CN102911181A - Preparation method of high-purity pyromellitic dianhydride - Google Patents
Preparation method of high-purity pyromellitic dianhydride Download PDFInfo
- Publication number
- CN102911181A CN102911181A CN2012104558412A CN201210455841A CN102911181A CN 102911181 A CN102911181 A CN 102911181A CN 2012104558412 A CN2012104558412 A CN 2012104558412A CN 201210455841 A CN201210455841 A CN 201210455841A CN 102911181 A CN102911181 A CN 102911181A
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- CN
- China
- Prior art keywords
- pyromellitic acid
- acid anhydride
- preparation
- pyromellitic dianhydride
- pyromellitic
- 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.)
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- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- VLDPXPPHXDGHEW-UHFFFAOYSA-N 1-chloro-2-dichlorophosphoryloxybenzene Chemical compound ClC1=CC=CC=C1OP(Cl)(Cl)=O VLDPXPPHXDGHEW-UHFFFAOYSA-N 0.000 title abstract 6
- CYIDZMCFTVVTJO-UHFFFAOYSA-N pyromellitic acid Chemical compound OC(=O)C1=CC(C(O)=O)=C(C(O)=O)C=C1C(O)=O CYIDZMCFTVVTJO-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000013078 crystal Substances 0.000 claims abstract description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 9
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 claims abstract description 8
- 150000004703 alkoxides Chemical class 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 3
- ANSXAPJVJOKRDJ-UHFFFAOYSA-N furo[3,4-f][2]benzofuran-1,3,5,7-tetrone Chemical compound C1=C2C(=O)OC(=O)C2=CC2=C1C(=O)OC2=O ANSXAPJVJOKRDJ-UHFFFAOYSA-N 0.000 claims description 34
- 238000002425 crystallisation Methods 0.000 claims description 7
- 230000008025 crystallization Effects 0.000 claims description 7
- 230000018044 dehydration Effects 0.000 claims description 5
- 238000006297 dehydration reaction Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 abstract 1
- 230000007062 hydrolysis Effects 0.000 abstract 1
- 238000006460 hydrolysis reaction Methods 0.000 abstract 1
- 239000012535 impurity Substances 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000000034 method Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 239000011810 insulating material Substances 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 1
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 1
- 239000004642 Polyimide Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229920003223 poly(pyromellitimide-1,4-diphenyl ether) Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 235000019633 pungent taste Nutrition 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
Landscapes
- Heterocyclic Carbon Compounds Containing A Hetero Ring Having Oxygen Or Sulfur (AREA)
Abstract
The invention relates to a preparation method of high-purity pyromellitic dianhydride. The preparation method comprises the following steps of: heating and dewatering crude pyromellitic acid in the absence of acetic anhydride so as to transform the pyromellitic acid to the pyromellitic dianhydride and enable an obtained product mixture to contain the pyromellitic acid and the pyromellitic dianhydride; then performing hydrolysis on the obtained mixture in a sufficient amount of alkoxide solution, decoloring by activated carbon, performing heat filtering, then re-crystallizing, and further centrifugating to obtain crude crystals of the pyromellitic dianhydride; and then separating impurities from the crude crystals at the temperature of 150-200 DEG C under vacuum conditions, and finally cooling to obtain a high-purity full-powder pyromellitic dianhydride product.
Description
Technical field
The present invention relates to a kind of preparation method of high purity pyromellitic acid anhydride, belong to chemical field.
Background technology
Pyromellitic acid anhydride is white in color to faint yellow needle crystal, density 1.68/cm3,284 ℃～288 ℃ of fusing points, neutralization equivalent 54.5 ± 0.2 easily distils, and is dissolved in acetone, vinyl acetic monomer, N,N-DIMETHYLACETAMIDE, it is imitative to be insoluble to high post, ether, and easily the moisture absorption is hydrolyzed into acid, pungency is arranged, it is the main raw material of polyimide heat-resistant engineering plastic and insulation film, epoxy curing agent, the synthesis material of stablizer and fuel etc.Be mainly used in the insulating material of aerospace, precision instrument etc., be used for the manufacturing enterprise of Kapton more than 95%, with high content of technology.
Because use range is mainly the aerospace of high-tech content, the insulating material of precision instrument, quality product requires extra-high-speed, and usual production purity can only reach about 99.9%, bring very large infringement to target product, that have even cause the accident, therefore the target customer wishes that urgently product content can reach more than 99.9%, to improve the target product quality and to reduce the loss that produces because of quality problems.
Summary of the invention
The purity to 99.999% of the pyromellitic acid anhydride that the preparation method who the purpose of this invention is to provide the full powder pyromellitic acid anhydride of a kind of high purity, the method produce, powder can arrive 99% simultaneously.
