CN116754598A - Method for testing gelation time of epoxy resin composition and application thereof - Google Patents
Method for testing gelation time of epoxy resin composition and application thereof Download PDFInfo
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- CN116754598A CN116754598A CN202310557278.8A CN202310557278A CN116754598A CN 116754598 A CN116754598 A CN 116754598A CN 202310557278 A CN202310557278 A CN 202310557278A CN 116754598 A CN116754598 A CN 116754598A
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- gelation time
- epoxy resin
- resin composition
- testing
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- 238000001879 gelation Methods 0.000 title claims abstract description 50
- 238000012360 testing method Methods 0.000 title claims abstract description 39
- 239000000203 mixture Substances 0.000 title claims abstract description 31
- 239000003822 epoxy resin Substances 0.000 title claims abstract description 28
- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 20
- 238000010998 test method Methods 0.000 claims abstract description 7
- 239000000523 sample Substances 0.000 claims description 45
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000002932 luster Substances 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 229920005989 resin Polymers 0.000 claims description 2
- 239000011347 resin Substances 0.000 claims description 2
- 239000004593 Epoxy Substances 0.000 abstract description 4
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- 238000005259 measurement Methods 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000004132 cross linking Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000003746 surface roughness Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/02—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Strength Of Materials By Application Of Mechanical Stress (AREA)
Abstract
The application discloses a method for testing the gelation time of an epoxy resin composition and application thereof, wherein the size of a sample to be tested is regulated, a contact piece is adopted for operation, meanwhile, the end point of the gelation time is quantified, the timing end point is accurately judged, the manual operation error is avoided, expensive instruments or customized instrument equipment are not required to be purchased, the cost is reduced, the operation error caused by the precision of the instruments and equipment can be avoided, the gelation time of the epoxy resin composition can be accurately measured, and particularly, the gelation time of the epoxy composition which is extremely fast and can not be tested or is easy to generate larger test error within 20s can be accurately measured by using the traditional test method, and the test cost is low and the operation is convenient.
Description
Technical Field
The application relates to the technical field of gelation time measurement, in particular to the field of I PC G01, and more particularly relates to a method for testing gelation time of an epoxy resin composition and application thereof.
Background
The gelation time refers to the time for the epoxy resin or other colloidal fluid to change from a viscous state to a gel solid state at a specific temperature, at which time the chain segment is initiated to grow, and as the reaction proceeds, the molecular chain is continuously increased to increase the molecular viscosity, and the gelation time can characterize the activity of the crosslinking reaction. Epoxy resins are widely used in various fields such as electronic devices, aviation, civil engineering, and automobile manufacturing. Because the resin has fluidity before the gel, the steps of pouring, infiltration and the like can be carried out, the gel time is judged to have great influence on the defects of bubble occurrence and insufficient casting solution of the production parts, the gelation process is mastered to effectively control the quality of the produced products, the operation risk is reduced, and the method has remarkable guiding significance for practical application.
At present, a plurality of existing testing methods and national standards all use a flat shovel to scrape a test sample, and when the test sample is subjected to resistance, the gelation time is considered to be stopped, and the judgment standard is based on the feeling of an operator, so that the error is larger. Other methods mainly rely on instruments for testing, and the epoxy composition has extremely high crosslinking and curing reaction speed at high temperature, and has high requirements on the testing precision of a testing instrument, and the existing high-precision equipment cannot meet the requirements on the testing precision and the testing range at the same time and cannot be used for packaging materials of the epoxy composition with extremely rapid gelation.
CN109342490a discloses a device and a method for measuring gelation time, wherein the end point of gelation time is determined by using torque data, and interference of human factors on test results is reduced, but the measurement process depends on the measuring device, so that the precision of the device cannot be determined, and influence errors on the data cannot be determined.
Disclosure of Invention
In order to solve the above problems, the first aspect of the present application provides a method for testing gelation time of an epoxy resin composition, comprising the steps of:
s1: setting the size of a sample wafer;
s2, prescribing the size of the L-shaped contact piece;
s3: the gelation time of the sample was measured.
Preferably, the specific steps of S1 are as follows: the epoxy resin composition was made into round plaques by a manual tablet press and a tablet die.
