CN101928212A - Method for intermittently recycling and separating light component waste in production of acetic acid - Google Patents
Method for intermittently recycling and separating light component waste in production of acetic acid Download PDFInfo
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- CN101928212A CN101928212A CN 201010264220 CN201010264220A CN101928212A CN 101928212 A CN101928212 A CN 101928212A CN 201010264220 CN201010264220 CN 201010264220 CN 201010264220 A CN201010264220 A CN 201010264220A CN 101928212 A CN101928212 A CN 101928212A
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Abstract
The invention relates to a method for intermittently recycling and separating light component waste in the production of acetic acid, and belongs to the technical field of chemical separation. Aldehyde, acraldehyde, methyl acetate, acetic acid methyl ester, water and acetic acid products are obtained by distillation through a rectifying system consisting of an intermittent rectifying tower. The number of theoretical plates of the rectifying tower is 10 to 40; the operating pressure of a tower top is -0.1 to 0.5Mpa; reflux ratio is 0.5 to 10; the temperature of the tower top is between 35 and 120 DEG C; and the temperature of a tower bottom is between 60 and 140 DEG C. The products such as the aldehyde with purity of 99.7 percent, the acetic acid with purity of 98 percent, mixed ester and the like can be obtained by the method. The method has the advantages of suitability for raw materials with different components, intermittent operation of the rectifying tower, suitability for increased pressure, normal pressure and reduced pressure operation, high separation efficiency and simple and reasonable process.
Description
Technical field: the device and method that the invention belongs to chemical separation process, the recovery process for purification that relates to light component waste in a kind of Processes for Producing Acetic Acid, especially be to isolate acetaldehyde from acetic acid waste light constituent, the batch fractionating of mixed ester and acetic acid reclaims separation method.
Background technology: acetic acid is a kind of important organic chemical industry's product, being mainly used in products such as producing Vinyl Acetate Monomer, aceticanhydride, terephthalic acid (PTA), polyvinyl alcohol, acetates, cellulose acetate and chloracetic acid etc., is the important source material of synthon, tackiness agent, medicine, agricultural chemicals and dyestuff.In addition, acetic acid still is good organic solvent, and therefore, purposes is very extensive in industries such as plastics, rubber, printing.In recent years, because the development of PTA and acetic acid derived product impels the production capacity of acetic acid and demand to increase rapidly.
Low-pressure methanol carbonyl compound established law is the main method of acetic acid production at present, and it has the following advantages: the raw material route variation; Transformation efficiency and selectivity height, product acetic acid quality is good; The catalyst activity height, the reaction conditions gentleness; Catalyst system is stable, the life-span is long, consumption is few, technical process is reasonable, and stable operation is reliable; Cost of material is cheap, the product yield height, and product cost is low, and its technology mainly comprises: operations such as reaction, refining, light constituent recovery, Preparation of Catalyst and regeneration are the first-selections of present Processes for Producing Acetic Acid, have been subjected to the attention of each big acetic acid enterprise.
Produce in the acetic acid technology at the low-pressure methanol carbonylation, behind acetic acid lightness-removing column, dehydration tower, enter the acetic acid treating tower through the reaction product behind the carbonylation reaction.Wherein the light component of lightness-removing column contains acetaldehyde, propenal, ritalin, vinyl acetic monomer, water in dividing, and components such as acetic acid generally are used as offal treatment.Industrial scale according to current 100,000/year acetic acid then can produce about 500 tons/year waste, produces acetate yield with domestic carbonylation in 2009 and has reached about 350～4,000,000 tons/year, therefore can produce about 17500～20000 tons solid gurry.Along with the requirement of current domestic energy-saving and emission-reduction and low-carbon economy, especially the solid refuse for chemical enterprise fully utilizes the attention that has caused country and enterprise.
Therefore, the recovery of light component separates in the Dichlorodiphenyl Acetate production technique, and the products such as acetaldehyde, acetate of therefrom purifying out have very high economic benefit and social benefit.
Summary of the invention: the method for intermittently recycling and separating that the objective of the invention is to propose light component waste in a kind of Processes for Producing Acetic Acid.This method can obtain products such as acetaldehyde, acetate from acetic acid light constituent mixture separation.
The present invention is achieved like this: mainly comprise acetaldehyde, propenal, ritalin, vinyl acetic monomer, water in the described light component waste, components such as acetic acid, it reclaims the distillation system that separates by a batch fractionating tower composition and finishes, be that the light component waste raw material enters batch fractionating Tata still, obtain acetaldehyde, propenal, ritalin, methyl acetate, water and acetic acid product in the cat head distillation successively.
