CN104262084B - The continuous distillation method of two (trichloromethyl) benzene and device - Google Patents
The continuous distillation method of two (trichloromethyl) benzene and device Download PDFInfo
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Abstract
The present invention relates to continuous distillation method and the device of a kind of two (trichloromethyl) benzene, enter after two (trichloromethyl) benzene crude product is preheated in the middle part of the 1st tower in three-tower rectification system, this tower steams thing and is partially in the middle part of the 2nd tower and carries out rectifying, the tower bottoms of the 1st tower and the 2nd tower all enters further rectifying in the middle part of the 3rd tower, steams available two (trichloromethyl) the benzene finished product of thing condensation from the 3rd column overhead.The present invention proposes a kind of two (trichloromethyl) continuous rectification production technology, has product purity high, and yield is high, low cost, low power consumption and other advantages.
Description
Technical field
The present invention relates to continuous distillation method and the device of a kind of two (trichloromethyl) benzene, especially relate to three tower continuous rectification methods and the device of a kind of two (trichloromethyl) benzene.
Background technology
Aramid fiber is that a class has high intensity, high-wearing feature, the special fibre of 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.World market is ever-increasing situation to the demand of aramid fiber, the coming years, and aramid fiber market, the whole world will increase with the high speed of annual about 20%.But due to reasons such as its technical difficulty are big, cost of investment is high, aramid fiber market is always by the monopolization of beautiful, Deng minority developed country.The Kevlar fiber of du pont company, the Technora fiber of Di Ren company of Japan are the matured products of position oneself at the forefront in the market.
Producing aramid fiber needs highly purified two (chloroformyl) benzene as initiation material, and otherwise aramid fiber difficult quality reaches regulation requirement.In prior art in the preparation method of two (chloroformyl) benzene; apply the thionyl chloride method most often with phthalic acid as raw material; but the phthalic acid needing purity to be 99.99% in this technique, cost is high, and this technique can produce byproduct hydrogen chloride and sulfur dioxide.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 isolation; being directly used in preparation two (chloroformyl) benzene, two (chloroformyl) the benzaldehyde product purity obtained after decompression distillation is 99%, does not reaches the requirement preparing aramid fiber.
The production technology of existing two (trichloromethyl) benzene is mainly with dimethylbenzene as raw material, and with radical initiator and/or light-initiated side chain free radical chlorination, two (trichloromethyl) benzene obtained takes recrystallization or vacuum distillation method to be purified further.But there is the problems such as production cost height, cycle length, low, the environmental pollution of yield in recrystallization method；There is the problems such as treating capacity is little, product yield is low, equipment investment is big, energy consumption is high, workman's intensity is big in vacuum distillation method.
In order to ensure two (trichloromethyl) benzaldehyde product Quality advance, can guarantee that again production efficiency, the purifying of two (trichloromethyl) benzene is used continuous rectificating technique.
Summary of the invention
Present invention aim at providing the continuous rectificating technique of a kind of two (trichloromethyl) benzene, solve the problems such as products obtained therefrom purity is low, treating 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:
The continuous distillation method of a kind of two (trichloromethyl) benzene, comprises the steps:
Entering in the middle part of the 1st tower in three-tower rectification system after (1) two (trichloromethyl) benzene crude product is preheated, the light component that tower top distills out enters and carries out further rectifying in the middle part of the 2nd tower；
(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 purified.
That discharges three-tower rectification system in step of the present invention (2) steams thing, it is optionally possible to carry out the most isolated and purified, and according to concrete conditions such as gains composition, purity, carries out utilizing legitimately.
The method of the invention, in the 1st tower, vacuum 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 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 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.
It is a further object of the present invention to provide the continuous rectification apparatus of a kind of two (trichloromethyl) benzene, including three rectifying columns and supporting reboiler thereof and condenser system, the 1st tower in three rectifying tower systems is that light component removes rectifying column continuously, 2nd tower is light Component seperation tower, and the 3rd tower is two (trichloromethyl) benzene rectifying column.
Device of the present invention, optionally, connects further after each condenser and has receiving slit.
Device of the present invention, tower bottom reboiler can use heating in tower body, it is possible to uses tower body external heat；Overhead condenser can use condensation in tower body, it is possible to uses tower body condensed exterior.
