CN103626629B - Rectification method of 3-chlorine-2-methyl diphenyl - Google Patents
Rectification method of 3-chlorine-2-methyl diphenyl Download PDFInfo
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- CN103626629B CN103626629B CN201310552745.4A CN201310552745A CN103626629B CN 103626629 B CN103626629 B CN 103626629B CN 201310552745 A CN201310552745 A CN 201310552745A CN 103626629 B CN103626629 B CN 103626629B
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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, particularly relate 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.Water-soluble, most organic solvent such as ethanol, ether, acetone, benzene.
Be difficult to obtain the higher 3-chloro-2-methyl biphenyl of purity to the rectificating method of 3-chloro-2-methyl biphenyl in prior art.
Therefore, the rectificating method proposing a kind of 3-chloro-2-methyl biphenyl is necessary.
Summary of the invention
The object of the present invention is to provide a kind of rectificating method 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 one: by hydrolyzation material through preheater preheats, wherein, described hydrolyzation material by 15% salinity and solvent composition, described solvent is made up of the component A of 56%, the B component of 44%;
Step 2: sent in precipitation tower by the hydrolyzation material after preheating and carry out rectifying, the THF in hydrolyzation material and the water removed overhead from precipitation tower;
Step 3: the material of precipitation tower tower bottom in step 2 is carried out washing workshop section, obtains washing material;
Step 4: the washing material obtained in step 3 is sent in lightness-removing column the light constituent removed wherein;
Step 5: the material in step 4 at the bottom of lightness-removing column tower is entered tower bottom buffering tank, then carry out rectifying by take away pump feeding finishing column, obtain 3-chloro-2-methyl biphenyl.
As a specific embodiment of the present invention, in step, the pH value of described hydrolyzation material is 1, described salt is divided into the mixture of magnesium chloride and sodium-chlor, described component A is made up of THF, water, benzene, toluene and ethylbenzene, described B component is made up 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 component A, 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:
The THF of 2%, water, benzene, toluene and ethylbenzene;
Ortho-chlorotolu'ene, bromobenzene, the 2,6-DCT of 5%;
2-methyl diphenyl, the biphenyl of 3%;
The 3-chloro-2-methyl biphenyl of 80%; And
The high boiling material of 10%.
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, also comprise in described step 5 and the light constituent without completely de-light process returned lightness-removing column to carry out circulation de-light, be describedly mainly 2-methyl diphenyl and biphenyl without the completely de-light constituent gently processed.
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 herein " embodiment " or " embodiment " refers to special characteristic, structure or the characteristic that can be contained at least one implementation of the present invention.Different local in this manual " in one embodiment " occurred not all refers to same embodiment, neither be independent or optionally mutually exclusive with other embodiments embodiment.
Rectifying of the present invention is the operation under multi-component complex situation, and adopt normal pressure and decompression and the distillation system deposited, 3-chloro-2-methyl biphenyl rectificating method of the present invention, it comprises the steps:
Step one: by the hydrolyzation material out-of-bounds sent here by flow control, through preheater preheats.Wherein, described hydrolyzation material by 15% salinity and solvent composition, the pH value of described hydrolyzation material is 1; Described solvent is made up of the component A of 56%, the B component of 44%.Described component A is made up of THF, water, benzene, toluene and ethylbenzene, and described B component is made up of ortho-chlorotolu'ene, bromobenzene, 2,6-DCT, 2-methyl diphenyl, biphenyl, 3-chloro-2-methyl biphenyl and high boiling material.Wherein, in described component A, 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 in precipitation tower and carries out rectifying, by the removed overhead of the light constituent THF in hydrolyzation material from precipitation tower.In precipitation tower, utilizing the boiling point of THF low, first distilled by THF, because THF and water exist azeotropism, is the mixture of THF and a small amount of water from the solution of precipitation column overhead condensation.In material after precipitation tower is separated, 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 carried out washing workshop section, obtains washing material.Wherein, what washing workshop section adopted is soda lye wash, and then carries out oily water separation, obtains the neutrality washing material that pH value is 6-7.In this step, component and the content of described washing material are as follows:
The THF of 2%, water, benzene, toluene and ethylbenzene;
Ortho-chlorotolu'ene, bromobenzene, the 2,6-DCT of 5%;
2-methyl diphenyl, the biphenyl of 3%;
The 3-chloro-2-methyl biphenyl of 80%; And
The high boiling material of 10%.