Usually, the number of theoretical plate of batch fractionating tower of the present invention is 10～40; Batch fractionating column overhead working pressure is-0.1～0.5MPa, and reflux ratio is 0.5～10; Tower top temperature is 35～120 ℃, and tower still temperature is 60～140 ℃; During from cat head distillation acetaldehyde product and acetaldehyde interim fraction, tower top temperature is in the time of 35～50 ℃, and the working pressure of rectifying tower is the band press operation, and pressure is 0.05～0.5MPa, is preferably 0.22MPa, and reflux ratio is preferably 3.When going out the acetic acid cut, tower top temperature is 90-120 ℃, and the working pressure of rectifying tower is little negative pressure, is preferably-0.05MPa, and tower still temperature is 70 ℃-120 ℃, and reflux ratio is preferably 2.When going out other cuts, the working pressure normal pressure of rectifying tower, tower top temperature is 50 ℃-100 ℃, and tower still temperature is 70 ℃-120 ℃, and reflux ratio is preferred 2.
Batch fractionating of the present invention reclaims separation method and has following characteristics:
(1) separation process scheme is simple, is separated into high value added products such as acetaldehyde, acetate as the light component raw material of acetic acid of waste liquid, makes the ortho-acetic acid device not have discharging of waste liquid, has favorable economic benefit and social benefit;
(2) flow operations technology is flexible, and when raw material changed in the light component waste liquid, rectifier unit also can meet the demands.
Description of drawings: accompanying drawing 1 embodiment of the invention batch fractionating reclaims the separation process scheme sketch.
In the accompanying drawing, 1-acetaldehyde rectifying tower; 2-acetaldehyde rectifying tower condenser; 3-acetate rectifying tower kettle-type reboiler.
Embodiment: below in conjunction with embodiment and accompanying drawing, further specify the present invention, but the present invention is not limited to embodiment.
Embodiment 1:
Light component waste stock liquid quality group becomes to see the following form.
| Component | Form (wt%) |
| Acetaldehyde | 92 |
| Acetate | 5 |
| Water | 1.2 |
| |
1 |
| Ethyl acetate | 0.8 |
Every batch of add-on of raw material is 10000kg, at first enter the tower still, during from cat head distillation acetaldehyde product and acetaldehyde interim fraction, the working pressure of rectifying tower is 0.22MPa, and tower top temperature is 42 ℃, and tower still temperature is 90 ℃, reflux ratio is 3, the acetaldehyde product that obtains, its content are 99.9% (wt%), and the rate of recovery of acetaldehyde is 85%;
When going out the acetic acid cut, the working pressure of rectifying tower is-0.05MPa, and tower top temperature is 100 ℃, and tower still temperature is 80 ℃ ℃, and reflux ratio is 2.The acetic acid product that obtains, 99.9% (wt%), the yield of acetate are 99.9%.
When going out other cuts, the working pressure normal pressure of rectifying tower, tower top temperature is 60 ℃, and tower still temperature is 70 ℃, and reflux ratio is 2.
Embodiment 2:
Light component waste stock liquid quality group becomes to see the following form.
| Component | Form (wt%) |
| Acetaldehyde | 54 |
| Acetate | 35 |
| Water | 5.2 |
| Methyl acetate | 4 |
| Ethyl acetate | 1.2 |
Every batch of add-on of raw material is 10000kg, at first enter the tower still, during from cat head distillation acetaldehyde product and acetaldehyde interim fraction, the working pressure of rectifying tower is 0.5MPa, and tower top temperature is 50 ℃, and tower still temperature is 70 ℃, reflux ratio is 3, the acetaldehyde product that obtains, its content are 99.9% (wt%), and the rate of recovery of acetaldehyde is 90%; When going out other cuts, the working pressure normal pressure of rectifying tower, tower top temperature is 90 ℃, and tower still temperature is 80 ℃, and reflux ratio is 2.When going out the acetic acid cut, the working pressure of rectifying tower is-0.05MPa, and tower top temperature is 120 ℃, and tower still temperature is 100 ℃, and reflux ratio is 2.The acetic acid product that obtains, 99.9% (wt%), the yield of acetate are 99.9%.
