CN104072327A - A preparing method of para-terphenyl - Google Patents
A preparing method of para-terphenyl Download PDFInfo
- Publication number
- CN104072327A CN104072327A CN201310101374.8A CN201310101374A CN104072327A CN 104072327 A CN104072327 A CN 104072327A CN 201310101374 A CN201310101374 A CN 201310101374A CN 104072327 A CN104072327 A CN 104072327A
- Authority
- CN
- China
- Prior art keywords
- terphenyl
- distillation
- biphenyl
- preparation
- product
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Abstract
The invention discloses a preparing method of para-terphenyl. A distillation residue liquid generated after biphenyl production by a high-temperature synthesis methods and biphenyl extraction by distillation is adopted as a raw material, and is subjected to secondary dissolution, filtration and secondary distillation to obtain the target product para-terphenyl. In specific, the method includes: (1) a step of fusion and filtration, namely a step of heating the distillation residue liquid, controlling the temperature to be 150-200 DEG C to fuse the residue liquid, and filtering 1-2 h later to remove mechanical impurities; (2) a step of dissolution, namely a step of dissolving the residue liquid with an organic solvent at 30-60 DEG C; and (3) a step of purification and separation, namely a step of distilling the product of the step (2) after the product is centrifuged and separated, subjecting the obtained solid to a repeat step (2), and performing secondary distillation after centrifugation and separation to obtain a target product. Compared with the prior art, the preparing method is more reasonable in process design, simpler in preparation conditions and safer and can obtain the para-terphenyl with extremely high purity.
Description
Technical field
The present invention relates to a kind of preparation method's of organic scintillation reagent, particularly a kind of p-terphenyl preparation method.
Background technology
P-terphenyl is a kind of organic scintillation reagent.In existing document, report that some methods of preparing p-terphenyl are as " Kirk-Othmer ", 2nd ed, vol. 7, pp.191-201,1963.What report is that the method that cuts the laggard one-step refining of narrow fraction from this mixing terphenyl of ortho-terphenyl, meta-terphenyl and p-terphenyl obtains.First, rectifying under the higher condition of reflux ratio, collects three cuts, and the cut of final stage is the mixture of meta-terphenyl and p-terphenyl.The fusing point of considering meta-terphenyl is 87.5 DEG C, and the fusing point of p-terphenyl is 212.7 DEG C, therefore this meta-terphenyl and p-terphenyl mixed fraction is cooled to 90-165 DEG C, maintains crystallization at this temperature, filtration, can obtain p-terphenyl product.This route need to be controlled at the mixture of a position and contraposition at 90-165 DEG C and filter, although now meta-terphenyl melting, but viscosity ratio is larger, be not easy to pass through filter cloth, it will be very difficult filtering, and the purity of the p-terphenyl obtaining also can only reach 99%, can not meet special user as the requirement of liquid crystal.
Summary of the invention
Technical problem to be solved by this invention is for the deficiencies in the prior art, provide a kind of design more reasonable, preparation condition is simple, safety and can obtain the preparation method that content is greater than 99.9% p-terphenyl, meets the particularly specific demand of LCD product of p-terphenyl user.
Technical problem to be solved by this invention is to realize by following technical scheme: a kind of preparation method of p-terphenyl, produce the vinasse that produces again of biphenyl as raw material after distillation extraction biphenyl taking high-temperature synthesis, obtain target product p-terphenyl through secondary dissolving, filtration, second distillation; Its concrete steps are as follows:
(1) melting, filtration: by vinasse heating, control temperature is 150-200 DEG C, makes its melting, removes by filter mechanical impurity after 1-2h;
(2) dissolve: at temperature 30-60 DEG C, with the above-mentioned raffinate of organic solvent dissolution;
(3) purify and separate: will after the centrifugation of previous step product, distill, gained solid is repeating step (2) again, and after centrifugation, second distillation obtains target product.
Vinasse described in step (1) is containing ortho-terphenyl, meta-terphenyl and p-terphenyl, and more than three accounts for the 80wt% of total amount, all the other are biphenyl and mix quaterphenyl.
