CN214514486U

CN214514486U - Trans-1, 2-dichloroethylene preparation system

Info

Publication number: CN214514486U
Application number: CN202120372119.7U
Authority: CN
Inventors: 菅盘铭; 郑亚威; 孙春辉; 陈明军; 刘新文; 张虎; 马小利
Original assignee: Ningxia Purui Chemical Co ltd
Current assignee: Ningxia Purui Chemical Co ltd
Priority date: 2021-02-08
Filing date: 2021-02-08
Publication date: 2021-10-29
Anticipated expiration: 2031-02-08

Abstract

The utility model provides a trans-1, 2-dichloroethylene preparation system, including the synthetic tower, the regenerator, the mother liquor storage tank, the regeneration storage tank, take off the light tower, the rectifying column, the gas phase entry is used for letting in acetylene gas at the bottom of the synthetic tower, the export of liquid phase access connection mother liquor jar at the bottom of the tower, synthetic tower top gas phase exit linkage condenser for synthesis, the top of the tower liquid phase entry of the exit linkage synthetic tower of condenser for synthesis, crude jar is still connected in the export of condenser for synthesis, the gas phase entry is used for letting in chlorine at the bottom of the tower of regenerator, regeneration tower top of the tower liquid phase access linkage regeneration storage tank, liquid phase exit linkage mother liquor storage tank at the bottom of the condenser for regeneration still sets up the dehydrogenation buffer tank for taking off the light tower, the light jar of keeping in, the transition buffer tank, still set up the rectification buffer tank for the rectifying column, heavy matter jar of keeping in, the finished product jar, this scheme is through setting up above the dichloroethylene boiling point, The rectification is carried out for the following two times, thereby ensuring that the purity of the dichloroethylene reaches 0.999.

Description

Trans-1, 2-dichloroethylene preparation system

Technical Field

The utility model relates to a trans-1, 2-dichloroethylene preparation technical field especially relates to a trans-1, 2-dichloroethylene preparation system.

Background

Trans-1, 2-dichloroethylene (hereinafter referred to as dichloroethylene) is a good solvent and chemical raw material, and is colorless and volatile liquid with slight pungent smell. The main application is as follows: the trans-1, 2-dichloroethylene is a novel environment-friendly organic solvent, and can be used as a solvent for paint, resin, wax, rubber and acetate fiber, a dry cleaning agent, an insecticide, a bactericide, an anesthetic, a low-temperature extractant, a refrigerant and the like. Due to the wide application of trans-1, 2-dichloroethylene, the preparation of the trans-1, 2-dichloroethylene also becomes a very concerned problem in the chemical industry.

In the existing equipment, acetylene gas and mother liquor are adopted to synthesize and produce a crude product of dichloroethylene, wherein the content of dichloroethylene in the crude product is about 98 percent, and the purity is lower.

Disclosure of Invention

It is necessary to provide a trans-1, 2-dichloroethylene production system.