Claims (4)
1. the method for intermittently recycling and separating of light component waste in the acetic acid production, mainly comprise acetaldehyde, propenal, ritalin, vinyl acetic monomer, water in the described light component waste, the acetic acid component, it is characterized in that reclaiming separation finishes by the distillation system of a batch fractionating tower composition, the light component waste raw material enters batch fractionating Tata still, obtain acetaldehyde, propenal, ritalin, methyl acetate, water and acetic acid product in the cat head distillation successively, the number of theoretical plate of batch fractionating tower is 10～40; Batch fractionating column overhead working pressure is-0.1～0.5MPa, and reflux ratio is 0.5～10; Tower top temperature is 35～120 ℃, and tower still temperature is 60～140 ℃; Tower top temperature is in the time of 35～50 ℃, and the working pressure of rectifying tower is the band press operation, and pressure is 0.05～0.5MPa; When going out the acetic acid cut, tower top temperature is 90-120 ℃, and the working pressure of rectifying tower is little negative pressure, and tower still temperature is 70 ℃-120 ℃; When going out other cuts, the working pressure normal pressure of rectifying tower, tower top temperature is 50 ℃-100 ℃, tower still temperature is 70 ℃-120 ℃.
2. the method for claim 1, the cat head working pressure is 0.22MPa when it is characterized in that batch fractionating tower from cat head distillation acetaldehyde product and acetaldehyde interim fraction, reflux ratio is 3.
3. the method for claim 1, the cat head working pressure is-0.05MPa when it is characterized in that batch fractionating tower from cat head distilled vinegar acid fraction, reflux ratio is 2.
4. the method for claim 1 is characterized in that batch fractionating tower when cat head distills out other cuts, and the cat head working pressure is a normal pressure, and reflux ratio is 2.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010102642207A CN101928212B (en) | 2010-08-27 | 2010-08-27 | Method for intermittently recycling and separating light component waste in production of acetic acid |
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| CN2010102642207A CN101928212B (en) | 2010-08-27 | 2010-08-27 | Method for intermittently recycling and separating light component waste in production of acetic acid |
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| CN101928212B CN101928212B (en) | 2012-11-21 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103087094A (en) * | 2013-01-30 | 2013-05-08 | 天津大学 | Method and device for rectifying and purifying triethyl phosphate in batches |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1031402C (en) * | 1992-06-03 | 1996-03-27 | 中国石油化工总公司上海石油化工总厂 | Refinement of acetic acid by ethyl aldehyde oxidation process |
| CN101391946A (en) * | 2008-11-04 | 2009-03-25 | 江苏索普（集团）有限公司 | Control method of acetaldehyde content during acetic acid synthesis from methanol carbonylation |
-
2010
- 2010-08-27 CN CN2010102642207A patent/CN101928212B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1031402C (en) * | 1992-06-03 | 1996-03-27 | 中国石油化工总公司上海石油化工总厂 | Refinement of acetic acid by ethyl aldehyde oxidation process |
| CN101391946A (en) * | 2008-11-04 | 2009-03-25 | 江苏索普（集团）有限公司 | Control method of acetaldehyde content during acetic acid synthesis from methanol carbonylation |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103087094A (en) * | 2013-01-30 | 2013-05-08 | 天津大学 | Method and device for rectifying and purifying triethyl phosphate in batches |
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Effective date of registration: 20160120 Address after: 210047 No. 157, general road, Nanjing chemical industry park, Jiangsu, China Patentee after: NANJING CHANGJIANG JIANGYU PETROCHEMICAL Co.,Ltd. Address before: The development zone of Liuhe District of Nanjing City, Jiangsu province 210048 geguan Road No. 385 No. -8 Patentee before: NANJING YANGCHI INDUSTRY GAS Co.,Ltd. |
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Address after: 210047 157 puqiao Road, Changlu street, Jiangbei new district, Nanjing City, Jiangsu Province Patentee after: Nanjing Changjiang Jiangyu Environmental Protection Technology Co.,Ltd. Address before: No.157, puqiao Road, Nanjing Chemical Industrial Park, Jiangsu 210047 Patentee before: NANJING CHANGJIANG JIANGYU PETROCHEMICAL Co.,Ltd. |
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Address after: 210047 157 puqiao Road, Changlu street, Jiangbei new district, Nanjing City, Jiangsu Province Patentee after: Nanjing Changjiang Jiangyu Environmental Protection Technology Co.,Ltd. Address before: 210047 157 puqiao Road, Changlu street, Jiangbei new district, Nanjing City, Jiangsu Province Patentee before: Nanjing Changjiang Jiangyu Environmental Protection Technology Co.,Ltd. |