CN208182895U - A kind of tetrahydrofuran fractional order reaction separator - Google Patents

A kind of tetrahydrofuran fractional order reaction separator Download PDF

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Publication number
CN208182895U
CN208182895U CN201820460628.3U CN201820460628U CN208182895U CN 208182895 U CN208182895 U CN 208182895U CN 201820460628 U CN201820460628 U CN 201820460628U CN 208182895 U CN208182895 U CN 208182895U
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order reaction
tower
rectification tower
separating rectification
reaction
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张利岗
周新明
赵中贤
王素霞
魏正学
成玉
鲁伟华
杜金成
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Ningxia Meibang World Chemical Co Ltd
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Ningxia Meibang World Chemical Co Ltd
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Abstract

The utility model relates to a kind of tetrahydrofuran fractional order reaction separators.It is made of head tank, charging pump, first order reaction separating rectification tower, second order reaction separating rectification tower, rear pump and connecting line.First order reaction separating rectification tower wall is provided, in sequence from bottom to top, with material inlet, mouth, reacting product outlet, overflow port, catalyst emission mouth is added in catalyst.Overflowing liquid import, reacting product outlet, catalyst addition mouth, catalyst emission mouth, kettle base solution outlet are successively arranged on second order reaction separating rectification tower wall.Heat exchanger, strainer, filler, demister, condenser are equipped in tower.Head tank is connected by charging pump, pipeline with first order reaction separating rectification tower, is connected between two towers by overflow pipe, the reacting product outlet of two towers is connected with reaction product pipeline.The kettle base solution outlet of second order reaction separating rectification tower is connected with rear pump.The fractional order reaction separator of the utility model is produced for tetrahydrofuran, improves the conversion ratio and yield of reaction.

