CN104262084A - Process and device for continuous rectification of bis(trichloromethyl)benzene - Google Patents
Process and device for continuous rectification of bis(trichloromethyl)benzene Download PDFInfo
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Abstract
The invention relates to a process and a device for continuous rectification of bis(trichloromethyl)benzene. According to the method, bis(trichloromethyl)benzene crude product is preheated and enters the middle part of a first tower of a three-tower rectification system, the distillate part of the first tower enters the middle part of a second tower for rectification, the tower bottoms of the first tower and the second tower enter the middle part of a third tower for further rectification, the distillate part coming out from the tower top of the third tower is condensed to obtain bis(trichloromethyl)benzene. The process for producing bis(trichloromethyl)benzene provided by the invention has the advantages of high product purity, high yield, low cost, low energy consumption and the like.
Description
Technical field
The present invention relates to a kind of continuous distillation method and device of two (trichloromethyl) benzene, especially relate to a kind of three tower continuous rectification methods and device of two (trichloromethyl) benzene.
Background technology
Aramid fiber is the special fibre that a class has high strength, high-wearing feature, the advantageous property such as high temperature resistant.Due to the application performance that it is good, aramid fiber all has boundless application prospect in many industries.The demand of world market to aramid fiber is ever-increasing situation, the coming years, and global aramid fiber market will increase with the high speed of annual about 20%.But due to reasons such as its technical difficulty are large, cost of investment is high, aramid fiber market is monopolized by beautiful, Deng minority developed country always.The Kevlar fiber of du pont company, the Technora fiber of Japanese Di Ren company are the matured products of position oneself at the forefront in the market.
Producing aramid fiber needs highly purified two (chloroformyl) benzene as starting raw material, otherwise aramid fiber difficult quality reaches specified requirement.In prior art two (chloroformyl) benzene preparation method in; application is most often the sulfur oxychloride method of raw material with phthalic acid; but need in this technique purity be 99.99% phthalic acid, cost is high, and this technique can produce byproduct hydrogen chloride and sulfurous gas.Wang Lumin; at " study on the synthesis of chlorination reaction ", (institute of Tonghua Teachers College reports Cui Bingcun etc.; 2005; 26 (4): 46-47); by two (trichloromethyl) benzene of reaction preparation without separation; be directly used in preparation two (chloroformyl) benzene, two (chloroformyl) benzaldehyde product purity obtained after underpressure distillation is 99%, does not reach the requirement preparing aramid fiber.
The production technique of existing two (trichloromethyl) benzene is mainly raw material with dimethylbenzene, and with radical initiator and/or light-initiated side chain free radical chlorination, two (trichloromethyl) benzene obtained takes recrystallization or vacuum distillation method to carry out purifying further.But the problems such as production cost is high, the cycle is long, yield is low, environmental pollution that recrystallization method exists; There is the problems such as treatment capacity is little, product yield is low, facility investment is large, energy consumption is high, workman's intensity is large in vacuum distillation method.
In order to ensure two (trichloromethyl) benzaldehyde product Quality advance, can production efficiency be ensured again, continuous rectificating technique is adopted to the purifying of two (trichloromethyl) benzene.
Summary of the invention
The object of the invention is the continuous rectificating technique providing a kind of two (trichloromethyl) benzene, solves the problems such as products obtained therefrom purity is low, treatment capacity is little, product yield is low, efficiency is low, energy consumption is high in current purification process.
The present invention is realized by the following technical programs:
A kind of continuous distillation method of two (trichloromethyl) benzene, comprises the steps:
(1) two (trichloromethyl) benzene crude product enters in the middle part of the 1st tower in three-tower rectification system after preheating, and the light constituent that tower top distills out enters in the middle part of the 2nd tower and carries out further rectifying;
(2) the 2nd column overhead steam thing and discharge three-tower rectification system;
(3) the 1st towers and the 2nd tower tower bottoms enter in the middle part of the 3rd tower, carry out further rectifying, collect the 3rd column overhead and steam thing, obtain two (trichloromethyl) benzene of purifying.
That discharges three-tower rectification system in step of the present invention (2) steams thing, optionally, can carry out further separation and purification, and according to particular cases such as gains composition, purity, carry out utilizing legitimately.
