CN102653512A - Integrated process for recovering acetic acid and methyl acetate in production process of aromatic carboxylic acid - Google Patents
Integrated process for recovering acetic acid and methyl acetate in production process of aromatic carboxylic acid Download PDFInfo
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- CN102653512A CN102653512A CN2011100498598A CN201110049859A CN102653512A CN 102653512 A CN102653512 A CN 102653512A CN 2011100498598 A CN2011100498598 A CN 2011100498598A CN 201110049859 A CN201110049859 A CN 201110049859A CN 102653512 A CN102653512 A CN 102653512A
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Abstract
The invention relates to an integrated process for recovering acetic acid and methyl acetate in a production process of aromatic carboxylic acid. The integrated process is as follows: water solution of acetic acid from an oxidation unit enters the upper part of a dehydrating tower, steam at the top of the dehydrating tower enters a condenser at the tower top for cooling, and concentrated acetic acid extracted from a tower kettle directly returns to an oxidation reactor; condensed fluid at the top of the dehydrating tower enters a phase splitter and is automatically splitted into an oil phase and a water phase, the oil phase enters an entrainer refining tower, methyl acetate is extracted from the tower top and is recovered, and the entrainer in the tower kettle returns to the top of the dehydrating tower; the water phase enters a methyl acetate recovering tower, methyl acetate extracted from the tower top and methyl acetate at the top of the entrainer refining tower are recovered together, water part in the tower kettle flows back to the top of the dehydrating tower, and part of water is extracted and treated. When the entrainer in the acetic acid of the tower kettle of the dehydrating tower is higher than 5 percent, the tower kettle material firstly enters an entrainer separating tower, the condensed acetic acid extracted from the tower top returns to the oxidation reactor, and excess entrainer is separated from the tower kettle. By utilizing the process, the quantity of the entrainer flowing back can be greatly reduced, and the oxidation reaction can be stably performed.
Description
Technical field
The present invention relates to reclaim in the aromatic carboxylic acid production process method of reaction solvent acetic acid and byproduct of reaction ritalin.The separation method that the present invention relates generally to is an azeotropic distillation.
Background technology
Aromatic carboxylic acid is one type of important chemical midbody, is the basic raw material of producing mechanicalss such as polyester, fiber, film, bottle class.Aromatic carboxylic acid such as terephthalic acid, m-phthalic acid generally makes through the substituted aromatic hydrocarbons compounds of its corresponding alkyl of catalyzed oxidation such as p-Xylol, m-xylene etc.Oxidizing reaction is solvent with acetic acid, and Cobaltous diacetate, manganese acetate, hydrogen bromide or tetrabromoethane are made catalyzer, under certain temperature and pressure, carry out, in this process with the generation of water.For the accumulation that prevents water in the oxidation reactor reduces efficiency, often discharge from oxidation reactor with the form of steam.Mainly contain acetic acid and water in the steam of discharging, also have a small amount of unreacted raw material and byproduct of reaction in addition.Therefore, remove the water in this strand material, the solvent acetic acid that reclaims wherein is very necessary.Main conventional distillation and the azeotropic distillation technology for recovery acetic acid of adopting in the industry.Because the conventional distillation energy consumption is higher, and therefore azeotropic distillation has characteristics such as good separating effect, energy consumption are low, operation stabilization become the main trend that reclaims acetic acid in the industrial production.
At present; Entrainer commonly used in the industrial production mainly is acetic acid alkyl ester (like n-butyl acetate, isobutyl acetate, a n-propyl acetate etc.), and when being entrainer with the acetic acid alkyl ester, the entrainer add-on must strictly be controlled; And a small amount of entrainer can get into reactor drum with acetic acid at the bottom of the tower; Reaction generates impurity, causes the consumption of entrainer, and quality product and dewatering unit are had very big influence.In addition, a small amount of unreacted aromatic hydrocarbon in the charging can constantly accumulate in tower, when its concentration is increased to a certain degree, will certainly reduce the separation performance of tower, influences separating effect.
