Determination method for insoluble substances in polymer

A measurement method and high polymer technology, applied in the field of chemical analysis, can solve the problems of insoluble impurity blockage, blockage removal trouble, funnel scrapping, etc.

Inactive Publication Date: 2013-10-09
LUCKY HUAGUANG GRAPHICS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

(2) Apparent ills of plates appear: insoluble matter in polymers is usually the main cause of apparent ills of plates
The filters used are mainly G3 type "glass sand core funnels", there are as many as 11 types, but the biggest problem with using sand core funnels is that insoluble impurities will block the filter holes of the sand core, and it is troublesome to remove these blockages. It even caused the funnel to be scrapped; there is another method to measure insoluble matter is to use centrifugation, and another 6 kinds use filter paper to filter
However, the scope of application of these standards is not included in the determination of the insoluble content of polymers

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Embodiment 1: a kind of assay method of insolubles in polymer, comprises the following steps:

[0031] a. Weigh 5.0176g of phenolic resin sample, record it as m0, put it into a 250mL conical flask, stir it with an electromagnetic stirrer to make it fully dissolve;

[0032] b. The dried and constant-weight 0.45 μm filter membrane is weighed to obtain m1=0.1010g, installed on a solvent filter, and the solution obtained in step a is vacuum-filtered through the filter to be nearly dry;

[0033] c. Use 20 mL of ethylene glycol monoethyl ether EC to wash the insoluble matter on the filter membrane three times, and continue vacuum filtration until no solvent drops;

[0034] d. Remove the filter membrane dried by suction in step C, put it in a glass desiccator, and evacuate it to 500mmHg, and leave it for 1 hour;

[0035] e. Take out the filter membrane after drying and constant weight in step D, and weigh m2=0.1084g;

[0036] f. According to formula (1), the content of insol...

Embodiment 2

[0037] Embodiment 2: a kind of assay method of insoluble matter in high polymer, comprises the following steps:

[0038] a. Weigh 5.9993g of epoxy resin modified phenolic resin sample, record it as m0, put it into a 250mL Erlenmeyer flask, place it overnight, and shake it before filtering to fully dissolve it;

[0039] b. The dried and constant-weight 0.45 μm filter membrane is weighed to obtain m1=0.1027g, installed on a solvent filter, and the solution obtained in step a is vacuum-filtered through the filter until nearly dry;

[0040] c. Use 20mL of EC to wash the insoluble matter on the filter membrane three times, and continue to vacuum filter until no solvent drops;

[0041] d. Remove the filter membrane dried by suction in step C, put it in a glass desiccator, and evacuate it to 500mmHg, and leave it for 1 hour;

[0042] e. Take out the filter membrane after drying and constant weight in step D, and weigh m2=0.1083g;

[0043] f. According to formula (1), the content of i...

Embodiment 3

[0044] Embodiment 3: a kind of assay method of insoluble matter in high polymer, comprises the following steps:

[0045] a. Weigh 6.0168g of alkylphenolic resin sample, record it as m0, put it into a 250mL Erlenmeyer flask, put it into an ultrasonic generator, and ultrasonically dissolve it fully;

[0046] b. The dried and constant-weight 0.45 μm filter membrane is weighed to obtain m1=0.1028g, installed on a solvent filter, and the solution obtained in step a is vacuum-filtered to nearly dry through the filter;

[0047] c. Use 20mL of ethylene glycol monodiether to wash the insoluble matter on the filter membrane three times, and continue vacuum filtration until no solvent drops;

[0048] d. Remove the filter membrane dried by suction in step C, put it in a glass desiccator, and evacuate it to 500mmHg, and leave it for 1 hour;

[0049] e. Take out the filter membrane after drying and constant weight in step D, and weigh m2=0.1580g;

[0050] f. According to formula (1), the ...

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PUM

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Abstract

The invention discloses a determination method for insoluble substances in a polymer. The determination method comprises the following steps of a. weighing the polymer, dissolving the polymer completely in ethylene glycol monoethyl ether; b. weighing a 0.40-0.55 [mu]m filter membrane, suction filtering with the 0.40-0.55 [mu]m filter membrane, the insoluble substances being left on the membrane, and suction filtering the filter membrane until the filter membrane is dried; c. taking the filter membrane down, putting the filter membrane into a vacuum drier with a vacuum degree of 450-550 mmHg, drying for 1-1.5 hours at a room temperature, taking out the filter membrane, weighing to obtain the weight of the residual substances; and d. calculating the content of the insoluble substances in the polymer. The content of the insoluble substances in the polymer is calculated by drying and weighing under a vacuum condition at the room temperature. Instrument and equipment used in the method are easily available and low in cost and can be easily popularized.

Description

technical field [0001] The invention belongs to the technical field of chemical analysis, in particular to a method for measuring insoluble matter in high polymers with ethylene glycol monoethyl ether (EC) solvent. It can be used for the analysis of samples with insoluble content of high polymer in ethylene glycol monoethyl ether solvent between 0.05% and 1.00%. Background technique [0002] If the high polymer used in the printing plate contains insoluble matter above 0.45 μm, such as ultra-high molecular weight polymers, cross-linked products, overheated oxidation products, etc., as well as solid particles mixed in during the synthesis process, these insoluble matter will be in During the plate production process, it will cause many problems in the coating solution. For example (1) Increase the replacement frequency of the filter element on the production line: If the insoluble content in the polymer is too high, the direct adverse consequences will increase the chance of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N5/04
Inventor 王怀功张涛高峰张刚
Owner LUCKY HUAGUANG GRAPHICS
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