CN102659555A - Acetic acid dehydration technology adopting partial condensation process - Google Patents
Acetic acid dehydration technology adopting partial condensation process Download PDFInfo
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- CN102659555A CN102659555A CN2012101128573A CN201210112857A CN102659555A CN 102659555 A CN102659555 A CN 102659555A CN 2012101128573 A CN2012101128573 A CN 2012101128573A CN 201210112857 A CN201210112857 A CN 201210112857A CN 102659555 A CN102659555 A CN 102659555A
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- acetic acid
- ritalin
- partial condensation
- acid dehydration
- butyl acetate
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Abstract
The invention relates to an acetic acid dehydration technology adopting a partial condensation process and belongs to the field of separation engineering of chemical engineering. The acetic acid dehydration technology provided by the invention aims at dehydration of an acetic acid containing a large amount of methyl acetate, and combines the conventional acetic acid dehydration technology and two-stage partial condensation. Through the acetic acid dehydration technology, a part of methyl acetate is extracted in a form of a gas phase in an entrainer recovery tower and thus a circulation amount of methyl acetate in an acetic acid dehydration tower is reduced so that energy-saving and consumption reduction of the acetic acid dehydration tower are realized.
Description
Technical field
The invention provides a kind of acetic acid dehydration and azeotropic distillation tower that contains ritalin adopts dephlegmator process to carry out the method that acetic acid reclaims.The invention belongs to the separation engineering field of chemical engineering, be specially adapted to contain in the dehydration tower charging the more operating mode of ritalin.
Background technology
Acetic acid has been widely used in industry, and it can be used as the solvent of oxidizing reaction, also can be used as the important source material of organic synthesis industry.In the acetic acid use, usually need acetic acid be purified, make with extra care, usually relate to acetic acid and separation of water solution.Because water and acetic acid relative volatility approach 1, adopt conventional distillation to need more stage number and bigger reflux ratio, energy consumption is bigger.And acetic acid content is also higher in the tower top discharge water, and the acetic acid loss is big, and the environmental protection treatment expense is high.Heterogeneous azeotropic rectification has characteristics such as less energy-consumption, required stage number are less, separation efficiency height, generally at present adopts this method to carry out acetic acid dehydration, and entrainer commonly used has n-propyl acetate, n-butyl acetate, isobutyl acetate etc.
When but acetic acid is used as solvent or reactant, can produce a certain amount of ritalin.When reclaiming acetic acid, need ritalin is reclaimed simultaneously.When acetic acid dehydrating tower adopted the acetates entrainer, ritalin contained in the dehydration tower charging had bigger influence to the tower load.Existing processes is not considered the influence of this impurity to system energy consumption.Because after the condensation of dehydration column overhead vapour phase, ritalin is different in the distribution of organic phase and water, most of acetic acid is back in the dehydration tower with ester mutually, and ritalin enrichment in dehydration tower causes the increase of thermal load and cat head refrigeration duty at the bottom of the Tata that dewaters.Especially in charging, contain under the situation of more ritalin, a large amount of ritalins constantly flows at dehydration tower and phase splitter internal recycle, thereby has caused unnecessary energy expenditure.Therefore, when ritalin content is high in the charging, need make certain improvements to existing processes, with the influence of reduction ritalin Dichlorodiphenyl Acetate dehydration tower, and then the energy consumption of reduction dehydration tower.
Summary of the invention
The improvement technology that the purpose of this invention is to provide a kind of acetic acid dehydration and azeotropic distillation method in conjunction with conventional acetic acid dehydration technology and dephlegmator process, is used to reduce the energy consumption of acetic acid dehydrating tower.
