CN108061692A - A kind of accurate method for measuring fine foreign matter content in pyromellitic acid anhydride - Google Patents
A kind of accurate method for measuring fine foreign matter content in pyromellitic acid anhydride Download PDFInfo
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- CN108061692A CN108061692A CN201711356964.XA CN201711356964A CN108061692A CN 108061692 A CN108061692 A CN 108061692A CN 201711356964 A CN201711356964 A CN 201711356964A CN 108061692 A CN108061692 A CN 108061692A
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- acid anhydride
- pyromellitic acid
- filter membrane
- foreign matter
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
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Abstract
The invention discloses a kind of accurate method for measuring fine foreign matter content in pyromellitic acid anhydride, including following detecting steps：1）Weigh sample；2）Filter membrane dimethylformamide is impregnated 10 minutes, the heat drying 20 minutes in the baking oven of 100 DEG C of temperature, re-dry cools down 20 minutes, weighs；3）Excess dimethyl formamide is added in the container equipped with pyromellitic acid anhydride sample and is sufficiently stirred；4）Filter membrane is fitted into sand core filter device, dimethyl formamide solution is poured into the sand core filter device equipped with filter membrane, is filtered by vacuum；5）The filter membrane in sand core filter device is removed, heat drying 20 minutes in 100 DEG C of baking oven, dry cooling 20 minutes weighs.The present invention dissolves pyromellitic acid anhydride using excessive dimethylformamide as solvent, and dissolved pyromellitic acid anhydride will not change, and the fine foreign matter weight that can be finally accurately detected in pyromellitic acid anhydride, levels of precision reaches 0.1mg.
Description
Technical field
The present invention relates to detection technique field, more particularly to a kind of inspection of fine foreign matter content in pyromellitic acid anhydride
Survey method.
Background technology
The Pyromellitic Acid of high-purity（Pyromellitic ACID, abridge PMA）With the pyromellitic acid anhydride of high-purity
（Pyromellitic Dianhydride, abridge PMDA）It is mainly used as synthesis high-end electronic grade Kapton
（Polyimide, abridge PI）Raw material.
PI films have good physical and chemical performance, at high temperature（300℃）Heating 1 year it is non-fusible do not burn, and
It has the stability to radiation and all solvents concurrently, it is each to be widely used in space flight, aviation, microelectronics and machinery, electric appliance etc.
Industry.
Chinese patent《The detection method of ultra-fine foreign material in Pyromellitic Acid, pyromellitic acid anhydride》, Application No.
200810023605.7 disclose a kind of detection side for the ultra-fine foreign material for detecting Pyromellitic Acid or pyromellitic acid anhydride
Sample to be tested is dissolved in solvent by method（Water）In, it is filtered with filter paper, then the filter paper after filtering is placed under microscope, in filter paper
On take point of observation observe stain, and then in two anhydride products foreign matter content carry out one detection.This method is two anhydride products
Dissolving is detected in a solvent, however the sample size of this method detection is less, and man's activity and contingency are bigger, inspection
The number that result is foreign matter is surveyed, can only probably be referred to as one of dianhydride product quality, result of the test is simultaneously inaccurate.Cause
This, being capable of the accurate quantitative fine foreign matter detected in pyromellitic acid anhydride there is an urgent need for one detection method of design
Content.
The content of the invention
The invention mainly solves the technical problem of providing fine foreign matters in a kind of accurate measure pyromellitic acid anhydride to contain
The method of amount.
In order to solve the above technical problems, one aspect of the present invention is：
A kind of accurate method for measuring fine foreign matter content in pyromellitic acid anhydride is provided, including following detecting steps：
1）Sample is weighed, a certain amount of pyromellitic acid anhydride sample is weighed, is placed in container, the pyromellitic acid anhydride examination
The weight tested is accurate to 0.01g；
2）Filter membrane processing impregnates filter membrane dimethylformamide 10 minutes, and the rear filter membrane that takes out is placed in baking oven, and oven temperature is set
100 DEG C are scheduled on, heat drying 20 minutes, rear taking-up filter membrane is placed in drier to be cooled down 20 minutes again, then is weighed；
3）Dissolved samples install excessive dimethylformamide addition in the container of pyromellitic acid anhydride sample, fully
Stirring, makes pyromellitic acid anhydride sample be dissolved completely in dimethylformamide；
4）Filtering, by step 2）In the filter membrane handled well be fitted into sand core filter device, step 3）In obtained dimethyl methyl
Amide solution is poured into the sand core filter device equipped with filter membrane, using vacuum filtration pumping filter；After filtering, then use dimethyl
Formamide cleaning filter membranes and residue at least 2 times；
5）Drying is weighed, and removes step 4）In sand core filter device, take out filter membrane be placed in baking oven, drying temperature is set as
100 DEG C, heat drying 20 minutes further takes out filter membrane and is placed in drier, cools down 20 minutes, is weighed with assay balance.
