CN1974500B - Serial trimethyl benzene separating apparatus and method - Google Patents
Serial trimethyl benzene separating apparatus and method Download PDFInfo
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- CN1974500B CN1974500B CN2006101304141A CN200610130414A CN1974500B CN 1974500 B CN1974500 B CN 1974500B CN 2006101304141 A CN2006101304141 A CN 2006101304141A CN 200610130414 A CN200610130414 A CN 200610130414A CN 1974500 B CN1974500 B CN 1974500B
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Abstract
The present invention relates to serial trimethyl benzene separating apparatus and method. The serial trimethyl benzene separating apparatus includes a pre-separating tower, a sym-trimethyl benzene tower and an unsym-trimethyl benzene tower, and features the condensator on the pre-separating tower connected to the outlet of the pre-separating tower, the reflux accumulator connected to the condensator and one vacuum unit, the reboiler in the bottom of the pre-separating tower connected between the outlet and the inlet of the sym-trimethyl benzene tower. The present invention adopts a serial three-tower process, can produce unsym-trimethyl benzene in purity over 99 % and sym-trimethyl benzene in purity over 35 % simultaneously in the yield over 90 % and power consumption 30 %-40 % lower than one normal pressure process.
Description
Technical field
The present invention relates to the fine chemistry industry separation technology field, specifically is serial trimethyl benzene separating apparatus and method.
Background technology
Carbon such as trimethylbenzene nine heavy aromaticss mainly come from refinery's reformer, and wherein unsym-trimethyl benzene and sym-trimethylbenzene are important fine chemical products, have very high added value.Wherein unsym-trimethyl benzene is of many uses as basic Organic Chemicals, is mainly used to isomerization and produces sym-trimethylbenzene, synthetic trimellitic acid 1,2-anhydride.With the enriched mesitylene is raw material, carries out catalytic alkylation reaction, can obtain the high purity sym-trimethylbenzene, and sym-trimethylbenzene can be used to produce 2,4,6-trimethylaniline, also can make dyestuff intermediate etc.
Domestic trimethylbenzene separation process adopts the normal pressure double-column process mostly, only produces unsym-trimethyl benzene, and a large amount of valuable sym-trimethylbenzene are used to do gasoline dope.Adopt three-column process flow under normal pressure, energy consumption is bigger, influences economic benefit.This is because each component of C9 aromatic hydrocarbons in the charging is a series of isomerss, boiling-point difference is little each other, want isolating sym-trimethylbenzene to have very much the component o-methylethylbenzene between the unsym-trimethyl benzene, wherein unsym-trimethyl benzene and o-methylethylbenzene boiling-point difference are 4.2 ℃, 0.5 ℃ of sym-trimethylbenzene and o-methylethylbenzene boiling-point difference, separating difficulty is big, and required each tower number of theoretical plate is more, and therefore the investment and the process cost of device are all higher.
Summary of the invention
Purpose of the present invention provides a kind of trimethylbenzene tripping device and method that cuts down the consumption of energy, and it adopts three tower serial process, presort tower and adopt negative-pressure operation, the sym-trimethylbenzene tower adopts normal pressure or pressurized operation, in production high purity unsym-trimethyl benzene, and the coproduction enriched mesitylene.
Technology of the present invention is as follows:
Serial trimethyl benzene separating apparatus of the present invention comprises through presorting tower 1, sym-trimethylbenzene tower 2 and unsym-trimethyl benzene tower 3; It is characterized in that presorting tower and be provided with condenser, a termination is presorted tower top outlet, and a termination return tank connects vacuum unit on the return tank.At the bottom of presorting tower reboiler 9 is set, two ends are connected with import with the sym-trimethylbenzene tower top outlet respectively.Sym-trimethylbenzene tower opening for feed with presort the tower bottom outlet and link to each other, unsym-trimethyl benzene tower opening for feed links to each other with sym-trimethylbenzene tower bottom outlet.
As required, the present invention can be provided with reboiler 16 again at the bottom of presorting tower, and two ends are connected with import with the unsym-trimethyl benzene tower top outlet respectively.
