CN108329327A - A kind of method of purification of the thick pyromellitic acid anhydride based on crystallization distillation - Google Patents
A kind of method of purification of the thick pyromellitic acid anhydride based on crystallization distillation Download PDFInfo
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Abstract
The present invention provides a kind of method of purification of the thick pyromellitic acid anhydride based on crystallization distillation, specifically includes：The thermal current come out from the reactor that durol is raw material is directly mixed with the inert gas containing ice crystal piece, is collected through column trap, centrifugation obtains pyromellitic acid anhydride crude product；Molybdenum trioxide one-dimensional rod-like material is added in PVP solution, after temperature reaction, drying, charing and pickling is washed, obtains the Bacilliform carbon material containing molybdenum oxide；Pyromellitic acid anhydride crude product is added in hydrolysis kettle, the Bacilliform carbon material containing molybdenum oxide, stirring hydrolysis decoloration hydrotreating is added, filtering obtains slightly hydrogenating Pyromellitic Acid crystal；Pyromellitic Acid crystal will slightly be hydrogenated to handle through fused salt thermal dehydration and distillation, obtain pyromellitic acid anhydride.The method of purification of the present invention is raw material through the inert gas of the piece containing ice crystal is in direct contact trapping after, and being carried out at the same time hydrolysis using the Bacilliform carbon material containing molybdenum oxide decolourizes hydrogenation reaction, obtains high-purity pyromellitic acid anhydride.
Description
Technical field
The invention belongs to pyromellitic acid anhydride purification technique fields, and in particular to a kind of thick equal benzene based on crystallization distillation
The method of purification of tetracarboxylic acid dianhydride.
Background technology
Pyromellitic acid anhydride is also referred to as equal acid anhydride, has special molecular structure, can be used for manufacturing heat resistance, electrical isolation
Property and the material of chemical resistance closed with aromatic diamine wherein most important purposes is the monomer as polyimides
At obtained polyimide plastic, but it is very high to the purity requirement of pyromellitic acid anhydride, it needs up to 99% or more.Current equal benzene
The method of purification of tetracarboxylic acid dianhydride has recrystallization method, solvent washing method, vacuum sublimation, adduct process, inert gas method, two level
Way of distillation etc..
Chinese patent CN 101580509B are disclosed to catch the method that crude anhydride produces electron level pyromellitic acid anhydride by two,
Crude anhydride and the solvent Hybrid Heating of washing are caught by two, after cooling down suction strainer, dehydration and decolorization obtains crystalline solids, by crystalline solids
It again after crystallisation by cooling, filters, obtains the pyromellitic acid anhydride crystalline solid containing mother liquor, most obtained after cooling through drying afterwards
Electron level pyromellitic acid anhydride, crystalline mother solution circulating and recovering.This method is produced through catalytic gas phase oxidation with durol
Crude product Pyromellitic Acid two catches crude anhydride as raw material, by the phthalic anhydride wherein contained, trimellitic acid through secondary trapping
Acid anhydride, Pyromellitic Acid, Pyromellitic Acid list acid anhydride and inclined three acid anhydrides of 5- methyl and mechanical admixture and ultra-fine foreign material, the present invention
Method of purification make to carry out in closed device, environmental pollution is small, and Recycling Mother Solution uses, and customer service Hydrolyze method lacks
It falls into, the purity of the Pyromellitic Acid of purification is higher than 99%, the purity level requirement of composite synthesis electron level PI films.Chinese patent CN
Purity is more than 98% Pyromellitic Acid by the preparation method of electronic grade hydrogenated pyromellitic acid anhydride disclosed in 103992330B
The catalyst of dianhydride, deionized water and the carbon containing noble metal is added in autoclave, be passed through into reaction kettle hydrogen simultaneously into
Row hydrolysis and catalytic hydrogenation reaction, obtain slightly hydrogenating Pyromellitic Acid, then with deionization and activated carbon to slightly hydrogenating equal benzene four
Formic acid carries out decolorizing and refining, obtains the hydrogenation Pyromellitic Acid that purity is more than 99.5%, finally carries out dehydration with acetic anhydride and obtain
It is more than 99.85% electronic grade hydrogenated pyromellitic acid anhydride to purity, which, which simplifies, first hydrolyzes again catalytic hydrogenation
Method improves the polycarboxylic purity of hydrogenated aromatic, and by suitable acetic anhydride on the basis of shortening dewatering time, saves
Solvent is removed, to more environment-friendly.By the above-mentioned prior art it is found that pyromellitic acid anhydride can be improved by the technique for improving trapping
Purification efficiency and purity, but at present all multi-methods it is still not mature enough, need further perfect.
