CN1250493C - Separation process for 1,2,3-trimethylbenzene - Google Patents
Separation process for 1,2,3-trimethylbenzene Download PDFInfo
- Publication number
- CN1250493C CN1250493C CN 200410021117 CN200410021117A CN1250493C CN 1250493 C CN1250493 C CN 1250493C CN 200410021117 CN200410021117 CN 200410021117 CN 200410021117 A CN200410021117 A CN 200410021117A CN 1250493 C CN1250493 C CN 1250493C
- Authority
- CN
- China
- Prior art keywords
- unsym
- trimethyl benzene
- removing column
- lightness
- tower
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- 238000000926 separation method Methods 0.000 title description 5
- FYGHSUNMUKGBRK-UHFFFAOYSA-N 1,2,3-trimethylbenzene Chemical compound CC1=CC=CC(C)=C1C FYGHSUNMUKGBRK-UHFFFAOYSA-N 0.000 title 2
- 239000000463 material Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 238000010992 reflux Methods 0.000 claims abstract description 6
- 239000000470 constituent Substances 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000012856 packing Methods 0.000 claims description 10
- 241000282326 Felis catus Species 0.000 claims description 8
- 239000000945 filler Substances 0.000 claims description 8
- 230000000994 depressogenic effect Effects 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 239000007791 liquid phase Substances 0.000 claims description 4
- 238000000605 extraction Methods 0.000 claims description 3
- 239000012071 phase Substances 0.000 claims description 3
- 239000000758 substrate Substances 0.000 claims description 3
- 238000009826 distribution Methods 0.000 claims description 2
- 238000005265 energy consumption Methods 0.000 abstract description 4
- GWHJZXXIDMPWGX-UHFFFAOYSA-N 1,2,4-trimethylbenzene Chemical compound CC1=CC=C(C)C(C)=C1 GWHJZXXIDMPWGX-UHFFFAOYSA-N 0.000 abstract 14
- SRPWOOOHEPICQU-UHFFFAOYSA-N trimellitic anhydride Chemical compound OC(=O)C1=CC=C2C(=O)OC(=O)C2=C1 SRPWOOOHEPICQU-UHFFFAOYSA-N 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 6
- 239000003599 detergent Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 2
- 125000003118 aryl group Chemical group 0.000 description 2
- 238000006317 isomerization reaction Methods 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- ARCGXLSVLAOJQL-UHFFFAOYSA-N trimellitic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C(C(O)=O)=C1 ARCGXLSVLAOJQL-UHFFFAOYSA-N 0.000 description 2
- AUHZEENZYGFFBQ-UHFFFAOYSA-N 1,3,5-trimethylbenzene Chemical compound CC1=CC(C)=CC(C)=C1 AUHZEENZYGFFBQ-UHFFFAOYSA-N 0.000 description 1
- AUFZRCJENRSRLY-UHFFFAOYSA-N 2,3,5-trimethylhydroquinone Chemical compound CC1=CC(O)=C(C)C(C)=C1O AUFZRCJENRSRLY-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 150000008065 acid anhydrides Chemical class 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000001833 catalytic reforming Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000007323 disproportionation reaction Methods 0.000 description 1
- SQNZJJAZBFDUTD-UHFFFAOYSA-N durene Chemical compound CC1=CC(C)=C(C)C=C1C SQNZJJAZBFDUTD-UHFFFAOYSA-N 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention discloses a technological method for separating pseudocumene, which has the characteristics of high purity of separated products and low energy consumption of devices. The present invention comprises a feed preheater for a light end removing column, a light end removing column, a reboiler arranged at the bottom of the light end removing column, a pseudocumene column, a heat exchanger and a machine pump, wherein the heat of a raw material is exchanged to the bubble point temperature after pressure of the raw material is boosted to enter the light end removing column, UT-SW high-efficiency filling materials are used by all the filling materials of the light end removing column operated by negative pressure, the gas phase of the top of the light end removing column is condensed to the bubble point temperature via an air cooler of the light end removing column, one part of the gas phase is used as back flow, the other part of the gas phase is flowed out of a boundary zone after the other part of the gas phase is cooled as a light component, the material at the bottom of the light end removing column enters a pseudocumene column via a feed pump for the pseudocumene column, UT-SW high-efficiency filling materials are used by all the filling materials of the pseudocumene column operated by pressurization, the most part of column top oil gas is used as a heat source of the reboiler arranged at the bottom of the light end removing column and is automatically pressed in a reflux tank arranged on the top of the pseudocumene column, and a part of the column top oil gas is used as pseudocumene products.