A trans-1, 2-dichloroethylene preparation system comprises a synthesis tower, a regeneration tower, a mother liquor storage tank, a regeneration storage tank, a light component removal tower and a rectification tower, wherein the synthesis tower and the regeneration tower are packed towers, a tower bottom liquid phase inlet is connected with an outlet of the mother liquor tank, a tower top gas phase outlet of the synthesis tower is connected with a condenser for synthesis, an outlet of the condenser for synthesis is connected with a tower top liquid phase inlet of the synthesis tower through a gas-water separator, an outlet of the condenser for synthesis is also connected with a crude product tank through the gas-water separator so as to input a semi-finished product containing dichloroethylene into the crude product tank, a tower bottom gas phase inlet of the regeneration tower is used for introducing chlorine, a tower top liquid phase inlet of the regeneration tower is connected with the regeneration storage tank, a tower bottom liquid phase outlet of the regeneration tower is connected with the mother liquor storage tank, the regeneration tower is provided with the condenser for regeneration, a tower top gas phase outlet of the regeneration tower is connected with the condenser for regeneration, an outlet of the condenser for regeneration is connected with the crude product tank through the gas-water separator, still set up pre-heater, intensifier between synthetic column and mother liquor storage tank, the exit of the entry linkage mother liquor storage tank of pre-heater, the liquid phase entry at the bottom of the exit linkage intensifier of pre-heater, the liquid phase entry at the bottom of the tower of the exit linkage synthetic column of intensifier, the gaseous phase entry linkage acetylene gas incoming material pipeline of intensifier, crude jar passes through pipeline and power pump and connects lightness-removing column, rectifying column, lightness-removing column is the packed column, still sets up dehydrogenation buffer tank, light temporary storage tank, transition buffer tank for lightness-removing column, crude jar connects the dehydrogenation buffer tank, and dehydrogenation buffer tank connects the liquid phase entry at the bottom of the tower of lightness-removing column, and dehydrogenation condenser is used in dehydrogenation of lightness-removing column top gaseous phase exit linkage, and light temporary storage tank is connected to the dehydrogenation condenser, and transition buffer tank is connected to the liquid phase exit at the bottom of lightness-removing column, and the rectifying column is the packed column, still sets up rectification buffer tank, heavy temporary storage tank for the rectifying column, The finished product tank, the transition buffer tank are connected with the rectification buffer tank, the rectification buffer tank is connected with the inlet at the bottom of the rectification tower, the gas phase outlet at the top of the rectification tower is connected with the condenser for rectification, the condenser for rectification is connected with the finished product tank, the outlet at the bottom of the rectification tower is connected with the heavy temporary storage tank, the temperature at the top of the light component removal tower is lower than the boiling temperature of trans-1, 2-dichloroethylene, and the temperature at the top of the rectification tower is higher than the boiling temperature of trans-1, 2-dichloroethylene.

The utility model discloses a cyclic regeneration of mother liquor uses, and regeneration process and synthetic process are incessant continuous reaction process, and the synthetic reaction of dichloroethylene and the regeneration of mother liquor supply each other do not influence, and the process of whole production dichloroethylene need not to stop, be interrupted, and equipment structure optimizes, and production efficiency is high.

The utility model discloses in, carry out light cryogenic rectification through taking off the light tower and handle the dichloroethylene in to the crude jar for the first time, make light impurity by the desorption, carry out heavy matter high temperature rectification for the second time through the rectifying column again, make high boiling point impurity by the desorption, the rectifying column tower overhead gas phase dichloroethylene is saved in the finished product jar after the condensation, and the dichloroethylene content that obtains through this secondary treatment can reach 0.999%.

Drawings

Fig. 1 is a schematic connection diagram of the present apparatus.

In the figure: the system comprises a synthesis tower 10, a condenser 11 for synthesis, a withdrawal control valve 111, an acetylene gas incoming pipeline 112, an acetylene recycling pipeline 113, a crude product tank 12, a preheater 13, a tower top temperature detector 14, a tower bottom temperature detector 15, a controller 16, an input control valve 17, a reinforcing device 18, a regeneration tower 20, a condenser 21 for regeneration, a mother liquor storage tank 30, a tail gas pipeline 31, a regeneration storage tank 40, a balance pipeline 41, a first condenser 42, a second condenser 43, a light component removal tower 50, a dehydrogenation buffer tank 51, a light component temporary storage tank 52, a transition buffer tank 53, a rectification tower 60, a rectification buffer tank 61, a heavy component temporary storage tank 62 and a finished product tank 63.

Detailed Description

In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to these drawings without creative efforts.