The method of the invention, in the 1st tower, vacuum tightness is 0.08 ~ 0.095MPa, and column bottom temperature is 145 ~ 210 ° of C, and in tower, temperature is 90 ~ 150 ° of C, and tower top temperature is 80 ~ 130 ° of C, and reflux ratio is 1 ~ 2.
The method of the invention, in the 2nd tower, vacuum tightness is 0.08 ~ 0.095MPa, and column bottom temperature is 145 ~ 210 ° of C, and in tower, temperature is 75 ~ 120 ° of C, and tower top temperature is 65 ~ 120 ° of C, and reflux ratio is 1 ~ 2.
The method of the invention, in the 3rd tower, vacuum tightness is 0.095 ~ 0.1MPa, and column bottom temperature is 250 ~ 300 ° of C, and in tower, temperature is 175 ~ 200 ° of C, and tower top temperature is 145 ~ 170 ° of C, and reflux ratio is 2 ~ 4.
Another object of the present invention is to provide a kind of continuous rectification apparatus of two (trichloromethyl) benzene, comprise three rectifying tower and supporting reboiler thereof and condenser system, the 1st tower in three rectifying tower systems is that light constituent removes rectifying tower continuously, 2nd tower is light constituent knockout tower, and the 3rd tower is two (trichloromethyl) benzene rectifying tower.
Device of the present invention, optionally, is connected with Receiving bin after each condenser further.
Device of the present invention, tower bottom reboiler can adopt heating in tower body, also can adopt tower body external heat; Overhead condenser can adopt condensation in tower body, also can adopt tower body condensed exterior.
In device of the present invention, tower bottom reboiler can adopt steam or heat-conducting oil heating, preferably adopts heat-conducting oil heating.
Two (trichloromethyl) benzene crude product provided in the embodiment of the present invention can obtain by the following method: two (methyl) benzene and chlorine react and prepares under illumination condition.The optical source wavelength of reaction conditions preferred illumination is about 350nm-700nm, light wave width is the most about 200nm, wherein start to pass into chlorine under temperature of reaction about 0 DEG C-85 DEG C, illuminance about 2000 Lux-about 55000 Lux, experience the first step of reaction that temperature of reaction under described illuminance is no more than about 120 DEG C; Then continue to pass into residual content chlorine until reacted under higher temperature of reaction.
In preferred implementations more of the present invention, two (trichloromethyl) benzene crude product is obtained by three tower continuous prodution modes.
" about " of the present invention, refers to that for temperature centered by this number, be worth variation is up and down no more than 2.5 DEG C; For illuminance, refer to that centered by this number, be worth variation is up and down no more than 2500Lux; For wavelength, refer to that centered by this number, be worth variation is up and down no more than 5nm; For light wave width, refer to that centered by this number, be worth variation is up and down no more than 3nm.
Beneficial effect of the present invention is:
(1) three tower continuous rectification techniques are introduced the purification process of two (trichloromethyl) benzene by the present invention, improve refining amount and the quality product of two (trichloromethyl) benzene, two (trichloromethyl) benzaldehyde product purity after process for purification process of the present invention reaches more than 99%;
(2) because two (trichloromethyl) benzene adopts three-tower rectification can realize continuous operation, improve device processes ability and product yield, constant product quality, reduce energy consumption of rectification, and easy handling.
Accompanying drawing explanation
Fig. 1: two (trichloromethyl) benzene refining process schematic flow sheet;
Wherein, 1-bis-(trichloromethyl) benzene crude product, 2-preheater, 3-the 1st tower, 4-the 1st tower reboiler, 5-the 1st tower condenser, 6-the 2nd tower, 7-the 2nd tower reboiler, 8-the 2nd tower condenser, 9-the 3rd tower, 10-the 3rd tower reboiler, 11-the 3rd tower condenser, 12-residue Receiving bin, two (trichloromethyl) benzene of 13-purifying
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in further details:
As described in Figure 1, two (trichloromethyl) benzene crude product (1) enters the 1st tower (3) middle part via preheater (2), rectifying is carried out through the 1st tower reboiler (4) heating, 1st column overhead steams thing by condenser (5) condensation, a part passes back into the 1st tower, rest part enters the 2nd tower (6) middle part, carries out rectifying through the 2nd tower reboiler (7) heating; 2nd column overhead steams thing by condenser (8) condensation, and a part passes back into the 2nd tower, and rest part discharges three-tower rectification system; The tower bottoms of the 1st tower and the tower bottoms of the 2nd tower all enter the 3rd tower (9) middle part, further rectifying is carried out through the 3rd tower reboiler (10) heating, 3rd tower steams thing by condenser (11) condensation, a part passes back into the 3rd tower, rest part is two (trichloromethyl) benzene (13) of purifying, be mainly distillation residual liquid at the bottom of 3rd tower tower, reclaim after proceeding to residue Receiving bin (12) process.