Embodiment of the present invention are; Feed stream 1 from a last operation (comprises acetic acid, water and ritalin; Wherein the mass ratio of ritalin and water is greater than 0.03) get into acetic acid dehydrating tower T01, under the effect of entrainer n-butyl acetate, the acetic acid stream 3 that obtains content 95% at the bottom of the tower is recycled; Cat head is mainly contained the vapor phase stream 2 of n-butyl acetate, water and ritalin; Be introduced into condensing surface E02 and be reduced to certain temperature; Introduce vapour liquid separator V02 again and separate, resulting liquid phase stream 4C introduces liquid liquid/gas separator V01 after introducing condensing surface E01 condensation, and resulting vapor phase stream 4A introduces condensing surface E03 and vapour liquid separator V03; Condense to certain temperature and separation; The liquid phase stream 4E that obtains gets into liquid liquid/gas separator V01 after introducing condensing surface E01 condensation, and resulting vapor phase stream 4D is rich in ritalin, introduces entrainer regenerating column T02.Through the adjustment first step and partial condensing temperature; The massfraction scope of ritalin is 0.026～0.096 among the control liquid phase stream 4E; The massfraction scope of ritalin is 0.042～0.39 among the liquid phase stream 4D, guarantees that simultaneously the condensing temperature of condensing surface E03 is lower than condensing surface E02.Ritalin is realized the pre-separation of ritalin and other components mainly through logistics 4D extraction dehydration tower, reduces the enriching quantity of ritalin in acetic acid dehydrating tower T01.The positive butyl ester of the little acetic acid that logistics 4D takes out of reclaims through the entrainer regenerating column.The liquid phase that gets into liquid liquid/gas separator V01 is divided into organic phase logistics 5 and water logistics 6.Organic phase logistics 5 contains n-butyl acetate, ritalin and less water, returns acetic acid dehydrating tower with reflux; Water logistics 6 contains water and the positive butyl ester of little acetic acid, ritalin, introduces the entrainer regenerating column and reclaims n-butyl acetate and ritalin.
Implementing foregoing invention vapor-liquid separation and the isolating device of liquid liquid can be the equipment of any realization above-mentioned functions, and the inventive method is not limited to any special type of equipment.
The present invention compared with prior art; Main benefit is to reduce the energy consumption of acetic acid dehydrating tower; And simple and easy to do, the expansion that is particularly useful for old factory can and be reconstructed, when ritalin content in the supplied materials of the upper reaches is big; Can increase and decrease the quantity of partial condensation device at any time, need not do big change existing equipment.
Description of drawings
Fig. 1 is conventional acetic acid dehydration heterogeneous azeotropic rectification process flow sheet.
Fig. 2 is improved acetic acid dehydration heterogeneous azeotropic rectification process flow sheet.
In the drawings: the T01-acetic acid dehydrating tower; T02-entrainer regenerating column; V01-liquid liquid phase splitter;
V03-vapour liquid separator; E02 condensing surface; The E04-interchanger;
S02-splitter; P02-pump
Embodiment
Explanation through following examples will help to understand the present invention, but not limit content of the present invention.The particular flow sheet of embodiment please refer to Fig. 1 and Fig. 2.
It is entrainer that the present invention adopts n-butyl acetate, is that 0.4 solution is pending solution with the acetic acid massfraction, and the acetic acid dehydration column overhead is 5kPag, and tower still pressure is 25kPag.In the present embodiment, the acetic acid dehydrating tower feed conditions is following: pressure is 30kPag; Temperature is 65.1 ℃; The acetic acid flow is 6000kg/h in the feed stream, and discharge is 9000kg/h, and the ritalin flow is 450kg/h, and promptly ritalin reaches 0.05 with the quality ratio.
Under full condensation process, dehydration tower T01 cat head vapour phase gets into liquid liquid phase splitter V01 after the whole condensations of condensing surface E01; Under dephlegmator process, dehydration tower T01 cat head vapor phase stream 2 is at first passed through the two-stage partial condensation, and vapor phase stream 4D directly introduces the entrainer regenerating column, and liquid phase gets into liquid liquid phase splitter V01.Wherein, first step partial condensation temperature is 88 ℃, and second stage partial condensation temperature is 85 ℃.
Two kinds of technological effect contrasts:
Adopt full condensation process, the ritalin mass rate in the liquid phase stream 4 is 4422.5kg/h, and its massfraction is for reaching 0.12.Ritalin flow in organic backflow 5 reaches 3955.3kg/h, and its massfraction reaches 0.14.The cat head refrigeration duty is 10.24MW, and the cat head thermal load is 10.22MW.