Concrete operation method of the present invention is: adopt serial trimethyl benzene separation method C9 aromatic raw material 4 after interchanger 5 heat exchange, enter and presort tower 1, it is presorted tower and adopts negative-pressure operation, cat head connects vacuum unit 8, the cat head gas phase enters return tank 7 behind condenser 6, phlegma partial reflux wherein, part is as lightnaphtha A extraction.The cat head gas phase of sym-trimethylbenzene tower 2 realizes thermal coupling as the thermal source of presorting tower bottom reboiler 9, and a cat head gaseous condensate part refluxes, a part is as the extraction of sym-trimethylbenzene product B, the bottoms material is behind reboiler 11, and a part is got back to the sym-trimethylbenzene tower, and another part enters unsym-trimethyl benzene tower 3.Unsym-trimethyl benzene cat head part phlegma is as the extraction of unsym-trimethyl benzene products C, extraction heavy naptha D at the bottom of the tower.
The present invention realizes thermal coupling presorting between tower and the sym-trimethylbenzene tower, as shown in Figure 1.
The present invention presorts pressure tower and is controlled at 30～80KPa, and tower top temperature is controlled at 100～160 ℃.The sym-trimethylbenzene pressure tower is controlled at 100～200KPa, and tower top temperature is controlled at 150～200 ℃.The unsym-trimethyl benzene pressure tower is controlled at 100～200KPa, and tower top temperature is controlled at 150～250 ℃.
Advantage of the present invention is:
(1) adopt three tower serial flow processs, the enriched mesitylene of coproduction purity more than 35% in the unsym-trimethyl benzene of production purity more than 99%, wherein the yield of unsym-trimethyl benzene and sym-trimethylbenzene is all more than 90%.
(1) adopt the differential pressure operation, the sym-trimethylbenzene tower adopts normal pressure or pressurization, presort tower and adopt decompression, with the cat head gas phase that reaches equal toluene tower as the thermal source of presorting tower bottom reboiler, the realization thermal coupling.
(2) the unsym-trimethyl benzene tower with presort tower and can carry out thermal coupling, also can not carry out thermal coupling.
(3) compare with the normal pressure flow process, unit consumption of energy can reduce by 30%～40%.
Description of drawings
Fig. 1: presort the trimethylbenzene separating technology figure that tower and sym-trimethylbenzene tower are realized thermal coupling
Fig. 2: presort the trimethylbenzene separating technology figure that all realizes thermal coupling between tower and sym-trimethylbenzene tower and the unsym-trimethyl benzene tower
1 for presorting tower, 2 is the sym-trimethylbenzene tower, and 3 is the unsym-trimethyl benzene tower, and 4 is the C9 aromatic feed, 5 is interchanger, 6 for presorting overhead condenser, and 7 is return tank, and 8 is vacuum unit, 9 for presorting tower bottom reboiler, 10 is sym-trimethylbenzene tower fresh feed pump, and 11 is the sym-trimethylbenzene tower bottom reboiler, and 12 is unsym-trimethyl benzene tower fresh feed pump, 13 is the unsym-trimethyl benzene tower bottom reboiler, 14 is the unsym-trimethyl benzene overhead condenser, and 15 is the unsym-trimethyl benzene return tank of top of the tower, and 16 are unsym-trimethyl benzene tower and presort interchanger between tower, A is a lightnaphtha, B is an enriched mesitylene, and C is a unsym-trimethyl benzene, and D is a heavy naptha.
Embodiment
Embodiment 1
Presort tower, sym-trimethylbenzene tower and unsym-trimethyl benzene tower and all adopt Sulzer packing.The thermal coupling process is shown as Fig. 2 for all realizing thermal coupling between tower and sym-trimethylbenzene tower and the unsym-trimethyl benzene tower presorting.C9 aromatic raw material 4 enters and presorts tower 1 after interchanger 5 heat exchange, and it is presorted tower and adopts the 30KPa operation, tower top temperature is controlled at 100 ℃, and cat head connects vacuum unit 8, and the cat head gas phase enters return tank 7 behind condenser 6, wherein the phlegma partial reflux partly goes out the battery limit (BL) as lightnaphtha A.The sym-trimethylbenzene pressure tower is controlled at 100KPa, tower top temperature is controlled at more than 150 ℃, make the cat head gas phase as the thermal source of presorting tower bottom reboiler 9, realize thermal coupling, a cat head gaseous condensate part refluxes, and a part goes out the battery limit (BL) as the sym-trimethylbenzene product B, and the bottoms material is behind reboiler 11, a part is got back to the sym-trimethylbenzene tower, and another part enters unsym-trimethyl benzene tower 3.The unsym-trimethyl benzene pressure tower is controlled at 100KPa, tower top temperature is controlled at more than 150 ℃, the most of gas phase of its cat head is as the thermal source of presorting interchanger 16 at the bottom of the tower, realize thermal coupling, a cat head gaseous condensate part refluxes, another part phlegma is as the extraction of unsym-trimethyl benzene products C, extraction heavy naptha D at the bottom of the tower.Gained unsym-trimethyl benzene purity reaches 99%, and yield is more than 90%, sym-trimethylbenzene purity 35%, and yield reaches 90%.