Step 4: the washing material obtained in step 3 is sent in lightness-removing column the light constituent removed wherein.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 in step 4 at the bottom of lightness-removing column tower is entered tower bottom buffering tank, then carry out rectifying by take away pump feeding finishing column, obtain 3-chloro-2-methyl biphenyl.A small amount of light constituent mainly 2-methyl diphenyl and biphenyl of finishing column tower top enrichment, this light constituent returns lightness-removing column, and to carry out circulation de-light, and the 3-chloro-2-methyl biphenyl product that side take-off is qualified in the middle part of finishing column, sends out-of-bounds after cooling.High boiling material at the bottom of finishing column then enters height and to boil tank, 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 constantly shifted toward gas phase from liquid phase, and difficult volatiles is moved in liquid phase by gas phase, mixture is constantly separated.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 in the middle part of tower, and tower is divided into two sections, epimere is rectifying section, and not containing charging, hypomere is profit reduction and reserving sections 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 fully discloses the specific embodiment of the present invention.It is pointed out that the scope be familiar with person skilled in art and any change that the specific embodiment of the present invention is done all do not departed to claims of the present invention.Correspondingly, the scope of claim of the present invention is also not limited only to previous embodiment.
Claims (6)
1. a rectificating method for 3-chloro-2-methyl biphenyl, is characterized in that: it comprises the steps:
Step one: by hydrolyzation material through preheater preheats, wherein, described hydrolyzation material by 15% salinity and solvent composition, described solvent is made up of the component A of 56%, the B component of 44%;
Step 2: sent in precipitation tower by the hydrolyzation material after preheating and carry out rectifying, the THF in hydrolyzation material and the water removed overhead from precipitation tower;
Step 3: the material of precipitation tower tower bottom in step 2 is carried out washing workshop section, obtains washing material;
Step 4: the washing material obtained in step 3 is sent in lightness-removing column the light constituent removed wherein;
Step 5: the material in step 4 at the bottom of lightness-removing column tower is entered tower bottom buffering tank, then carry out rectifying by take away pump feeding finishing column, obtain 3-chloro-2-methyl biphenyl,
In step, the pH value of described hydrolyzation material is 1, described salt is divided into the mixture of magnesium chloride and sodium-chlor, described component A is made up of THF, water, benzene, toluene and ethylbenzene, described B component is by ortho-chlorotolu'ene, bromobenzene, 2,6-toluene dichloride, 2-methyl diphenyl, biphenyl, 3-chloro-2-methyl biphenyl and high boiling material form
In described component A, the content of THF is 61%, the content of water is 36%.
2. the rectificating method of 3-chloro-2-methyl biphenyl according to claim 1, is characterized in that: in step 3, and the pH value of described washing material is 6-7, and described washing material component is:
The THF of 2%, water, benzene, toluene and ethylbenzene;
Ortho-chlorotolu'ene, bromobenzene, the 2,6-DCT of 5%;
2-methyl diphenyl, the biphenyl of 3%;
The 3-chloro-2-methyl biphenyl of 80%; And
The high boiling material of 10%.
3. 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%.
4. the rectificating method of 3-chloro-2-methyl biphenyl according to claim 1, is characterized in that: in step 4, and the pressure of lightness-removing column is negative pressure.
5. the rectificating method of 3-chloro-2-methyl biphenyl according to claim 1, is characterized in that: in step 4, and light constituent comprises water, benzene, toluene, ethylbenzene, ortho-chlorotolu'ene, bromobenzene, 2,6-DCT, 2-methyl diphenyl and biphenyl.
6. the rectificating method of 3-chloro-2-methyl biphenyl according to claim 1, it is characterized in that: also comprise in described step 5 and the light constituent without completely de-light process returned lightness-removing column to carry out circulation de-light, be describedly mainly 2-methyl diphenyl and biphenyl without the completely de-light constituent gently processed.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4423234A (en) * | 1982-05-17 | 1983-12-27 | Fmc Corporation | Copper-catalyzed biaromatic coupling process |
| 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 |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0825922B2 (en) * | 1987-05-26 | 1996-03-13 | 有機合成薬品工業株式会社 | Process for producing asymmetric biphenyl derivative |
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2013
- 2013-11-08 CN CN201310552745.4A patent/CN103626629B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4423234A (en) * | 1982-05-17 | 1983-12-27 | Fmc Corporation | Copper-catalyzed biaromatic coupling process |
| 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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