CN101870644B - Device for removing acetone in carbonyl synthesis process of acetic anhydride - Google Patents
Device for removing acetone in carbonyl synthesis process of acetic anhydride Download PDFInfo
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- CN101870644B CN101870644B CN 201010231131 CN201010231131A CN101870644B CN 101870644 B CN101870644 B CN 101870644B CN 201010231131 CN201010231131 CN 201010231131 CN 201010231131 A CN201010231131 A CN 201010231131A CN 101870644 B CN101870644 B CN 101870644B
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Abstract
The invention relates to a device for removing acetone in a carbonyl synthesis process of acetic anhydride, belonging to the preparation of acetic anhydride. The device comprises the following operating units: a, a prefractionation unit using an acetone-enriching rectifying tower (2) as the main body; b, an azeotropic acetone separating unit using an azeotropic fractionation rectifying tower (6) as the main body; and c, an extracting and phase-splitting unit using a double-cavity extracting overflow phase separator (9) as the main body, wherein the extracting and phase-separating unit mainly comprises the double-cavity extracting overflow phase separator (9), a water inlet pipeline (10), a normal pentane inlet pipeline (11), and a refluxing cavity (13) and a water extracting and phase-separating cavity (14) which are separated by a barrier (12).The device for removing acetone in a carbonyl synthesis process of acetic anhydride has the advantages of simple process, high acetone removalrate and less waste water production. The chroma of the acetic anhydride is no more than 5 Hazen units, the carbon monoxide conversion rate is up to 95%, and the service life of the catalyst is prolonged.
Description
Technical field
The present invention is the device of removing acetone in a kind of carbonyl synthesis process of acetic anhydride.Belong to the preparation of carboxylic acid anhydride, particularly the method for employing oxo process prepares the removal device of the impurity acetone that produces in the process of acetic anhydride process.
Background technology
Obtain acetic acid and diacetyl oxide by methyl acetate and methyl alcohol or methyl alcohol and dme and reaction of carbon monoxide, namely to prepare diacetyl oxide be the novel process that grows up the 1980s to carbonylic preparation method.Energy consumption is little, cost is lower because it has, and is conducive to large-scale industrial production, and before ketenes method and acetaldehyde oxidation are progressively replaced by oxo synthesis.
But a small amount of acetone that produces in the carbonylation processes is removed as untimely, will become " tar ".The disadvantageous effect of bringing thus is as follows:
1. acetone can reduce the transformation efficiency of carbon monoxide.
2. the colourity variation that causes the aceticanhydride product.
3. the tar that produces owing to the accumulation of acetone sticks to the surface of catalyst rhodium, has reduced its catalytic activity.
Describe a kind of method of complexity in the U.S. Patent No. 4252748, needed four distillations and single extraction.Device and technological process are too complicated.China's patent 00817411.3,92111407.9,92105695.8, utilize water and acetone to dissolve each other, and the solubleness of water in ritalin and methyl iodide is extremely low, thus water acetone is separated from acetone, ritalin and methyl iodide, but need to produce a large amount of trade effluents.
Summary of the invention
The object of the invention is to avoid above-mentioned weak point of the prior art, and a kind of simple structure is provided, the acetone clearance is high, produces the less device of removing acetone from carbonyl synthesis process of acetic anhydride of waste water.Comparatively ideal avoiding because the existence of the impurity acetone in the reaction product, and the reduction of the transformation efficiency of the carbon monoxide that brings, the colourity variation of diacetyl oxide product, and the tar that produces owing to the accumulation of acetone sticks to the surface of catalyst rhodium, reduced the problems of its catalytic activity.