Description
Technical field:
The present invention relates to chemical technology field, exactly it is the processing method of separating unsym-trimethyl benzene in a kind of heavy aromatics.
Background technology:
Unsym-trimethyl benzene (1,2,4-Three methyl Benzene) is a kind of important Organic Chemicals, is mainly derived from the heavy aromatics of catalytic reforming.Unsym-trimethyl benzene is of many uses as basic Organic Chemicals, and derived product is a lot, and added value is higher.The unsym-trimethyl benzene main application is as follows: synthetic trimellitic acid and trimellitic acid 1,2-anhydride; Sym-trimethylbenzene is produced in isomerization; Durol is produced in disproportionation and isomerization; Synthon 2,3,5-Trimethylhydroquinone.Wherein, the synthetic trimellitic acid 1,2-anhydride of unsym-trimethyl benzene becomes the unsym-trimethyl benzene main application, state, inside and outside with 20% rate of growth demand trimellitic acid 1,2-anhydride, very high (general requirement purity is more than 98.5% because synthetic trimellitic acid 1,2-anhydride is to the unsym-trimethyl benzene purity requirement, now domestic basic import unsym-trimethyl benzene is produced trimellitic acid 1,2-anhydride), therefore produce the high unsym-trimethyl benzene of purity, significant to further production trimellitic acid 1,2-anhydride.
Produce unsym-trimethyl benzene both at home and abroad, all from carbon nine heavy aromaticss, separate, separate back gained unsym-trimethyl benzene and do not contain alkene, good stability.The separation and the application of domestic unsym-trimethyl benzene are started in the seventies, Nanjing, Nanjing petrochemical corporation (complex) takes the lead in building up the heavy aromatics comprehensive utilization device in nineteen eighty-two, isolate unsym-trimethyl benzene, original design production unsym-trimethyl benzene 100t/a can produce unsym-trimethyl benzene 600t/a after the transformation.Nanjing, Nanjing petrochemical corporation (complex) newly built up the new device of a cover unsym-trimethyl benzene throughput 20000t/a in 2000.The separation of domestic unsym-trimethyl benzene is generally produced with order separation, micro-pressure operation, product purity the highest by 98.5% (WT).Domestic unsym-trimethyl benzene throughput is as follows:
Domestic unsym-trimethyl benzene throughput of table 3.1 and technology
| Manufacturer | Throughput (t/a) | Output (t) | Production technology | Product purity % (wt) |
| Jinling Petrochemical Co. | 20000 | 1800 | Order is separated, micro-pressure operation | 98.2 |
| Liaoyang quintessence company | 4000 | 2200 | The same | 98 |
| Jinzhou Tianyuan company | 8700 | 5600 | The same | 98.2 |
Find out from above data, the tripping device of existing unsym-trimethyl benzene all employing separate in proper order, micro-pressure operation, product yield is generally 70%, product purity is generally 98%.Material purity as trimellitic acid 1,2-anhydride is not enough, and general requirement purity is more than 98.5 (wt).Cause the existing unsym-trimethyl benzene can not be as the raw material of trimellitic acid 1,2-anhydride, the tripping device energy consumption of existing unsym-trimethyl benzene be higher (generally 610.56 * 10 simultaneously
4The kcal/t unsym-trimethyl benzene).
From as can be seen above, in the past technology all employing separate in proper order, micro-pressure operation, cause unsym-trimethyl benzene purity low, the energy consumption height, product yield is low.Its structure mainly has following characteristics:
A) adopt common plate ripple packing or valve tray.
B) lightness-removing column and unsym-trimethyl benzene tower adopt micro-pressure operation, and cat head is all used the low-temperature receiver condensation.