Organic solvent described in step (2) is selected from the one in dehydrated alcohol, ethyl acetate or acetone.
The vacuum tightness of the distillation described in step (3) is 10-15 KPa, reflux ratio 3-10:1, and the aperture of described centrifugation filter bag used is 10-30 μ m.
Compared with prior art, technological design of the present invention is more reasonable, and preparation condition is simple, safety and can obtain the preparation method of the p-terphenyl of very high purity.
Embodiment
Below further describe concrete technical scheme of the present invention, so that those skilled in the art understands the present invention further, and do not form the restriction to its right.
A kind of preparation method of p-terphenyl, the by product vinasse that the method produces in the time that high-temperature synthesis is produced biphenyl after distillation extraction biphenyl is as raw material, (this vinasse is containing ortho-terphenyl, meta-terphenyl and p-terphenyl finally to obtain target product p-terphenyl through secondary dissolving, filtration, second distillation, more than three accounts for the 80wt% of total amount, all the other are biphenyl and mix quaterphenyl); Its step is as follows:
(1) melting, filtration: by the heating of biphenyl vinasse, control temperature is 150-200 DEG C, makes its melting; After 1-2h, filter, to remove mechanical impurity;
(2) dissolve: under temperature 30-60 DEG C condition, with this vinasse of anhydrous alcohol solution, p-terphenyl component is in addition dissolved as far as possible;
(3) centrifugation: by the whizzer centrifugation of previous step product, filter bag aperture is 10-30 μ m; Its solid part is mainly p-terphenyl;
(4) distillation: the solid product that centrifugation is obtained drops into rectifying tower reactor, underpressure distillation, vacuum tightness is 10-15 KPa, reflux ratio 3-10:1 will obtain purer p-terphenyl;
(5) dissolving, centrifugal again: by centrifugation again after previous step product repeating step (2);
(6) second distillation: by the underpressure distillation for the second time of previous step product, by the target product p-terphenyl that obtains content and be greater than 99.9%.
Embodiment 1
A p-terphenyl preparation method experiment, its concrete steps are as follows:
(1) in raw materials melt device, drop into the vinasse (it includes p-terphenyl 24wt%) producing when 50kg produces biphenyl with high-temperature synthesis, be heated to start agitator when temperature reaches 150-160 DEG C and stir 1-2h, in the time of the whole melting of material, open drain hole valve, after Stainless Steel Wire net filtration, flow in dissolving tank;
(2) dissolving tank is equipped with thermometer and electric mixer, and volume is 1m
3, in material, add 800L dehydrated alcohol, heat while stirring, temperature is controlled at 30-40 DEG C, keeps 1h;
(3), by the whizzer centrifugation of previous step product, filter bag aperture is 20 μ m.Solid in filtering bag of centrifuge is p-terphenyl (11kg), yield 82.5%, GC measurement result content approximately 90%;
(4) solid in filter bag obtained in the previous step is dropped into underpressure distillation in rectifying tower reactor, vacuum tightness is 15 KPa, and reflux ratio 5:1 will extract the p-terphenyl product (9kg) that obtains the about 98wt% of content, yield 89.1%;
(5) previous step product is dropped in dissolving tank again, add 700L dehydrated alcohol, heat while stirring, control temperature 30 DEG C ± 5, keep 1h;
(6) previous step product is used to whizzer centrifugation again, filter bag aperture is 50 μ m, and the solid in filter bag is p-terphenyl (8.4kg), yield 96.2%.GC measurement result content can reach 99%.
(7) this solid is dropped in rectifying tower reactor again, underpressure distillation, vacuum tightness is 10KPa, and reflux ratio 10:1 measures with GC after the target product obtaining oven dry, and target product p-terphenyl content is up to 99.9%.Weight is 7.8kg, yield 65%.