Purpose of the present invention can reach by following measure:
Remove the device of acetone in the carbonyl synthesis process of acetic anhydride of the present invention, it is characterized in that comprising the following operating unit that is connected with pipe fitting by pipeline:
A. the prefractionation unit take acetone enrichment rectifying tower 2 as main body mainly is formed by connecting by pipeline and pipe fitting by conveying pipeline A1, acetone enrichment rectifying tower 2, reboiler A3, condenser A4;
B. the azeotropic separation acetone unit take azeotropic fractionation rectifying tower 6 as main body mainly is formed by connecting by pipeline and pipe fitting by conveying pipeline B 5, azeotropic fractionation rectifying tower 6, reboiler B 7, condenser B 8, return line 15;
C. the extraction take two-chamber extraction overflow phase splitter 9 as main body divides facies unit, mainly enters pipeline 11 by two-chamber extraction overflow phase splitter 9, back with water inlet line 10, Skellysolve A, and consists of by dividing plate 12 separated back cavity 13 and water extraction, phase-splitting chambeies 14;
Wherein, operating unit a is connected conveying pipeline B 5 and connects with operating unit b, and operating unit b is connected return line 15 with operating unit c and condenser B 8 connects;
Technological process comprises following operation steps:
A. prefractionation
Contain methyl acetate, CH from the oxo process system
3The low boiling mixture of I, acetone and micro-acetic acid enters acetone enrichment rectifying tower 2 by conveying pipeline A 1 from the middle part of acetone enrichment rectifying tower 2, is rich in ritalin, and a small amount of CH
3The overhead product of I and acetone, after condenser A4 condensation, wherein part is as trim the top of column, and all the other send into the carbonylation reaction system as recycle stock; Acetone enters azeotropic fractionation rectifying tower 6 by conveying pipeline B 5 middle parts from azeotropic fractionation rectifying tower 6 after further enrichment at the bottom of the tower;
B. azeotropic separation acetone
From mixture flow at the bottom of acetone enrichment rectifying tower 2 towers, in azeotropic fractionation rectifying tower 6, be fractionated, Skellysolve A and acetone azeotrope distillate from cat head, after condenser B 8 condensations, all enter two-chamber extraction overflow phase splitter 9, phase-splitting to be extracted; Materials at bottom of tower constantly is admitted to the utilization of carbonylation reaction systemic circulation;
C. extract phase-splitting
From the overhead product of step b, enter in the water extraction, phase-splitting chamber 14 of two-chamber extraction overflow phase splitter 9, mix with water from back with water inlet line 10, be extracted phase-splitting; Organic phase is crossed dividing plate 12 overflows and is entered back cavity 13, and enters the Skellysolve A that pipeline 11 adds from Skellysolve A and converges, and total reflux enters azeotropic fractionation rectifying tower 6, continues to carry out the task that azeotropic is taken acetone out of, and lower layer of water is carried the acetone of dissolving and sent into treatment and finishing section.
Purpose of the present invention can also reach by following measure, and the below discloses preferred technical scheme:
Remove the method for acetone in the carbonyl synthesis process of acetic anhydride of the present invention, contain methyl acetate, CH from the oxo process system described in the step a
3The low boiling mixture percent by weight of I, acetone and micro-acetic acid consists of: ritalin 50～65, CH
3I20～50, acetone 4～12, acetic acid 0.5～5.
Remove the method for acetone in the carbonyl synthesis process of acetic anhydride of the present invention, the bottom still liquid temp of the enrichment of acetone described in step a rectifying tower 2 remains on 55～65 ℃, 40～50 ℃ of top exhaust gas stream temperature.
Remove the method for acetone in the carbonyl synthesis process of acetic anhydride of the present invention, the trim the top of column ratio of the enrichment of acetone described in step a rectifying tower 2 is controlled between 2.5:1～1.5:1.
Remove the method for acetone in the carbonyl synthesis process of acetic anhydride of the present invention, it is characterized in that 50～60 ℃ of the bottom still liquid temps of azeotropic fractionation rectifying tower 6 described in the step b, 30～40 ℃ of top exhaust gas temperatures.Remove the method for acetone in the carbonyl synthesis process of acetic anhydride of the present invention, the phegma flow of described azeotropic fractionation rectifying tower 6 is 1:0.1～0.1:1 with the feed rate ratio of acetone enrichment rectifying tower 2.
Remove the method for acetone in the carbonyl synthesis process of acetic anhydride disclosed by the invention, following positively effect arranged compared to existing technology:
1. provide a kind of technique simple, the acetone clearance is high, produces the less method of removing acetone from carbonyl synthesis process of acetic anhydride of waste water.Comparatively ideal having avoided because the existence of the impurity acetone in the reaction product, and the reduction of the transformation efficiency of the carbon monoxide that brings, the colourity variation of diacetyl oxide product, and the tar that produces owing to the accumulation of acetone sticks to the surface of catalyst rhodium, reduced the problems of its catalytic activity.
2. can be used for as required continuous or semi-continuous concentration with the acetone in the carbonylation reactor is reduced in the predetermined scope.
3. can produce high-quality diacetyl oxide, the color of diacetyl oxide product be improved significantly.Diacetyl oxide colourity Hazen unit≤5.
4. the carbon monoxide transformation efficiency brings up to 95% by original 75%.
5. activity and the work-ing life of catalyst rhodium have been prolonged.