Embodiment 1
1, the preparation of 3-bis-(trichloromethyl) benzene crude product: three lass lining reaction towers with thermometric, reflux exchanger, LED irradiating unit and heating-cooling device are composed in series serialization photochlorination apparatus, wherein lass lining reaction tower is followed successively by the first tower, the second tower and the 3rd tower.Reaction unit is through pressure testing, leak test, cleaning, after drying waits the preparatory stage, start initial start-up, and improve charging capacity gradually, after optical chlorinating reaction is stable, 1, 3-bis-(methyl) benzene adds the first tower continuously with the speed of 95kg/h, mono-Ta Tawen controls at 80 DEG C ~ 120 DEG C by heating or refrigerating unit, first tower incident light central peak wavelength is 460nm, in tower, average light illumination is 20000 ~ 39000Lux, at the bottom of tower, pass into chlorine with the flow of 135kg/h carries out continuous chlorination reaction simultaneously, the speed controlling heating or cooling makes the first tower temperature be no more than 120 DEG C, the reaction solution of the first tower overflows to the second tower at the bottom of tower, second tower incident light central peak wavelength is 505nm, average light illumination in second tower is 40000 ~ 61000 Lux, and the second tower temperature controls, at 135 ~ 145 DEG C, to pass into chlorine with the flow of 128kg/h in the second tower, the reaction solution of the second tower overflows to the 3rd tower at the bottom of tower, 3rd tower incident light central peak wavelength is 586nm, average light illumination in 3rd tower is 60000 ~ 86000 Lux, 3rd tower temperature controls at 170 ~ 180 DEG C, in the 3rd tower, pass into chlorine with the flow of 148kg/h, in the reaction system be made up of three towers, total passes into amount of chlorine is 411kg/h.Sample from the 3rd tower outlet gained reaction mixture, gas chromatograph is analyzed this sample, and wherein the purity of 1,3-bis-(trichloromethyl) benzene is 93.1%.
Be 93.1% 1 by the purity obtained, 3-bis-(trichloromethyl) benzene crude product, 100 DEG C are heated to via preheater (2) by the speed of 300 kg/h, join the 1st tower (3) middle part of three tower continuous rectification tower groups continuously, 1st tower vacuum tightness is 0.09MPa, through the 1st tower reboiler (4) heating, maintaining column bottom temperature is 165 ~ 175 DEG C, in tower, temperature is 100 ~ 130 DEG C, tower top temperature is 85 ~ 110 DEG C, 1st column overhead steams thing, by condenser (5) condensation, low boiling point component and a small amount of principal constituent 1, 3-bis-(trichloromethyl) benzene flows out from the 1st overhead condenser, partial reflux enters the 1st top of tower, partial continuous enter in the middle part of the 2nd tower, reflux ratio is 1.4,
2nd tower vacuum tightness is 0.09MPa, through the 2nd tower reboiler (7) heating, maintaining column bottom temperature is 165 ~ 175 DEG C, and in tower, temperature is 80 ~ 100 DEG C, tower top temperature is 75 ~ 95 DEG C, 2nd column overhead steams thing, and by condenser (8) condensation, a part is not substantially containing principal constituent 1, the light constituent of 3-bis-(trichloromethyl) benzene, discharge three-tower rectification system, a part passes back into the 2nd tower, and reflux ratio is 1.0;
The tower bottoms of the 1st tower and the tower bottoms of the 2nd tower are mixed into the 3rd tower (9) middle part, 3rd tower vacuum tightness is 0.098MPa, through the 3rd tower reboiler (10) heating, maintaining column bottom temperature is 270 ~ 290 DEG C, in tower, temperature is 180 ~ 190 DEG C, tower top temperature is 150 ~ 160 DEG C, 3rd tower steams thing by condenser (11) condensation, a part passes back into the 3rd tower, reflux ratio is 2.7, rest part obtain that purity is 99.3% 1, 3-bis-(trichloromethyl) benzene (13), 8 hourly average flow 252kg/h, with 1, 3-bis-(trichloromethyl) benzene meter, 8 hourly average rectification yields 84%, distillation residual liquid is mainly at the bottom of 3rd tower tower, reclaim after proceeding to residue Receiving bin (12) process.