Invention content
The technical problem to be solved in the present invention is to provide a kind of purifications of the thick pyromellitic acid anhydride based on crystallization distillation
The inert gas of method, thermal current and the piece containing ice crystal through being come out from the reactor that durol is raw material is in direct contact trapping
Afterwards, it is carried out at the same time hydrolysis decoloration hydrogenation reaction using the Bacilliform carbon material containing molybdenum oxide, obtains high-purity pyromellitic acid anhydride.
In order to solve the above technical problems, the technical scheme is that：
A kind of method of purification of the thick pyromellitic acid anhydride based on crystallization distillation, it is characterised in that：Include the following steps：
（1）The thermal current come out from the reactor that durol is raw material is directly mixed with the inert gas containing ice crystal piece,
It is collected through column trap, centrifugation obtains pyromellitic acid anhydride crude product；
（2）By step（1）The pyromellitic acid anhydride crude product of preparation is added in hydrolysis kettle, and the rodlike carbon materials containing molybdenum oxide are added
Material, stirring hydrolysis decoloration hydrotreating, filtering obtain slightly hydrogenating Pyromellitic Acid crystal；
（3）By step（2）The thick hydrogenation Pyromellitic Acid crystal prepared is handled through fused salt thermal dehydration and distillation, obtains equal benzene four
Formic acid dianhydride.
As a preferred embodiment of the above technical solution, the step（1）In, the volume of thermal current and the inert gas for having ice crystal piece
Than being 1:0.5-0.8.
As a preferred embodiment of the above technical solution, the step（1）In, ice crystal piece contains in the inert gas containing ice crystal piece
Amount is 1-4%, gas velocity 0.05-0.5m/s.
As a preferred embodiment of the above technical solution, the step（2）In, the temperature of steam is 90-100 DEG C in hydrolysis kettle, pressure
Power is 0.2MPa.
As a preferred embodiment of the above technical solution, the step（2）In, the preparation method of the Bacilliform carbon material containing molybdenum oxide
For：Molybdenum trioxide one-dimensional rod-like material is added in PVP solution, 120-130 DEG C of reaction 2-3d is warming up to, takes out crystal, wash,
Vacuum drying, the charing process at 590-620 DEG C obtain the Bacilliform carbon material containing molybdenum oxide through hydrofluoric acid pickling.
As a preferred embodiment of the above technical solution, the step（2）In, the dosage of the Bacilliform carbon material containing molybdenum oxide is equal benzene
The 1-5% of tetracarboxylic acid dianhydride crude product quality.
As a preferred embodiment of the above technical solution, the step（2）In, the time of hydrolysis decoloration hydrotreating is 3-6h.
As a preferred embodiment of the above technical solution, the step（3）In, the technique of fused salt thermal dehydration and distillation processing is：
First under the pressure of -0.09MPa, it is warming up to 220-230 DEG C with the rate of 10-20 DEG C/min, keeps the temperature 30-60min, then with 1-3
DEG C/rate of min is warming up to 240-250 DEG C, keep the temperature 60-120min.
As a preferred embodiment of the above technical solution, the step（3）In, fused salt is the mixture of potassium nitrate and sodium nitrate.
As a preferred embodiment of the above technical solution, the step（3）In, the purity of pyromellitic acid anhydride is more than 99.8%.
