Method for detecting moisture of filler-containing epoxy resin

Abstract

The invention discloses a method for detecting moisture of filler-containing epoxy resin. The method comprises the following steps: step 1, weighing a sample: weighing 4-8g of filler-type epoxy resin to be detected; 2, dissolving a sample: adding 10-20g of an organic solvent, and dissolving and mixing the filler type epoxy resin to be detected; 3, sample dispersion: stirring the mixed solution in the step 2 for 10-30 minutes for uniform dispersion; step 4, extracting clear liquid: putting the solution which is uniformly dispersed in the step 3 into a high-speed centrifugal machine to be centrifugally dispersed for 30 to 60 minutes, and extracting supernate; 5, moisture detection, wherein the content of trace moisture in the supernate is detected. In the detection process, components influencing moisture detection result errors in the filler type epoxy resin are effectively removed only by using a balance, a magnetic stirrer, a centrifugal machine and other instruments commonly used in a laboratory, and then the moisture content in supernate is detected through a high-precision analysis instrument, so that the purpose of detecting the trace moisture content in the filler type epoxy resin is achieved. The detection process is easy to operate and the detection result is accurate.

Description

Technical Field

[0001] The invention relates to the technical field of a detection method for epoxy resin containing fillers, in particular to a moisture detection method for epoxy resin containing fillers. Background Art

[0002] With the development of integrated circuits and electronic technology, the requirements for heat resistance of corresponding materials are constantly increasing. Cured epoxy resin has excellent chemical resistance, corrosion resistance, dimensional stability, mechanical and electrical properties, and has been widely used, but the commonly used epoxy resin cannot meet the requirements of use under high temperature conditions.

[0003] Filler-type epoxy resin is a new type of epoxy additive material. Its most prominent feature is the use of atomic stabilization technology. By modifying the complexing group, a small amount of it added into the epoxy formula can effectively stabilize the polymer chain between 320℃-350℃, prevent the decomposition reaction from proceeding, and thus improve the heat resistance of epoxy products.

[0004] Filler-type epoxy resins can be applied to epoxy glass fiber composites, epoxy carbon fiber composites, high temperature resistant epoxy structural adhesives, epoxy electronic adhesives and other fields, and have broad market prospects.

[0005] The performance of filled epoxy resin is greatly affected by moisture. The Karl Fischer method is applicable to the determination of water content in a variety of organic and inorganic substances, but the determination results are affected by many factors. Metal complexes and other components in filled epoxy resin can react quantitatively with Karl Fischer reagents, causing errors in moisture test results. Therefore, there are currently few methods available for accurate detection of trace moisture in filled epoxy resin. Summary of the invention

[0006] In order to overcome the above problems, the present invention provides a method for detecting moisture in epoxy resin containing fillers.

[0007] The technical solution adopted by the present invention is:

[0008] A method for detecting moisture in epoxy resin containing fillers comprises the following steps:

[0009] Step 1: Sample weighing: weigh 4g-8g of the filler-type epoxy resin to be tested into a sample cup;

[0010] Step 2: Sample dissolution: Add 10g-20g of organic solvent into the sample cup and stir with a glass rod to fully dilute and dissolve the filler-type epoxy resin to obtain a filler-type epoxy resin dilution solution;

[0011] Step 3: Sample dispersion: Place the filler-type epoxy resin dilution in step 2 on a magnetic stirrer and stir for 10-30 minutes to uniformly disperse the filler-type epoxy resin dilution to obtain a uniform dispersion of the filler-type epoxy resin;

[0012] Step 4: Extraction of supernatant: Use a pipette to place the uniform dispersion of filler-type epoxy resin in step 3 into centrifuge tubes of the same specifications, and place them symmetrically in a high-speed centrifuge for centrifugal dispersion for 30 minutes to 60 minutes to extract the supernatant of filler-type epoxy resin;

[0013] Step 5: Repeat step 3 and step 4 2-3 times until the clarity of the filler-type epoxy resin supernatant meets the requirements;

[0014] Step 6: Moisture detection: Detect the trace moisture content in the supernatant of the filled epoxy resin.

[0015] Wherein, the organic solvent in step 2 is one or more of methanol, ethanol, ether, acetone, butanone, 1-propanol, butyl acetate, isopropyl acetate, dimethyl sulfoxide, ethyl acetate, acetonitrile, toluene, N,N-dimethylformamide, xylene, and propylene glycol monomethyl ether acetate.

[0016] Among them, the trace moisture content in step six is ​​detected by a Karl Fischer moisture meter.

[0017] Among them, depending on the clarity of the filler-type epoxy resin supernatant, the above-mentioned dispersion and supernatant extraction steps are repeated 2-3 times, so that the filler-type epoxy resin supernatant can be effectively extracted and its trace water content can be accurately detected.

[0018] The advantages of the present invention are as follows:

[0019] During the detection process, only commonly used laboratory instruments such as balances, magnetic stirrers and centrifuges are used to effectively remove the components in the filled epoxy resin that affect the error of the moisture detection result, and then the moisture content in the supernatant is detected by high-precision analytical instruments, thereby achieving the purpose of detecting the trace moisture content in the filled epoxy resin. The detection process is easy to operate, the test results are accurate, and the detection effect is excellent. DETAILED DESCRIPTION

[0020] The present invention will be further described below, but the present invention is not limited to these contents.