The technical solution used in the present invention is:
A kind of preparation method of high purity pyromellitic acid anhydride, its step comprises: thick Pyromellitic Acid thermal dehydration in situation about existing without diacetyl oxide is processed, so that Pyromellitic Acid is converted into pyromellitic acid anhydride, include very pyromellitic acid anhydride of Pyromellitic Acid in the product mixtures that obtains thus; Then resulting mixture is hydrolyzed in alkoxide solution, by again crystallization behind activated carbon decolorizing and the heat filtering, again through the centrifugal coarse crystal that obtains pyromellitic acid anhydride; Then with coarse crystal removing foreign matter under the condition of 180-200 ℃ and vacuum, namely obtain highly purified full powder pyromellitic acid anhydride product after the cooling at last.
The purity of described Pyromellitic Acid is 99.7%-99.9% by weight.
The consumption of described alkoxide solution is q.s.
The temperature of described crystallization is 190-210 ℃.
Advantage of the present invention is: by the purity to 99.999% of the method production pyromellitic acid anhydride, powder can arrive 99% simultaneously, and the method is simple to operate, production efficiency is high.
Embodiment
Embodiment 1
A kind of preparation method of high purity pyromellitic acid anhydride, its step comprises: thick Pyromellitic Acid thermal dehydration in the situation that does not have diacetyl oxide is processed, so that the Pyromellitic Acid of 99.7 % is converted into pyromellitic acid anhydride by weight, include very pyromellitic acid anhydride of Pyromellitic Acid in the product mixtures that obtains thus; Then resulting mixture is hydrolyzed in the alkoxide solution of q.s, by again crystallization under 190 ℃ temperature behind activated carbon decolorizing and the heat filtering, again through the centrifugal coarse crystal that obtains pyromellitic acid anhydride; Then with coarse crystal removing foreign matter under the condition of 150 ℃ and vacuum, cool off at last postscript and obtain highly purified full powder pyromellitic acid anhydride product.
Embodiment 2
A kind of preparation method of high purity pyromellitic acid anhydride, its step comprises: thick Pyromellitic Acid thermal dehydration in the situation that does not have diacetyl oxide is processed, so that 99.9% Pyromellitic Acid is converted into pyromellitic acid anhydride by weight, include very pyromellitic acid anhydride of Pyromellitic Acid in the product mixtures that obtains thus; Then resulting mixture is hydrolyzed in the alkoxide solution of q.s, by again crystallization under 210 ℃ temperature behind activated carbon decolorizing and the heat filtering, again through the centrifugal coarse crystal that obtains pyromellitic acid anhydride; Then with coarse crystal removing foreign matter under the condition of 200 ℃ and vacuum, cool off at last postscript and obtain highly purified full powder pyromellitic acid anhydride product.
Embodiment 3
A kind of preparation method of high purity pyromellitic acid anhydride, its step comprises: thick Pyromellitic Acid thermal dehydration in the situation that does not have diacetyl oxide is processed, so that the Pyromellitic Acid of 99.8 % is converted into pyromellitic acid anhydride by weight, include very pyromellitic acid anhydride of Pyromellitic Acid in the product mixtures that obtains thus; Then resulting mixture is hydrolyzed in the alkoxide solution of q.s, by again crystallization under 200 ℃ temperature behind activated carbon decolorizing and the heat filtering, again through the centrifugal coarse crystal that obtains pyromellitic acid anhydride; Then with coarse crystal removing foreign matter under the condition of 180 ℃ and vacuum, cool off at last postscript and obtain highly purified full powder pyromellitic acid anhydride product.
Claims (4)
1. the preparation method of a high purity pyromellitic acid anhydride, it is characterized in that: its step comprises: thick Pyromellitic Acid thermal dehydration in situation about existing without diacetyl oxide is processed, so that Pyromellitic Acid is converted into pyromellitic acid anhydride, include very pyromellitic acid anhydride of Pyromellitic Acid in the product mixtures that obtains thus; Then resulting mixture is hydrolyzed in alkoxide solution, by again crystallization behind activated carbon decolorizing and the heat filtering, again through the centrifugal coarse crystal that obtains pyromellitic acid anhydride; Then with coarse crystal removing foreign matter under the condition of 180-200 ℃ and vacuum, namely obtain highly purified full powder pyromellitic acid anhydride product after the cooling at last.
2. the preparation method of a kind of high purity pyromellitic acid anhydride according to claim 1 is characterized in that: the purity of described Pyromellitic Acid is 99.7%-99.9% by weight.
3. the preparation method of a kind of high purity pyromellitic acid anhydride according to claim 1, it is characterized in that: the consumption of described alkoxide solution is q.s.