Adopt dephlegmator process, after first step partial condensation, ritalin among the vapor phase stream 4A and n-butyl acetate mass rate are respectively 372.7kg/h and 925.4kg/h, and its massfraction is respectively 0.22 and 0.55; Ritalin 1083.3kg/h among the liquid phase stream 4C, its massfraction are 0.33.After the partial condensation of the second stage, ritalin among the vapor phase stream 4D and n-butyl acetate mass rate are respectively 326.5kg/h and 420.6kg/h, and its massfraction is respectively 0.35 and 0.45; The ritalin mass rate is 46.2kg/h among the liquid phase stream 4E, and its massfraction is 0.06.After the two-stage partial condensation, 72.6% of contained ritalin with the extraction of vapour phase form in the charging, directly introduces the entrainer regenerating column.Vapor phase stream 4D takes the part n-butyl acetate out of and reclaims through the entrainer regenerating column.Ritalin in organic backflow 5 has only 1001.8kg/h, and its massfraction has only 0.04.The cat head refrigeration duty is 9.32MW, and the cat head thermal load is 9.57MW.
Both compare, and adopt dephlegmator process can reduce by 6.39% thermal load and 9.83% refrigeration duty, have obvious energy-saving effect.
Claims (4)
1. one kind is adopted the technological acetic acid dehydration and azeotropic distillation technology of partial condensation; It is characterized in that: the operating mode that contains the impurity ritalin in the acetic acid dehydrating tower charging; Through being the acetic acid dehydration and azeotropic distillation tower of entrainer with the n-butyl acetate, obtain accords with production high density acetic acid that requires and the vapor phase stream that contains n-butyl acetate, water and ritalin; Through between cat head and liquid liquid phase splitter, increasing by two cover partial condensation devices; Extraction part ritalin is to the entrainer regenerating column; Adopt two-stage partial condensation technology, make ritalin and n-butyl acetate, water realize pre-separation, thereby reduce the enriching quantity of ritalin in acetic acid dehydrating tower; Reclaim n-butyl acetate and ritalin through the entrainer regenerating column.
2. technology according to claim 1 is characterized in that: ritalin compares greater than 0.03 with quality in the handled feed stream.
3. partial condensation device according to claim 1 is characterized in that: the partial condensation device is made up of a condensing surface and a vapour liquid separator.
4. partial condensation device according to claim 3; It is characterized in that: first step partial condensation obtains the massfraction of ritalin in the liquid phase stream and is reduced in 0.026～0.096 the scope, and the massfraction of ritalin is reduced in 0.042～0.39 the scope in the liquid phase stream that second stage partial condensation obtains; Simultaneously, partial condensation temperature in the second stage is lower than first step partial condensation temperature.
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| CN2012101128573A CN102659555A (en) | 2012-04-17 | 2012-04-17 | Acetic acid dehydration technology adopting partial condensation process |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1150583A (en) * | 1995-09-29 | 1997-05-28 | 昭和电工株式会社 | Process for purifying acetic acid |
| US5980696A (en) * | 1994-08-23 | 1999-11-09 | E. I. Du Pont De Nemours And Company | Dehydration of acetic acid by azeotropic distillation in the production of an aromatic acid |
| CN1867537A (en) * | 2003-08-12 | 2006-11-22 | Amt国际股份有限公司 | System and method for acetic acid recovery during terephthalic acid production |
-
2012
- 2012-04-17 CN CN2012101128573A patent/CN102659555A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5980696A (en) * | 1994-08-23 | 1999-11-09 | E. I. Du Pont De Nemours And Company | Dehydration of acetic acid by azeotropic distillation in the production of an aromatic acid |
| CN1150583A (en) * | 1995-09-29 | 1997-05-28 | 昭和电工株式会社 | Process for purifying acetic acid |
| CN1867537A (en) * | 2003-08-12 | 2006-11-22 | Amt国际股份有限公司 | System and method for acetic acid recovery during terephthalic acid production |
Non-Patent Citations (1)
| Title |
|---|
| 唐守胜等: "醋酸甲酯对醋酸脱水共沸精馏过程的影响", 《华东理工大学学报（自然科学版）》 * |
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Application publication date: 20120912 |