CN103626629A - Rectification method of 3-chlorine-2-methyl diphenyl - Google Patents
Rectification method of 3-chlorine-2-methyl diphenyl Download PDFInfo
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- CN103626629A CN103626629A CN201310552745.4A CN201310552745A CN103626629A CN 103626629 A CN103626629 A CN 103626629A CN 201310552745 A CN201310552745 A CN 201310552745A CN 103626629 A CN103626629 A CN 103626629A
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Abstract
The invention provides a rectification method of 3-chlorine-2-methyl diphenyl. The rectification method comprises the following steps: step one. preheating a hydrolysis material by using a preheater; step two. feeding the preheated hydrolysis material into a desolventizing tower so as to rectify the preheated hydrolysis material, and removing THF (tetrahydrofuran) and water in the hydrolysis material on the top of the desolventizing tower; step three. washing a material at the bottom of the desolventizing tower so as to obtain a wash material; step four. feeding the wash material obtained in the step three into a light component removal tower so as to remove light components in the wash material; and step five. feeding a material at the bottom of the light component removal tower in the step four into a buffer tank at the tower bottom, then feeding the materail into a finished product tower by using a feeding pump so as to rectify the material, thus obtaining the 3-chlorine-2-methyl diphenyl. Compared with the prior art, the rectification method of the 3-chlorine-2-methyl diphenyl has the advantages that the technology is simple, the rectification effect is good, the recovery rate of the 3-chlorine-2-methyl diphenyl product obtained by rectification is higher than or equal to 95%, and the purity of the 3-chlorine-2-methyl diphenyl product is higher than or equal to 98%.
Description
Technical field
The present invention relates to a kind of rectificating method, relate in particular to a kind of rectificating method of 3-chloro-2-methyl biphenyl.
Background technology
THF(Tetrahydrofuran, Chinese: tetrahydrofuran (THF)) be a kind of important organic synthesis raw material and be the solvent of excellent property.Tetrahydrofuran (THF) is heterocycle organic compound.It is one of the strongest polarity ethers, is used as a kind of solvent of middle polarity when chemical reaction and extraction.Colourless volatile liquid, has the smell of similar ether.Most organic solvents such as water-soluble, ethanol, ether, acetone, benzene.
In prior art, the rectificating method of 3-chloro-2-methyl biphenyl is difficult to obtain the 3-chloro-2-methyl biphenyl that purity is higher.
Therefore, be necessary to propose a kind of rectificating method of 3-chloro-2-methyl biphenyl.
Summary of the invention
The rectificating method that the object of the present invention is to provide a kind of 3-chloro-2-methyl biphenyl, its technique is simple, and rectification effect is good.
For reaching aforementioned object, the rectificating method of a kind of 3-chloro-2-methyl of the present invention biphenyl, it comprises the steps:
Step 1: through preheater preheating, wherein, described hydrolyzation material is by 15% salinity and solvent composition by hydrolyzation material, and described solvent is comprised of 56% A component, 44% B component;
Step 2: the hydrolyzation material after preheating is sent into and carried out rectifying in precipitation tower, the removed overhead the THF in hydrolyzation material and water from precipitation tower;
Step 3: the material of precipitation tower tower bottom in step 2 is washed to workshop section, obtain washing material;
Step 4: the washing material obtaining in step 3 is sent into and removed light constituent wherein in lightness-removing column;
Step 5: the material at the bottom of lightness-removing column tower in step 4 is entered to tower bottom buffering tank, then send into finishing column by take away pump and carry out rectifying, obtain 3-chloro-2-methyl biphenyl.
As a specific embodiment of the present invention, in step 1, the pH value of described hydrolyzation material is 1, described salt is divided into the mixture of magnesium chloride and sodium-chlor, described A component is comprised of THF, water, benzene, toluene and ethylbenzene, described B component is comprised of ortho-chlorotolu'ene, bromobenzene, 2,6-DCT, 2-methyl diphenyl, biphenyl, 3-chloro-2-methyl biphenyl and high boiling material.
As a specific embodiment of the present invention, in described A component, the content of THF is 61%, the content of water is 36%.