Embodiment 2
Presort tower, sym-trimethylbenzene tower and unsym-trimethyl benzene tower and all adopt Sulzer packing.The thermal coupling process is shown as Fig. 2 for all realizing thermal coupling between tower and sym-trimethylbenzene tower and the unsym-trimethyl benzene tower presorting.C9 aromatic raw material 4 enters and presorts tower 1 after interchanger 5 heat exchange, and it is presorted tower and adopts the 50KPa operation, tower top temperature is controlled at 130 ℃, and cat head connects vacuum unit 8, and the cat head gas phase enters return tank 7 behind condenser 6, wherein the phlegma partial reflux partly goes out the battery limit (BL) as lightnaphtha A.The sym-trimethylbenzene pressure tower is controlled at 120KPa, tower top temperature is controlled at about 170 ℃, make the cat head gas phase as the thermal source of presorting tower bottom reboiler 9, realize thermal coupling, a cat head gaseous condensate part refluxes, and a part goes out the battery limit (BL) as the sym-trimethylbenzene product B, and the bottoms material is behind reboiler 11, a part is got back to the sym-trimethylbenzene tower, and another part enters unsym-trimethyl benzene tower 3.The unsym-trimethyl benzene pressure tower is controlled at 110KPa, tower top temperature is controlled at about 170 ℃, the most of gas phase of its cat head is as the thermal source of presorting interchanger 16 at the bottom of the tower, realize thermal coupling, a cat head gaseous condensate part refluxes, another part phlegma is as the extraction of unsym-trimethyl benzene products C, extraction heavy naptha D at the bottom of the tower.Gained unsym-trimethyl benzene purity reaches 99%, and yield is more than 90%, sym-trimethylbenzene purity 35%, and yield reaches 90%.
Embodiment 3
Presort tower, sym-trimethylbenzene tower and unsym-trimethyl benzene tower and all adopt Sulzer packing.The thermal coupling process is shown as Fig. 2 for all realizing thermal coupling between tower and sym-trimethylbenzene tower and the unsym-trimethyl benzene tower presorting.C9 aromatic raw material 4 enters and presorts tower 1 after interchanger 5 heat exchange, and it is presorted tower and adopts the 80KPa operation, tower top temperature is controlled at 160 ℃, and cat head connects vacuum unit 8, and the cat head gas phase enters return tank 7 behind condenser 6, wherein the phlegma partial reflux partly goes out the battery limit (BL) as lightnaphtha A.The sym-trimethylbenzene pressure tower is controlled at 160KPa, tower top temperature is controlled at 185 ℃, make the cat head gas phase as the thermal source of presorting tower bottom reboiler 9, realize thermal coupling, a cat head gaseous condensate part refluxes, and a part goes out the battery limit (BL) as the sym-trimethylbenzene product B, and the bottoms material is behind reboiler 11, a part is got back to the sym-trimethylbenzene tower, and another part enters unsym-trimethyl benzene tower 3.The unsym-trimethyl benzene pressure tower is controlled at 200KPa, tower top temperature is controlled at 250 ℃, the most of gas phase of its cat head is as the thermal source of presorting interchanger 16 at the bottom of the tower, realize thermal coupling, a cat head gaseous condensate part refluxes, another part phlegma is as the extraction of unsym-trimethyl benzene products C, extraction heavy naptha D at the bottom of the tower.Gained unsym-trimethyl benzene purity reaches 99%, and yield is more than 90%, sym-trimethylbenzene purity 35%, and yield reaches 90%.