Referring to fig. 1, an embodiment of the present invention provides a trans-1, 2-dichloroethylene preparation system, which includes a synthesis tower 10, a regeneration tower 20, a mother liquor storage tank 30, a regeneration storage tank 40, a lightness-removing tower 50, and a rectification tower 60, where the synthesis tower 10 and the regeneration tower 20 are packed towers, a liquid phase inlet at the bottom of the tower is connected to an outlet of the mother liquor tank, a gas phase outlet at the top of the synthesis tower 10 is connected to a condenser 11 for synthesis, an outlet of the condenser 11 for synthesis is connected to a liquid phase inlet at the top of the synthesis tower 10 through a gas-water separator, an outlet of the condenser 11 for synthesis is further connected to a crude product tank 12 through a gas-water separator, so as to input a semi-finished product containing dichloroethylene into the crude product tank 12, a gas phase inlet at the bottom of the regeneration tower 20 is used for introducing chlorine gas, a liquid phase inlet at the top of the regeneration tower 20 is connected to the regeneration storage tank 40, a liquid phase outlet at the bottom of the regeneration tower 20 is connected to the mother liquor storage tank 30, the regeneration tower 20 is provided with a condenser 21 for regeneration, a gas phase outlet at the top of the regeneration tower 20 is connected with a regeneration condenser 21, an outlet of the regeneration condenser 21 is connected with a crude product tank 12 through a gas-water separator, a balance pipeline 41, a first condenser 42 and a second condenser 43 are arranged between a regeneration storage tank 40 and the crude product tank 12, the balance pipeline 41 is connected between an inlet of the first condenser 42 and the regeneration storage tank 40, a gas phase outlet of the first condenser 42 is connected with an inlet of the second condenser 43, a liquid phase outlet of the first condenser 42 and a liquid phase outlet of the second condenser 43 are connected with the crude product tank 12, a tail gas pipeline 31 is arranged between a mother liquid storage tank 30 and the regeneration condenser 21, a preheater 13 and a reinforcer 18 are arranged between the synthesis tower 10 and a mother liquid storage tank 30, an inlet of the preheater 13 is connected with an outlet of the mother liquid storage tank 30, an outlet of the preheater 13 is connected with a liquid phase inlet at the bottom of the reinforcer 18, an outlet at the top of the reinforcer 18 is connected with a liquid phase inlet at the bottom of the synthesis tower 10, the gas phase inlet of the intensifier 18 is connected to the acetylene gas feed line 112. The crude product tank 12 is connected with a lightness-removing tower 50 and a rectifying tower 60 through pipelines and a power pump, the lightness-removing tower 50 is a packed tower, the lightness-removing tower 50 is also provided with a dehydrogenation buffer tank 51, a light temporary storage tank 52 and a transition buffer tank 53, the crude product tank is connected with the dehydrogenation buffer tank 51, the dehydrogenation buffer tank 51 is connected with a tower bottom liquid phase inlet of the lightness-removing tower 50, a tower top gas phase outlet of the lightness-removing tower 50 is connected with a dehydrogenation condenser, the dehydrogenation condenser is connected with the light temporary storage tank 52, a tower bottom liquid phase outlet of the lightness-removing tower 50 is connected with the transition buffer tank 53, the rectifying tower 60 is a packed tower, the rectifying tower 60 is also provided with a rectifying buffer tank 61, a heavy temporary storage tank 62 and a finished product tank 63, the transition buffer tank 53 is connected with a rectifying buffer tank 61, the rectifying buffer tank 61 is connected with a tower bottom inlet of the rectifying tower 60, a tower bottom gas phase outlet of the rectifying tower 60 is connected with a rectifying condenser, the rectifying condenser is connected with a finished product tank 63, a tower bottom outlet of the rectifying tower 60 is connected with a heavy temporary storage tank 62, the temperature of the top of the light component removal tower 50 is lower than the boiling point temperature of trans-1, 2-dichloroethylene, and the temperature of the top of the rectifying tower 60 is higher than the boiling point temperature of trans-1, 2-dichloroethylene.

