阅读说明：本技术 一种偏苯三酸三辛酯残液中辛醇的提取装置和方法 (Device and method for extracting octanol from trioctyl trimellitate residual liquid ) 是由 蒋国强 吴晓明 黄小磊 丁书平 王忠法 万鹏 周国君 陶植 邹淼 于 2020-06-24 设计创作，主要内容包括：本发明涉及有机化工技术领域,具体公开了一种偏苯三酸三辛酯残液中辛醇的提取装置和方法,包括脱重塔、脱重塔进料预热器、脱重塔再沸器、脱重塔一级冷凝器、脱重塔二级冷凝器、脱重塔冷凝液罐、脱轻塔进料预热器、脱轻塔再沸器、脱轻塔一级冷凝器、脱轻塔二级冷凝器、脱轻塔回流罐和脱轻塔,通过脱重塔将粗品提出,冷凝后再进入脱轻塔,通过脱轻塔进一步提出精品,本发明操作简单,通过连续进料,能够回收高含量的辛醇进行回用,减少了偏苯三酸三辛酯生产的物耗,同时减少了偏苯三酸三辛酯生产过程中废液的产生量,有利于环保。(The invention relates to the technical field of organic chemical industry, and particularly discloses a device and a method for extracting octanol from trioctyl trimellitate residual liquid.)

1. The utility model provides an extraction element of octanol in trioctyl trimellitate raffinate which characterized in that: comprises a heavy component removal tower (1), a heavy component removal tower feeding preheater (2), a heavy component removal tower reboiler (3), a heavy component removal tower first-stage condenser (5), a heavy component removal tower second-stage condenser (6), a heavy component removal tower condensate tank (7), a light component removal tower feeding preheater (9), a light component removal tower reboiler (10), a light component removal tower first-stage condenser (12), a light component removal tower second-stage condenser (13), a light component removal tower reflux tank (14) and a light component removal tower (16),

a feed inlet on the left side of the de-weighting tower (1) is connected with a discharge outlet on the top end of the de-weighting tower feed preheater (2), and a trioctyl trimellitate residual liquid feed inlet containing octanol is formed in the bottom end of the de-weighting tower feed preheater (2);

a feed inlet at the lower part of the right side of the heavy component removal tower (1) is connected with an outlet at the bottom end of the heavy component removal tower reboiler (3), and an inlet at the top end of the heavy component removal tower reboiler (3) is connected with a residual liquid discharge outlet at the bottom end of the heavy component removal tower (1) through a heavy component removal tower bottom circulating pump (401); a pipeline between a raffinate discharge hole at the bottom end of the de-heavy tower (1) and a de-heavy tower bottom circulating pump (401) is connected with a de-heavy tower bottom waste liquid extraction pump (402);

the gas-phase crude octanol discharge port at the top end of the de-weighting tower (1) is connected with the inlet at the left top of the first-stage condenser (5) of the de-weighting tower, the gas-phase outlet at the right top of the first-stage condenser (5) of the de-weighting tower is connected with the inlet at the left top of the second-stage condenser (6) of the de-weighting tower, and the outlet at the bottom end of the first-stage condenser (5) of the de-weighting tower and the outlet at the bottom end of the second-stage condenser (6) of the de-weighting tower are connected in parallel to the octanol;

a crude product condensate outlet at the lower part of the right side of the heavy component removal tower condensate tank (7) is connected with an inlet at the bottom of the light component removal tower feed preheater (9) through a light component removal tower feed pump (802); an outlet at the top of the light component removal tower feeding preheater (9) is connected with a feeding hole at the lower part of the left side of the light component removal tower (16);

the gas-phase refined octanol discharge port at the top end of the lightness-removing tower (16) is connected with the inlet at the left top of the first-stage condenser (12) of the lightness-removing tower, the outlet at the right top of the first-stage condenser (12) of the lightness-removing tower is connected with the inlet at the left top of the second-stage condenser (13) of the lightness-removing tower, and the outlet at the bottom end of the first-stage condenser (12) of the lightness-removing tower and the outlet at the bottom end of the second-stage condenser (13) of the lightness-removing tower are connected in parallel to the liquid-phase;