As a specific embodiment of the present invention, in step 3, the pH value of described washing material is 6-7, and described washing material component is:
2% THF, water, benzene, toluene and ethylbenzene;
5% ortho-chlorotolu'ene, bromobenzene, 2,6-DCT;
3% 2-methyl diphenyl, biphenyl;
80% 3-chloro-2-methyl biphenyl; And
10% high boiling material.
As a specific embodiment of the present invention, in the material of step 3, the content of THF is less than 2%.
As a specific embodiment of the present invention, in step 4, the pressure of lightness-removing column is negative pressure.
As a specific embodiment of the present invention, in step 4, light constituent comprises water, benzene, toluene, ethylbenzene, ortho-chlorotolu'ene, bromobenzene, 2-6-toluene dichloride, 2-methyl diphenyl and biphenyl.
As a specific embodiment of the present invention, in described step 5, also comprise and circulate de-gently by return to lightness-removing column without the completely de-light light constituent of processing, the described light constituent without completely de-light processing is mainly 2-methyl diphenyl and biphenyl.
Beneficial effect of the present invention: compared with prior art, the rectificating method of 3-chloro-2-methyl biphenyl of the present invention, technique is simple, and rectification effect is good, 3-chloro-2-methyl biphenyl product recovery rate >=95%, purity >=98% that rectifying obtains.
Embodiment
Below the present invention is described in further detail.
Alleged " embodiment " or " embodiment " refers to special characteristic, structure or the characteristic that can be contained at least one implementation of the present invention herein.Different local in this manual " in one embodiment " that occur not all refer to same embodiment, neither be independent or the embodiment mutually exclusive with other embodiment optionally.
Rectifying of the present invention is the operation under multi-component complex situation, the distillation system that adopts normal pressure and decompression and deposit, and 3-chloro-2-methyl biphenyl rectificating method of the present invention, it comprises the steps:
Step 1: by the hydrolyzation material of out-of-bounds sending here by flow control, through preheater preheating.Wherein, described hydrolyzation material is by 15% salinity and solvent composition, and the pH value of described hydrolyzation material is 1; Described solvent is comprised of 56% A component, 44% B component.Described A component is comprised of THF, water, benzene, toluene and ethylbenzene, and described B component is comprised of ortho-chlorotolu'ene, bromobenzene, 2,6-DCT, 2-methyl diphenyl, biphenyl, 3-chloro-2-methyl biphenyl and high boiling material.Wherein, in described A component, the content of THF is 61%, the content of water is 36%.In one embodiment, described salt is MgCl
2with the mixture of NaCl, wherein MgCl
2unrestricted with the blending ratio of NaCl.
Step 2: the hydrolyzation material after preheating is sent into and carried out rectifying, the removed overhead by the light constituent THF in hydrolyzation material from precipitation tower in precipitation tower.In precipitation tower, utilize the boiling point of THF low, first THF is distilled, because THF and water exist azeotropism, from the solution of precipitation column overhead condensation, be the mixture of THF and a small amount of water.In material after the separation of precipitation tower, the content of THF is less than 2%.In this step, benzene+toluene level≤3% in described THF decreasing ratio >=99.5%, recovery THF.In one embodiment, the number of times of atmospheric distillation is at least once.
Step 3: the material of precipitation tower tower bottom in step 2 is washed to workshop section, obtain washing material.Wherein, what washing workshop section adopted is soda lye wash, and then carries out oily water separation, and obtaining pH value is the neutrality washing material of 6-7.In this step, component and the content of described washing material are as follows:
2% THF, water, benzene, toluene and ethylbenzene;
5% ortho-chlorotolu'ene, bromobenzene, 2,6-DCT;
3% 2-methyl diphenyl, biphenyl;
80% 3-chloro-2-methyl biphenyl; And
10% high boiling material.
Step 4: the washing material obtaining in step 3 is sent into and removed light constituent wherein in lightness-removing column.This step adopts continuous negative pressure distillation technology, removes the light constituent in washing material: water, benzene, toluene, ethylbenzene, ortho-chlorotolu'ene, bromobenzene, 2,6-DCT, 2-methyl diphenyl and biphenyl.In one embodiment, the number of times of negative pressure rectifying is at least twice.