Embodiment 2
A p-terphenyl preparation method experiment, its concrete steps are as follows:
(1) in raw materials melt device, drop into the vinasse (it includes p-terphenyl 30wt%) producing when 100kg produces biphenyl with high-temperature synthesis, be heated to start agitator when temperature reaches 190-200 DEG C and stir 1-2h, in the time of the whole melting of material, open drain hole valve, after Stainless Steel Wire net filtration, flow in dissolving tank;
(2) dissolving tank is equipped with thermometer and electric mixer, and volume is 1m
3, in material, add 800L ethyl acetate, heat while stirring, temperature is controlled at 50-60 DEG C, keeps 1h;
(3), by the whizzer centrifugation of previous step product, filter bag aperture is 10 μ m.Solid in filtering bag of centrifuge is p-terphenyl (25kg), yield 83.3%, GC measurement result content approximately 88%;
(4) solid in filter bag obtained in the previous step is dropped into underpressure distillation in rectifying tower reactor, vacuum tightness is 10 KPa, and reflux ratio 3:1 will extract the p-terphenyl product (20.4kg) that obtains the about 97wt% of content, yield 81.6%;
(5) previous step product is dropped in dissolving tank again, add 800L ethyl acetate, heat while stirring, control temperature 60 DEG C ± 5, keep 1h;
(6) previous step product is used to whizzer centrifugation again, filter bag aperture is 30 μ m, and the solid in filter bag is p-terphenyl (18.3kg), yield 89.7%.GC measurement result content can reach 98.5%.
(7) this solid is dropped in rectifying tower reactor again, underpressure distillation, vacuum tightness is 12KPa, and reflux ratio 10:1 measures with GC after the target product obtaining oven dry, and target product p-terphenyl content is up to 99.9%.Weight is 17.5kg, yield 58%.
Claims (4)
1. a preparation method for p-terphenyl, is characterized in that described method produces the vinasse that produces after distillation extraction biphenyl again of biphenyl as raw material taking high-temperature synthesis, obtains target product p-terphenyl through secondary dissolving, filtration, second distillation; Its concrete steps are as follows:
(1) melting, filtration: by vinasse heating, control temperature is 150-200 DEG C, makes its melting, removes by filter mechanical impurity after 1-2h;
(2) dissolve: at temperature 30-60 DEG C, with the above-mentioned raffinate of organic solvent dissolution;
(3) purify and separate: will after the centrifugation of previous step product, distill, gained solid is repeating step (2) again, and after centrifugation, second distillation obtains target product.
2. the preparation method of p-terphenyl according to claim 1, is characterized in that the vinasse described in step (1) is containing ortho-terphenyl, meta-terphenyl and p-terphenyl, and more than three accounts for the 80wt% of total amount, all the other are biphenyl and mix quaterphenyl.
3. the preparation method of p-terphenyl according to claim 1, is characterized in that the organic solvent described in step (2) is selected from the one in dehydrated alcohol, ethyl acetate or acetone.
4. the preparation method of p-terphenyl according to claim 1, the vacuum tightness that it is characterized in that the distillation described in step (3) is 10-15 KPa, reflux ratio 3-10:1, the aperture of described centrifugation filter bag used is 10-30 μ m.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310101374.8A CN104072327A (en) | 2013-03-26 | 2013-03-26 | A preparing method of para-terphenyl |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310101374.8A CN104072327A (en) | 2013-03-26 | 2013-03-26 | A preparing method of para-terphenyl |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104072327A true CN104072327A (en) | 2014-10-01 |
Family
ID=51593979
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310101374.8A Pending CN104072327A (en) | 2013-03-26 | 2013-03-26 | A preparing method of para-terphenyl |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104072327A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2767518C1 (en) * | 2021-08-20 | 2022-03-17 | Общество с ограниченной ответственностью «БИОЛАЙТ» | Method of producing para-terphenyl of scintillation quality |