Embodiment 2
1, the preparation of 4-bis-(trichloromethyl) benzene crude product: three lass lining reaction towers with thermometric, reflux exchanger, LED irradiating unit and heating-cooling device are composed in series serialization photochlorination apparatus, wherein lass lining reaction tower is followed successively by the first tower, the second tower and the 3rd tower.Reaction unit is through pressure testing, leak test, cleaning, after drying waits the preparatory stage, start initial start-up, and improve charging capacity gradually, after optical chlorinating reaction is stable, 1, 4-bis-(methyl) benzene adds the first tower continuously with the speed of 100kg/h, mono-Ta Tawen controls at 80 DEG C ~ 120 DEG C by heating or refrigerating unit, first tower incident light central peak wavelength is 470nm, in tower, average light illumination is 25000 ~ 37000Lux, at the bottom of tower, pass into chlorine with the flow of 140kg/h carries out continuous chlorination reaction simultaneously, the speed controlling heating or cooling makes the first tower temperature be no more than 120 DEG C, the reaction solution of the first tower overflows to the second tower at the bottom of tower, second tower incident light central peak wavelength is 502nm, average light illumination in second tower is 45000 ~ 61000 Lux, and the second tower temperature controls, at 135 ~ 145 DEG C, to pass into chlorine with the flow of 150kg/h in the second tower, the reaction solution of the second tower overflows to the 3rd tower at the bottom of tower, 3rd tower incident light central peak wavelength is 555nm, average light illumination in 3rd tower is 70000 ~ 85000 Lux, 3rd tower temperature controls at 170 ~ 180 DEG C, in the 3rd tower, pass into chlorine with the flow of 145kg/h, in the reaction system be made up of three towers, total passes into amount of chlorine is 435kg/h.Sample from the 3rd tower outlet gained reaction mixture, gas chromatograph is analyzed this sample, and wherein the purity of Isosorbide-5-Nitrae-two (trichloromethyl) benzene is 92.5%.
Be 92.5% 1 by the purity obtained, 4-bis-(trichloromethyl) benzene crude product, 120 DEG C are heated to via preheater (2) by the speed of 300 kg/h, join the 1st tower (3) middle part of three tower continuous rectification tower groups continuously, 1st tower vacuum tightness is 0.09MPa, through the 1st tower reboiler (4) heating, maintaining column bottom temperature is 175 ~ 195 DEG C, in tower, temperature is 120 ~ 140 DEG C, tower top temperature is 110 ~ 120 DEG C, 1st column overhead steams thing, by condenser (5) condensation, low boiling point component and a small amount of principal constituent 1, 4-bis-(trichloromethyl) benzene flows out from the 1st overhead condenser, partial reflux enters the 1st top of tower, partial continuous enter in the middle part of the 2nd tower, reflux ratio is 1.6,
2nd tower vacuum tightness is 0.09MPa, through the 2nd tower reboiler (7) heating, maintaining column bottom temperature is 165 ~ 175 DEG C, and in tower, temperature is 100 ~ 110 DEG C, tower top temperature is 95 ~ 105 DEG C, 2nd column overhead steams thing, and by condenser (8) condensation, a part is not substantially containing principal constituent 1, the light constituent of 4-bis-(trichloromethyl) benzene, discharge three-tower rectification system, a part passes back into the 2nd tower, and reflux ratio is 1.1;
The tower bottoms of the 1st tower and the tower bottoms of the 2nd tower are mixed into the 3rd tower (9) middle part, 3rd tower vacuum tightness is 0.098MPa, through the 3rd tower reboiler heating, maintaining column bottom temperature is 280 ~ 300 DEG C, in tower, temperature is 180 ~ 190 DEG C, tower top temperature is 150 ~ 160 DEG C, 3rd tower steam thing by condenser (11) condensation, a part passes back into the 3rd tower, reflux ratio is 3.1, rest part obtain that purity is 99.19% 1, 4-bis-(trichloromethyl) benzene (13), 8 hourly average flow 230kg/h, with 1, 4-bis-(trichloromethyl) benzene meter, 8 hourly average rectification yields 82.2%, distillation residual liquid is mainly at the bottom of 3rd tower tower, reclaim after proceeding to residue Receiving bin (12) process.