Step 5: the material at the bottom of lightness-removing column tower in step 4 is entered to tower bottom buffering tank, then send into finishing column by take away pump and carry out rectifying, obtain 3-chloro-2-methyl biphenyl.A small amount of light constituent of finishing column tower top enrichment is mainly 2-methyl diphenyl and biphenyl, and this light constituent returns to lightness-removing column and circulates de-ly light, at the qualified 3-chloro-2-methyl biphenyl product of finishing column middle part side line extraction, after cooling, sends out-of-bounds.High boiling material at the bottom of finishing column enters the height tank that boils, and sends out-of-bounds, processes in addition.In this embodiment, 3-chloro-2-methyl biphenyl product recovery rate >=95%, purity >=98%.
The treatment capacity of method hydrolyzation material of the present invention is 55～60t/d, and the treatment capacity of washing material is 20t/d.
The present invention utilizes the difference of each component volatilization ability in hydrolyzation material, by the backflow of liquid and gas, make gas, the reverse MULTI CONTACT of liquid two-phase, under the constraint of heat-driven and phase equilibrium relationship, volatile components (light constituent) is shifted constantly from liquid phase toward gas phase, and difficult volatiles is moved in liquid phase by gas phase, make mixture obtain continuous separation.In this process, heat transfer, mass transfer process are carried out simultaneously, belong to mass transfer process and control.Raw material enters tower from appropriate location, tower middle part, and tower is divided into two sections, and epimere is rectifying section, and not containing charging, hypomere is profit reduction and reserving section containing feed plate, and condenser provides liquid-phase reflux from tower top, and reboiler provides gas phase to reflux at the bottom of tower.
The rectificating method of 3-chloro-2-methyl biphenyl of the present invention, technique is simple, and rectification effect is good, 3-chloro-2-methyl biphenyl product recovery rate >=95%, purity >=98% that rectifying obtains.
Above-mentioned explanation has fully disclosed the specific embodiment of the present invention.It is pointed out that being familiar with any change that person skilled in art does the specific embodiment of the present invention does not all depart from the scope of claims of the present invention.Correspondingly, the scope of claim of the present invention is also not limited only to previous embodiment.
Claims (8)
1. a rectificating method for 3-chloro-2-methyl biphenyl, is characterized in that: it comprises the steps:
Step 1: through preheater preheating, wherein, described hydrolyzation material is by 15% salinity and solvent composition by hydrolyzation material, and described solvent is comprised of 56% A component, 44% B component;
Step 2: the hydrolyzation material after preheating is sent into and carried out rectifying in precipitation tower, the removed overhead the THF in hydrolyzation material and water from precipitation tower;
Step 3: the material of precipitation tower tower bottom in step 2 is washed to workshop section, obtain washing material;
Step 4: the washing material obtaining in step 3 is sent into and removed light constituent wherein in lightness-removing column;
Step 5: the material at the bottom of lightness-removing column tower in step 4 is entered to tower bottom buffering tank, then send into finishing column by take away pump and carry out rectifying, obtain 3-chloro-2-methyl biphenyl.
2. the rectificating method of 3-chloro-2-methyl biphenyl according to claim 1, it is characterized in that: in step 1, the pH value of described hydrolyzation material is 1, described salt is divided into the mixture of magnesium chloride and sodium-chlor, described A component is comprised of THF, water, benzene, toluene and ethylbenzene, described B component is comprised of ortho-chlorotolu'ene, bromobenzene, 2,6-DCT, 2-methyl diphenyl, biphenyl, 3-chloro-2-methyl biphenyl and high boiling material.
3. the rectificating method of 3-chloro-2-methyl biphenyl according to claim 2, is characterized in that: in described A component, the content of THF is 61%, the content of water is 36%.