In a preferred embodiment of the present invention, in step 3）In, using magnetic stirring apparatus, cooperation, which is placed in container, to be turned
Son is stirred dissolving to pyromellitic acid anhydride sample.
In a preferred embodiment of the present invention, the filter membrane is polytetrafluoroethylcomposite composite film.
In a preferred embodiment of the present invention, the aperture of the filter membrane is 1 μm.
In a preferred embodiment of the present invention, the filter aperture of the sand core filter device is 10 μm.
In a preferred embodiment of the present invention, the sieve plate material of the sand core filter device is high-boron-silicon glass.
In a preferred embodiment of the present invention, the purity of the dimethylformamide of use is more than 99.5%, and density is
0.945 ~ 0.950 g/ml, evaporation residue≤0.005%.
In a preferred embodiment of the present invention, step 5）The middle weight that filter membrane is weighed using assay balance, is accurate to
0.1mg。
The beneficial effects of the invention are as follows：This detection method of the present invention, using excessive dimethylformamide as solvent
Dissolve pyromellitic acid anhydride, hydrolysis or other changes will not occur for dissolved pyromellitic acid anhydride, finally being capable of essence
Really detect the fine foreign matter weight in pyromellitic acid anhydride, levels of precision reaches 0.1mg.
Specific embodiment
Presently preferred embodiments of the present invention is described in detail below so that advantages and features of the invention can be easier to by
It will be appreciated by those skilled in the art that so as to make a clearer definition of the protection scope of the present invention.
Embodiment 1：
1）Sample is weighed, the pyromellitic acid anhydride sample of 200g is weighed with assay balance, is placed in beaker, the equal benzene tetramethyl
The weight of acid dianhydride experiment is accurate to 0.01g；
2）Filter membrane processing impregnates filter membrane dimethylformamide 10 minutes, and the rear filter membrane that takes out is placed in baking oven, and oven temperature is set
100 DEG C are scheduled on, heat drying 20 minutes, rear taking-up filter membrane is placed in drier to be cooled down 20 minutes again, is weighed again with assay balance,
Weight is accurate to 0.1mg；
3）The dimethylformamide of 3L excess is added in the beaker equipped with pyromellitic acid anhydride sample, burnt by dissolved samples
Rotor is put into cup, and beaker is placed on magnetic stirring apparatus, beaker mouth is sealed with preservative film, is opened magnetic stirring apparatus, is filled
Divide stirring, pyromellitic acid anhydride sample is made to be dissolved completely in dimethylformamide, obtains dimethyl formamide solution；
4）Filtering, by step 2）In the filter membrane handled well be fitted into sand core filter device, step 3）In obtained dimethyl methyl
Amide solution is poured into the filter tunnel of the sand core filter device equipped with filter membrane, opens valve, and the solution filtered down flows into filter
In cup, vacuum filtration pumping filter is opened；After filtering, then with 150g dimethylformamides cleaning filter membranes and residue at least 2
It is secondary；
5）Drying is weighed, and after filtering and cleaning, removes step 4）In sand core filter device, the filter membrane taken out above is placed in
In baking oven, drying temperature is set as 100 DEG C, and heat drying 20 minutes further takes out filter membrane and is placed in drier, cools down 20 minutes,
It is weighed with assay balance, is accurate to 0.1mg.
As a result calculate：
U=1000 × (W2-W1)/200,
In formula：
Insoluble matter content/ppm in U-pyromellitic acid anhydride,
Filter membrane weight/mg after W2-filtering,
W1-filtering front filter weight/mg,
Under similarity condition, at least three groups of insoluble impurities content analysis experiments are done to same pyromellitic acid anhydride sample, are made even
Average.
Following table is the result measured using the method in the present embodiment：
As can be seen from the above table, totally 10 groups of foreign matter content analysis experiments, the average value of 10 groups of experiments is 9.66, reaches the requirement 15 of client
Below ppm.
Embodiment 2：
In step 1）The weight that middle pyromellitic acid anhydride sample weighs by 160 ~ 200g etc., last calculation formula be changed to U=
1000 × (W2-W1)/n, n be the pyromellitic acid anhydride sample weighed weight, unit g.Remaining test procedure, parameter
It is same as Example 1.
Following table is the result measured using the method in the present embodiment：
As can be seen from the above table, totally 10 groups of foreign matter content analysis experiments, the average value of 10 groups of experiments is 9.22ppm, reaches wanting for client
Seek 15 below ppm.
In the above-described embodiments, the experimental facilities of use is as follows：
Assay balance：It is accurate to 0.1 mg；
Baking oven：It can be controlled in 100 DEG C ± 1 DEG C；
Beaker：5 L of capacity；
Drier：Built-in efficient drying agent；
Filter membrane：Filter membrane is the composite membrane of polytetrafluoroethylene (PTFE), and a diameter of 47 mm, aperture is 1 μm；
Sand core filter device：Rise T-50 in model Tianjin, 10 μm of filter aperture, sieve plate material be high-boron-silicon glass, filter bowl 500
ML, 5 L of filter tunnel, receiving bottle 5 L, matching used a diameter of 47 mm of filter membrane；
Vacuum filtration pump：Negative pressure is provided for sand core filter device.
