CN103524288A - Purification method for durene - Google Patents
Purification method for durene Download PDFInfo
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- CN103524288A CN103524288A CN201310467290.6A CN201310467290A CN103524288A CN 103524288 A CN103524288 A CN 103524288A CN 201310467290 A CN201310467290 A CN 201310467290A CN 103524288 A CN103524288 A CN 103524288A
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- durol
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- mother solution
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Abstract
The invention relates to a purification method for durene. A durene solution (4) is added into a freezing crystallizer (1) for freezing crystallization, wherein a clod source is obtained through feed (11) of a cooling medium of the freezing crystallizer and discharge (12) of the cooling medium. After the freezing crystallization, durene crystals (5) containing crystallization mother liquor are obtained. The crystallization mother liquor is separated by a centrifugal separation device (2) to obtain crystallization mother liquor (7) and a solid product (6) after centrifugation. The solid product is squeezed by a squeezer (3) to obtain a durene product (8) and squeezed crystallization mother liquor (8) According to the purification method for the durene, the durene with a high concentration can be obtained, thus bringing great economic benefit and social benefit.
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 solvents 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 is to produce pyromellitic acid anhydride.Pyromellitic acid anhydride can be produced 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 suitability for industrialized production scale.Therefore being necessary to open up reasonable, efficient production method reduces production costs.
The present invention mainly provides a kind of method that durol can be purified
Summary of the invention
The present invention has provided a kind of method of purification of durol, can, by obtaining the durol of higher concentration, have huge economic benefit and social benefit.
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 that contains crystalline mother solution; With centrifugal separating device, crystalline mother solution is separated, 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 squeezing out.
The service temperature of described freezing and crystallizing device is-15 ℃～20 ℃; 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 whizzer operation, 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, 4. in lower concentration durol solution, 5. durol xln, 6. centrifugal rear solid phase prod, 7. crystalline mother solution, 8. durol product, 9. the crystalline mother solution squeezing 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 and in freezing and crystallizing device 1, carries out freezing and crystallizing, this freezing and crystallizing device heat-eliminating medium enter 11 and the discharge 12 of heat-eliminating medium, obtain low-temperature receiver, after freezing and crystallizing, obtain the durol xln 5 that contains crystalline mother solution; With centrifugal separating device 2, crystalline mother solution is separated, 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 squeezing out.
In the method raw material durol solution, durol mass concentration is 50%～70%; The service temperature of freezing and crystallizing device is-15 ℃～20 ℃; Whizzer operation revolution is 600～1800r/min; The squeezing machine operating time is 30～180min; Heat-eliminating medium is recirculated water or refrigerated water; According to whizzer, operation can be added washing lotion 10, is 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 ℃, and this freezing and crystallizing device heat-eliminating medium adopts refrigerated water, obtains the durol xln 5 that contains crystalline mother solution after freezing and crystallizing; With centrifugal separating device 2, adopting rotating speed is that 600r/min is separated by crystalline mother solution, 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 squeezing 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 ℃, and this freezing and crystallizing device heat-eliminating medium adopts refrigerated water, obtains the durol xln 5 that contains crystalline mother solution after freezing and crystallizing; With centrifugal separating device 2, adopting rotating speed is that 1200r/min is separated by crystalline mother solution, this process adds the washing lotion gasoline that accounts 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 squeezing 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 ℃, and this freezing and crystallizing device heat-eliminating medium adopts refrigerated water, obtains the durol xln 5 that contains crystalline mother solution after freezing and crystallizing; With centrifugal separating device 2, adopting rotating speed is that 1800r/min is separated by crystalline mother solution, this process adds the washing lotion solar oil that accounts 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 squeezing out.
The method of purification of a kind of durol that the present invention proposes, by preferred embodiment, be described, person skilled obviously can be within not departing from content of the present invention, spirit and scope to structure as herein described with technological method is changed or suitably change and 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 artly, they are deemed to be included in spirit of the present invention, scope and content.
Claims (6)
1. a method of purification for durol, is characterized in that: raw material durol solution, through freezing and crystallizing device freezing and crystallizing, obtains the durol xln that contains crystalline mother solution; With centrifugal separating device, crystalline mother solution is separated, 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 squeezing out.
2. as the method under claim 1, the service temperature that it is characterized in that freezing and crystallizing device is-15 ℃～20 ℃; Heat-eliminating medium is recirculated water or refrigerated water.
3. as the method under claim 1, it is characterized in that raw material durol mass concentration is 50%～70%.
4. as the method under claim 1, it is characterized in that centrifugal separating device operation revolution is 600～1800r/min.
5. as the method under claim 1, it is characterized in that the squeezing machine operating time is 30～180min.
6. as the method under claim 1, while it is characterized in that whizzer operation, add gasoline or solar oil washing lotion, addition is less than or equal to durol quality 10% in raw material.
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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 true CN103524288A (en) | 2014-01-22 |
| CN103524288B CN103524288B (en) | 2015-11-25 |
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Cited By (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 |
| CN105541543A (en) * | 2016-02-15 | 2016-05-04 | 天津市兴源化工有限公司 | Durene purifying method |
| CN106242937A (en) * | 2016-08-06 | 2016-12-21 | 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 |
| WO2021223068A1 (en) * | 2020-05-05 | 2021-11-11 | 鹏辰新材料科技股份有限公司 | Refrigeration liquid delivery device for durene 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 |
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 |
-
2013
- 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 |
Cited By (8)
| 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 |
| CN105541543A (en) * | 2016-02-15 | 2016-05-04 | 天津市兴源化工有限公司 | Durene purifying method |
| 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 |
| CN106242937A (en) * | 2016-08-06 | 2016-12-21 | 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 |
| WO2021223068A1 (en) * | 2020-05-05 | 2021-11-11 | 鹏辰新材料科技股份有限公司 | Refrigeration liquid delivery device for durene 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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| CN103524288B (en) | 2015-11-25 |
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