The utility model discloses in, carry out light cryogenic rectification through taking off the dichloroethylene of light tower 50 in to the crude jar and handle for the first time, make light impurity by the desorption, carry out heavy matter high temperature rectification for the second time through rectifying column 60 again, make heavy matter impurity by the desorption, rectifying column 60 top of the tower distills gaseous phase dichloroethylene, saves in finished product jar 63 after the condensation, and the dichloroethylene content that obtains through this secondary treatment can reach 0.999%. This scheme is when realizing, through control lightness-removing tower inner tower top temperature, makes it be less than the dichloroethylene boiling point, distills off light impurity and collects alone, and heavy component such as dichloroethylene gets into the rectifying column rectification once more, and control rectifying column top temperature is higher than the dichloroethylene boiling point, makes dichloroethylene be gaseous phase discharge to the condensation is collected, and other heavy components are collected alone. According to the scheme, the light impurities and the heavy impurities are discharged in batches by performing rectification twice above and below the boiling point of the dichloroethylene, so that the purity of the dichloroethylene is ensured to reach 0.999.

The utility model discloses in, the acetylene is the material that preceding step preparation formed, as the raw materials of production dichloroethylene, get into the converter 10 with the catalyst mother liquor in the mother liquor storage tank 30, the two reaction generates the crude that contains dichloroethylene, the mother liquor of depriving a chloridion discharges into regeneration storage tank 40, liquid in the regeneration storage tank 40 is pumped to in the regeneration tower 20, regeneration tower 20 lets in chlorine, a chloridion in the chlorine is absorbed by the mother liquor that lacks chloridion, realize the regeneration of mother liquor, the mother liquor after the regeneration is stored in mother liquor storage tank 30, squeeze into converter 10 once more and use, there is some dichloroethylene still at the top of the tower of regeneration tower 20, in being regenerated with condenser 21 condensation reflux to crude tank 12, and then improve the conversion of the inside dichloroethylene of system, improve the yield of dichloroethylene in the crude tank 12. A part of dichloroethylene still exists at the top of the regeneration tower 20, and is condensed and refluxed to the crude product tank 12 by a regeneration condenser 21. The mother liquor is copper chloride solution with copper chloride content not lower than 98%, and the mother liquor with one chloride ion being deprived is cuprous chloride solution with cuprous chloride content not lower than 98%.

The scheme is that a tail gas pipeline 31 is arranged on the mother liquor storage tank 30 and is used for absorbing gas which is discharged into the mother liquor storage tank 30 in the regeneration process of the regeneration tower 20, the entrained gas is discharged into a regeneration condenser 21 along the tail gas pipeline 31, and the gas is condensed and then separated and sent into a tail gas treatment system.

This scheme still sets up balanced pipeline 41, first condenser 42, second condenser 43 for regeneration storage tank 40, the mother liquor temperature of discharging from the synthetic tower 10 like regeneration storage tank 40 is higher, and inside its part secretly carries partial gaseous dichloroethylene, gets into regeneration storage tank 40 inside, causes the big problem of regeneration storage tank 40 internal pressure easily, and this scheme discharges gaseous dichloroethylene into first condenser 42 and second condenser 43, and the dichloroethylene after the condensation gets into in crude jar 12 to improve the conversion of dichloroethylene in the synthetic tower 10. The first condenser 42 and the second condenser 43 adopt a series reinforcement mode, so that the substance which is not cooled in the first condenser is secondarily condensed by the second condenser, and the gas-phase ethylene dichloride is fully collected. This scheme still sets up balanced pipeline, first condenser, second condenser for the regeneration storage tank, and is higher at the synthetic tower exhaust mother liquor temperature, and it is inside to smuggle partial gaseous dichloroethylene secretly, gets into inside the regeneration storage tank, causes the big problem of regeneration storage tank internal pressure easily, and this scheme emits gaseous dichloroethylene into first condenser and second condenser, and the dichloroethylene after being condensed gets into in the crude jar to improve the conversion of dichloroethylene in the synthetic tower.

The scheme is that the mother liquor storage tank is provided with a tail gas pipeline for absorbing gas which is discharged into the mother liquor storage tank in the regeneration process of the regeneration tower and is entrained along the tail gas pipeline, the entrained gas is discharged into a regeneration condenser, the gas is condensed and then separated and sent into a tail gas treatment system, meanwhile, part of gas-phase dichloroethylene is also entrained in the gas and is discharged into the regeneration condenser along the tail gas pipeline, and the condensed gas enters a crude product tower.