a feed inlet at the lower part of the right side of the lightness-removing column (16) is connected with an outlet at the bottom end of the lightness-removing column reboiler (10), and an inlet at the top end of the lightness-removing column reboiler (10) is connected with a discharge outlet of raffinate at the bottom end of the lightness-removing column (16) through a circulation pump (1101) at the bottom of the lightness-removing column; a pipeline between a residual liquid discharge port at the bottom end of the lightness-removing tower (16) and a circulation pump (1101) at the bottom of the lightness-removing tower is connected with a pump (1102) for pumping the waste liquid at the bottom of the lightness-removing tower;

and a refined condensate outlet at the lower part of the left side of the light component removal tower reflux tank (14) is connected with a condensate feed inlet at the upper part of the right side of the light component removal tower (16) through a light component removal tower reflux pump (1501).

2. The device for extracting octanol from trioctyl trimellitate raffinate according to claim 1, wherein a pipeline between the heavy component removal tower condensate tank (7) and the light component removal tower feed pump (802) is connected with a heavy component removal tower condensate tank circulating pump (801), and the heavy component removal tower condensate tank circulating pump (801) is connected with the heavy component removal tower condensate tank (7) through a pipeline A.

3. The device for extracting octanol from trioctyl trimellitate raffinate according to claim 2, wherein the outlet of the lightness-removing column feed pump (802) is connected with the inlet at the bottom of the lightness-removing column feed preheater (9) through a pipeline B, and a pipeline C is arranged between the pipeline B and the pipeline A.

4. The device for extracting octanol from trioctyl trimellitate raffinate according to claim 1, wherein a lightness-removing column reflux tank circulating pump (1502) is connected to the pipeline between the lightness-removing column reflux tank (14) and the lightness-removing column reflux pump (1501), and the lightness-removing column reflux tank circulating pump (1502) is connected to the lightness-removing column reflux tank (14) through a pipeline D.

5. The device for extracting octanol from trioctyl trimellitate raffinate according to claim 4, wherein an outlet of the light component removal tower reflux pump (1501) is connected with a condensate feed inlet at the upper part of the light component removal tower (16) through a pipeline E, and a pipeline F is arranged between the pipeline E and the pipeline D.

6. The device for extracting octanol from trioctyl trimellitate raffinate according to claim 1, wherein the de-heavy column bottom waste liquid extraction pump (402) discharges waste liquid through a pipeline G, the top outlet of the de-heavy column bottom circulation pump (401) is connected with the top inlet of the de-heavy column reboiler (3) through a pipeline H, and a pipeline I is arranged between the pipeline G and the pipeline H.

7. The device for extracting the octanol from the trioctyl trimellitate raffinate according to claim 1, wherein the lightness-removing column bottom waste liquid extraction pump (1102) discharges the waste liquid through a pipeline J, a top outlet of the lightness-removing column bottom circulating pump (1101) is connected with a top inlet of the lightness-removing column reboiler (10) through a pipeline K, and a pipeline L is arranged between the pipeline J and the pipeline K.

8. The device for extracting octanol from trioctyl trimellitate raffinate according to claim 1, wherein the right outlet at the top of the second-stage condenser (6) of the heavy component removal tower and the right outlet at the top of the second-stage condenser (13) of the light component removal tower are respectively connected to a vacuum system.

9. A method for extracting octanol from trioctyl trimellitate residual liquid, which adopts the device for extracting octanol from trioctyl trimellitate residual liquid according to any one of claims 1 to 8 to recover, and is characterized in that: the recovery method comprises the following process steps:

s1, after the de-weighting tower (1) is vacuumized, preheating trioctyl trimellitate residual liquid (a sampling mark is S0) containing octanol through a de-weighting tower feeding preheater (2) and then pumping into the de-weighting tower (1);

s2, after the liquid level of the heavy component removal tower (1) reaches 1m, starting a heavy component removal tower bottom circulating pump (401), starting a heavy component removal tower reboiler (3) for heating and raising the temperature, controlling the kettle temperature at 125-135 ℃, and after the tower bottom liquid (sampling mark is S1) detects that the octanol content is lower than 10%, pumping the heavy component removal tower bottom waste liquid by using a heavy component removal tower bottom waste liquid pump (402);