4. the preparation method of a kind of high purity pyromellitic acid anhydride according to claim 1, it is characterized in that: the temperature of described crystallization is 190-210 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012104558412A CN102911181A (en) | 2012-11-14 | 2012-11-14 | Preparation method of high-purity pyromellitic dianhydride |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012104558412A CN102911181A (en) | 2012-11-14 | 2012-11-14 | Preparation method of high-purity pyromellitic dianhydride |
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| Publication Number | Publication Date |
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| CN102911181A true CN102911181A (en) | 2013-02-06 |
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| CN2012104558412A Pending CN102911181A (en) | 2012-11-14 | 2012-11-14 | Preparation method of high-purity pyromellitic dianhydride |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114516882A (en) * | 2020-11-19 | 2022-05-20 | 烟台弘邦医药科技有限公司 | Preparation method of cycloalkane tetracarboxylic dianhydride |
| CN117327086A (en) * | 2022-06-27 | 2024-01-02 | 中国石油化工股份有限公司 | A preparation method of high-purity pyromellitic dianhydride and the obtained high-purity pyromellitic dianhydride |
| CN117683039A (en) * | 2022-09-05 | 2024-03-12 | 中国石油化工股份有限公司 | Method for producing pyromellitic anhydride by pyromellitic acid dehydration process |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1280562A (en) * | 1969-06-13 | 1972-07-05 | Veba Chemie Ag | Process for the purification of pyromellitic acid dianhydride |
| US4370487A (en) * | 1980-04-25 | 1983-01-25 | Gerhard Meyer | Process for, respectively, the production and purification of dicarboxylic and polycarboxylic acid anhydrides |
| US4694089A (en) * | 1985-09-10 | 1987-09-15 | Mitsubishi Gas Chemical Company, Inc. | Process for preparing pyromellitic dianhydride |
| JPH03294272A (en) * | 1990-04-13 | 1991-12-25 | Hitachi Ltd | Production method of high purity tetracarboxylic dianhydride |
| JP2002069073A (en) * | 2000-08-23 | 2002-03-08 | Mitsubishi Gas Chem Co Inc | Method for producing high-purity pyromellitic anhydride |
| EP1199298A1 (en) * | 2000-08-23 | 2002-04-24 | Mitsubishi Gas Chemical Company, Inc. | Process for producing refined pyromellitic acid and refined pyromellitic anhydride |
| CN1970560A (en) * | 2005-07-21 | 2007-05-30 | 三菱瓦斯化学株式会社 | Method for producing high-purity pyromellitic dianhydride |
| CN101250190A (en) * | 2008-04-10 | 2008-08-27 | 常熟市联邦化工有限公司 | Method for refining pyromellitic anhydride by solvent |
| US20110319620A1 (en) * | 2009-03-11 | 2011-12-29 | National University Corporation Nagoya University | Method for producing carboxylic anhydride and arylboronic acid compound |
-
2012
- 2012-11-14 CN CN2012104558412A patent/CN102911181A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1280562A (en) * | 1969-06-13 | 1972-07-05 | Veba Chemie Ag | Process for the purification of pyromellitic acid dianhydride |
| US4370487A (en) * | 1980-04-25 | 1983-01-25 | Gerhard Meyer | Process for, respectively, the production and purification of dicarboxylic and polycarboxylic acid anhydrides |
| US4694089A (en) * | 1985-09-10 | 1987-09-15 | Mitsubishi Gas Chemical Company, Inc. | Process for preparing pyromellitic dianhydride |
| JPH03294272A (en) * | 1990-04-13 | 1991-12-25 | Hitachi Ltd | Production method of high purity tetracarboxylic dianhydride |
| JP2002069073A (en) * | 2000-08-23 | 2002-03-08 | Mitsubishi Gas Chem Co Inc | Method for producing high-purity pyromellitic anhydride |
| EP1199298A1 (en) * | 2000-08-23 | 2002-04-24 | Mitsubishi Gas Chemical Company, Inc. | Process for producing refined pyromellitic acid and refined pyromellitic anhydride |
| CN1970560A (en) * | 2005-07-21 | 2007-05-30 | 三菱瓦斯化学株式会社 | Method for producing high-purity pyromellitic dianhydride |
| CN101250190A (en) * | 2008-04-10 | 2008-08-27 | 常熟市联邦化工有限公司 | Method for refining pyromellitic anhydride by solvent |
| US20110319620A1 (en) * | 2009-03-11 | 2011-12-29 | National University Corporation Nagoya University | Method for producing carboxylic anhydride and arylboronic acid compound |
Non-Patent Citations (3)
| Title |
|---|
| AKIRA SAKAKURA,等: "Bronsted Base-Assisted Boronic Acid Catalysis for the Dehydrative Intramolecular Condensation of Dicarboxylic Acids", 《ORGANIC LETTERS》 * |
| 丁志平，等: "精均苯四甲酸二酐的研制", 《涂料工业》 * |
| 王玉珊，等: "均苯四甲酸二酐的分离精制", 《石油化工》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114516882A (en) * | 2020-11-19 | 2022-05-20 | 烟台弘邦医药科技有限公司 | Preparation method of cycloalkane tetracarboxylic dianhydride |
| CN117327086A (en) * | 2022-06-27 | 2024-01-02 | 中国石油化工股份有限公司 | A preparation method of high-purity pyromellitic dianhydride and the obtained high-purity pyromellitic dianhydride |
| CN117683039A (en) * | 2022-09-05 | 2024-03-12 | 中国石油化工股份有限公司 | Method for producing pyromellitic anhydride by pyromellitic acid dehydration process |
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Application publication date: 20130206 |