CN108333269A - A kind of purity analysis method of bibenzene tetracarboxylic dianhydride - Google Patents
A kind of purity analysis method of bibenzene tetracarboxylic dianhydride Download PDFInfo
- Publication number
- CN108333269A CN108333269A CN201810100033.1A CN201810100033A CN108333269A CN 108333269 A CN108333269 A CN 108333269A CN 201810100033 A CN201810100033 A CN 201810100033A CN 108333269 A CN108333269 A CN 108333269A
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- CN
- China
- Prior art keywords
- analysis method
- tetracarboxylic dianhydride
- bibenzene tetracarboxylic
- purity
- sample
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- 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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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/067—Preparation by reaction, e.g. derivatising the sample
Abstract
The present invention relates to the purity analysis method of bibenzene tetracarboxylic dianhydride, analytical instrument used in the analysis method is LC 20AT type high performance liquid chromatographs, and the analysis condition of the high performance liquid chromatograph is：Pillar C18,25 DEG C, sample size 5ml, Detection wavelength 250mau, detection time 10min of column temperature, mobile phase：Acetonitrile: 0.1 formic acid=3 weight %:7.In the purity analysis method, sample preparation step is：It weighs 0.01g bibenzene tetracarboxylic dianhydride samples to be contained in 10ml dry reaction bottles, 5ml absolute methanols is added, after being heated to reflux 3~4 hours, you can sample presentation detects.High-purity bibenzene tetracarboxylic dianhydride sample is detected by the analysis method of the present invention, testing result is 99.8wt% 99.9wt% purity.
Description
One, technical fields
The present invention relates to the purity analysis methods of bibenzene tetracarboxylic dianhydride, it more particularly relates to polyimides
With the purity analysis method of monomer bibenzene tetracarboxylic dianhydride.
Two, background technologies
Polyimides is to adapt to aerospace, microelectronics industry, the needs of automobile and other industries, to the matter of polyimides itself
Amount proposes new requirement.High request is proposed to the acid anhydrides and diamines quality of synthesis of polyimides, it is desirable that both raw materials
Purity is in 99.5wt% or more.
It is required to meet user, needs to be rigid in checking up to the acid anhydrides quality that manufacturer produces, it is desirable that engineering technology
The analysis method of personnel searching fast accurate.For the purity analysis of bibenzene tetracarboxylic dianhydride (BPDA), chemist surely can
Chromatograph method is expected to analyze.With liquid chromatogram or gas chromatography analysis methodWhat analysis condition is, analyzes sample
Product produce equal technical characteristics, it is necessary to by experiment, pay hard working to realize.
Three, invention contents
For the present inventors in order to find precisely, quick analysis method has made particular study, first to gas chromatography
It contrasts with high performance liquid chromatography purposes, they think that gas-chromatography is mainly used in permanent gas and some small molecules and has
The separation and analysis of machine object gas.Early seventies high performance liquid chromatography have evolved into it is a kind of it is strong separation with analysis
Means, development speed have been more than gas chromatography.High performance liquid chromatography can analyze general fluid sample, and particularly suitable
In analysis higher boiling, macromolecular is highly polar, thermal instability compound and various ionic compounds.Therefore it is widely answered
For amino acid, protein, steroid, carbohydrate, organic acid, product, drug, antibiotic, vitamin, pesticide, Gao Ju
The separation and analysis of object and various inorganic salts.The boiling point 399~400 for the sample bibenzene tetracarboxylic dianhydride that the present invention is analyzed
DEG C, facile hydrolysis decomposes.Mp299~301 DEG C of bibenzene tetracarboxylic dianhydride,>300 DEG C of decomposition.They belong to organic acid, selection
High-efficient liquid phase chromatogram technique analysis is more reasonable.
Compared by experiment, LC-20AT type high performance liquid chromatographs is selected to analyze bibenzene tetracarboxylic dianhydride purity, analyzes item
Part is set to：Pillar C18,25 DEG C, sample size 5ml, Detection wavelength 250mau, detection time 10min of column temperature, mobile phase：Acetonitrile:
0.1 formic acid=3 weight %:7.
Acid anhydrides esterification is made bibenzene tetracarboxylic dianhydride be transformed into four methyl esters of bibenzene tetracarboxylic by present invention absolute methanol.
It is contained in 10ml dry reaction bottles so weighing 0.01g bibenzene tetracarboxylic dianhydride samples, 5ml absolute methanols is added, are heated to reflux
It 3-4 hours can sample presentation detection.
It can detect the purity of bibenzene tetracarboxylic dianhydride by the analysis method of the present invention, new chemical materials are created in detection Shanghai admittedly to be had
The high-purity bibenzene tetracarboxylic dianhydride sample that limit company provides, testing result are 99.8wt%-99.9wt% purity.
Four, are illustrated
Fig. 1 is the chromatogram of high efficiency liquid chromatography instrument LC-20AT detection bibenzene tetracarboxylic dianhydride purity.
Five, specific implementation modes
In order to more preferably implement the present invention, special illustration, but embodiment is not limitation of the present invention.
Embodiment 1
It weighs 0.01g bibenzene tetracarboxylic dianhydrides to be contained in 10ml dry reaction bottles, 5ml absolute methanols is added, are heated to reflux
3.5 hours, you can sample presentation detects.
The bibenzene tetracarboxylic dianhydride sample of methanol esterification is detected with high efficiency liquid chromatography instrument Shimadzu LC-20AT.Control
Testing conditions processed are：Pillar C18,25 DEG C, sample size 5ml, Detection wavelength 250mAU of column temperature, detection time 10min.Mobile phase：
Acetonitrile: 0.1% (weight) formic acid=3:7.Testing result is as shown in Figure 1, bibenzene tetracarboxylic dianhydride purity is 99.8wt%.