Embodiment 3
1, the preparation of 3-bis-(trichloromethyl) benzene crude product: three lass lining reaction towers with thermometric, reflux exchanger, LED irradiating unit and heating-cooling device are composed in series serialization photochlorination apparatus, wherein lass lining reaction tower is followed successively by the first tower, the second tower and the 3rd tower.Reaction unit is through pressure testing, leak test, cleaning, after drying waits the preparatory stage, start initial start-up, and improve charging capacity gradually, after optical chlorinating reaction is stable, 1, 3-bis-(methyl) benzene adds the first tower continuously with the speed of 100kg/h, mono-Ta Tawen controls at 60 DEG C ~ 120 DEG C by heating or refrigerating unit, first tower incident light central peak wavelength is 405nm, in tower, average light illumination is 5000 ~ 15000Lux, at the bottom of tower, pass into chlorine with the flow of 142kg/h carries out continuous chlorination reaction simultaneously, the speed controlling heating or cooling makes the first tower temperature be no more than 120 DEG C, the reaction solution of the first tower overflows to the second tower at the bottom of tower, second tower incident light central peak wavelength is 465nm, average light illumination in second tower is 20000 ~ 35000 Lux, and the second tower temperature controls, at 130 ~ 140 DEG C, to pass into chlorine with the flow of 148kg/h in the second tower, the reaction solution of the second tower overflows to the 3rd tower at the bottom of tower, 3rd tower incident light central peak wavelength is 505nm, average light illumination in 3rd tower is 42000 ~ 55000 Lux, 3rd tower temperature controls at 170 ~ 180 DEG C, in the 3rd tower, pass into chlorine with the flow of 147kg/h, in the reaction system be made up of three towers, total passes into amount of chlorine is 437kg/h.Sample from the 3rd tower outlet gained reaction mixture, gas chromatograph is analyzed this sample, and wherein the purity of 1,3-bis-(trichloromethyl) benzene is 84.2%.
Be 84.2% 1 by the purity obtained, 3-bis-(trichloromethyl) benzene crude product, 113 DEG C are heated to via preheater (2) by the speed of 300 kg/h, join the 1st tower (3) middle part of three tower continuous rectification tower groups continuously, 1st tower vacuum tightness is 0.09MPa, through the 1st tower reboiler (4) heating, maintain column bottom temperature 165 ~ 175 DEG C, in tower, temperature is 100 ~ 125 DEG C, tower top temperature is 87 ~ 108 DEG C, 1st column overhead steams thing, by condenser (5) condensation, low boiling point component and a small amount of principal constituent 1, 3-bis-(trichloromethyl) benzene flows out from the 1st overhead condenser, partial reflux enters the 1st top of tower, partial continuous enter in the middle part of the 2nd tower, reflux ratio is 1.8,
2nd tower vacuum tightness is 0.09MPa, through the 2nd tower reboiler (7) heating, maintaining column bottom temperature is 165 ~ 175 DEG C, and in tower, temperature is 80 ~ 100 DEG C, tower top temperature is 75 ~ 95 DEG C, 2nd column overhead steams thing, and by condenser (8) condensation, a part is not substantially containing principal constituent 1, the light constituent of 3-bis-(trichloromethyl) benzene, discharge three-tower rectification system, a part passes back into the 2nd tower, and reflux ratio is 1.0;
The tower bottoms of the 1st tower and the tower bottoms of the 2nd tower all enter the 3rd tower (9) middle part, 3rd tower vacuum tightness is 0.098MPa, through the 3rd tower reboiler (10) heating, maintaining column bottom temperature is 280 ~ 290 DEG C, in tower, temperature is 180 ~ 190 DEG C, tower top temperature is 150 ~ 160 DEG C, 3rd tower steams thing by condenser (11) condensation, a part passes back into the 3rd tower, reflux ratio is 3.5, rest part obtain that purity is 99.05 % 1, 3-bis-(trichloromethyl) benzene (13), 8 hourly average flow 206.3kg/h, with 1, 3-bis-(trichloromethyl) benzene meter, 8 hourly average rectification yield 80.9 %, distillation residual liquid is mainly at the bottom of 3rd tower tower, reclaim after proceeding to residue Receiving bin (12) process.