In device of the present invention, tower bottom reboiler can use steam or heat-conducting oil heating, it is preferred to use 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 under illumination condition and prepares.The optical source wavelength of reaction condition preferred illumination is about 350nm-700nm, light wave amplitude is the largest of about 200nm, wherein starting to be passed through chlorine under reaction temperature about 0 DEG C-85 DEG C, illuminance about 2000 Lux-about 55000 Lux, experience reaction temperature under described illuminance is no more than about first stage of reaction of 120 DEG C；Then continue to be passed through surplus chlorine until having reacted under higher reaction temperature.
In some preferred embodiments of the present invention, two (trichloromethyl) benzene crude product is obtained by three tower continuous prodution modes.
" about " of the present invention, refers to be worth variation up and down centered by this number less than 2.5 DEG C for temperature；For illuminance, refer to be worth variation up and down centered by this number less than 2500Lux；For wavelength, refer to be worth variation up and down centered by this number less than 5nm;For light wave amplitude, refer to be worth variation up and down centered by this number less than 3nm.
The beneficial effects of the present invention is:
(1) three tower continuous rectification techniques are introduced the purification process of two (trichloromethyl) benzene by the present invention, improving refined amount and the product quality of two (trichloromethyl) benzene, two (trichloromethyl) the benzaldehyde product purity after process for purification of the present invention processes reaches more than 99%；
(2) use three-tower rectification can realize running continuously due to two (trichloromethyl) benzene, improve equipment disposal ability and product yield, constant product quality, reduce energy consumption of rectification, and easily operated.
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 slit, two (trichloromethyl) benzene that 13-purifies
Detailed description of the invention
With detailed description of the invention, the present invention is described in further details below in conjunction with the accompanying drawings:
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 is steamed thing and is condensed by condenser (5), a part passes back into the 1st tower, remainder enters the 2nd tower (6) middle part, carries out rectifying through the 2nd tower reboiler (7) heating；2nd column overhead is steamed thing and is condensed by condenser (8), and a part passes back into the 2nd tower, and remainder 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 is steamed thing and is condensed by condenser (11), a part passes back into the 3rd tower, remainder is two (trichloromethyl) benzene (13) purified, it is mainly distillation residual liquid at the bottom of 3rd tower tower, proceeds to reclaim after residue receiving slit (12) processes.
Embodiment 1
1, the preparation of 3-bis-(trichloromethyl) benzene crude product: three enamel reaction towers with thermometric, reflux condenser, LED irradiation unit and heating-cooling device are composed in series serialization photochlorination apparatus, and wherein enamel reaction tower is followed successively by the first tower, the second tower and the 3rd tower.Reaction unit is through pressure testing, leak test, clean, it is dried after waiting the preparatory stage, start initial start-up, and gradually step up inventory, after optical chlorinating reaction is stable, 1, 3-bis-(methyl) benzene is added continuously the first tower with the speed of 95kg/h, mono-Ta Tawen controls at 80 DEG C ~ 120 DEG C by heating or cooling device, first tower incident light central peak wavelength is 460nm, in tower, average light illumination is 20000 ~ 39000Lux, simultaneously carry out continuous chlorination reaction from being passed through chlorine with the flow of 135kg/h at the bottom of tower, the speed controlling to be heated or cooled makes the first tower temperature less than 120 DEG C；The reactant liquor of the first tower is from overflowing 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 be passed through chlorine with the flow of 128kg/h in the second tower；The reactant liquor of the second tower is from overflowing 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, being passed through chlorine with the flow of 148kg/h in the 3rd tower, in the reaction system being made up of three towers, total is passed through amount of chlorine is 411kg/h.Sample from the 3rd tower outlet gained reactant mixture, gas chromatograph analyzes this sample, wherein 1, the purity of 3-bis-(trichloromethyl) benzene is 93.1%.
Purity is 93.1% 1 will obtained, 3-bis-(trichloromethyl) benzene crude product, it is heated to 100 DEG C via preheater (2) by the speed of 300 kg/h, it is continuously added to the 1st tower (3) middle part of three tower continuous rectification tower groups, 1st tower vacuum is 0.09MPa, heat through the 1st tower reboiler (4), 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, condensed by condenser (5), low boiling point component and a small amount of principal component 1, 3-bis-(trichloromethyl) benzene flows out from the 1st overhead condenser, partial reflux enters the 1st top of tower, part continuous print enters in the middle part of the 2nd tower, reflux ratio is 1.4；
2nd tower vacuum is 0.09MPa, heating through the 2nd tower reboiler (7), 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, is condensed by condenser (8), and a part is substantially free of principal component 1, the light component of 3-bis-(trichloromethyl) benzene, discharging 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 is 0.098MPa, heat through the 3rd tower reboiler (10), 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 is steamed thing and is condensed by condenser (11), a part passes back into the 3rd tower, reflux ratio is 2.7, remainder obtains 1 that purity is 99.3%, 3-bis-(trichloromethyl) benzene (13), 8 hourly average flow 252kg/h, with 1, 3-bis-(trichloromethyl) benzene meter, 8 hourly average rectification yields 84%, it is mainly distillation residual liquid at the bottom of 3rd tower tower, proceed to reclaim after residue receiving slit (12) processes.