[0021] Example 1

[0022] A method for detecting moisture in epoxy resin containing fillers comprises the following steps:

[0023] Step 1: Sample weighing: Use an analytical balance to accurately weigh 4g (accurate to 0.01g) of the filler-type epoxy resin to be tested into a sample cup;

[0024] Step 2: Sample dissolution: Add 10g of organic solvent into the sample cup and stir with a glass rod to fully dilute and dissolve the filler-type epoxy resin to obtain a filler-type epoxy resin dilution solution;

[0025] Step 3: Sample dispersion: Place the filler-type epoxy resin dilution in step 2 on a magnetic stirrer and stir for 30 minutes to uniformly disperse the filler-type epoxy resin dilution to obtain a uniform dispersion of the filler-type epoxy resin;

[0026] Step 4: Extraction of supernatant: Use a pipette to place the uniform dispersion of filler-type epoxy resin in step 3 into centrifuge tubes of the same specifications, and place them symmetrically in a high-speed centrifuge for centrifugal dispersion for 30 minutes to extract the supernatant of filler-type epoxy resin;

[0027] Step 5: Water content detection: Use a Karl Fischer moisture meter to detect the trace water content in the supernatant of the filler-type epoxy resin in step 4.

[0028] Embodiment 2:

[0029] A method for detecting moisture in epoxy resin containing fillers comprises the following steps:

[0030] Step 1: Sample weighing: Use an analytical balance to accurately weigh 8g (accurate to 0.01g) of the filler-type epoxy resin to be tested into a sample cup;

[0031] Step 2: Sample dissolution: Add 20g of organic solvent into the sample cup and stir with a glass rod to fully dilute and dissolve the filler-type epoxy resin to obtain a filler-type epoxy resin dilution solution;

[0032] Step 3: Sample dispersion: Place the filler-type epoxy resin dilution in step 2 on a magnetic stirrer and stir for 30 minutes to uniformly disperse the filler-type epoxy resin dilution to obtain a uniform dispersion of the filler-type epoxy resin;

[0033] Step 4: Extraction of supernatant: Use a pipette to place the uniform dispersion of filler-type epoxy resin in step 3 into centrifuge tubes of the same specifications, and place them symmetrically in a high-speed centrifuge for centrifugal dispersion for 60 minutes to extract the supernatant of filler-type epoxy resin;

[0034] Step 5: Water content detection: Use a Karl Fischer moisture meter to detect the trace water content in the supernatant of the filler-type epoxy resin in step 4.

[0035] Example 3

[0036] On the basis of Example 1 and Example 2, depending on the clarity of the filler-type epoxy resin supernatant, steps 3 and 4 are repeated 2-3 times, so that the filler-type epoxy resin supernatant can be effectively extracted and its trace moisture content can be accurately detected.

[0037] It is pointed out that, for those skilled in the art, several modifications and improvements can be made without departing from the concept of the present invention, and these all fall within the protection scope of the present invention.

Claims

1. A method for detecting moisture in epoxy resin containing fillers, characterized in that: The following steps are involved: Step 1: Sample weighing: weigh 4g-8g of the filler-type epoxy resin to be tested into a sample cup; Step 2: Sample dissolution: Add 10g-20g of organic solvent into the sample cup and stir with a glass rod to fully dilute and dissolve the filler-type epoxy resin to obtain a filler-type epoxy resin dilution solution; Step 3: Sample dispersion: Place the filler-type epoxy resin dilution in step 2 on a magnetic stirrer and stir for 10-30 minutes to uniformly disperse the filler-type epoxy resin dilution to obtain a uniform dispersion of the filler-type epoxy resin; Step 4: Extraction of supernatant: Use a pipette to place the uniform dispersion of filler-type epoxy resin in step 3 into centrifuge tubes of the same specifications, and place them symmetrically in a high-speed centrifuge for centrifugal dispersion for 30 minutes to 60 minutes to extract the supernatant of filler-type epoxy resin; Step 5: Repeat step 3 and step 4 2-3 times until the clarity of the filler-type epoxy resin supernatant meets the requirements; Step 6: Moisture detection: Detect the trace moisture content in the supernatant of the filled epoxy resin.

2. The method for detecting moisture in epoxy resin containing fillers according to claim 1, characterized in that: The organic solvent in step 2 is one or more of methanol, ethanol, ether, acetone, butanone, 1-propanol, butyl acetate, isopropyl acetate, dimethyl sulfoxide, ethyl acetate, acetonitrile, toluene, N,N-dimethylformamide, xylene, and propylene glycol monomethyl ether acetate.

3. The method for detecting moisture in epoxy resin containing fillers according to claim 1, characterized in that: The trace moisture content in step 6 is detected by using a Karl Fischer moisture meter.

4. The method for detecting moisture in epoxy resin containing fillers according to claim 1, characterized in that: Depending on the clarity of the filler-type epoxy resin supernatant, the above-mentioned dispersion and supernatant extraction steps can be repeated 2-3 times to effectively extract the filler-type epoxy resin supernatant and accurately detect its trace water content.