Presort tower, sym-trimethylbenzene tower and unsym-trimethyl benzene tower and all adopt Sulzer packing, realize thermal coupling presorting between tower and the sym-trimethylbenzene tower, as shown in Figure 1.C9 aromatic raw material 4 enters and presorts tower 1 after interchanger 5 heat exchange, and it is presorted tower and adopts the 30KPa operation, tower top temperature is controlled at 100 ℃, and cat head connects vacuum unit 8, and the cat head gas phase enters return tank 7 behind condenser 6, wherein the phlegma partial reflux partly goes out the battery limit (BL) as lightnaphtha A.The sym-trimethylbenzene pressure tower is controlled at 120KPa, tower top temperature is controlled at 165 ℃, make the cat head gas phase as the thermal source of presorting tower bottom reboiler 9, realize thermal coupling, a cat head gaseous condensate part refluxes, and a part goes out the battery limit (BL) as the sym-trimethylbenzene product B, and the bottoms material is behind reboiler 11, a part is got back to the sym-trimethylbenzene tower, and another part enters unsym-trimethyl benzene tower 3.The unsym-trimethyl benzene pressure tower is controlled at 100KPa, and tower top temperature is controlled at 170 ℃, and its cat head gas phase enters return tank 15 through condenser 14, and a part of phlegma refluxes, and another part phlegma is as the extraction of unsym-trimethyl benzene products C, extraction heavy naptha D at the bottom of the tower.Gained unsym-trimethyl benzene purity reaches 99%, and yield is more than 90%, sym-trimethylbenzene purity 35%, and yield reaches 90%.
Presort tower, sym-trimethylbenzene tower and unsym-trimethyl benzene tower and all adopt Sulzer packing, realize thermal coupling presorting between tower and the sym-trimethylbenzene tower, as shown in Figure 1.C9 aromatic raw material 4 enters and presorts tower 1 after interchanger 5 heat exchange, and it is presorted tower and adopts the 50KPa operation, tower top temperature is controlled at 130 ℃, and cat head connects vacuum unit 8, and the cat head gas phase enters return tank 7 behind condenser 6, wherein the phlegma partial reflux partly goes out the battery limit (BL) as lightnaphtha A.The sym-trimethylbenzene pressure tower is controlled at 120KPa, tower top temperature is controlled at 172 ℃, make the cat head gas phase as the thermal source of presorting tower bottom reboiler 9, realize thermal coupling, a cat head gaseous condensate part refluxes, and a part goes out the battery limit (BL) as the sym-trimethylbenzene product B, and the bottoms material is behind reboiler 11, a part is got back to the sym-trimethylbenzene tower, and another part enters unsym-trimethyl benzene tower 3.The unsym-trimethyl benzene pressure tower is controlled at 100KPa, and tower top temperature is controlled at 170 ℃, and its cat head gas phase enters return tank 15 through condenser 14, and a part of phlegma refluxes, and another part phlegma is as the extraction of unsym-trimethyl benzene products C, extraction heavy naptha D at the bottom of the tower.Gained unsym-trimethyl benzene purity reaches 99%, and yield is more than 90%, sym-trimethylbenzene purity 35%, and yield reaches 90%.
Embodiment 6
Presort tower, sym-trimethylbenzene tower and unsym-trimethyl benzene tower and all adopt Sulzer packing, realize thermal coupling presorting between tower and the sym-trimethylbenzene tower, as shown in Figure 1.C9 aromatic raw material 4 enters and presorts tower 1 after interchanger 5 heat exchange, and it is presorted tower and adopts the 80KPa operation, tower top temperature is controlled at 150 ℃, and cat head connects vacuum unit 8, and the cat head gas phase enters return tank 7 behind condenser 6, wherein the phlegma partial reflux partly goes out the battery limit (BL) as lightnaphtha A.The sym-trimethylbenzene pressure tower is controlled at about 200KPa, tower top temperature is controlled at 200 ℃, make the cat head gas phase as the thermal source of presorting tower bottom reboiler 9, realize thermal coupling, a cat head gaseous condensate part refluxes, and a part goes out the battery limit (BL) as the sym-trimethylbenzene product B, and the bottoms material is behind reboiler 11, a part is got back to the sym-trimethylbenzene tower, and another part enters unsym-trimethyl benzene tower 3.The unsym-trimethyl benzene pressure tower is controlled at 100KPa, and tower top temperature is controlled at 170 ℃, and its cat head gas phase enters return tank 15 through condenser 14, and a part of phlegma refluxes, and another part phlegma is as the extraction of unsym-trimethyl benzene products C, extraction heavy naptha D at the bottom of the tower.Gained unsym-trimethyl benzene purity reaches 99%, and yield is more than 90%, sym-trimethylbenzene purity 35%, and yield reaches 90%.