Embodiment 2
1, the preparation of 4-bis-(trichloromethyl) benzene crude product: three enamel reaction towers with thermometric, reflux condenser, LED irradiation unit and heating-cooling device are composed in series serialization photochlorination apparatus, and wherein enamel reaction tower is followed successively by the first tower, the second tower and the 3rd tower.Reaction unit is through pressure testing, leak test, clean, it is dried after waiting the preparatory stage, start initial start-up, and gradually step up inventory, after optical chlorinating reaction is stable, 1, 4-bis-(methyl) benzene is added continuously the first tower with the speed of 100kg/h, mono-Ta Tawen controls at 80 DEG C ~ 120 DEG C by heating or cooling device, first tower incident light central peak wavelength is 470nm, in tower, average light illumination is 25000 ~ 37000Lux, simultaneously carry out continuous chlorination reaction from being passed through chlorine with the flow of 140kg/h at the bottom of tower, the speed controlling to be heated or cooled makes the first tower temperature less than 120 DEG C；The reactant liquor of the first tower is from overflowing 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 be passed through chlorine with the flow of 150kg/h in the second tower；The reactant liquor of the second tower is from overflowing 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, being passed through chlorine with the flow of 145kg/h in the 3rd tower, in the reaction system being made up of three towers, total is passed through amount of chlorine is 435kg/h.Sampling from the 3rd tower outlet gained reactant mixture, analyze this sample on gas chromatograph, wherein the purity of Isosorbide-5-Nitrae-two (trichloromethyl) benzene is 92.5%.
Purity is 92.5% 1 will obtained, 4-bis-(trichloromethyl) benzene crude product, it is heated to 120 DEG C via preheater (2) by the speed of 300 kg/h, it is continuously added to the 1st tower (3) middle part of three tower continuous rectification tower groups, 1st tower vacuum is 0.09MPa, heat through the 1st tower reboiler (4), 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, condensed by condenser (5), low boiling point component and a small amount of principal component 1, 4-bis-(trichloromethyl) benzene flows out from the 1st overhead condenser, partial reflux enters the 1st top of tower, part continuous print enters in the middle part of the 2nd tower, reflux ratio is 1.6；
2nd tower vacuum is 0.09MPa, heating through the 2nd tower reboiler (7), 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, is condensed by condenser (8), and a part is substantially free of principal component 1, the light component of 4-bis-(trichloromethyl) benzene, discharging 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 is 0.098MPa, heat through the 3rd tower reboiler, 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, the thing that steams of the 3rd tower is condensed by condenser (11), a part passes back into the 3rd tower, reflux ratio is 3.1, remainder obtains 1 that purity is 99.19%, 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%, it is mainly distillation residual liquid at the bottom of 3rd tower tower, proceed to reclaim after residue receiving slit (12) processes.
Embodiment 3
1, the preparation of 3-bis-(trichloromethyl) benzene crude product: three enamel reaction towers with thermometric, reflux condenser, LED irradiation unit and heating-cooling device are composed in series serialization photochlorination apparatus, and wherein enamel reaction tower is followed successively by the first tower, the second tower and the 3rd tower.Reaction unit is through pressure testing, leak test, clean, it is dried after waiting the preparatory stage, start initial start-up, and gradually step up inventory, after optical chlorinating reaction is stable, 1, 3-bis-(methyl) benzene is added continuously the first tower with the speed of 100kg/h, mono-Ta Tawen controls at 60 DEG C ~ 120 DEG C by heating or cooling device, first tower incident light central peak wavelength is 405nm, in tower, average light illumination is 5000 ~ 15000Lux, simultaneously carry out continuous chlorination reaction from being passed through chlorine with the flow of 142kg/h at the bottom of tower, the speed controlling to be heated or cooled makes the first tower temperature less than 120 DEG C；The reactant liquor of the first tower is from overflowing 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 be passed through chlorine with the flow of 148kg/h in the second tower；The reactant liquor of the second tower is from overflowing 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, being passed through chlorine with the flow of 147kg/h in the 3rd tower, in the reaction system being made up of three towers, total is passed through amount of chlorine is 437kg/h.Sample from the 3rd tower outlet gained reactant mixture, gas chromatograph analyzes this sample, wherein 1, the purity of 3-bis-(trichloromethyl) benzene is 84.2%.