s3, condensing the gas phase of the heavy component removal tower through a first-stage condenser (5) of the heavy component removal tower and a second-stage condenser (6) of the heavy component removal tower, feeding the condensate into a condensate tank (7) of the heavy component removal tower, and analyzing the octanol content of the condensate (the sampling mark is S2); opening a circulating pump (801) of the heavy component removal tower condensed liquid tank, and continuously circulating the condensed liquid in the heavy component removal tower condensed liquid tank (7);

s4, after the liquid level of the heavy component removal tower condensate tank (7) reaches 1m, establishing vacuum in the light component removal tower (16), starting a light component removal tower feed pump (802), preheating heavy component removal tower condensate by a light component removal tower feed preheater (9), and then pumping the heavy component removal tower condensate into the light component removal tower (16);

s5, after the liquid level of the light component removal tower (16) reaches 1m, starting a circulating pump (1101) at the bottom of the light component removal tower, starting a reboiler (10) of the light component removal tower for heating, and controlling the kettle temperature to be 85-95 ℃;

s6, condensing the gas phase of the lightness-removing tower through a first-stage condenser (12) of the lightness-removing tower and a second-stage condenser (13) of the lightness-removing tower, and then feeding the liquid phase into a reflux tank (14) of the lightness-removing tower; opening a circulating pump (1502) of a reflux tank of the light component removal tower, and continuously circulating the condensate in the reflux tank (14) of the light component removal tower;

s7, after the liquid level of a light component removal tower reflux tank (14) reaches 1m, starting a light component removal tower reflux pump (1501), and controlling the tower top temperature to be 75-80 ℃;

s8, extracting octanol from the middle part of the light component removal tower (16) (the sampling mark is S3) and analyzing the content of the octanol, and extracting the octanol when the content reaches more than 95 percent; and pumping out the light component removal tower bottom waste liquid by using a light component removal tower bottom waste liquid pumping pump (1102).

Technical Field

The invention relates to the technical field of organic chemical industry, in particular to a device and a method for extracting octanol from trioctyl trimellitate residual liquid.

Background

The trioctyl trimellitate is liquid at normal temperature, is convenient to transport and use, and the ester has high boiling point, low volatility and moderate molecular weight, contains some branched chains in molecules, is good for improving the plasticity and flexibility of plastics and rubber, and is commonly used as a plasticizer, so that the temperature resistance grade of PVC plastics, rubber, resin and the like can be obviously improved. It is also used in automobile decoration material, waterproof layer of swimming pool, soaking oil of capacitor, etc.

At present, the industrial production method of trioctyl trimellitate is generally produced by directly esterifying trimellitic acid and octanol. The industrial production method comprises the steps of oxidizing trimellitic benzene in a liquid phase by air to prepare trimellitic acid, dehydrating the trimellitic acid at high temperature to form anhydride, rectifying the anhydride at high temperature and high vacuum to obtain trimellitic anhydride with the content of over 95 percent, carrying out esterification reaction on the trimellitic anhydride and octanol under the action of a catalyst to obtain crude trioctyl trimellitate, and rectifying and purifying the crude trioctyl trimellitate to obtain a finished product of trioctyl trimellitate.

A certain amount of residual liquid containing octanol and trioctyl trimellitate is generated in the reaction process and the rectification process, the color number of the residual liquid is high, the purification difficulty is high, the residual liquid is directly discarded, the residual liquid treatment burden is increased, and the unit consumption of products is increased.

Disclosure of Invention

The invention aims to solve the technical problems that the treatment burden is increased and the unit consumption of products is increased due to the fact that trioctyl trimellitate residual liquid containing octanol generated in the existing production process is directly discarded.

In order to solve the technical problems, the invention provides a device for extracting octanol from trioctyl trimellitate raffinate, which comprises a heavy component removal tower, a heavy component removal tower feeding preheater, a heavy component removal tower reboiler, a heavy component removal tower first-stage condenser, a heavy component removal tower second-stage condenser, a heavy component removal tower condensate tank, a light component removal tower feeding preheater, a light component removal tower reboiler, a light component removal tower first-stage condenser, a light component removal tower second-stage condenser, a light component removal tower reflux tank and a light component removal tower,

a feed inlet on the left side of the de-weighting tower is connected with a discharge outlet on the top end of a feed preheater of the de-weighting tower, and a feed inlet for trioctyl trimellitate residual liquid containing octanol is arranged at the bottom end of the feed preheater of the de-weighting tower;