Preferably, the surface area of the round sample wafer is 6-10cm 2 。
Preferably, the diameter of the circular sample wafer is 28mm,thickness of 1mm and surface area of 6.16cm 2 。
Preferably, the dimension of the L-shaped contact piece is from bottom surface to length of 35 mm multiplied by width of 30 mm multiplied by thickness of 1 mm; terminal-width 30 mm x high 5 mm x thick 1 mm; the arithmetic mean deviation Ra of the surface roughness profile is 0.050.
Preferably, the L-shaped contact piece is made of 15Cr10NI stainless steel.
Preferably, the specific step of S3 is as follows:
(1) Placing the round sample on a heating plate, and heating the sample;
(2) The bottom surface of the L-shaped contact piece is horizontally covered on the surface of the sample piece, timing is started immediately when the surface of the sample piece has luster, and then the thrust meter probe vertically presses the L-shaped contact piece to a first thrust value.
(3) And then the probe of the thrust meter is vertically pushed to the tail end of the L-shaped contact piece, when the reasoning value displayed by the thrust meter reaches a second thrust value, the timing is stopped, the test is completed, and the gelation time is recorded.
Preferably, the sample wafer is heated to a temperature of 174-176 ℃.
Preferably, the sample wafer is heated to 175 ℃.
Preferably, the first thrust value is 0.20kgf.
Preferably, the second thrust value is 1.2kgf.
In a second aspect the present application provides the use of a method of testing the gelation time of an epoxy resin composition as described above for determining the gelation time of an epoxy resin composition.
On one hand, the specification of a test sample in the gelation time test process of the epoxy resin composition is accurately regulated, so that the consumption of the sample meets the national standard, and measurement errors caused by different areas and thicknesses of the sample during different measurements are avoided; meanwhile, the measurement focus of the gelation time is quantified, the problems that the traditional measurement mode depends on manual judgment of a timing end point through the sense of the level of resistance of the production, the repeatability of the test and the accuracy of the result are affected are solved, in addition, the defects that the gelation time tester cannot meet the precision requirement of the gelation time test and the testability range of the instrument cannot meet the test range requirement of a sample are avoided, expensive instrument equipment is not required to be customized and purchased, the operation cost is reduced, and the accuracy of the test result is improved.
The beneficial effects are that:
1. the application provides a method for testing the gelation time of an epoxy resin composition, which adopts a contact piece to operate and simultaneously quantifies the end point of the gelation time, accurately judges the timing end point, avoids manual operation errors, can accurately test the gelation time of the epoxy resin composition, and particularly accurately tests the gelation time of the epoxy resin composition within 20s, which cannot be tested or is easy to generate larger test errors by using the traditional testing method, and has low testing cost and convenient operation.
2. The application provides the size of the sample to be measured, so that the area of the sample can meet the requirements of national standard GB/T40564-2021, and the measurement error caused by different sample consumption and different area and thickness after sample tiling can be avoided.
3. The application adopts the thrust meter probe to vertically press the L-shaped contact piece to the first thrust value so as to ensure that the round sample piece is fully contacted with the bottom surface of the L-shaped contact piece, so that a specific friction force exists between the round sample piece and the bottom surface of the L-shaped contact piece, and data errors caused by different friction forces are avoided.
4. According to the application, the thrust of the L-shaped contact piece pushed by the thrust meter probe reaches the second thrust value as the gelation time end point, so that the gelation state end point is quantified, the operation error of artificial feel judgment is reduced, and the repeatability of the test can be improved.
5. The method for testing the gelation time does not need to purchase expensive instruments or custom-made instruments, reduces the cost and can avoid operation errors caused by the precision of the instruments and the equipment.
Detailed Description
Examples
Example 1 provides a method of testing the gelation time of an epoxy resin composition comprising the steps of:
s1: setting the size of a sample wafer;
s2, prescribing the size of the L-shaped contact piece;
s3: the gelation time of the sample was measured.
The specific steps of S1 are as follows: the epoxy resin composition was made into round plaques by a manual tablet press and a tablet die.