A kind of serial trimethyl benzene separating apparatus and method that the present invention proposes, be described by embodiment, person skilled obviously can be changed or suitably change and combination content as herein described in not breaking away from content of the present invention, spirit and scope, realizes the present invention.Special needs to be pointed out is, the replacement that all are similar and change apparent to those skilled in the artly, they are regarded as being included in the utility model spirit, scope and the content.
Claims (5)
1. a serial trimethyl benzene separating apparatus comprises and presorts tower (1), sym-trimethylbenzene tower (2) and unsym-trimethyl benzene tower (3); It is characterized in that presorting tower and be provided with condenser, a termination is presorted tower top outlet, and a termination return tank connects vacuum unit on the return tank; At the bottom of presorting tower reboiler (9) is set, two ends are connected with import with the sym-trimethylbenzene tower top outlet respectively; Sym-trimethylbenzene tower opening for feed with presort the tower bottom outlet and link to each other, unsym-trimethyl benzene tower opening for feed links to each other with sym-trimethylbenzene tower bottom outlet.
2. the working method of serial trimethyl benzene separating apparatus as claimed in claim 1, it is characterized in that adopting the serial trimethyl benzene separation method, C9 aromatic raw material (4) is after interchanger (5) heat exchange, enter and presort tower (1), it is presorted tower and adopts negative-pressure operation, and cat head connects vacuum unit (8), and the cat head gas phase enters return tank (7) behind condenser (6), phlegma partial reflux wherein, part is as lightnaphtha (A) extraction; The cat head gas phase of sym-trimethylbenzene tower (2) is as presorting the thermal source of tower bottom reboiler (9), realize thermal coupling, a cat head gaseous condensate part refluxes, a part is as sym-trimethylbenzene product (B) extraction, the bottoms material is behind reboiler (11), a part is got back to the sym-trimethylbenzene tower, and another part enters unsym-trimethyl benzene tower (3); Unsym-trimethyl benzene cat head part phlegma is as unsym-trimethyl benzene product (C) extraction, extraction heavy naptha (D) at the bottom of the tower.
3. method according to claim 2 is characterized in that: presort pressure tower and be controlled at 30～80KPa, tower top temperature is controlled at 100～160 ℃.
4. method according to claim 2 is characterized in that: the sym-trimethylbenzene pressure tower is controlled at 100～200KPa, and tower top temperature is controlled at 150～200 ℃.
5. method according to claim 2 is characterized in that: the unsym-trimethyl benzene pressure tower is controlled at 100～200KPa, and tower top temperature is controlled at 150～250 ℃.
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| CN2006101304141A CN1974500B (en) | 2006-12-20 | 2006-12-20 | Serial trimethyl benzene separating apparatus and method |
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| CN2006101304141A CN1974500B (en) | 2006-12-20 | 2006-12-20 | Serial trimethyl benzene separating apparatus and method |
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| CN102580338B (en) * | 2012-02-23 | 2014-04-16 | 淄博市临淄齐泉工贸有限公司 | Method for continuously rectifying 3-chloropropyl triethoxysilane |
| CN104591952A (en) * | 2014-12-25 | 2015-05-06 | 天津大学 | Method for refining mesitylene by virtue of differential pressure thermal coupling rectification |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1557793A (en) * | 2004-02-06 | 2004-12-29 | 抚顺石油化工设计院 | Separation process for 1,2,3-trimethylbenzene |
| CN1569781A (en) * | 2004-04-29 | 2005-01-26 | 天津天大天久科技股份有限公司 | Method and device for separating 1,2,3-trimethylbenzene |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1557793A (en) * | 2004-02-06 | 2004-12-29 | 抚顺石油化工设计院 | Separation process for 1,2,3-trimethylbenzene |
| CN1569781A (en) * | 2004-04-29 | 2005-01-26 | 天津天大天久科技股份有限公司 | Method and device for separating 1,2,3-trimethylbenzene |
Non-Patent Citations (2)
| Title |
|---|
| 张卫江 王文喜等.均三甲苯生产与分离技术新进展.化学工业与工程19 3.2002,19(3),265-270. * |
| 杨智生.重整重芳烃中偏三甲苯的分离和利用.辽宁化工 3.1987,(3),42-44. * |
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