Compared with prior art, the invention has the advantages that：
（1）The present invention is that the inert gas of the thermal current and the piece containing ice crystal that are come out from the reactor that durol is raw material directly connects
It touches, thermal current is cooled crystallization of sublimating, and compared with water contact is cooling, cooling effect is more preferably good, and reduces durol turn
It is melted into propylene glycol methyl ether acetate, and due to the weight of ice crystal piece, reduces the feelings that thick Pyromellitic Acid crystal is crystallized in wall surface
Condition, and collected using column trap, good effect of heat exchange, cooling velocity is fast, yield higher, and also contains inertia in cooling gas
Gas reduces water and effect that acid anhydride is transformed into acid, further improves the yield of product.And the Pyromellitic Acid two after trapping
Acid anhydride crude product is carried out at the same time hydrolysis decoloration hydrogenation reaction using the Bacilliform carbon material containing molybdenum oxide, this contains the Bacilliform carbon material of molybdenum oxide
For club-shaped material, large specific surface area, high active of hydrogenation catalysis is big, and due to porous carbon materials with certain decolorization,
So that hydrolysis decoloration plus hydrogen is carried out at the same time, reduce the time of reaction, improve the purity of reaction efficiency and product, is conducive to continuous
Change reaction.
（2）Preparation method of the present invention is simple, and using the Bacilliform carbon material containing molybdenum oxide as catalyst, it is de- to be carried out at the same time hydrolysis
Color hydrogenation reaction, refinement is efficient, and product purity is high, and controllability is strong, and byproduct is few, and product purity is high.
Specific implementation mode
Below in conjunction with specific embodiment, the present invention will be described in detail, herein illustrative examples and explanation of the invention
For explaining the present invention, but it is not as a limitation of the invention.
Embodiment 1：
（1）It is 1 by volume ratio:0.5 slave durol be raw material reactor come out thermal current with contain the lazy of ice crystal piece
Property gas directly mix, wherein in the inert gas containing ice crystal piece ice crystal piece content be 1%, gas velocity 0.05m/s,
It is collected through column trap, centrifugation obtains pyromellitic acid anhydride crude product.
（2）Molybdenum trioxide one-dimensional rod-like material is added in PVP solution, 120 DEG C of reaction 2d is warming up to, takes out crystal, wash
It washs, is dried in vacuo, the charing process at 590 DEG C obtains the Bacilliform carbon material containing molybdenum oxide through hydrofluoric acid pickling.
（3）Pyromellitic acid anhydride crude product is added in hydrolysis kettle, the temperature of steam is 90 DEG C in hydrolysis kettle, and pressure is
0.2MPa, is added 1% Bacilliform carbon material containing molybdenum oxide that dosage is pyromellitic acid anhydride crude product quality, and stirring hydrolysis is de-
Color hydrotreating 3h, filtering, obtains slightly hydrogenating Pyromellitic Acid crystal.
（4）It is 1 that Pyromellitic Acid crystal, which will slightly be hydrogenated, through mass ratio:At 1 potassium nitrate and the mixture fused salt of sodium nitrate
Reason is warming up to 220 DEG C with the rate of 10 DEG C/min, keeps the temperature 30min, then with the speed of 1 DEG C/min first under the pressure of -0.09MPa
Rate is warming up to 240 DEG C, keeps the temperature 60min, carries out thermal dehydration and distillation processing, obtains pyromellitic acid anhydride.
Embodiment 2：
（1）It is 1 by volume ratio:0.8 slave durol be raw material reactor come out thermal current with contain the lazy of ice crystal piece
Property gas directly mix, wherein in the inert gas containing ice crystal piece ice crystal piece content be 4%, gas velocity 0.5m/s, warp
Column trap is collected, and centrifugation obtains pyromellitic acid anhydride crude product.
（2）Molybdenum trioxide one-dimensional rod-like material is added in PVP solution, 130 DEG C of reaction 3d is warming up to, takes out crystal, wash
It washs, is dried in vacuo, the charing process at 620 DEG C obtains the Bacilliform carbon material containing molybdenum oxide through hydrofluoric acid pickling.
（3）Pyromellitic acid anhydride crude product is added in hydrolysis kettle, the temperature of steam is 100 DEG C in hydrolysis kettle, and pressure is
0.2MPa, is added 5% Bacilliform carbon material containing molybdenum oxide that dosage is pyromellitic acid anhydride crude product quality, and stirring hydrolysis is de-
Color hydrotreating 6h, filtering, obtains slightly hydrogenating Pyromellitic Acid crystal.