This detection method of the present invention dissolves Pyromellitic Acid two using excessive dimethylformamide as solvent
Acid anhydride, dissolved pyromellitic acid anhydride will not occur hydrolysis or other changes, can finally be accurately detected Pyromellitic Acid
Fine foreign matter weight in dianhydride, levels of precision reach 0.1mg.
The foregoing is merely the embodiment of the present invention, are not intended to limit the scope of the invention, every to utilize this hair
The equivalent structure or equivalent flow shift that bright description is made directly or indirectly is used in other relevant technology necks
Domain is included within the scope of the present invention.
Claims (8)
- A kind of 1. accurate method for measuring fine foreign matter content in pyromellitic acid anhydride, which is characterized in that including following detections Step：1）Sample is weighed, a certain amount of pyromellitic acid anhydride sample is weighed, is placed in container, the pyromellitic acid anhydride examination The weight tested is accurate to 0.01g；2）Filter membrane processing impregnates filter membrane dimethylformamide 10 minutes, and the rear filter membrane that takes out is placed in baking oven, and oven temperature is set 100 DEG C are scheduled on, heat drying 20 minutes, rear taking-up filter membrane is placed in drier to be cooled down 20 minutes again, then is weighed；3）Dissolved samples install excessive dimethylformamide addition in the container of pyromellitic acid anhydride sample, fully Stirring, makes pyromellitic acid anhydride sample be dissolved completely in dimethylformamide；4）Filtering, by step 2）In the filter membrane handled well be fitted into sand core filter device, step 3）In obtained dimethyl methyl Amide solution is poured into the sand core filter device equipped with filter membrane, using vacuum filtration pumping filter；After filtering, then use dimethyl Formamide cleaning filter membranes and residue at least 2 times；5）Drying is weighed, and removes step 4）In sand core filter device, take out filter membrane be placed in baking oven, drying temperature is set as 100 DEG C, heat drying 20 minutes further takes out filter membrane and is placed in drier, cools down 20 minutes, is weighed with assay balance.
- 2. the accurate method for measuring fine foreign matter content in pyromellitic acid anhydride according to claim 1, feature exist In in step 3）In, using magnetic stirring apparatus, cooperation is placed in the rotor in container, pyromellitic acid anhydride sample is stirred Mix dissolving.
- 3. the accurate method for measuring fine foreign matter content in pyromellitic acid anhydride according to claim 1, feature exist In the filter membrane is polytetrafluoroethylcomposite composite film.
- 4. the accurate method for measuring fine foreign matter content in pyromellitic acid anhydride according to claim 1, feature exist In the aperture of the filter membrane is 1 μm.
- 5. the accurate method for measuring fine foreign matter content in pyromellitic acid anhydride according to claim 1, feature exist In the filter aperture of the sand core filter device is 10 μm.
- 6. the accurate method for measuring fine foreign matter content in pyromellitic acid anhydride according to claim 1, feature exist In the sieve plate material of the sand core filter device is high-boron-silicon glass.
- 7. the accurate method for measuring fine foreign matter content in pyromellitic acid anhydride according to claim 1, feature exist It is more than 99.5% in the purity of, the dimethylformamide of use, density is 0.945 ~ 0.950 g/ml, evaporation residue≤0.005%.
- 8. the accurate method for measuring fine foreign matter content in pyromellitic acid anhydride according to claim 1, feature exist In step 5）The middle weight that filter membrane is weighed using assay balance, is accurate to 0.1mg.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112763370A (en) * | 2020-12-21 | 2021-05-07 | 山东省产品质量检验研究院 | Method for removing film material on surface of fabric and application thereof |
Citations (2)
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| CN101251494A (en) * | 2008-04-11 | 2008-08-27 | 常熟市联邦化工有限公司 | Method for detecting ultra-minuteness foreign body in pyromellitic acid and pyromellitic acid anhydride |
| CN103344518A (en) * | 2013-06-21 | 2013-10-09 | 乐凯华光印刷科技有限公司 | Determination method for insoluble substances in polymer |
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2017
- 2017-12-16 CN CN201711356964.XA patent/CN108061692A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101251494A (en) * | 2008-04-11 | 2008-08-27 | 常熟市联邦化工有限公司 | Method for detecting ultra-minuteness foreign body in pyromellitic acid and pyromellitic acid anhydride |
| CN103344518A (en) * | 2013-06-21 | 2013-10-09 | 乐凯华光印刷科技有限公司 | Determination method for insoluble substances in polymer |
Non-Patent Citations (2)
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| 李广宇 等: "《胶黏剂原材料手册》", 31 August 2004, 北京：国防工业出 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112763370A (en) * | 2020-12-21 | 2021-05-07 | 山东省产品质量检验研究院 | Method for removing film material on surface of fabric and application thereof |
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Application publication date: 20180522 |