Aromatic hydrocarbon as reactant not only can form low-boiling-point substance with water; And its band outlet capacity also is better than acetic acid alkyl esters entrainer; Therefore; If directly the aromatic hydrocarbon with one of reactant is entrainer, just can solve above-mentioned when being entrainer with the acetic acid alkyl ester, the entrainer consumption of existence and the problem that aromatic hydrocarbon accumulates in dehydration tower.For above-mentioned imagination, the existing report of patent US 2005/0272951 A1, US 2006/0235242 A1 and US 2007/0027340 A1.But the mentioned technology entrainer quantity of reflux of above-mentioned patent is bigger, causes acetic acid removal process energy consumption higher; In addition, excessive entrainer directly and the processing mode of acetic acid Returning oxidation reactor will inevitably increase the control difficulty of oxidation feed in the dehydration Tata still of mentioning in the above-mentioned patent, influences the stable of oxidizing reaction and carries out.In the entrainer that dehydration tower refluxes, still contain a certain amount of ritalin; If can ritalin wherein be separated; Not only can improve the separating effect of dehydration tower; Also can improve the economy of tripping device, for ritalin process for separating and recovering in the above-mentioned entrainer, not seeing at present has bibliographical information.
Summary of the invention
The present invention be directed to the substituted aromatic hydrocarbon based compound for catalysis oxidation of alkyl and generate the aromatic carboxylic acid process, a kind of integrated technique that reclaims solvent acetic acid and by-product methyl acetate thereof is provided, this integrated technique is realized through following technical scheme:
A kind of integrated technique that reclaims acetic acid and ritalin in the aromatic carboxylic acid production process that reclaims; This technology comprises dehydration tower, phase splitter, entrainer treating tower, ritalin regenerating column, entrainer knockout tower and corresponding pipeline composition; It is characterized in that being provided with in this integrated technique an entrainer treating tower, this tower is used for the little acetic acid methyl esters of separation and azeotropic agent; This technology also is provided with an entrainer knockout tower, when entrainer content is higher than 5% in the tower still material, is used for the entrainer of knockout tower still material.
A kind of integrated technique that reclaims acetic acid and ritalin in the aromatic carboxylic acid production process that reclaims; As shown in Figure 1; It is characterized in that this integrated technique is an entrainer with the aromatic hydrocarbon of one of reactant in the aromatic carboxylic acid production process; Utilize operation stepss such as azeotropic distillation, overhead oil water sepn, entrainer are made with extra care, ritalin recovery, entrainer separation to form, carry out according to following steps successively:
Step 1. comes the unitary aqueous acetic acid of automatic oxidation reaction to get into dehydration tower top, and the dehydration overhead vapours is minimum azeotropic mixture and the little acetic acid methyl esters that water and entrainer form, and tower bottoms is concentrated acetic acid,
Dehydration tower tower bottoms in step 2. step 1 concentrates the direct Returning oxidation reactor of acetic acid as solvent, gets into phase splitter behind the dehydration column overhead vapor condensation in the step 1 simultaneously, and overhead product is divided into oil phase and water in phase splitter,
Oil phase in step 3. step 2 in the cat head phase splitter gets into the entrainer treating tower, and the little acetic acid methyl esters is from refining cat head extraction of entrainer and recovery in the entrainer, and the entrainer after making with extra care is back to the dehydration tower top, gets into dehydration tower, uses as entrainer; Water gets into the ritalin regenerating column, and the ritalin of cat head extraction and entrainer treating tower cat head ritalin merge, and reclaims together, and tower still material is the water that contains acetate in minute,
Ritalin reclaims the water section that the Tata still contains acetate in minute and is back to the dehydration tower top in step 4. step 3, and the part extraction is handled,
When step 5. was higher than 5% when the entrainer content in the acetic acid of the dehydration Tata still in the step 2, the acetic acid of tower still was introduced into the entrainer knockout tower, the entrainer that the extraction of tower still is excessive, cat head high-content acetic acid Returning oxidation reactor.
The above-mentioned recovery acetic acid and the integrated technique of ritalin, the described dehydration tower of step 1 is the rectifying tower of 10-100 theoretical tray.
The above-mentioned recovery acetic acid and the integrated technique of ritalin, the rectifying tower that the described entrainer treating tower of step 3 is the 10-80 theoretical tray.
The above-mentioned recovery acetic acid and the integrated technique of ritalin, the rectifying tower that the described ritalin regenerating column of step 3 is the 5-60 theoretical tray.
The above-mentioned recovery acetic acid and the integrated technique of ritalin, the described dehydration tower top azeotropic dosage that is back to of step 3 is 0.5 ~ 5 with getting into dehydration tower Total Water ratio, preferred 1 ~ 2.5.