（4）It is 1 that Pyromellitic Acid crystal, which will slightly be hydrogenated, through mass ratio:1.5 potassium nitrate and the mixture fused salt of sodium nitrate
Processing is warming up to 230 DEG C with the rate of 20 DEG C/min, keeps the temperature 60min, then with 3 DEG C/min's first under the pressure of -0.09MPa
Rate is warming up to 250 DEG C, keeps the temperature 120min, carries out thermal dehydration and distillation processing, obtains pyromellitic acid anhydride.
Embodiment 3：
（1）It is 1 by volume ratio:0.6 slave durol be raw material reactor come out thermal current with contain the lazy of ice crystal piece
Property gas directly mix, wherein in the inert gas containing ice crystal piece ice crystal piece content be 2%, gas velocity 0.15m/s,
It is collected through column trap, centrifugation obtains pyromellitic acid anhydride crude product.
（2）Molybdenum trioxide one-dimensional rod-like material is added in PVP solution, 125 DEG C of reaction 2.5d is warming up to, takes out crystal,
Washing, vacuum drying, the charing process at 600 DEG C obtain the Bacilliform carbon material containing molybdenum oxide through hydrofluoric acid pickling.
（3）Pyromellitic acid anhydride crude product is added in hydrolysis kettle, the temperature of steam is 95 DEG C in hydrolysis kettle, and pressure is
0.2MPa, is added 2% Bacilliform carbon material containing molybdenum oxide that dosage is pyromellitic acid anhydride crude product quality, and stirring hydrolysis is de-
Color hydrotreating 4h, filtering, obtains slightly hydrogenating Pyromellitic Acid crystal.
（4）It is 1 that Pyromellitic Acid crystal, which will slightly be hydrogenated, through mass ratio:1.3 potassium nitrate and the mixture fused salt of sodium nitrate
Processing is warming up to 225 DEG C with the rate of 15 DEG C/min, keeps the temperature 45min, then with 2 DEG C/min's first under the pressure of -0.09MPa
Rate is warming up to 245 DEG C, keeps the temperature 80min, carries out thermal dehydration and distillation processing, obtains pyromellitic acid anhydride.
Embodiment 4：
（1）It is 1 by volume ratio:0.7 slave durol be raw material reactor come out thermal current with contain the lazy of ice crystal piece
Property gas directly mix, wherein in the inert gas containing ice crystal piece ice crystal piece content be 2.5%, gas velocity 0.3m/s,
It is collected through column trap, centrifugation obtains pyromellitic acid anhydride crude product.
（2）Molybdenum trioxide one-dimensional rod-like material is added in PVP solution, 128 DEG C of reaction 2d is warming up to, takes out crystal, wash
It washs, is dried in vacuo, the charing process at 610 DEG C obtains the Bacilliform carbon material containing molybdenum oxide through hydrofluoric acid pickling.
（3）Pyromellitic acid anhydride crude product is added in hydrolysis kettle, the temperature of steam is 95 DEG C in hydrolysis kettle, and pressure is
0.2MPa, is added 4% Bacilliform carbon material containing molybdenum oxide that dosage is pyromellitic acid anhydride crude product quality, and stirring hydrolysis is de-
Color hydrotreating 5h, filtering, obtains slightly hydrogenating Pyromellitic Acid crystal.
（4）It is 1 that Pyromellitic Acid crystal, which will slightly be hydrogenated, through mass ratio:1.4 potassium nitrate and the mixture fused salt of sodium nitrate
Processing is warming up to 225 DEG C with the rate of 13 DEG C/min, keeps the temperature 40min, then with 2.5 DEG C/min first under the pressure of -0.09MPa
Rate be warming up to 246 DEG C, keep the temperature 90min, carry out thermal dehydration and distillation processing, obtain pyromellitic acid anhydride.
Embodiment 5：
（1）It is 1 by volume ratio:0.5 slave durol be raw material reactor come out thermal current with contain the lazy of ice crystal piece
Property gas directly mix, wherein in the inert gas containing ice crystal piece ice crystal piece content be 4%, gas velocity 0.05m/s,
It is collected through column trap, centrifugation obtains pyromellitic acid anhydride crude product.