The chromatogram of bibenzene tetracarboxylic dianhydride purity is detected referring to Fig. 1 high efficiency liquid chromatography instrument LC-20AT.It is with height below
Effect liquid chromatograph Shimadzu LC-20AT reports the chromatography that the bibenzene tetracarboxylic dianhydride sample of methanol esterification is detected.
BPDA chromatography are reported
Spectrogram file：E：Liquid phase [2] oop orgData BPDA BPDA [GC0120170905001] 000001.smp
Sample name and type：BPDA (1=samples)
Lot number：GC0120170905
Method：BPDA- normalization methods (area normalization method)
Analysis of results table
Claims (2)
1. a kind of purity analysis method of bibenzene tetracarboxylic dianhydride, which is characterized in that analytical instrument used in the analysis method is LC-
20AT type high performance liquid chromatographs, the analysis condition of the high performance liquid chromatograph are：Pillar C18,25 DEG C, sample size 5ml of column temperature,
Detection wavelength 250mau, detection time 10min, mobile phase：Acetonitrile: 0.1 formic acid=3 weight %:7.
2. a kind of purity analysis method of bibenzene tetracarboxylic dianhydride according to claim 1, which is characterized in that described is pure
It spends in analysis method, sample preparation step is：0.01g bibenzene tetracarboxylic dianhydride samples are weighed to be contained in 10ml dry reaction bottles,
5ml absolute methanols are added, after being heated to reflux 3~4 hours, you can sample presentation detects.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810100033.1A CN108333269A (en) | 2018-02-01 | 2018-02-01 | A kind of purity analysis method of bibenzene tetracarboxylic dianhydride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201810100033.1A CN108333269A (en) | 2018-02-01 | 2018-02-01 | A kind of purity analysis method of bibenzene tetracarboxylic dianhydride |
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| CN108333269A true CN108333269A (en) | 2018-07-27 |
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| CN201810100033.1A Pending CN108333269A (en) | 2018-02-01 | 2018-02-01 | A kind of purity analysis method of bibenzene tetracarboxylic dianhydride |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3719492A4 (en) * | 2018-10-05 | 2021-04-14 | Lg Chem, Ltd. | Dianhydride analysis method |
Citations (6)
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|---|---|---|---|---|
| CN1436780A (en) * | 2003-03-03 | 2003-08-20 | 中国科学院长春应用化学研究所 | Prepn process of 2,3,3',4'-diphenyl tetraformic dianhydride and its derivative |
| CN101251515A (en) * | 2008-04-10 | 2008-08-27 | 常熟市联邦化工有限公司 | Method for testing pyromellitic acid anhydride purity and organic impurity |
| CN101659647A (en) * | 2008-08-26 | 2010-03-03 | 比亚迪股份有限公司 | Method for preparing diphenyl tetracarboxylic dianhydride |
| CN102040573A (en) * | 2009-10-17 | 2011-05-04 | 比亚迪股份有限公司 | Biphenyltetracarboxylic di-anhydride, preparation method thereof and polymide synthesized by using same |
| CN102558119A (en) * | 2004-06-28 | 2012-07-11 | 三菱化学株式会社 | Biphenyltetracarboxylic acid dianhydride, method for producing the same, polyimide using the same and method for producing polyimide using the same |
| CN106279085A (en) * | 2016-08-17 | 2017-01-04 | 万华化学集团股份有限公司 | A kind of preparation method mixing isomery bis ether tetracarboxylic acid dianhydride |
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2018
- 2018-02-01 CN CN201810100033.1A patent/CN108333269A/en active Pending
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| CN1436780A (en) * | 2003-03-03 | 2003-08-20 | 中国科学院长春应用化学研究所 | Prepn process of 2,3,3',4'-diphenyl tetraformic dianhydride and its derivative |
| CN102558119A (en) * | 2004-06-28 | 2012-07-11 | 三菱化学株式会社 | Biphenyltetracarboxylic acid dianhydride, method for producing the same, polyimide using the same and method for producing polyimide using the same |
| CN101251515A (en) * | 2008-04-10 | 2008-08-27 | 常熟市联邦化工有限公司 | Method for testing pyromellitic acid anhydride purity and organic impurity |
| CN101659647A (en) * | 2008-08-26 | 2010-03-03 | 比亚迪股份有限公司 | Method for preparing diphenyl tetracarboxylic dianhydride |
| CN102040573A (en) * | 2009-10-17 | 2011-05-04 | 比亚迪股份有限公司 | Biphenyltetracarboxylic di-anhydride, preparation method thereof and polymide synthesized by using same |
| CN106279085A (en) * | 2016-08-17 | 2017-01-04 | 万华化学集团股份有限公司 | A kind of preparation method mixing isomery bis ether tetracarboxylic acid dianhydride |
Non-Patent Citations (2)
| Title |
|---|
| WENXI HUANG等: "Synthesis and miscibility studies of rodlike/ flexible polyimide molecular composites via para-para linked aromatic poly(amic ester) precursors", 《POLYMER》 * |
| 张金芳等: "一种测定3,3′,4,4′-联苯四甲酸二酐纯度的新方法", 《理化检验-化学分册》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3719492A4 (en) * | 2018-10-05 | 2021-04-14 | Lg Chem, Ltd. | Dianhydride analysis method |
| US11327059B2 (en) | 2018-10-05 | 2022-05-10 | Lg Chem, Ltd. | Dianhydride analysis method |
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