CN103524288B - A kind of method of purification of durol - Google Patents
A kind of method of purification of durol Download PDFInfo
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- CN103524288B CN103524288B CN201310467290.6A CN201310467290A CN103524288B CN 103524288 B CN103524288 B CN 103524288B CN 201310467290 A CN201310467290 A CN 201310467290A CN 103524288 B CN103524288 B CN 103524288B
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Abstract
The present invention relates to a kind of method of purification of durol, durol solution (4) enters in freezing and crystallizing device (1) and carries out freezing and crystallizing, the discharge (12) entering (11) and heat-eliminating medium of this freezing and crystallizing device heat-eliminating medium, obtain low-temperature receiver, after freezing and crystallizing, obtain the durol xln (5) containing crystalline mother solution; Be separated by crystalline mother solution with centrifugal separating device (2), obtain crystalline mother solution (7) and centrifugal rear solid phase prod (6), this solid phase prod adopts squeezing machine (3) to squeeze, and obtains durol product (8), and the crystalline mother solution squeezed out (9).The present invention gives a kind of method of purification of durol, by obtaining the durol of higher concentration, huge economic benefit and social benefit can be had.
Description
Technical field
The present invention relates to a kind of durol preparation field, be specifically related to the method for purification of durol in middle lower concentration raw material.
Background technology
Durol, i.e. 1，2，4，5-tetramethylbenzene, camphor stink, white crystal, is dissolved in the organic solvent such as ether, ethanol, water insoluble, can distil, and under high temperature and nitric acid, Vanadium Pentoxide in FLAKES catalysis, oxidation generates pyromellitic dianhydride.
The topmost purposes of durol produces pyromellitic acid anhydride.Pyromellitic acid anhydride can produce polyimide.Along with the market consumption of polyimide constantly expands, the demand of durol also grows with each passing day.But, present stage the output of durol less, not yet form industrial production scale.Therefore be necessary to open up reasonable, the production cost of production method reduction efficiently.
The present invention mainly provides a kind of method durol can being carried out purifying
Summary of the invention
The present invention gives a kind of method of purification of durol, by obtaining the durol of higher concentration, huge economic benefit and social benefit can be had.
The equipment that the present invention adopts is: freezing and crystallizing device, centrifugal separating device and squeezing machine.
A method of purification for durol, technical scheme is:
Raw material durol solution, through freezing and crystallizing device freezing and crystallizing, obtains the durol xln containing crystalline mother solution; Be separated by crystalline mother solution with centrifugal separating device, obtain crystalline mother solution and centrifugal rear solid phase prod, solid phase prod adopts squeezing machine to squeeze, and obtains durol product, and the crystalline mother solution squeezed out.
The service temperature of described freezing and crystallizing device is-15 DEG C ~ 20 DEG C; Heat-eliminating medium is recirculated water or refrigerated water.
Described raw material durol mass concentration is 50% ~ 70%.
Described centrifugal separating device operation revolution is 600 ~ 1800r/min.
The described squeezing machine operating time is 30 ~ 180min.
During described centrifuge operations, add gasoline or solar oil washing lotion, addition is less than or equal to durol quality 10% in raw material.
The concentration of durol in lower concentration durol solution during the present invention can effectively improve, after purifying, durol concentration can reach 70-80%, operates fairly simple.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of durol method of purification;
In figure, 1. freezing and crystallizing device, 2. whizzer, 3. squeezing machine, lower concentration durol solution 4., 5. durol xln, 6. centrifugal rear solid phase prod, 7. crystalline mother solution, 8. durol product, 9. the crystalline mother solution squeezed out, 10. washing lotion, 11. heat-eliminating mediums enter, and 12. heat-eliminating mediums are discharged.
Embodiment
Below in conjunction with accompanying drawing, technology provided by the present invention is further detailed.
The present invention is achieved through the following technical solutions:
As shown in Figure 1, technical process of the present invention is: raw material durol solution 4 enters in freezing and crystallizing device 1 and carries out freezing and crystallizing, the discharge 12 entering 11 and heat-eliminating medium of this freezing and crystallizing device heat-eliminating medium, obtains low-temperature receiver, obtains the durol xln 5 containing crystalline mother solution after freezing and crystallizing; Be separated by crystalline mother solution with centrifugal separating device 2, obtain crystalline mother solution 7 and centrifugal rear solid phase prod 6, this solid phase prod adopts squeezing machine 3 to squeeze, and obtains durol product 8, and the crystalline mother solution 9 squeezed out.
In the method raw material durol solution, durol mass concentration is 50% ~ 70%; The service temperature of freezing and crystallizing device is-15 DEG C ~ 20 DEG C; Centrifuge operations revolution is 600 ~ 1800r/min; The squeezing machine operating time is 30 ~ 180min; Heat-eliminating medium is recirculated water or refrigerated water; Washing lotion 10 can be added according to centrifuge operations, be mainly gasoline or solar oil.
Embodiment 1:
Operating process is: 50% durol solution 4 enters in freezing and crystallizing device 1 and carries out freezing and crystallizing, and service temperature is-15 DEG C, and this freezing and crystallizing device heat-eliminating medium adopts refrigerated water, obtains the durol xln 5 containing crystalline mother solution after freezing and crystallizing; Rotating speed is adopted to be that crystalline mother solution is separated by 600r/min with centrifugal separating device 2, obtain crystalline mother solution 7 and centrifugal rear solid phase prod 6, this solid phase prod adopts squeezing machine 3 to carry out press operation 30min, and obtaining durol product 8 concentration is 60%, and the crystalline mother solution 9 squeezed out.