（2）Molybdenum trioxide one-dimensional rod-like material is added in PVP solution, 130 DEG C of reaction 2d is warming up to, takes out crystal, wash
It washs, is dried in vacuo, the charing process at 620 DEG C obtains the Bacilliform carbon material containing molybdenum oxide through hydrofluoric acid pickling.
（3）Pyromellitic acid anhydride crude product is added in hydrolysis kettle, the temperature of steam is 90 DEG C in hydrolysis kettle, and pressure is
0.2MPa, is added 5% Bacilliform carbon material containing molybdenum oxide that dosage is pyromellitic acid anhydride crude product quality, and stirring hydrolysis is de-
Color hydrotreating 3h, filtering, obtains slightly hydrogenating Pyromellitic Acid crystal.
（4）It is 1 that Pyromellitic Acid crystal, which will slightly be hydrogenated, through mass ratio:1.5 potassium nitrate and the mixture fused salt of sodium nitrate
Processing is warming up to 230 DEG C with the rate of 10 DEG C/min, keeps the temperature 30min, then with 3 DEG C/min's first under the pressure of -0.09MPa
Rate is warming up to 240 DEG C, keeps the temperature 120min, carries out thermal dehydration and distillation processing, obtains pyromellitic acid anhydride.
Embodiment 6：
（1）It is 1 by volume ratio:0.8 slave durol be raw material reactor come out thermal current with contain the lazy of ice crystal piece
Property gas directly mix, wherein in the inert gas containing ice crystal piece ice crystal piece content be 1%, gas velocity 0.5m/s, warp
Column trap is collected, and centrifugation obtains pyromellitic acid anhydride crude product.
（2）Molybdenum trioxide one-dimensional rod-like material is added in PVP solution, 120 DEG C of reaction 3d is warming up to, takes out crystal, wash
It washs, is dried in vacuo, the charing process at 590 DEG C obtains the Bacilliform carbon material containing molybdenum oxide through hydrofluoric acid pickling.
（3）Pyromellitic acid anhydride crude product is added in hydrolysis kettle, the temperature of steam is 100 DEG C in hydrolysis kettle, and pressure is
0.2MPa, is added 1% Bacilliform carbon material containing molybdenum oxide that dosage is pyromellitic acid anhydride crude product quality, and stirring hydrolysis is de-
Color hydrotreating 6h, filtering, obtains slightly hydrogenating Pyromellitic Acid crystal.
（4）It is 1 that Pyromellitic Acid crystal, which will slightly be hydrogenated, through mass ratio:At 1 potassium nitrate and the mixture fused salt of sodium nitrate
Reason is warming up to 220 DEG C with the rate of 20 DEG C/min, keeps the temperature 60min, then with the speed of 1 DEG C/min first under the pressure of -0.09MPa
Rate is warming up to 250 DEG C, keeps the temperature 60min, carries out thermal dehydration and distillation processing, obtains pyromellitic acid anhydride.
After testing, the purity for the pyromellitic acid anhydride that prepared by embodiment 1-6 and the result of yield are as follows：
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | |
| Purity（%） | 99.83 | 99.85 | 99.89 | 99.86 | 99.82 | 99.83 |
| Yield（%） | 99.3 | 99.6 | 99.5 | 99.4 | 99.5 | 99.6 |
As seen from the above table, the present invention is based on Pyromellitic Acids prepared by the method for purification of the thick pyromellitic acid anhydride of crystallization distillation
The purity and high income of dianhydride.
The above-described embodiments merely illustrate the principles and effects of the present invention, and is not intended to limit the present invention.It is any ripe
The personage for knowing this technology can all carry out modifications and changes to above-described embodiment without violating the spirit and scope of the present invention.Cause
This, institute is complete without departing from the spirit and technical ideas disclosed in the present invention by those of ordinary skill in the art such as
At all equivalent modifications or change, should by the present invention claim be covered.