Description

A kind of tetrahydrofuran fractional order reaction separator
Technical field
The utility model relates to a kind of chemical reaction equipment, especially a kind of tetrahydrofuran fractional order reaction separator belongs to Reactive distillation tower apparatus in Chemical Manufacture.
Background technique
Rectifying column is the common separation equipment of chemical production field.Reactive distillation is while being reacted with rectifying side Method isolates the process of product.Promote to react with rectifying, reaction product is constantly removed by rectifying, to improve reaction conversion ratio And yield.In the prior art, the production process of tetrahydrofuran is under the effect of the catalyst, to be dehydrated ring using 1,4-butanediol Change method prepares tetrahydrofuran, and reactor therein uses reactive distillation column, is 140-150 in the temperature control of tower bottom reaction zone DEG C, the temperature control of top of tower is 70-80 DEG C, and reactive distillation pressure tower is normal pressure.Catalyst is added from the middle and lower part of tower to anti- It answers in rectifying column, reaction zone of the 1,4-butanediol dehydration in tower lower part carries out, during the reaction, the tetrahydro reacted Furans under temperature environment is gaseous state in tower, is discharged to obtain tetrahydrofuran gas phase from tower top, after subsequent dehydrating and removing impurities To tetrahydrofuran product.Using the conversion ratio about 90% or so of such reactive distillation column 1,4-butanediol, there is nearly 10% Isosorbide-5-Nitrae-fourth Glycol is not reacted by as the residual discharge of kettle, can reuse after needing further progress removal of impurities to handle, energy consumption is caused to increase Add, product yield is low, in order to further increase the conversion ratio of 1,4-butanediol, reduces energy consumption, improves the receipts of product tetrahydrofuran Rate, it is necessary to which existing tetrahydrofuran Reaction Separation rectifier unit is improved.
Summary of the invention
The purpose of the utility model is to provide a kind of tetrahydrofuran fractional order reaction separators, to improve reaction raw materials Isosorbide-5-Nitrae- The conversion ratio of butanediol, improves the yield of product tetrahydrofuran, while reducing energy consumption.
The technical scheme in the invention for solving the technical problem is such.A kind of tetrahydrofuran fractional order reaction point From device, including head tank, charging pump, first order reaction separating rectification tower, second order reaction separating rectification tower, rear pump and connection Pipeline.Feed opening is equipped at the top of head tank, bottom is equipped with outlet, and head tank is passed through by piping connection charging pump, charging pump Piping connection first order reaction separating rectification tower, first order reaction separating rectification tower tower bottom is equipped with catalyst emission mouth, lower part is equipped with Material inlet, middle part are equipped with catalyst and mouth are added, and top is built-in with condenser, and middle part is packing layer, are equipped with and remove above packing layer Foam device.First order reaction separating rectification tower tower top has reacting product outlet, and tower lower part is built-in with heat exchanger, and middle part is equipped with reaction hydrorrhea Head piece is connected by overflow pipe with the overflowing liquid import of second order reaction separating rectification tower.Second order reaction separating rectification tower bottom is set There are kettle base solution outlet and catalyst emission mouth, tower reactor to be built-in with heat exchanger, middle part is built-in with packing layer, and the top of packing layer is equipped with Demister, top of tower are built-in with condenser, and tower top is equipped with reacting product outlet, and the middle part of tower is equipped with catalyst and mouth is added.Level-one The reacting product outlet at the top of reacting product outlet, second order reaction separating rectification tower at the top of Reaction Separation rectifying column passes through respectively Pipeline is connect with Product pipeline, and the kettle base solution outlet of second order reaction separating rectification tower bottom is connected with rear pump.
The top that mouth is located at reaction solution overflow port in tower, raw material is added in catalyst on the first order reaction separating rectification tower The lower part of liquid level is reacted in import in tower, is equipped with strainer at first order reaction separating rectification tower reaction solution overflow port.
Mouth is added in the top of overflowing liquid import and reaction liquid level in the catalyst of the second order reaction separating rectification tower, and two The kettle base solution exit of order reaction separating rectification tower bottom is equipped with strainer.
Height locating for reaction solution overflow port position on the first order reaction separating rectification tower is separated higher than second order reaction Overflowing liquid import on rectifying column can ensure that in first order reaction separating rectification tower the complete reaction solution of unreacted from overflow port in this way It naturally, is smoothly flowed into second order reaction separating rectification tower after spilling.
The reaction zone temperature of the first order reaction separating rectification tower tower bottom is by being passed through automatic steam control, temperature into heat exchanger It is 120-125 DEG C, the temperature of tower top is 70-80 DEG C by being passed through cooling water control, temperature into condenser, and pressure is normal pressure.
The reaction zone temperature of the second order reaction separating rectification tower tower bottom is by being passed through automatic steam control, temperature into heat exchanger It is 140-150 DEG C, the temperature of tower top is 70-80 DEG C by being passed through cooling water control, temperature into condenser, and pressure is normal pressure.
The working principle of the utility model is as follows:
Be added from feed opening into head tank by pretreated raw material 1,4-butanediol, then from outlet through charging pump, Material inlet is delivered in first order reaction separating rectification tower, while catalyst is added mouth from catalyst and is added.In first order reaction point It is 120~125 DEG C by heat exchanger control tower bottom reaction zone temperature, after stopping 45min, in the work of catalyst from rectifying column Under, 1,4-butanediol occurs cyclodehydration and reacts to obtain tetrahydrofuran and water, since the boiling point of tetrahydrofuran is 66 DEG C, water Boiling point is 100 DEG C, and reaction product tetrahydrofuran and water are vaporizated into gaseous state and are moved upward to tower top, is 70 in tower top temperature Under conditions of~80 DEG C, water and a small amount of 1,4-butanediol are condensed, and tetrahydrofuran gas phase is overflowed from reacting product outlet, When reaction solution liquid level to overflow open height, unreacted 1,4-butanediol solution is 1,4-butanediol clear liquid through strainer filtering, Catalyst is trapped in first order reaction separating rectification tower by strainer, and 1,4-butanediol clear liquid is anti-through overflow port, overflow pipe, second level Separating rectification tower overflowing liquid import is answered to enter in second order reaction separating rectification tower.In second order reaction separating rectification tower, catalyst It is added from catalyst inlet, is 140-150 DEG C by heat exchanger control tower bottom reaction zone temperature, under the effect of the catalyst, not The 1,4-butanediol of reaction continues cyclodehydration and reacts to obtain tetrahydrofuran and water, is vaporizated into gaseous state and moves up To tower top, under conditions of tower top temperature is 70~80 DEG C, water and a small amount of 1,4-butanediol are condensed, tetrahydrofuran gas It mutually overflows from reacting product outlet, is converged with the tetrahydrofuran gas phase overflowed from the reacting product outlet of first order reaction separating rectification tower It flow to reaction product pipeline after conjunction and obtains product tetrahydrofuran after subsequent dehydrating and removing impurities.Raw material 1,4-butanediol is through fractional order reaction Conversion ratio reaches 95% or more after separation, and it is clear that the kettle base solution of the remaining 1,4-butanediol containing unreacted through strainer filtering obtains bottom Liquid, catalyst are trapped in second order reaction separating rectification tower, and bottom clear liquid exports discharge from kettle base solution and receipts are discharged through rear pump Collection is back to 1,4-butanediol pretreatment of raw material process, be recycled after handling again.
When detecting the conversion ratio of 1,4-butanediol lower than 95%, illustrate that the activity of catalyst reduces, by periodically from two A Reaction Separation rectifying column catalyst outlet discharge part catalyst, then the catalyst that mouth adds homogenous quantities is added from catalyst Mode, to guarantee the high conversion of 1,4-butanediol.
The material of two Reaction Separation rectifying column Inner filter nets is 316L, and filtering accuracy is 30-100 mesh.
The beneficial effect that the utility model obtains is:
It is increased using fractional order reaction separator technology due to increasing 1,4-butanediol catalysis reaction time The contact area of 1,4-butanediol and catalyst can be such that the conversion ratio of 1,4-butanediol improves from 90% to 95% or more, tetrahydro furan The yield muttered also improves 5% or more;The content of 1,4-butanediol is reduced to 5% or so from 10% in kettle base solution, subsequent pretreated Energy consumption can reduce by 2% or so in journey.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the utility model.
Figure label meaning is as follows:
A, head tank B, charging pump C, first order reaction separating rectification tower D, second order reaction separating rectification tower E, defeated It pumps out.
1, feed opening 2, outlet 3, material inlet 4, catalyst emission mouth 5, heat exchanger 6, condensate outlet 7, steam inlet 8, reaction solution overflow port 9, overflow pipe 10, overflowing liquid import 11, strainer 12, kettle base solution outlet 13, catalyst emission mouth 14, condensate outlet 15, heat exchanger 16, steam inlet 17, catalyst are added mouth 18, fill out Material 19, demister 20, circulating water intake 21, circulating water outlet 22, condenser 23, reacting product outlet 24, Reaction product pipeline 25, condenser 27, circulating water outlet 28, circulating water intake 29, removes reacting product outlet 26 Mouth 32, strainer is added in foam device 30, filler 31, catalyst.
Specific embodiment
With reference to the accompanying drawing and the specific embodiment that provides of attached drawing is further described the utility model.
As shown in Figure 1, a kind of tetrahydrofuran fractional order reaction separator, including head tank (A), charging pump (B), head tank (A) top is equipped with feed opening 1, and bottom is equipped with outlet 2, and for head tank (A) by piping connection charging pump (B), charging pump (B) is logical Cross piping connection first order reaction separating rectification tower (C).The first order reaction separating rectification tower bottom (C) be equipped with catalyst emission mouth 4, under Portion is equipped with material inlet 3, and middle part is equipped with catalyst and mouth 31 is added, and top is built-in with condenser 26, has circulating water intake in tower wall 28, circulating water outlet 27, the middle part of tower are packing layer 30, are demister 29 above packing layer 30, tower top has reacting product outlet 25, tower lower part is built-in with heat exchanger 5, and tower wall is equipped with steam inlet 7, condensate outlet 6, is equipped with reaction solution overflow port 8 in the middle part of tower, Strainer 32 is equipped at reaction solution overflow port 8, reaction solution overflow port 8 is overflow by overflow pipe 9 and second order reaction separating rectification tower (D's) Flow liquid import 10 is connected.The second order reaction separating rectification tower bottom (D) is equipped with kettle base solution outlet 12 and catalyst emission mouth 13, kettle Strainer 11 is equipped at bottom liquid outlet 12, tower reactor is built-in with heat exchanger 15, and tower reactor wall is equipped with steam inlet 16, condensate outlet 14, Packing layer 18 is built-in in the middle part of tower, the top of packing layer 18 is equipped with demister 19, and top of tower is built-in with condenser 22, sets in tower wall There are circulating water outlet 21, circulating water intake 20, tower top is equipped with reacting product outlet 23, and the middle part of tower is equipped with catalyst and mouth is added 17.The reacting product outlet of the reacting product outlet 25 of first order reaction separating rectification tower (C), second order reaction separating rectification tower (D) 23 are connect by pipeline with Product pipeline 24 respectively.The kettle base solution outlet 12 and output of the bottom second order reaction separating rectification tower (D) (E) is pumped to be connected.
Mouth 31 is added in the top of its reaction liquid level in catalyst in the middle part of first order reaction separating rectification tower (C), that is, The top of reaction solution overflow port 8.Material inlet 3 is in the lower part of reaction liquid level.
Catalyst in the middle part of second order reaction separating rectification tower (D) is added mouth 17 and exists in the top of overflowing liquid import 10, and all It reacts liquid level or more.
8 position height of reaction solution overflow port on first order reaction separating rectification tower (C) is higher than second order reaction separating rectification tower (D) the overflowing liquid import 10 on.
Strainer material in first order reaction separating rectification tower (C), second order reaction separating rectification tower (D) is 316L, filtering essence Degree is 50 mesh.