Embodiment 2:
Operating process is: 60% durol solution 4 enters in freezing and crystallizing device 1 and carries out freezing and crystallizing, and service temperature is 0 DEG C, and this freezing and crystallizing device heat-eliminating medium adopts refrigerated water, obtains the durol xln 5 containing crystalline mother solution after freezing and crystallizing; Rotating speed is adopted to be that crystalline mother solution is separated by 1200r/min with centrifugal separating device 2, this process adds the washing lotion gasoline accounting for durol quality 5% in raw material, obtain crystalline mother solution 7 and centrifugal rear solid phase prod 6, this solid phase prod adopts squeezing machine 3 to carry out press operation 120min, obtaining durol product 8 concentration is 70%, and the crystalline mother solution 9 squeezed out.
Embodiment 3:
Operating process is: 70% durol solution 4 enters in freezing and crystallizing device 1 and carries out freezing and crystallizing, and service temperature is 20 DEG C, and this freezing and crystallizing device heat-eliminating medium adopts refrigerated water, obtains the durol xln 5 containing crystalline mother solution after freezing and crystallizing; Rotating speed is adopted to be that crystalline mother solution is separated by 1800r/min with centrifugal separating device 2, this process adds the washing lotion solar oil accounting for durol quality 10% in raw material, obtain crystalline mother solution 7 and centrifugal rear solid phase prod 6, this solid phase prod adopts squeezing machine 3 to carry out press operation 180min, obtaining durol product 8 concentration is 80%, and the crystalline mother solution 9 squeezed out.
The method of purification of a kind of durol that the present invention proposes, be described by preferred embodiment, person skilled obviously can not depart from content of the present invention, spirit and scope structure as herein described and technological method 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 (1)
1. a method of purification for durol, is characterized in that: raw material durol mass concentration be 50% ~ 70% solution through freezing and crystallizing device freezing and crystallizing, temperature is-15 DEG C, obtains the durol xln containing crystalline mother solution; Add gasoline or solar oil washing lotion, addition is less than or equal to durol quality 10% in raw material, be that crystalline mother solution is separated by 600 ~ 1800r/min with centrifugal separating device revolution, obtain crystalline mother solution and centrifugal rear solid phase prod, solid phase prod adopts squeezing machine to carry out 30 ~ 180min squeezing, obtain durol product, and the crystalline mother solution squeezed out.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310467290.6A CN103524288B (en) | 2013-09-30 | 2013-09-30 | A kind of method of purification of durol |
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| CN201310467290.6A CN103524288B (en) | 2013-09-30 | 2013-09-30 | A kind of method of purification of durol |
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| CN103524288A CN103524288A (en) | 2014-01-22 |
| CN103524288B true CN103524288B (en) | 2015-11-25 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104945214A (en) * | 2015-05-19 | 2015-09-30 | 常熟联邦化工股份有限公司 | Purification method of coproduct durene enrichment solution in process of preparing gasoline from methanol |
| CN105541543B (en) * | 2016-02-15 | 2018-03-13 | 天津市兴源化工有限公司 | The method of purification of durol |
| CN106242937B (en) * | 2016-08-06 | 2019-02-26 | 江苏华伦化工有限公司 | A kind of method of purification of durol |
| CN107827697A (en) * | 2017-12-16 | 2018-03-23 | 常熟联邦化工股份有限公司 | Durol crystallization kettle freezing liquid conveying equipment |
| CN109232158A (en) * | 2018-10-26 | 2019-01-18 | 江苏华伦化工有限公司 | Durol continuous crystallisation process |
| DE212020000055U1 (en) * | 2020-05-05 | 2020-06-04 | Pengchen New Material Technology Co., Ltd. | A freezing liquid delivery device for the 1,2,4,5-tetramethylbenzene crystallization kettle |
| CN115231997A (en) * | 2021-04-25 | 2022-10-25 | 中国石油化工股份有限公司 | Crystallization refining method of crude pyromellitic acid |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101279886A (en) * | 2008-05-22 | 2008-10-08 | 天津市大港区兴源化工厂 | Technological process for preparing durene with reformed C10 aromatic |
| CN101318874A (en) * | 2008-06-18 | 2008-12-10 | 常熟市联邦化工有限公司 | Process for joint production of aromatic solvent, stone oil naphthalin and durene line products with C10 heavy aromatic raw material |
| CN101973840A (en) * | 2010-10-14 | 2011-02-16 | 江苏华伦化工有限公司 | Method for separating durene by freezing crystallization |
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- 2013-09-30 CN CN201310467290.6A patent/CN103524288B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101279886A (en) * | 2008-05-22 | 2008-10-08 | 天津市大港区兴源化工厂 | Technological process for preparing durene with reformed C10 aromatic |
| CN101318874A (en) * | 2008-06-18 | 2008-12-10 | 常熟市联邦化工有限公司 | Process for joint production of aromatic solvent, stone oil naphthalin and durene line products with C10 heavy aromatic raw material |
| CN101973840A (en) * | 2010-10-14 | 2011-02-16 | 江苏华伦化工有限公司 | Method for separating durene by freezing crystallization |
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