Description of drawings
Fig. 1 is the method process flow diagram of removing acetone in the carbonyl synthesis process of acetic anhydride of the present invention
Among the figure
1-conveying pipeline A
2-acetone enrichment rectifying tower
3-reboiler A
4-condenser A
5-conveying pipeline B
6-azeotropic fractionation rectifying tower
7-reboiler B
8-condenser B
9-two-chamber extraction overflow phase splitter
The 10-back with water inlet line
The 11-Skellysolve A enters pipeline
The 12-dividing plate
The 13-back cavity
The extraction of 14-water, phase-splitting chamber
The 15-return line
Embodiment
The present invention will now be further detailed embodiment:
Embodiment 1
Remove the device of acetone in a kind of carbonyl synthesis process of acetic anhydride, it is characterized in that comprising the following operating unit that is connected with pipe fitting by pipeline:
A. the prefractionation unit take acetone enrichment rectifying tower 2 as main body mainly is formed by connecting by pipeline and pipe fitting by conveying pipeline A 1, acetone enrichment rectifying tower 2, reboiler A 3, condenser A4;
B. the azeotropic separation acetone unit take azeotropic fractionation rectifying tower 6 as main body mainly is formed by connecting by pipeline and pipe fitting by conveying pipeline B 5, azeotropic fractionation rectifying tower 6, reboiler B 7, condenser B 8, return line 15;
C. the extraction take two-chamber extraction overflow phase splitter 9 as main body divides facies unit, mainly enters pipeline 11 by two-chamber extraction overflow phase splitter 9, back with water inlet line 10, Skellysolve A, and consists of by dividing plate 12 separated back cavity 13 and water extraction, phase-splitting chambeies 14;
Wherein, operating unit a is connected conveying pipeline B 5 and connects with operating unit b, and operating unit b is connected return line 15 with operating unit c and condenser B 8 connects;
Utilize the device of removing acetone in the carbonyl synthesis process of acetic anhydride of the present invention, remove the method for acetone in a kind of carbonyl synthesis process of acetic anhydride, its technological process comprises following operation steps:
A. prefractionation
Contain ritalin 50～65, CH from the oxo process system
3I 20～50, acetone 4～12, and the low boiling mixture of acetic acid 0.5～5 enters acetone enrichment rectifying tower 2 by conveying pipeline A 1 from the middle part of acetone enrichment rectifying tower 2, and its flow is 1.2m3/h.Control tower reactor temperature 60 C, 49 ℃ of tower top temperatures are rich in ritalin, and a small amount of CH
3The overhead product of I and acetone, after condenser A 4 condensations, wherein part is as trim the top of column, and control of reflux ratio is at 2.5:1, and all the other send into the carbonylation reaction system as recycle stock; Acetone enters azeotropic fractionation rectifying tower 6 by conveying pipeline B 5 middle parts from azeotropic fractionation rectifying tower 6 after further enrichment at the bottom of the tower;
B. azeotropic separation acetone
From mixture flow at the bottom of acetone enrichment rectifying tower 2 towers, enter azeotropic fractionation rectifying tower 6 by conveying pipeline B 5 middle parts from azeotropic fractionation rectifying tower 6; 55 ℃ of the bottom still liquid temps of control azeotropic fractionation rectifying tower 6,35 ℃ of top exhaust gas temperatures.Be fractionated in azeotropic fractionation rectifying tower 6, Skellysolve A and acetone azeotrope distillate from cat head, after condenser B 8 condensations, all enter two-chamber extraction overflow phase splitter 9, phase-splitting to be extracted; Materials at bottom of tower constantly is admitted to the utilization of carbonylation reaction systemic circulation;
C. extract phase-splitting
From the overhead product of step b, enter in the water extraction, phase-splitting chamber 14 of two-chamber extraction overflow phase splitter 9, mix with water from back with water inlet line 10, the flow of water is 0.15m3/h, is extracted phase-splitting; Organic phase is crossed dividing plate 12 overflows and is entered back cavity 13, with enter the Skellysolve A that pipeline 11 adds from Skellysolve A and converge, enter azeotropic fractionation rectifying tower 6 by return line 15 total refluxs, continue to carry out the task that azeotropic is taken acetone out of, lower layer of water is carried the acetone of dissolving and is sent into treatment and finishing section.In the said process, the phegma flow of azeotropic fractionation rectifying tower 6 is 1:0.1 with the feed rate ratio of acetone enrichment rectifying tower 2.