a feed inlet at the lower part of the right side of the heavy component removal tower is connected with an outlet at the bottom end of a reboiler of the heavy component removal tower, and an inlet at the top end of the reboiler of the heavy component removal tower is connected with a residual liquid discharge outlet at the bottom end of the heavy component removal tower through a circulating pump at the bottom of the heavy component removal tower; a pipeline between the residual liquid discharge port at the bottom end of the de-heavy tower and the circulating pump at the bottom of the de-heavy tower is connected with a waste liquid extraction pump at the bottom of the de-heavy tower;

the outlet of the gas phase crude octanol at the top end of the de-weighting tower is connected with the inlet of the left side of the top of the first-stage condenser of the de-weighting tower, the outlet of the gas phase at the right side of the top of the first-stage condenser of the de-weighting tower is connected with the inlet of the left side of the top of the second-stage condenser of the de-weighting tower, and the outlet of the bottom end of the first-stage condenser of the de-weighting tower and the outlet of the bottom end of the second-stage condenser;

a crude product condensate outlet at the lower part of the right side of the heavy component removal tower condensate tank is connected with an inlet at the bottom of a light component removal tower feeding preheater through a light component removal tower feeding pump; an outlet at the top of the feed preheater of the lightness-removing column is connected with a feed inlet at the lower part of the left side of the lightness-removing column;

the gas-phase refined octanol discharge port at the top end of the lightness-removing tower is connected with the left inlet at the top of the first-stage condenser of the lightness-removing tower, the right outlet at the top of the first-stage condenser of the lightness-removing tower is connected with the left inlet at the top of the second-stage condenser of the lightness-removing tower, and the outlet at the bottom end of the first-stage condenser of the lightness-removing tower and the outlet at the bottom end of the second-stage condenser of the lightness-removing tower are connected in parallel to the;

a feed inlet at the lower part of the right side of the light component removal tower is connected with an outlet at the bottom end of a reboiler of the light component removal tower, and an inlet at the top end of the reboiler of the light component removal tower is connected with a residual liquid discharge outlet at the bottom end of the light component removal tower through a circulating pump at the bottom of the light component removal tower; a pipeline between a residual liquid discharge port at the bottom end of the light component removing tower and a circulating pump at the bottom of the light component removing tower is connected with a waste liquid extracting pump at the bottom of the light component removing tower;

and a refined condensate outlet at the lower part of the left side of the light component removal tower reflux tank is connected with a condensate inlet at the upper part of the right side of the light component removal tower through a light component removal tower reflux pump.

Furthermore, a circulating pump of the heavy component removal tower condensate tank is connected to a pipeline between the heavy component removal tower condensate tank and the light component removal tower feed pump, and the circulating pump of the heavy component removal tower condensate tank is connected with the heavy component removal tower condensate tank through a pipeline A.

Furthermore, an outlet of the light component removal tower feeding pump is connected with an inlet at the bottom of the light component removal tower feeding preheater through a pipeline B, and a pipeline C is arranged between the pipeline B and the pipeline A.

Furthermore, a circulating pump of the light component removal tower reflux tank is connected to a pipeline between the light component removal tower reflux tank and the light component removal tower reflux pump, and the circulating pump of the light component removal tower reflux tank is connected with the light component removal tower reflux tank through a pipeline D.

Further, an outlet of the reflux pump of the light component removal tower is connected with a condensate feeding port at the upper part of the light component removal tower through a pipeline E, and a pipeline F is arranged between the pipeline E and the pipeline D.

Further, a waste liquid pumping pump at the bottom of the heavy component removal tower discharges waste liquid through a pipeline G, an outlet at the top end of a circulating pump at the bottom of the heavy component removal tower is connected with an inlet at the top end of a reboiler of the heavy component removal tower through a pipeline H, and a pipeline I is arranged between the pipeline G and the pipeline H.

Further, the waste liquid at the bottom of the light component removing tower is discharged by a waste liquid extracting pump through a pipeline J, an outlet at the top end of a circulating pump at the bottom of the light component removing tower is connected with an inlet at the top end of a reboiler of the light component removing tower through a pipeline K, and a pipeline L is arranged between the pipeline J and the pipeline K.

Further, the right outlet at the top of the secondary condenser of the heavy component removal tower and the right outlet at the top of the secondary condenser of the light component removal tower are respectively connected with a vacuum system.