Summary of the invention:
The object of the invention provides the processing method of separating unsym-trimethyl benzene in a kind of heavy aromatics, it adopts the continuous rectification technology, the order cutting and separating obtains light aromatic hydrocarbon oil cut, unsym-trimethyl benzene and heavy aromatics cut, adopt heavy duty detergent UT-SW filler and proprietary liquid distributor, make the tower pressure drop reduce, thereby reduce tower still temperature, reduce energy expenditure.Mainly contain following characteristics on the structure:
A) adopt heavy duty detergent UT-SW filler and proprietary liquid distributor;
B) lightness-removing column adopts negative-pressure operation, increases relative volatilities light, heavy constituent;
C) the unsym-trimethyl benzene tower adopts pressurized operation, simultaneously unsym-trimethyl benzene cat head oil gas as the lightness-removing column tower at the bottom of thermal source, make full use of heat;
D) control the DCS system that adopts automatically, operator can implement full-automatic, semi-automatic to device and the manual operation supervision by the DCS system, and can realize the automatic control to technological operation.
E) the bubble point temperature charging is adopted in the lightness-removing column charging, avoids the filler decrease in efficiency.
It comprises lightness-removing column feed preheater (3), lightness-removing column (4), vacuum pump (7), reboiler at the bottom of the lightness-removing column (8), unsym-trimethyl benzene tower (12), a series of interchanger, pump, jar, it is characterized in that: raw material is after battery limit (BL) feedstock pump (1) boosts, enter lightness-removing column (4) with hot water heat exchanger (3) heat exchange to bubble point temperature, it is 8 sections that the lightness-removing column filler is divided into, all adopt the UT-SW high efficiency packing, lightness-removing column adopts negative-pressure operation, lightness-removing column top gas phase is condensed to bubble point temperature through lightness-removing column head space cooler (5), a part is as refluxing, another part goes out the battery limit (BL) after cooling off as light constituent, lightness-removing column substrate material through unsym-trimethyl benzene tower fresh feed pump (11) to unsym-trimethyl benzene tower (12), the unsym-trimethyl benzene tower packing is divided into 6 sections, all adopt the UT-SW high efficiency packing, the unsym-trimethyl benzene tower adopts pressurized operation, overhead oil most of thermal source as reboiler at the bottom of the lightness-removing column (8) of drawing last breath is depressed into unsym-trimethyl benzene return tank of top of the tower (13) voluntarily after heat exchange; Another small portion oil gas is depressed into unsym-trimethyl benzene return tank of top of the tower (13) voluntarily after unsym-trimethyl benzene cat head water cooler (14) heat exchange, liquid phase is through unsym-trimethyl benzene trim the top of column pump (17) output in the unsym-trimethyl benzene return tank of top of the tower, and a part refluxes as the unsym-trimethyl benzene tower; A part is as the unsym-trimethyl benzene product, after unsym-trimethyl benzene water cooler (18) cooling to the battery limit (BL); Unsym-trimethyl benzene bottoms material after unsym-trimethyl benzene tower still extraction pump (16) pressurization, is cooled to 40 ℃ through heavy constituent water cooler (19), to the battery limit (BL) as heavy constituent.Said lightness-removing column, pressure-controlling are at 0.01～0.09MPa (A), and tower top temperature is controlled at 80～180 ℃.Said unsym-trimethyl benzene tower, pressure-controlling are at 0.12～0.5MPa (A), and tower top temperature is controlled at 160～250 ℃.Utilize unsym-trimethyl benzene column overhead oil gas as the lightness-removing column reboiler.Said two towers all adopt UT-SW high efficiency packing and special distribution device.
Advantage of the present invention is:
(1) lightness-removing column adopts negative-pressure operation, increases relative volatilities light, heavy constituent;
(2) the unsym-trimethyl benzene tower adopts pressurized operation, simultaneously unsym-trimethyl benzene cat head oil gas as the lightness-removing column tower at the bottom of thermal source, make full use of heat;
(3) adopt heavy duty detergent UT-SW filler and proprietary liquid distributor, reduce the packing tower height;
(4) the bubble point temperature charging is adopted in the lightness-removing column charging, avoids the filler decrease in efficiency;
(5) the unsym-trimethyl benzene product purity reaches more than 99%, meets as inclined to one side acid anhydride ingredient requirement;
(6) the unsym-trimethyl benzene rate of recovery is more than 90%;
(7) plant energy consumption is 365.94 * 10
4The kcal/t unsym-trimethyl benzene, for the whole nation minimum.