The above-mentioned recovery acetic acid and the integrated technique of ritalin, the described ritalin of step 4 reclaim at the bottom of the Tata aqueous-phase reflux amount and produced quantity than 0.01 ~ 0.4, and preferred 0.05 ~ 0.2.
The above-mentioned recovery acetic acid and the integrated technique of ritalin, the rectifying tower that the described entrainer knockout tower of step 5 is the 10-80 theoretical tray.
The aqueous phase acetic acid content of the integrated technique extraction of recovery acetic acid of the present invention and ritalin is 0.01wt% ~ 0.08wt%; Water-content is 0.1wt% ~ 10wt% in the acetic acid of Returning oxidation reactor, and entrainer content is 0.1wt% ~ 5wt%.
Entrainer treating tower and ritalin regenerating column cat head extraction ritalin content are 90wt% ~ 99wt% in the integrated technique of recovery acetic acid of the present invention and ritalin.
Reclaim the integrated technique of acetic acid and ritalin in a kind of aromatic carboxylic acid production process of the present invention; Can significantly reduce the entrainer quantity of reflux; In reducing water acetic acid content, reclaim in the ritalin; Also may command tower still water and entrainer content help that oxidizing reaction is stable carries out, and have avoided existing technology to have that process is complicated, energy consumption is high, the problem of entrainer loss.
Description of drawings
Fig. 1 is the schematic flow sheet that reclaims the integrated technique of acetic acid and ritalin in the aromatic carboxylic acid production process of the present invention, and wherein: T1 is a dehydration tower; T2 is the entrainer treating tower; T3 is the ritalin regenerating column; T4 is the entrainer knockout tower; V1 is a phase splitter; 1 is the aqueous acetic acid from oxidation unit; 2 is dehydration column overhead steam; 3 is the dehydration column overhead phlegma; 4 concentrated acetic acid for dehydration Tata still; 5 is the oil phase in the phase splitter; 6 is the water in the phase splitter; 7 entrainers for the refining Tata still of entrainer; 8 the water that contain acetate in minute that are back to dehydration tower for ritalin recovery Tata still; 9 is the ritalin of entrainer treating tower cat head extraction; 10 is the ritalin of ritalin regenerating column cat head extraction; 11 reclaim the water that contains acetate in minute of the extraction of Tata still for ritalin; 12 is the high-load acetic acid of entrainer knockout tower cat head extraction, Returning oxidation reactor; 13 excessive entrainers for the extraction of entrainer separation Tata still.
Embodiment
Do detailed explanation below in conjunction with 1 pair of technological process of the present invention of accompanying drawing.Aqueous acetic acid (1) from oxidation unit gets into dehydration tower T1 top, and dehydration column overhead steam (2) gets into the overhead condenser cooling, and the extraction of tower still concentrates directly Returning oxidation reactor of acetic acid (4); Dehydration column overhead phlegma (3) gets into phase splitter V1, is divided into oil phase and water automatically, and oil phase in the phase splitter (5) gets into entrainer treating tower T2, and cat head extraction ritalin (9) also reclaims, and tower still entrainer (7) is back to dehydration tower T1 top; Water in the phase splitter (6) gets into ritalin regenerating column T3, and the ritalin of cat head extraction (10) reclaims with entrainer treating tower cat head ritalin, and tower still water section refluxes (8) to the dehydration tower top, and partly (11) extraction is handled.When entrainer concentration was higher than 5% in the dehydration Tata still acetic acid, tower still material was introduced into entrainer knockout tower T4, and the cat head extraction concentrates acetic acid (12) Returning oxidation reactor, and the tower still is isolated excessive entrainer (13).
Below pass through to reclaim acetic acid and the concrete application of the present invention of ritalin process explanation in the Production of Terephthalic Acid, but range of application of the present invention does not receive the restriction of the following example.
[embodiment 1]
Terephthalic acid is to be raw material with p-Xylol (PX), and catalyzed oxidation makes under catalyzer and certain temperature and pressure, and the aqueous acetic acid in the production process after the reactor head steam cooling gets into dehydration tower T1 top.