Purity is 84.2% 1 will obtained, 3-bis-(trichloromethyl) benzene crude product, it is heated to 113 DEG C via preheater (2) by the speed of 300 kg/h, it is continuously added to the 1st tower (3) middle part of three tower continuous rectification tower groups, 1st tower vacuum is 0.09MPa, heat through the 1st tower reboiler (4), 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, condensed by condenser (5), low boiling point component and a small amount of principal component 1, 3-bis-(trichloromethyl) benzene flows out from the 1st overhead condenser, partial reflux enters the 1st top of tower, part continuous print enters in the middle part of the 2nd tower, reflux ratio is 1.8；
2nd tower vacuum is 0.09MPa, heating through the 2nd tower reboiler (7), 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, is condensed by condenser (8), and a part is substantially free of principal component 1, the light component of 3-bis-(trichloromethyl) benzene, discharging 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 is 0.098MPa, heat through the 3rd tower reboiler (10), 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 is steamed thing and is condensed by condenser (11), a part passes back into the 3rd tower, reflux ratio is 3.5, remainder obtains 1 that purity is 99.05 %, 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 %, it is mainly distillation residual liquid at the bottom of 3rd tower tower, proceed to reclaim after residue receiving slit (12) processes.
Two (trichloromethyl) benzene continuous rectificating technique technology and equipment that the present invention proposes are described by preferred embodiment, structure as herein described and equipment substantially can be modified in without departing from present invention, spirit and scope or suitably change and combine by person skilled, realizes 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 considered as being included in present invention spirit, scope and content.
Claims (5)
1. the continuous distillation method of (trichloromethyl) benzene, it is characterised in that comprise the steps:
Enter after (1) two (trichloromethyl) benzene crude product is preheated in the middle part of the 1st tower in three-tower rectification system, tower
The light component that top distills out enters and carries out further rectifying in the middle part of the 2nd tower；
(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
Steam thing, obtain two (trichloromethyl) benzene purified；
Described two (trichloromethyl) benzene crude product obtains by the following method: dimethylbenzene and chlorine are under illumination condition
Reaction prepares, reaction condition be the optical source wavelength of illumination be 350nm-700nm, light wave amplitude for maximum
200nm, wherein starts to be passed through chlorine under reaction temperature 0 DEG C-85 DEG C, illuminance 2000Lux-55000Lux,
Experience is the reaction temperature first stage of reaction less than 120 DEG C under described illuminance；Then in higher reaction
At a temperature of continue to be passed through surplus chlorine until having reacted.
The continuous distillation method of a kind of two (trichloromethyl) benzene the most according to claim 1, it is characterised in that step
That suddenly discharges three-tower rectification system in (2) steams thing, is further purified.
3., according to the continuous distillation method of two (trichloromethyl) benzene a kind of described in any one of claim 1-2, it is special
Levying and be that vacuum is 0.08～0.095MPa in the 1st tower, column bottom temperature is 145～210 DEG C, temperature in tower
Being 90～150 DEG C, tower top temperature is 80～130 DEG C, and reflux ratio is 1～2.
The continuous distillation method of a kind of two (trichloromethyl) benzene the most according to claim 1, it is characterised in that the
In 2 towers, vacuum is 0.08～0.095MPa, and 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.
The continuous distillation method of a kind of two (trichloromethyl) benzene the most according to claim 1, it is characterised in that the
In 3 towers, vacuum is 0.095～0.1MPa, and 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.
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Effective date of registration: 20160721 Address after: 223100 Huaian city of Jiangsu province Hongze County Bridge salt chemical industry zone, on the west side of TGI Avenue South Guo Applicant after: FININGS Co.,Ltd. Address before: 200122 Shanghai city Pudong New Area Pudian No. 438 Shuangge building room 16-C Applicant before: SHANGHAI FANGLUN NEW MATERIAL TECHNOLOGY Co.,Ltd. |
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Address after: 223100 west of Taibo Avenue and south of Guoqiao Road, salt chemical industry zone, Hongze County, Huai'an City, Jiangsu Province Patentee after: Fangyuan New Material Technology Co.,Ltd. Address before: 223100 west of Taibo Avenue and south of Guoqiao Road, salt chemical industry zone, Hongze County, Huai'an City, Jiangsu Province Patentee before: FININGS Co.,Ltd. |
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