The method for extracting the octanol from the trioctyl trimellitate residual liquid adopts the device for extracting the octanol from the trioctyl trimellitate residual liquid for recovery, and comprises the following process steps:

s1, after the de-weighting tower is vacuumized, preheating trioctyl trimellitate residual liquid (sampling mark is S0) containing octanol through a feed preheater of the de-weighting tower, and then pumping the residual liquid into the de-weighting tower;

s2, after the liquid level of the de-weighting tower reaches 1m, starting a de-weighting tower bottom circulating pump, starting a de-weighting tower reboiler to heat and raise the temperature, controlling the kettle temperature at 125-135 ℃, and after the octanol content of the tower bottom liquid (sampled and marked as S1) is detected to be lower than 10%, pumping out the de-weighting tower bottom waste liquid by using a de-weighting tower bottom waste liquid pump;

s3, condensing the gas phase of the heavy component removal tower through a first-stage condenser of the heavy component removal tower and a second-stage condenser of the heavy component removal tower, feeding the condensate into a condensate tank of the heavy component removal tower, and analyzing the octanol content of the condensate (the sampling mark is S2); opening a circulating pump of a condensation liquid tank of the de-weighting tower, and continuously circulating the condensation liquid in the condensation liquid tank of the de-weighting tower;

s4, after the liquid level of a heavy component removal tower condensate tank reaches 1m, establishing vacuum on the light component removal tower, starting a light component removal tower feed pump, preheating heavy component removal tower condensate by a light component removal tower feed preheater, and then pumping into the light component removal tower;

s5, after the liquid level of the light component removal tower reaches 1m, starting a circulating pump at the bottom of the light component removal tower, starting a reboiler of the light component removal tower for heating and raising the temperature, wherein the kettle temperature is controlled to be 85-95 ℃;

s6, condensing the gas phase of the light component removal tower through a first-stage condenser of the light component removal tower and a second-stage condenser of the light component removal tower, and then feeding the liquid phase into a reflux tank of the light component removal tower; opening a circulating pump of a light component removal tower reflux tank, and continuously circulating the condensate in the light component removal tower reflux tank;

s7, after the liquid level of a light component removal tower reflux tank reaches 1m, starting a light component removal tower reflux pump, and controlling the tower top temperature to be 75-80 ℃;

s8, extracting octanol from the middle part of the light component removal tower (the sampling mark is S3), analyzing the content of the octanol, and extracting the octanol when the content reaches more than 95 percent; and pumping out the waste liquid at the bottom of the light component removal tower by using a pump for pumping the waste liquid at the bottom of the light component removal tower.

The invention has the advantages that:

the method is simple to operate, can recover high-content octanol for reuse through continuous feeding, reduces the material consumption of trioctyl trimellitate production, reduces the generation amount of waste liquid in the trioctyl trimellitate production process, and is beneficial to environmental protection.

Drawings

In order to more clearly illustrate the technical solution of the present invention, the drawings needed for the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.

FIG. 1 is a schematic diagram showing the structure of the octanol extraction process in the trioctyl trimellitate residue according to the present invention;

in the figure: 1-heavy component removal tower, 2-heavy component removal tower feeding preheater, 3-heavy component removal tower reboiler, 401-heavy component removal tower bottom circulating pump, 402-heavy component removal tower bottom waste liquid extraction pump, 5-heavy component removal tower first-stage condenser, 6-heavy component removal tower second-stage condenser, 7-heavy component removal tower condensate tank, 801-heavy component removal tower condensate tank circulating pump, 802-light component removal tower feeding pump, 9-light component removal tower feeding preheater, 10-light component removal tower reboiler, 1101-light component removal tower bottom circulating pump, 1102-light component removal tower bottom waste liquid extraction pump, 12-light component removal tower first-stage condenser, 13-light component removal tower second-stage condenser, 14-light component removal tower reflux tank, 1501-light component removal tower reflux, 1502-light component removal tower reflux circulating pump and 16-light component removal tower.

Detailed Description

The following describes the specific embodiments of the present invention with reference to examples, so that the technical solutions and the advantages thereof are more clear and clear. The following described embodiments are exemplary and are intended to be illustrative of the invention, but are not to be construed as limiting the invention.