Description of drawings:
Fig. 1 is a process flow sheet of the present invention.
As shown in the figure: the 1st, C9 aromatic raw material, the 2nd, lightness-removing column fresh feed pump, the 3rd, lightness-removing column feed preheater, the 4th, lightness-removing column, the 5th, lightness-removing column head space cooler, the 6th, lightness-removing column top return tank, the 7th, vacuum pump, the 8th, reboiler at the bottom of the lightness-removing column, the 9th, lightness-removing column top pump, the 10th, light constituent water cooler, the 11st, pump at the bottom of the lightness-removing column, the 12nd, unsym-trimethyl benzene tower, the 13rd, unsym-trimethyl benzene return tank of top of the tower, the 14th, unsym-trimethyl benzene overhead condenser, the 15th, the unsym-trimethyl benzene tower bottom reboiler, the 16th, unsym-trimethyl benzene column bottoms pump, the 17th, unsym-trimethyl benzene cat head pump, the 18th, unsym-trimethyl benzene reactor product cooler, the 19th, the heavy constituent water cooler, the 20th, light constituent, the 22nd, heavy constituent, the 23rd, unsym-trimethyl benzene.
Embodiment:
40 ℃ C9 aromatic after hot water heat exchanger 3 heat exchange to 132 ℃, enters the 3rd section filler of lightness-removing column 4 after the battery limit (BL) is boosted by feedstock pump 1.Lightness-removing column top gas phase is cooled to 115 ℃ through lightness-removing column head space cooler 5, enters lightness-removing column top return tank 6.Non-condensable gas in the return tank of lightness-removing column top enters atmosphere through vacuum pump 7, and the control tower top pressure is 0.04MPaA.A liquid phase part is as the backflow of lightness-removing column in the return tank of lightness-removing column top, a part as the light constituent product through light constituent water cooler 10 to the battery limit (BL).Lightness-removing column substrate material through unsym-trimethyl benzene tower fresh feed pump 11 to unsym-trimethyl benzene tower 12, a cat head oil gas part as lightness-removing column at the bottom of the thermal source of reboiler 8, after heat exchange from being depressed into unsym-trimethyl benzene return tank of top of the tower 13; Another part oil gas is depressed into unsym-trimethyl benzene return tank of top of the tower 13 certainly after 14 heat exchange of unsym-trimethyl benzene cat head water cooler, this part oil gas is that the control tower top pressure is 0.20MPaA as adjusting unsym-trimethyl benzene tower top pressure.Liquid phase is through 17 outputs of unsym-trimethyl benzene trim the top of column pump in the unsym-trimethyl benzene return tank of top of the tower, and a part refluxes as the unsym-trimethyl benzene tower; A part is as the unsym-trimethyl benzene product, after unsym-trimethyl benzene water cooler 18 cooling to the battery limit (BL).Unsym-trimethyl benzene bottoms material after 16 pressurizations of unsym-trimethyl benzene tower still extraction pump, is cooled to 40 ℃ through heavy constituent water cooler 19, to the battery limit (BL) as heavy constituent.
