de-dirt lateral line discharging azeotropic distillation extracts the method containing acetic acid in the aqueous acetic acid of charcoal ash, employing azeotropic distillation is separated, it is characterized in that: side line discharge is set on azeotropy rectification column, tower reactor bottom connects dust-settling compartment, described method comprises the steps, aqueous acetic acid containing charcoal ash is squeezed in azeotropy rectification column tower reactor, when liquid level reach azeotropy rectification column tower reactor volume 1/3 time, open the water coolant of overhead condenser and side line condenser, start heating, when azeotropic distillation column overhead, when column bottom temperature is stablized, controlling azeotropy rectification column trim the top of column ratio is 4～5:1, continue to add the aqueous acetic acid containing charcoal ash, and add entrainer from azeotropic distillation column overhead, entrainer is the mixed solution of hexanaphthene and N-BUTYL ACETATE, the mass ratio of described hexanaphthene and N-BUTYL ACETATE is 1:1, until azeotropic distillation column overhead and column bottom temperature continue stable after, containing the aqueous acetic acid of charcoal ash from the charging of azeotropy rectification column underfeed mouth, the continuous extraction of tower top and side line, lateral line discharging is that mass content reaches more than 95.6% acetic acid,
In described method, the aqueous acetic acid that contains charcoal ash is 40～55% acetic acid and 1～4% charcoal ash containing mass percent, and all the other are water and trace impurity; Azeotropic distillation column overhead drop temperature is that 80.5～81.5 ℃, lateral line discharging temperature are that 116.8～117.9 ℃ and tower reactor temperature are 121.5～123.6 ℃.
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| CN201210392100.4A CN102875353B (en) | 2012-10-16 | 2012-10-16 | Method for extracting acetic acid from carbon-soot-containing acetic acid water solution through dust removal/side-stream discharge/azeotropic rectification |
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| CN201210392100.4A CN102875353B (en) | 2012-10-16 | 2012-10-16 | Method for extracting acetic acid from carbon-soot-containing acetic acid water solution through dust removal/side-stream discharge/azeotropic rectification |
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| CN102875353B true CN102875353B (en) | 2014-11-26 |
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| CN104844444B (en) * | 2015-03-26 | 2017-03-01 | 南京师范大学 | Unilateral line is thermally integrated the method that azeotropic distillation extracts acetic acid in saliferous aqueous acetic acid |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101172941A (en) * | 2006-11-02 | 2008-05-07 | 中国石油化工股份有限公司 | Method for recycling acetic acid in dilute acetic acid |
| CN101306981A (en) * | 2007-05-16 | 2008-11-19 | 中国石油化工股份有限公司 | Azeotropy process for catalyzing, rectifying and hydrolyzing methyl acetate |
| CN101445444A (en) * | 2008-12-17 | 2009-06-03 | 中国石化仪征化纤股份有限公司 | Method for recovering dilute acetic acid by extraction and azeotropic distillation |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101172941A (en) * | 2006-11-02 | 2008-05-07 | 中国石油化工股份有限公司 | Method for recycling acetic acid in dilute acetic acid |
| CN101306981A (en) * | 2007-05-16 | 2008-11-19 | 中国石油化工股份有限公司 | Azeotropy process for catalyzing, rectifying and hydrolyzing methyl acetate |
| CN101445444A (en) * | 2008-12-17 | 2009-06-03 | 中国石化仪征化纤股份有限公司 | Method for recovering dilute acetic acid by extraction and azeotropic distillation |
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Application publication date: 20130116 Assignee: Binhai torch dyestuff Co., Ltd. Assignor: Jiangsu Yanjiang Chemical Resources Development Institute Co., Ltd. Contract record no.: 2015320000008 Denomination of invention: Method for extracting acetic acid from carbon-soot-containing acetic acid water solution through dust removal/side-stream discharge/azeotropic rectification Granted publication date: 20141126 License type: Exclusive License Record date: 20150115 |
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