Claims (10)
1. a kind of method of purification of the thick pyromellitic acid anhydride based on crystallization distillation, it is characterised in that：Include the following steps：
（1）The thermal current come out from the reactor that durol is raw material is directly mixed with the inert gas containing ice crystal piece,
It is collected through column trap, centrifugation obtains pyromellitic acid anhydride crude product；
（2）By step（1）The pyromellitic acid anhydride crude product of preparation is added in hydrolysis kettle, and the rodlike carbon materials containing molybdenum oxide are added
Material, stirring hydrolysis decoloration hydrotreating, filtering obtain slightly hydrogenating Pyromellitic Acid crystal；
（3）By step（2）The thick hydrogenation Pyromellitic Acid crystal prepared is handled through fused salt thermal dehydration and distillation, obtains equal benzene four
Formic acid dianhydride.
2. a kind of method of purification of thick pyromellitic acid anhydride based on crystallization distillation according to claim 1, feature
It is：The step（1）In, the volume ratio of thermal current and the inert gas for having ice crystal piece is 1:0.5-0.8.
3. a kind of method of purification of thick pyromellitic acid anhydride based on crystallization distillation according to claim 1, feature
It is：The step（1）In, the content of ice crystal piece is 1-4%, gas velocity 0.05- in the inert gas containing ice crystal piece
0.5m/s。
4. a kind of method of purification of thick pyromellitic acid anhydride based on crystallization distillation according to claim 1, feature
It is：The step（2）In, the temperature of steam is 90-100 DEG C in hydrolysis kettle, pressure 0.2MPa.
5. a kind of method of purification of thick pyromellitic acid anhydride based on crystallization distillation according to claim 1, feature
It is：The step（2）In, the preparation method of the Bacilliform carbon material containing molybdenum oxide is：Molybdenum trioxide one-dimensional rod-like material is added
Enter in PVP solution, is warming up to 120-130 DEG C of reaction 2-3d, takes out crystal, wash, vacuum drying carbonizes at 590-620 DEG C
Processing, through hydrofluoric acid pickling, obtains the Bacilliform carbon material containing molybdenum oxide.
6. a kind of method of purification of thick pyromellitic acid anhydride based on crystallization distillation according to claim 1, feature
It is：The step（2）In, the dosage of the Bacilliform carbon material containing molybdenum oxide is the 1-5% of pyromellitic acid anhydride crude product quality.
7. a kind of method of purification of thick pyromellitic acid anhydride based on crystallization distillation according to claim 1, feature
It is：The step（2）In, the time of hydrolysis decoloration hydrotreating is 3-6h.
8. a kind of method of purification of thick pyromellitic acid anhydride based on crystallization distillation according to claim 1, feature
It is：The step（3）In, the technique of fused salt thermal dehydration and distillation processing is：First under the pressure of -0.09MPa, with 10-
The rate of 20 DEG C/min is warming up to 220-230 DEG C, keeps the temperature 30-60min, then be warming up to 240-250 with the rate of 1-3 DEG C/min
DEG C, keep the temperature 60-120min.
9. a kind of method of purification of thick pyromellitic acid anhydride based on crystallization distillation according to claim 1, feature
It is：The step（3）In, fused salt is the mixture of potassium nitrate and sodium nitrate.
10. a kind of method of purification of thick pyromellitic acid anhydride based on crystallization distillation according to claim 1, feature
It is：The step（3）In, the purity of pyromellitic acid anhydride is more than 99.8%.
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| CN111892610A (en) * | 2020-08-18 | 2020-11-06 | 连云港鹏辰特种新材料有限公司 | Method for efficiently trapping and purifying pyromellitic dianhydride |
| CN113583016A (en) * | 2021-09-01 | 2021-11-02 | 潍坊弘润新材料有限公司 | Method for improving purity of crude pyromellitic dianhydride, device and application thereof |
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Denomination of invention: A purification method of crude pyromellitic dianhydride based on crystal sublimation Effective date of registration: 20210918 Granted publication date: 20200714 Pledgee: Bank of Nanjing Co.,Ltd. Lianyungang Branch Pledgor: LIANYUNGANG PENGCHEN SPECIAL NEW MATERIAL Co.,Ltd. Registration number: Y2021320000235 |