Remove the method for acetone in a kind of carbonyl synthesis process of acetic anhydride, its technological process comprises following operation steps:
A. prefractionation
Contain ritalin 50～65, CH from the oxo process system
3I 20～50, acetone 4～12, and the low boiling mixture of acetic acid 0.5～5 enters acetone enrichment rectifying tower 2 by conveying pipeline A 1 from the middle part of acetone enrichment rectifying tower 2, and its flow is 0.7m3/h.57 ℃ of control tower reactor temperature, 48 ℃ of tower top temperatures are rich in ritalin, and a small amount of CH
3The overhead product of I and acetone, after condenser A 4 condensations, wherein part is as trim the top of column, and control of reflux ratio is at 1.5:1, and all the other send into the carbonylation reaction system as recycle stock; Acetone enters azeotropic fractionation rectifying tower 6 by conveying pipeline B 5 middle parts from azeotropic fractionation rectifying tower 6 after further enrichment at the bottom of the tower;
B. azeotropic separation acetone
From mixture flow at the bottom of acetone enrichment rectifying tower 2 towers, enter azeotropic fractionation rectifying tower 6 by conveying pipeline B 5 middle parts from azeotropic fractionation rectifying tower 6; 60 ℃ of the bottom still liquid temps of control azeotropic fractionation rectifying tower 6,40 ℃ of top exhaust gas temperatures.Be fractionated in azeotropic fractionation rectifying tower 6, Skellysolve A and acetone azeotrope distillate from cat head, after condenser B 8 condensations, all enter two-chamber extraction overflow phase splitter 9, phase-splitting to be extracted; Materials at bottom of tower constantly is admitted to the utilization of carbonylation reaction systemic circulation;
C. extract phase-splitting
From the overhead product of step b, enter in the water extraction, phase-splitting chamber 14 of two-chamber extraction overflow phase splitter 9, mix with water from back with water inlet line 10, the flow of water is 0.2m3/h, is extracted phase-splitting; Organic phase is crossed dividing plate 12 overflows and is entered back cavity 13, with enter the Skellysolve A that pipeline 11 adds from Skellysolve A and converge, enter azeotropic fractionation rectifying tower 6 by return line 15 total refluxs, continue to carry out the task that azeotropic is taken acetone out of, lower layer of water is carried the acetone of dissolving and is sent into treatment and finishing section.In the said process, the phegma flow of azeotropic fractionation rectifying tower 6 is 0.1:1 with the feed rate ratio of acetone enrichment rectifying tower 2.
Claims (5)
1. remove the device of acetone in the carbonyl synthesis process of acetic anhydride, it is characterized in that comprising the following operating unit that is connected with pipe fitting by pipeline:
A. the prefractionation unit take acetone enrichment rectifying tower (2) as main body is mainly by conveying pipeline A(1), acetone enrichment rectifying tower (2), reboiler A(3), condenser A(4) be formed by connecting by pipeline and pipe fitting;
B. the azeotropic separation acetone unit take azeotropic fractionation rectifying tower (6) as main body is mainly by conveying pipeline B(5), azeotropic fractionation rectifying tower (6), reboiler B(7), condenser B(8), return line (15) is formed by connecting by pipeline and pipe fitting;
C. the extraction take two-chamber extraction overflow phase splitter (9) as main body divides facies unit, mainly enter pipeline (11) by two-chamber extraction overflow phase splitter (9), back with water inlet line (10), Skellysolve A, and consist of by dividing plate (12) separated back cavity (13) and water extraction, phase-splitting chamber (14);
Wherein, operating unit a is connected conveying pipeline B(5 with operating unit b) connect, operating unit b is connected return line (15) and condenser B(8 with operating unit c) connect;
Technological process comprises following operation steps:
A. prefractionation
Contain methyl acetate, CH from the oxo process system
3The low boiling mixture of I, acetone and micro-acetic acid is by conveying pipeline A(1) enter acetone enrichment rectifying tower (2) from the middle part of acetone enrichment rectifying tower (2), be rich in ritalin, and a small amount of CH
3The overhead product of I and acetone is through condenser A(4) after the condensation, wherein part is as trim the top of column, and all the other send into the carbonylation reaction system as recycle stock; Acetone is after further enrichment at the bottom of the tower, by conveying pipeline B(5) enter azeotropic fractionation rectifying tower (6) from the middle part of azeotropic fractionation rectifying tower (6);
Describedly contain methyl acetate, CH from the oxo process system
3The low boiling mixture percent by weight of I, acetone and micro-acetic acid consists of: ritalin 50～65, CH
3I 20～50, acetone 4～12, and acetic acid 0.5～5, each component concentration sum is absolutely;
B. azeotropic separation acetone
From mixture flow at the bottom of acetone enrichment rectifying tower (2) tower, be fractionated in azeotropic fractionation rectifying tower (6), Skellysolve A and acetone azeotrope distillate from cat head, through condenser B(8) after the condensation, all enter two-chamber extraction overflow phase splitter (9), phase-splitting to be extracted; Materials at bottom of tower constantly is admitted to the utilization of carbonylation reaction systemic circulation;
C. extract phase-splitting
From the overhead product of step b, enter in the water extraction, phase-splitting chamber (14) of two-chamber extraction overflow phase splitter (9), mix with water from back with water inlet line (10), be extracted phase-splitting; Organic phase is crossed dividing plate (12) overflow and is entered back cavity (13), with enter the Skellysolve A that pipeline (11) adds from Skellysolve A and converge, enter azeotropic fractionation rectifying tower (6) by return line (15) total reflux, continue to carry out the task that azeotropic is taken acetone out of, lower layer of water is carried the acetone of dissolving and is sent into treatment and finishing section.