The intensifier 18 is a packed tower, the acetylene gas enters the post-preheating mother liquor to be premixed in the intensifier 18, the acetylene gas and the preheated mother liquor begin to react, the mixture at the outlet of the intensifier 18 enters the synthesis tower to be further mixed and reacted, the arrangement of the intensifier 18 can lead the materials to be contacted and reacted in advance, the materials are contacted and reacted fully, the material reaction time is prolonged, the acetylene gas and the synthesis tower are fully mixed in advance, the reaction begins in advance, and the full preparation is made for the reaction in the synthesis tower.

Further, an acetylene recycling pipeline 113 is arranged for the second condenser, the other end of the acetylene recycling pipeline 113 is connected with an acetylene gas incoming pipeline 112, and a pipeline for connecting the second condenser is arranged on a gas-liquid separator of the condenser for synthesis. The gas phase remained in the gas-liquid separator and not condensed enters a second condenser, the gas-phase dichloroethylene is condensed and then enters a crude product tank, and part of acetylene gas flows back along an acetylene recycling pipeline 113 for secondary utilization. The scheme does not need to arrange a gas phase balance port for the second condenser, and can recycle the gas phase, thereby improving the utilization rate of acetylene.

According to the scheme, the mother liquor is preheated in advance before entering the synthesis tower 10, the preheating temperature is 88-93 ℃, the preheated mother liquor enters the synthesis tower 10, the required heat is less, the time point of the synthesis reaction of the mother liquor and acetylene gas can be advanced, the time required by the synthesis reaction is shortened, and the reaction efficiency is improved.

Further, a tower top temperature detector 14 and a tower bottom temperature detector 15 are arranged at both the tower top and the tower bottom of the synthesis tower 10, a controller 16 (of course, the controller 16 is not used for controlling the on-off of the acetylene input pipeline, but is used as a carrier for installing the controller 16) and an input control valve 17 are arranged on the pipeline for inputting acetylene, a recovery control valve 111 is arranged on the pipeline for connecting the synthesis condenser 11 and the crude product tank 12, and the controller 16 is connected with the tower top temperature detector 14, the tower bottom temperature detector 15, the input control valve 17 and the recovery control valve 111. The scheme forms an interlocking control system by a temperature controller 16 and a temperature detector, the temperature controller 16 adopts the existing equipment in the prior art, a tower top temperature detector 14 is used for detecting the temperature at the top of the synthesis tower 10, a tower bottom temperature detector 15 is used for detecting the temperature at the bottom of the synthesis tower 10, when the real-time temperature detected by the tower top temperature detector 14 is higher than the set value, which indicates that the content of high boiling point heavy components in the product produced at the tower top is higher, multiple times of reflux condensation separation are needed, the controller 16 controls the extraction control valve 111 to close and controls the input control valve 17 to close, otherwise, when the real-time temperature detected by the tower top temperature detector 14 is lower than the set value, which indicates that the content of dichloroethylene in the product produced at the tower top is higher, at this time, the controller 16 controls the extraction control valve 111 to be intermittently opened to extract the semi-finished product, and controls the input control valve 17 to be opened to input acetylene gas. The controller can be realized by adopting a switch circuit in the prior art.

The embodiment of the utility model provides a module or unit in the device can merge, divide and delete according to actual need.

The above disclosure is only illustrative of the preferred embodiments of the present invention, which should not be taken as limiting the scope of the invention, but rather the invention can be embodied in other specific forms without departing from the spirit or essential characteristics thereof. It will be understood by those skilled in the art that all or part of the above-described embodiments may be implemented and equivalents thereof may be made to the claims of the present invention while remaining within the scope of the invention. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.

Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.