4. the rectificating method of 3-chloro-2-methyl biphenyl according to claim 1, is characterized in that: in step 3, the pH value of described washing material is 6-7, and described washing material component is:
2% THF, water, benzene, toluene and ethylbenzene;
5% ortho-chlorotolu'ene, bromobenzene, 2,6-DCT;
3% 2-methyl diphenyl, biphenyl;
80% 3-chloro-2-methyl biphenyl; And
10% high boiling material.
5. the rectificating method of 3-chloro-2-methyl biphenyl according to claim 1, is characterized in that: in the material of step 3, the content of THF is less than 2%.
6. the rectificating method of 3-chloro-2-methyl biphenyl according to claim 1, is characterized in that: in step 4, the pressure of lightness-removing column is negative pressure.
7. the rectificating method of 3-chloro-2-methyl biphenyl according to claim 1, is characterized in that: in step 4, light constituent comprises water, benzene, toluene, ethylbenzene, ortho-chlorotolu'ene, bromobenzene, 2-6-toluene dichloride, 2-methyl diphenyl and biphenyl.
8. the rectificating method of 3-chloro-2-methyl biphenyl according to claim 1, it is characterized in that: in described step 5, also comprise and circulate de-gently by return to lightness-removing column without the completely de-light light constituent of processing, the described light constituent without completely de-light processing is mainly 2-methyl diphenyl and biphenyl.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4423234A (en) * | 1982-05-17 | 1983-12-27 | Fmc Corporation | Copper-catalyzed biaromatic coupling process |
| JPS63295520A (en) * | 1987-05-26 | 1988-12-01 | Yuki Gosei Yakuhin Kogyo Kk | Production of unsymmetrical biphenyl derivative |
| CN1935761A (en) * | 2006-09-27 | 2007-03-28 | 荆和祥 | Method for preparing 2-methyl-3-phenyl benzil alcohol |
| CN101130485A (en) * | 2007-08-24 | 2008-02-27 | 盐城科菲特生化技术有限公司 | Process for producing 2- methyl group -3- phenylbenzene methanol cleanly |
-
2013
- 2013-11-08 CN CN201310552745.4A patent/CN103626629B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4423234A (en) * | 1982-05-17 | 1983-12-27 | Fmc Corporation | Copper-catalyzed biaromatic coupling process |
| JPS63295520A (en) * | 1987-05-26 | 1988-12-01 | Yuki Gosei Yakuhin Kogyo Kk | Production of unsymmetrical biphenyl derivative |
| CN1935761A (en) * | 2006-09-27 | 2007-03-28 | 荆和祥 | Method for preparing 2-methyl-3-phenyl benzil alcohol |
| CN101130485A (en) * | 2007-08-24 | 2008-02-27 | 盐城科菲特生化技术有限公司 | Process for producing 2- methyl group -3- phenylbenzene methanol cleanly |
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Address after: 224100, No. two, No. 2, chemical industry zone, Dafeng Marine Economic Development Zone, Jiangsu, Yancheng City Province Patentee after: JIANGSU CONFIDENT BIOCHEMICAL TECHNOLOGY CO.,LTD. Address before: 224100 chemical industry zone of marine economic comprehensive development zone, Dafeng, Jiangsu, Yancheng City Patentee before: YANCHENG CONFIDENT BIOCHEMICAL TECHNOLOGY Co.,Ltd. |
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Effective date of registration: 20220420 Address after: 224100 6, Jinfeng South Street, Dafeng District, Yancheng City, Jiangsu. Patentee after: Dafeng District Productivity Promotion Center, Yancheng City Address before: 224100 No. 2, Weier Road, chemical industry park, Dafeng marine economic comprehensive development zone, Yancheng City, Jiangsu Province Patentee before: JIANGSU CONFIDENT BIOCHEMICAL TECHNOLOGY CO.,LTD. |
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Application publication date: 20140312 Assignee: JIANGSU HUIFENG BIO AGRICULTURE Co.,Ltd. Assignor: Dafeng District Productivity Promotion Center, Yancheng City Contract record no.: X2023980042603 Denomination of invention: Distillation method of 3-chloro-2-methylbiphenyl Granted publication date: 20150520 License type: Common License Record date: 20230926 |
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