| CN114959872A (en) * | 2022-05-05 | 2022-08-30 | 北京工业大学 | Preparation method of p-terphenyl organic scintillation monocrystal |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS55167230A (en) * | 1979-06-14 | 1980-12-26 | Nippon Steel Chem Co Ltd | Separation and purification of terphenyl |
| US4250237A (en) * | 1977-05-25 | 1981-02-10 | Eastman Kodak Company | P-Terphenyl organic photoconductors and heterogeneous compositions thereof |
| SU1165677A1 (en) * | 1981-08-04 | 1985-07-07 | Предприятие П/Я В-8952 | Method of obtaining diphenyl |
| US20030082858A1 (en) * | 2001-10-10 | 2003-05-01 | Seiko Epson Corporation | Method for forming thin film and method for forming electronic device |
-
2013
- 2013-03-26 CN CN201310101374.8A patent/CN104072327A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4250237A (en) * | 1977-05-25 | 1981-02-10 | Eastman Kodak Company | P-Terphenyl organic photoconductors and heterogeneous compositions thereof |
| JPS55167230A (en) * | 1979-06-14 | 1980-12-26 | Nippon Steel Chem Co Ltd | Separation and purification of terphenyl |
| SU1165677A1 (en) * | 1981-08-04 | 1985-07-07 | Предприятие П/Я В-8952 | Method of obtaining diphenyl |
| US20030082858A1 (en) * | 2001-10-10 | 2003-05-01 | Seiko Epson Corporation | Method for forming thin film and method for forming electronic device |
Non-Patent Citations (1)
| Title |
|---|
| 傅伟安等: "对三联苯闪烁体的制备", 《原子能科学技术》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2767518C1 (en) * | 2021-08-20 | 2022-03-17 | Общество с ограниченной ответственностью «БИОЛАЙТ» | Method of producing para-terphenyl of scintillation quality |
| CN114959872A (en) * | 2022-05-05 | 2022-08-30 | 北京工业大学 | Preparation method of p-terphenyl organic scintillation monocrystal |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103570568A (en) | Clean production process of glycine in coproduction with ammonium chloride | |
| CN104910059A (en) | Dicumyl peroxide (DCP) apparatus circulating mother liquor recovery method | |
| CN104072327A (en) | A preparing method of para-terphenyl | |
| CN104059019B (en) | Caprolactam purification method and device | |
| CN106543156A (en) | It is a kind of to reduce epoxychloropropane residue in triglycidyl isocyanurate (TGIC) | |
| CN107266294A (en) | A kind of purification process of the guaiacol first product synthesized for catechol with methanol oxidation | |
| CN105111049B (en) | Preparation method of 2, 2'-dihydroxybiphenyl | |
| CN104262110A (en) | Method for preparing 4-tert-butyl-2-(alpha-methylbenzyl)phenol | |
| CN104311380B (en) | The method that coupling fusion-crystallization prepares high-purity biphenyl | |
| CN104479707B (en) | A kind of method for preparing needle coke | |
| CN104418706B (en) | The process for purification of two (2-hydroxyisopropyl) benzene | |
| CN106117094B (en) | A kind of method for reclaiming dimethyl sulfoxide (DMSO) DMSO abraum salt organic matters | |
| CN106928172A (en) | A kind of process for refining of dibenzofuran | |
| CN106748978A (en) | It is a kind of to extract the method for being coupled with rectifying and realizing the dehydration of 2 picolines | |
| CN102367181A (en) | Process for preparing potassium manganate by liquid phase method | |
| CN106431879A (en) | Method for separating all trans-teprenone under low temperature | |
| CN105566209A (en) | Purifying method of beta-trifluoromethylpyridine chloride | |
| CN102910638B (en) | Preparation method of anhydrous lithium metaborate | |
| CN104119261B (en) | A kind of preparation method of L-Glutimic acid | |
| CN102898303A (en) | Method for extracting methyl stearate from stearoylbenzoylmethane raffinate | |
| CN114591149A (en) | 6-tert-butyl metacresol purification system and method | |
| CN108409536A (en) | A method of recycling pentaerythrite from the alcoholysis liquid filter residue of antioxidant 1010 mother liquor | |
| CN111099953B (en) | Separation and purification method of isomer | |
| CN112341316A (en) | Method for preparing 2, 2' -dihydroxybiphenyl by using dibenzofuran fraction as raw material | |
| CN111056938A (en) | Purification method and purification device for pentaerythritol byproduct crude sodium formate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20141001 |