Claims

1. A trans-1, 2-dichloroethylene preparation system is characterized in that: comprises a synthetic tower, a regeneration tower, a mother liquor storage tank, a regeneration storage tank, a light component removal tower and a rectification tower, wherein the synthetic tower and the regeneration tower are packed towers, a liquid phase inlet at the bottom of the tower is connected with an outlet of the mother liquor tank, a gas phase outlet at the top of the synthetic tower is connected with a condenser for synthesis, an outlet of the condenser for synthesis is connected with a liquid phase inlet at the top of the synthetic tower through a gas-water separator, an outlet of the condenser for synthesis is also connected with a crude product tank through the gas-water separator, a gas phase inlet at the bottom of the regeneration tower is used for introducing chlorine, a liquid phase inlet at the top of the regeneration tower is connected with the regeneration storage tank, a liquid phase outlet at the bottom of the regeneration tower is connected with the mother liquor storage tank, the regeneration tower is provided with the condenser for regeneration, a gas phase outlet at the top of the regeneration tower is connected with the crude product tank through the gas-water separator, a preheater and a reinforcer are also arranged between the synthetic tower and the mother liquor storage tank, an inlet of the preheater is connected with an outlet of the mother liquor storage tank, the outlet of the preheater is connected with the tower bottom liquid phase inlet of the intensifier, the tower top outlet of the intensifier is connected with the tower bottom liquid phase inlet of the synthesis tower, the gas phase inlet of the intensifier is connected with an acetylene gas incoming material pipeline, the crude product tank is connected with the light component removal tower and the rectification tower through a pipeline and a power pump, the light component removal tower is a packed tower, the light component removal tower is also provided with a dehydrogenation buffer tank, a light temporary storage tank and a transition buffer tank, the crude product tank is connected with the dehydrogenation buffer tank, the dehydrogenation buffer tank is connected with the tower bottom liquid phase inlet of the light component removal tower, the tower top gas phase outlet of the light component removal tower is connected with a dehydrogenation condenser, the dehydrogenation condenser is connected with the light temporary storage tank, the tower bottom liquid phase outlet of the light component removal tower is connected with the transition buffer tank, the rectification tower is provided with the packed tower, the rectification buffer tank, the heavy temporary storage tank and a finished product tank are also connected with the transition buffer tank, the rectification buffer tank is connected with the tower bottom inlet of the rectification buffer tank, the tower bottom gas phase outlet of the rectification tower is connected with a rectification condenser, the condenser for rectification is connected with a finished product tank, the outlet at the bottom of the rectifying tower is connected with a heavy temporary storage tank, the temperature at the top of the light component removal tower is lower than the boiling point temperature of trans-1, 2-dichloroethylene, and the temperature at the top of the rectifying tower is higher than the boiling point temperature of trans-1, 2-dichloroethylene.

2. The trans-1, 2-dichloroethylene production system of claim 1, wherein: the top and bottom of the synthetic tower are provided with a top temperature detector and a bottom temperature detector, a pipeline for inputting acetylene is provided with a controller and an input control valve, a pipeline for connecting the condenser for synthesis and the crude product tank is provided with a production control valve, and the controller is connected with the top temperature detector, the bottom temperature detector, the input control valve and the production control valve.

3. The trans-1, 2-dichloroethylene production system of claim 1, wherein: still set up balanced pipeline, first condenser, second condenser between regeneration storage tank and crude jar, balanced pipeline connects between the entry of first condenser and regeneration storage tank, and the gaseous phase export of first condenser and the entry linkage of second condenser, and the liquid phase export of first condenser and the liquid phase export of second condenser connect crude jar, still sets up the tail gas pipeline between mother liquor storage tank and the condenser for regeneration.

4. The trans-1, 2-dichloroethylene production system according to claim 3, wherein: and an acetylene recycling pipeline is also arranged for the second condenser, the other end of the acetylene recycling pipeline is connected with an acetylene gas incoming pipeline, and a gas-liquid separator of the condenser for synthesis is provided with a pipeline for connecting the second condenser.