Claims (5)
1, the isolating method of unsym-trimethyl benzene, it comprises lightness-removing column feed preheater (3), lightness-removing column (4), vacuum pump (7), reboiler at the bottom of the lightness-removing column (8), unsym-trimethyl benzene tower (12), a series of interchanger, pump, jar, it is characterized in that: raw material is after battery limit (BL) feedstock pump (1) boosts, enter lightness-removing column (4) with hot water heat exchanger (3) heat exchange to bubble point temperature, it is 8 sections that the lightness-removing column filler is divided into, all adopt the UT-SW high efficiency packing, lightness-removing column adopts negative-pressure operation, lightness-removing column top gas phase is condensed to bubble point temperature through lightness-removing column head space cooler (5), a part is as refluxing, another part goes out the battery limit (BL) after cooling off as light constituent, lightness-removing column substrate material through unsym-trimethyl benzene tower fresh feed pump (11) to unsym-trimethyl benzene tower (12), the unsym-trimethyl benzene tower packing is divided into 6 sections, all adopt the UT-SW high efficiency packing, the unsym-trimethyl benzene tower adopts pressurized operation, overhead oil most of thermal source as reboiler at the bottom of the lightness-removing column (8) of drawing last breath, and is depressed into unsym-trimethyl benzene return tank of top of the tower (13) after heat exchange voluntarily; Another small portion oil gas is depressed into unsym-trimethyl benzene return tank of top of the tower (13) voluntarily after unsym-trimethyl benzene cat head water cooler (14) heat exchange, liquid phase is through unsym-trimethyl benzene trim the top of column pump (17) output in the unsym-trimethyl benzene return tank of top of the tower, and a part refluxes as the unsym-trimethyl benzene tower; A part is as the unsym-trimethyl benzene product, after unsym-trimethyl benzene water cooler (18) cooling to the battery limit (BL); Unsym-trimethyl benzene bottoms material after unsym-trimethyl benzene tower still extraction pump (16) pressurization, is cooled to 40 ℃ through heavy constituent water cooler (19), to the battery limit (BL) as heavy constituent.
2, the isolating method of unsym-trimethyl benzene according to claim 1 is characterized in that: the lightness-removing column pressure-controlling is at 0.01～0.09MPa, and tower top temperature is controlled at 80～180 ℃.
3, the isolating method of unsym-trimethyl benzene according to claim 1, it is characterized in that: the unsym-trimethyl benzene pressure tower is controlled at 0.12～0.5MPa, and tower top temperature is controlled at 160～250 ℃.
4, the isolating method of unsym-trimethyl benzene according to claim 1 is characterized in that: utilize unsym-trimethyl benzene column overhead oil gas as the lightness-removing column reboiler.
5, the isolating method of unsym-trimethyl benzene according to claim 1 is characterized in that: lightness-removing column and unsym-trimethyl benzene tower all adopt UT-SW high efficiency packing and special distribution device.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410021117 CN1250493C (en) | 2004-02-06 | 2004-02-06 | Separation process for 1,2,3-trimethylbenzene |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410021117 CN1250493C (en) | 2004-02-06 | 2004-02-06 | Separation process for 1,2,3-trimethylbenzene |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1557793A CN1557793A (en) | 2004-12-29 |
| CN1250493C true CN1250493C (en) | 2006-04-12 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200410021117 Expired - Lifetime CN1250493C (en) | 2004-02-06 | 2004-02-06 | Separation process for 1,2,3-trimethylbenzene |
Country Status (1)
| Country | Link |
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| CN (1) | CN1250493C (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1974500B (en) * | 2006-12-20 | 2010-08-18 | 天津大学 | Serial trimethyl benzene separating apparatus and method |
| CN101768467B (en) * | 2010-01-26 | 2013-05-08 | 天津大学 | Device and process for separation and purification of methanol synthetic oil containing high-content aromatic hydrocarbon |
| CN101787306B (en) * | 2010-01-26 | 2012-10-10 | 天津大学 | Method and device for refining methanol synthetic oil |
| CN102304011B (en) * | 2011-07-22 | 2013-09-11 | 江苏正丹化学工业股份有限公司 | Method for producing 1,2,4-trimethylbenzene by C9 aromatic hydrocarbon isomerization |
| CN107056577A (en) * | 2016-12-05 | 2017-08-18 | 长沙博能科技股份有限公司 | The technique of pseudocumene in a kind of next door tower heat pump distillation separation C9 aromatic |
| CN111057572A (en) * | 2019-12-09 | 2020-04-24 | 盘锦锦阳化工有限公司 | Connecting structure of light component removing tower |
-
2004
- 2004-02-06 CN CN 200410021117 patent/CN1250493C/en not_active Expired - Lifetime
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| Publication number | Publication date |
|---|---|
| CN1557793A (en) | 2004-12-29 |
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