As shown in Figure 1, dehydration tower T1 theoretical plate number 40, entrainer treating tower theoretical plate number 15, ritalin regenerating column theoretical plate number is 10, entrainer knockout tower theoretical plate number is 20.The aqueous acetic acid flow that gets into dehydration tower is 1000kg/hr, wherein contains acetic acid 75 wt%, moisture 24.5 wt%; Quality 0.5 wt% that contains ritalin is from the 10th column plate charging of dehydration tower, after overhead vapours (2) condensation; Phlegma (3) gets into phase splitter V1; Oil phase in the phase splitter (5) gets into the 5th block of column plate of entrainer treating tower, and entrainer treating tower cat head extraction ritalin (9) content is 98.5%, and tower still extraction content is that 99.5% PX (7) is back to the 1st block of column plate of dehydration tower; Quantity of reflux is 550kg/hr, and oil phase quantity of reflux and the total amount that gets into dehydration tower water are than 2.0; Water in the phase splitter (6) gets into the ritalin regenerating column; Cat head extraction ritalin (10) content is 95.6%, and extraction aqueous phase acetic acid content is 0.03% at the bottom of the tower, aqueous portion extraction (11); Flow is 215kg/hr; The 3rd block of column plate of partial reflux (8) to dehydration tower, quantity of reflux is 30kg/hr, backflow is 0.14 with the extraction ratio.Moisture 1.9% in the dehydration Tata still extraction acetic acid, contain PX 2.3%
Other condition is constant among [embodiment 2] maintenance embodiment 1; The PX quantity of reflux is 220kg/hr, and oil phase quantity of reflux and the total amount that gets into dehydration tower water be than 0.8, separates that acetic acid content is 0.06% in the back ritalin recovery Tata still recovered water; In the dehydration Tata still extraction acetic acid moisture 2.5%; Contain PX 1.1%, entrainer treating tower cat head extraction ritalin content is 98.4%, and it is 96.0% that ritalin reclaims cat head extraction ritalin content.
Other condition is constant among [embodiment 3] maintenance embodiment 1, and the aqueous-phase reflux amount is 15kg/hr, and produced quantity is 230kg/hr; Aqueous-phase reflux and extraction ratio are 0.07; Separate the back ritalin and reclaim in the Tata still recovered water and contain acetic acid 0.04%, moisture 2.0% in the dehydration Tata still extraction acetic acid, contain PX 1.2%; Entrainer treating tower cat head extraction ritalin content is 98.6%, and it is 96.5% that ritalin reclaims cat head extraction ritalin content.
[embodiment 4]
Keep other condition among the embodiment 1 constant; Changing entrainer PX quantity of reflux is 900kg/hr; Oil phase quantity of reflux and the total amount that gets into dehydration tower water are than 3.3, and PX content is 12.9% in the Tata still extraction of dewatering, and this material is introduced into the 8th block of column plate of entrainer knockout tower T4; Moisture 1.2% in the cat head extraction acetic acid, contain PX 2.0%; Separate back ritalin recovery Tata still extraction aqueous phase and contain acetic acid 0.01%, entrainer treating tower cat head extraction ritalin content is 98.1%, and it is 96.3% that the extraction of ritalin recovery cat head contains ritalin content.
Claims (9)
1. one kind is reclaimed the integrated technique that reclaims acetic acid and ritalin in the aromatic carboxylic acid production process; It is characterized in that: this integrated technique is an entrainer with the aromatic hydrocarbon of one of reactant in the aromatic carboxylic acid production process; Utilize operation stepss such as azeotropic distillation, overhead oil water sepn, entrainer are made with extra care, ritalin recovery, entrainer separation to form, carry out according to following steps successively:
Step 1. comes the unitary aqueous acetic acid of automatic oxidation reaction to get into dehydration tower top, and the dehydration overhead vapours is minimum azeotropic mixture and the little acetic acid methyl esters that water and entrainer form, and tower bottoms is concentrated acetic acid,
Dehydration tower tower bottoms in step 2. step 1 concentrates the direct Returning oxidation reactor of acetic acid as solvent, gets into phase splitter behind the dehydration column overhead vapor condensation in the step 1 simultaneously, and overhead product is divided into oil phase and water in phase splitter,
Oil phase in step 3. step 2 in the cat head phase splitter gets into the entrainer treating tower, and the little acetic acid methyl esters is from refining cat head extraction of entrainer and recovery in the entrainer, and the entrainer after making with extra care is back to the dehydration tower top, gets into dehydration tower, uses as entrainer; Water gets into the ritalin regenerating column, and the ritalin of cat head extraction and entrainer treating tower cat head ritalin merge, and reclaims together, and tower still material is the water that contains acetate in minute,
Ritalin reclaims the water section that the Tata still contains acetate in minute and is back to the dehydration tower top in step 4. step 3, and the part extraction is handled,
When step 5. was higher than 5% when the entrainer content in the acetic acid of the dehydration Tata still in the step 2, the acetic acid of tower still was introduced into the entrainer knockout tower, the entrainer that the extraction of tower still is excessive, cat head high-content acetic acid Returning oxidation reactor.