Claims (4)

1. a kind of tetrahydrofuran fractional order reaction separator, including head tank (A), charging pump (B), first order reaction separating rectification tower (C), second order reaction separating rectification tower (D), rear pump (E), it is characterised in that feed opening (1), bottom are equipped at the top of head tank (A) Equipped with outlet (2), head tank (A) passes through piping connection first order reaction point by piping connection charging pump (B), charging pump (B) Material inlet (3) from rectifying column (C), first order reaction separating rectification tower (C) tower bottom are equipped with catalyst emission mouth (4), lower part It is built-in with heat exchanger (5), following side is equipped with material inlet (3), middle part is equipped with catalyst addition mouth (31), top is built-in with condensation Device (26), middle part are packing layer (30), and packing layer (30) top is equipped with demister (29), tower top has reacting product outlet (25), Reaction solution overflow port (8) in the middle part of first order reaction separating rectification tower (C) passes through overflow pipe (9) and second order reaction separating rectification tower (D) overflowing liquid import (10) is connected;The second order reaction separating rectification tower bottom (D) is equipped with kettle base solution outlet (12) and catalyst row It puts mouth (13), tower reactor is built-in with heat exchanger (15), and middle part is packing layer (18), and the top of packing layer (18) is equipped with demister (19), top of tower is built-in with condenser (22), and tower top is equipped with reacting product outlet (23), and the middle part of tower is equipped with catalyst and mouth is added (17);The reaction product of the reacting product outlet (25) of first order reaction separating rectification tower (C), second order reaction separating rectification tower (D) Outlet (23) is connect by pipeline with Product pipeline (24) respectively, the kettle base solution outlet of the bottom second order reaction separating rectification tower (D) (12) it is connected with rear pump (E).
2. fractional order reaction separator according to claim 1, it is characterised in that first order reaction separating rectification tower (C's) urges The top that mouth (31) are located at reaction solution overflow port (8) is added in agent, and material inlet (3) reacts the lower part of liquid level, level-one in tower Strainer (32) are equipped at the reaction solution overflow port (8) of Reaction Separation rectifying column (C).
3. fractional order reaction separator according to claim 1, it is characterised in that second order reaction separating rectification tower (D's) urges Mouth (17) are added in the top of overflowing liquid import (10) and reaction liquid level, the kettle of the bottom second order reaction separating rectification tower (D) in agent Bottom liquid exports and is equipped with strainer (11) at (12).
4. fractional order reaction separator according to claim 1, it is characterised in that first order reaction separating rectification tower (C) it is anti- Hydrorrhea head piece (8) position is answered to be higher than the overflowing liquid import (10) of second order reaction separating rectification tower (D).
CN201820460628.3U 2018-04-03 2018-04-03 A kind of tetrahydrofuran fractional order reaction separator Active CN208182895U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111318236A (en) * 2020-03-02 2020-06-23 宁夏美邦寰宇化学有限公司 Device and method for preparing tetrahydrofuran
CN114456131A (en) * 2020-10-21 2022-05-10 中国石油化工股份有限公司 Tetrahydrofuran production system and preparation method

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111318236A (en) * 2020-03-02 2020-06-23 宁夏美邦寰宇化学有限公司 Device and method for preparing tetrahydrofuran
CN114456131A (en) * 2020-10-21 2022-05-10 中国石油化工股份有限公司 Tetrahydrofuran production system and preparation method

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