2. according to the device of removing acetone in the carbonyl synthesis process of acetic anhydride of claim 1, it is characterized in that the bottom still liquid temp of the rectifying tower of acetone enrichment described in the step a (2) remains on 55～65 ℃, 40～50 ℃ of top exhaust gas stream temperature.
3. according to the device of removing acetone in the carbonyl synthesis process of acetic anhydride of claim 1, it is characterized in that the trim the top of column ratio of the rectifying tower of acetone enrichment described in the step a (2) is controlled between 2.5:1～1.5:1.
4. according to the device of removing acetone in the carbonyl synthesis process of acetic anhydride of claim 1, it is characterized in that 50～60 ℃ of the bottom still liquid temps of azeotropic fractionation rectifying tower described in the step b (6), 30～40 ℃ of top exhaust gas temperatures.
5. according to the device of removing acetone in the carbonyl synthesis process of acetic anhydride of claim 1, it is characterized in that the phegma flow of described azeotropic fractionation rectifying tower (6) and the feed rate ratio of acetone enrichment rectifying tower (2) are 1:0.1～0.1:1.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4444624A (en) * | 1981-09-11 | 1984-04-24 | Hoechst Aktiengesellschaft | Process for separating acetone from carbonylation mixtures |
| US4717454A (en) * | 1981-12-11 | 1988-01-05 | Hoechst Aktiengesellschaft | Process for removing acetone from reaction mixtures of carbonylation reactions |
| CN1061400A (en) * | 1990-10-01 | 1992-05-27 | 伊斯曼柯达公司 | Acetone removal process |
| CN1069021A (en) * | 1991-06-12 | 1993-02-17 | 英国石油化学品有限公司 | From the mixture that contains acetone, methyl acetate and methyl-iodide, remove the method for acetone |
| CN1071412A (en) * | 1991-10-09 | 1993-04-28 | 伊斯曼柯达公司 | By the method for removing acetone in the carbonylation processes |
| CN1411432A (en) * | 1999-12-22 | 2003-04-16 | 伊斯曼化学公司 | Process for enhanced acetone removal from carbonylation processes |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2204357A1 (en) * | 2009-01-06 | 2010-07-07 | BP Chemicals Limited | Process for removing acetone from a stream comprising acetone, methyl acetate and methyl iodide |
-
2010
- 2010-07-20 CN CN 201010231131 patent/CN101870644B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4444624A (en) * | 1981-09-11 | 1984-04-24 | Hoechst Aktiengesellschaft | Process for separating acetone from carbonylation mixtures |
| US4717454A (en) * | 1981-12-11 | 1988-01-05 | Hoechst Aktiengesellschaft | Process for removing acetone from reaction mixtures of carbonylation reactions |
| CN1061400A (en) * | 1990-10-01 | 1992-05-27 | 伊斯曼柯达公司 | Acetone removal process |
| CN1069021A (en) * | 1991-06-12 | 1993-02-17 | 英国石油化学品有限公司 | From the mixture that contains acetone, methyl acetate and methyl-iodide, remove the method for acetone |
| CN1071412A (en) * | 1991-10-09 | 1993-04-28 | 伊斯曼柯达公司 | By the method for removing acetone in the carbonylation processes |
| CN1411432A (en) * | 1999-12-22 | 2003-04-16 | 伊斯曼化学公司 | Process for enhanced acetone removal from carbonylation processes |
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