The diameter of the round sample piece is 28mm, the thickness is 1mm, and the surface area is 6.16cm 2 。
The L-shaped contact piece has the dimensions of bottom surface-length of 35 mm multiplied by width of 30 mm multiplied by thickness of 1 mm; terminal-width 30 mm x high 5 mm x thick 1 mm; the arithmetic mean deviation Ra of the surface roughness profile is 0.050.
The L-shaped contact piece is made of 15Cr10Ni stainless steel.
The specific steps of S3 are as follows:
(1) Placing the round sample on a heating plate, and heating the sample;
(2) The bottom surface of the L-shaped contact piece is horizontally covered on the surface of the sample piece, timing is started immediately when the surface of the sample piece has luster, and then the thrust meter probe vertically presses the L-shaped contact piece to a first thrust value.
(3) And then the probe of the thrust meter is vertically pushed to the tail end of the L-shaped contact piece, when the thrust value displayed by the thrust meter reaches a second thrust value, the timing is stopped, the test is completed, and the gelation time is recorded.
The sample piece was heated to 175 ℃.
The first thrust value was 0.20kgf.
The second thrust value was 1.2kgf.
The testing method comprises the following steps:
the epoxy compositions were tested for gelation time using example 1 of the present application and national standard GB/T40564-2021, respectively, GT for gelation time, 1-6# for six groups of samples, GT1-6 for six parallel runs of each group of samples, and gelation time, standard deviation, relative standard deviation are reported in Table 1.
TABLE 1
Claims (10)
1. A method of testing the gelation time of an epoxy resin composition comprising the steps of:
s1: setting the size of a sample wafer;
s2, prescribing the size of the L-shaped contact piece;
s3: the gelation time of the sample was measured.
2. The method for testing the gelation time of an epoxy resin composition according to claim 1, wherein the specific steps of S1 are: the epoxy resin composition was made into round plaques by a manual tablet press and a tablet die.
3. The method for measuring gelation time of an epoxy resin composition according to claim 2, wherein the surface area of said round coupon is 6 to 10cm 2 。
4. The method for testing the gelation time of an epoxy resin composition according to claim 1, wherein the circular coupon has a diameter of 28mm and a thickness of 1mm.
5. The method for testing the gelation time of an epoxy resin composition according to claim 1, wherein the L-shaped contact piece is made of 15Cr10Ni stainless steel.
6. The method for testing the gelation time of an epoxy resin composition according to claim 1, wherein the specific step of S3 is:
(1) Placing the round sample on a heating plate, and heating the sample;
(2) The bottom surface of the L-shaped contact piece is horizontally covered on the surface of the sample piece, when the surface of the sample piece has luster, the timing is started immediately, and then the thrust meter probe vertically presses the L-shaped contact piece to a first thrust value.
(3) And then the probe of the thrust meter is vertically pushed to the tail end of the L-shaped contact piece, when the thrust value displayed by the thrust meter reaches a second thrust value, the timing is stopped, the test is completed, and the gelation time is recorded.
7. The method for testing the gelation time of an epoxy resin composition according to claim 6, wherein the sample wafer has a heating temperature of 174 to 176 ℃.
8. The method of testing the gelation time of an epoxy resin composition according to claim 6, wherein said first thrust force value is 0.20kgf.
9. The method of testing the gelation time of an epoxy resin composition according to claim 6, wherein the second thrust force value is 1.2kgf.
10. A method of testing the gelation time of an epoxy resin composition according to any one of claims 1 to 9, comprising the use of the method in the determination of gelation time of the resin and its composition.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310557278.8A CN116754598A (en) | 2023-05-17 | 2023-05-17 | Method for testing gelation time of epoxy resin composition and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310557278.8A CN116754598A (en) | 2023-05-17 | 2023-05-17 | Method for testing gelation time of epoxy resin composition and application thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116754598A true CN116754598A (en) | 2023-09-15 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310557278.8A Pending CN116754598A (en) | 2023-05-17 | 2023-05-17 | Method for testing gelation time of epoxy resin composition and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116754598A (en) |
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2023
- 2023-05-17 CN CN202310557278.8A patent/CN116754598A/en active Pending
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