2. the integrated technique of recovery acetic acid according to claim 1 and ritalin is characterized in that: the described dehydration tower of step 1 is the rectifying tower of 10-100 theoretical tray.
3. the integrated technique of recovery acetic acid according to claim 1 and ritalin is characterized in that: the rectifying tower that the described entrainer treating tower of step 3 is the 10-80 theoretical tray.
4. the integrated technique of recovery acetic acid according to claim 1 and ritalin is characterized in that: the rectifying tower that the described ritalin regenerating column of step 3 is the 5-60 theoretical tray.
5. the integrated technique of recovery acetic acid according to claim 1 and ritalin is characterized in that: the described dehydration tower top azeotropic dosage that is back to of step 3 is 0.5 ~ 5 with getting into dehydration tower Total Water ratio.
6. the integrated technique of recovery acetic acid according to claim 1 and ritalin is characterized in that: the described dehydration tower top azeotropic dosage that is back to of step 3 is 1 ~ 2.5 with getting into dehydration tower Total Water ratio.
7. the integrated technique of recovery acetic acid according to claim 1 and ritalin is characterized in that: the aqueous-phase reflux amount is 0.01 ~ 0.4 with the produced quantity ratio at the bottom of the described ritalin recovery of step 4 Tata.
8. the integrated technique of recovery acetic acid according to claim 1 and ritalin is characterized in that: the aqueous-phase reflux amount is 0.05 ~ 0.2 with the produced quantity ratio at the bottom of the described ritalin recovery of step 4 Tata.
9. the integrated technique of recovery acetic acid according to claim 1 and ritalin is characterized in that: the rectifying tower that the described entrainer knockout tower of step 5 is the 10-80 theoretical tray.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104513150A (en) * | 2013-09-27 | 2015-04-15 | 中国石油化工股份有限公司 | Method for optimizing operation of solvent dehydration system during production process of aromatic acid |
| CN106397184A (en) * | 2015-07-27 | 2017-02-15 | 中国石化扬子石油化工有限公司 | Method for dewatering solvent during aromatic acid production process |
| CN109467497A (en) * | 2018-08-03 | 2019-03-15 | 内蒙古蒙维科技有限公司 | A kind of recovery process and device of polyvinyl alcohol alcohol hydrolysis mother liquor |
| CN111718256A (en) * | 2019-03-20 | 2020-09-29 | 中国石油化工股份有限公司 | Acetic acid dehydration method |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104513150A (en) * | 2013-09-27 | 2015-04-15 | 中国石油化工股份有限公司 | Method for optimizing operation of solvent dehydration system during production process of aromatic acid |
| CN104513150B (en) * | 2013-09-27 | 2016-06-29 | 中国石油化工股份有限公司 | A kind of method of solvent dehydration system optimized operation in aromatic acid production process |
| CN106397184A (en) * | 2015-07-27 | 2017-02-15 | 中国石化扬子石油化工有限公司 | Method for dewatering solvent during aromatic acid production process |
| CN109467497A (en) * | 2018-08-03 | 2019-03-15 | 内蒙古蒙维科技有限公司 | A kind of recovery process and device of polyvinyl alcohol alcohol hydrolysis mother liquor |
| CN109467497B (en) * | 2018-08-03 | 2023-11-10 | 内蒙古蒙维科技有限公司 | Recovery process and device for polyvinyl alcohol alcoholysis mother liquor |
| CN111718256A (en) * | 2019-03-20 | 2020-09-29 | 中国石油化工股份有限公司 | Acetic acid dehydration method |
| CN111718256B (en) * | 2019-03-20 | 2022-05-27 | 中国石油化工股份有限公司 | Acetic acid dehydration method |
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