Two (trichloromethyl) benzene continuous rectificating technique technology that the present invention proposes and equipment are described by preferred embodiment, person skilled obviously can not depart from content of the present invention, spirit and scope structure as herein described and equipment are changed or suitably change with combination, realize the technology of the present invention.Special needs to be pointed out is, all similar replacements and change apparent to those skilled in the art, they are deemed to be included in spirit of the present invention, scope and content.
Claims (10)
1. the continuous distillation method of two (trichloromethyl) benzene, is characterized in that comprising the steps:
(1) two (trichloromethyl) benzene crude product enters in the middle part of the 1st tower in three-tower rectification system after preheating, and the light constituent that tower top distills out enters in the middle part of the 2nd tower and carries out further rectifying;
(2) the 2nd column overhead steam thing and discharge three-tower rectification system;
(3) the 1st towers and the 2nd tower tower bottoms enter in the middle part of the 3rd tower, carry out further rectifying, collect the 3rd column overhead and steam thing, obtain two (trichloromethyl) benzene of purifying.
2. the continuous distillation method of a kind of two (trichloromethyl) benzene according to claim 1, what it is characterized in that discharging in step (2) three-tower rectification system steams thing, optionally, can be further purified.
3. a kind of continuous distillation method of two (trichloromethyl) benzene according to any one of claim 1-2, it is characterized in that in the 1st tower, vacuum tightness is 0.08 ~ 0.095MPa, column bottom temperature is 145 ~ 210 DEG C, and in tower, temperature is 90 ~ 150 DEG C, tower top temperature is 80 ~ 130 DEG C, and reflux ratio is 1 ~ 2.
4. a kind of continuous distillation method of two (trichloromethyl) benzene according to any one of claim 1-3, it is characterized in that in the 2nd tower, vacuum tightness is 0.08 ~ 0.095MPa, column bottom temperature is 145 ~ 210 DEG C, and in tower, temperature is 75 ~ 120 DEG C, tower top temperature is 65 ~ 120 DEG C, and reflux ratio is 1 ~ 2.
5. a kind of continuous distillation method of two (trichloromethyl) benzene according to claim 1-4, it is characterized in that in the 3rd tower, vacuum tightness is 0.095 ~ 0.1 MPa, column bottom temperature is 250 ~ 300 DEG C, and in tower, temperature is 175 ~ 200 DEG C, tower top temperature is 145 ~ 170 DEG C, and reflux ratio is 2 ~ 4.
6. method according to any one of claim 1-5, is characterized in that two (trichloromethyl) benzene crude product can obtain by the following method: two (methyl) benzene and chlorine react and prepares under illumination condition.
7. implement the claims a device for method described in 1 ~ 6 any one, comprise three rectifying tower and supporting reboiler thereof and condenser system.
8. device according to claim 7, is characterized in that reboiler can adopt heating in tower body, also can adopt tower body external heat; Condenser can adopt condensation in tower body, also can adopt tower body condensed exterior.
9. device according to claim 7, is characterized in that tower bottom reboiler can adopt steam or heat-conducting oil heating, preferably adopts heat-conducting oil heating.
10. device according to claim 7, is characterized in that optionally, is connected with Receiving bin further after each condenser.
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