A method of testing electronic grade solid polyphenyl ether resin for glue and a glue

Abstract

The present application relates to a kind of electronic grade solid polyphenyl ether resin impurity inspection glue and method, comprising the following weight parts components: PPO polyphenyl ether resin 30~100 parts, dicyandiamide 1~30 parts, solvent 100~300 parts;Method includes the following steps: (1) PPO polyphenyl ether resin is dissolved after stirring in solvent, and filtration is obtained PPO polyphenyl ether resin solution;(2) dicyandiamide is dissolved after stirring in solvent, and filtration is obtained dicyandiamide solution;(3) dicyandiamide solution is added to PPO polyphenyl ether resin solution, and filtration is obtained after stirring mixing;(4) the filtered impurity is washed with solvent and dried, and observed using microscope.Compared with prior art, the present application detection method is easy to operate, realizes the effective inspection of electronic grade solid resin impurity influence on glue, fills the quality control loophole, strengthens the quality control of raw material, enhances the rigor of inspection, improves the glue timeliness, both guarantee raw material resin quality stability and effectively improve the detection ability of detection department, also protect the strictness of formula.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of copper-clad plate production, in particular to a glue for testing impurities of electronic-grade solid polyphenyl ether resin and a method thereof. BACKGROUND

[0002] The use of electronic-grade solid resin (PPO polyphenyl ether resin) in copper-clad plates has become a common method for various copper-clad plate enterprises to solve technical problems, but the use of electronic-grade solid resin inevitably brings some technical problems, such as impurities (composite magnetic body, carbon oxide compound, etc.); the quality detection items of the electronic-grade solid resin currently include appearance, solubility, color, impurities, etc. However, the impurities of the solid resin escape filtration due to small particle size and low solubility, which leads to incomplete filtration during glue mixing and thus the impurities are mixed into the glue. It is difficult to detect and determine in advance according to the current detection means and methods, and the abnormal impurities occur after the batch is put into production, which seriously affects the performance verification of the customer's PCB product and causes a large loss due to scrap. SUMMARY

[0003] The purpose of the present application is to provide a glue for testing impurities of electronic-grade solid polyphenyl ether resin and a method thereof, which realizes effective testing of the influence of impurities of electronic-grade solid resin on glue mixing.

[0004] The purpose of the present application can be achieved by the following technical solution: a glue for testing impurities of electronic-grade solid polyphenyl ether resin, comprising the following components by weight:

[0005] PPO polyphenyl ether resin 30-100 parts;

[0006] Dicyandiamide 1-30 parts;

[0007] Solvent 100-300 parts.

[0008] Preferably, the PPO polyphenyl ether resin and the dicyandiamide are both electronic-grade.

[0009] Preferably, the PPO polyphenyl ether resin has a molecular weight Mn of 2200-2600 g / mol and a solubility viscosity of 200-300 mpa·s.

[0010] Preferably, the PPO polyphenyl ether resin is a common low-hydroxyl PPO polyphenyl ether resin.

[0011] Preferably, the solvent is selected from one or more of acetone, butanone, and cyclohexanone.

[0012] Preferably, the glue comprises PPO polyphenyl ether resin 70-100 parts.

[0013] A method for detecting impurities of electronic grade solid polyphenyl ether resin, using the above-mentioned glue, comprising the following steps:

[0014] (1) After stirring and dissolving PPO polyphenyl ether resin in a solvent, filtering to obtain a PPO polyphenyl ether resin solution;

[0015] (2) After stirring and dissolving dicyandiamide in a solvent, filtering to obtain a dicyandiamide solution;

[0016] (3) Add the dicyandiamide solution to the PPO polyphenyl ether resin solution, stir and mix, and then filter;

[0017] (4) After washing and drying the filtered impurities with a solvent, observe them under a microscope.

[0018] Preferably, the stirring speed in step (1) is 800-1000 rpm, and the time is 1-3 h.

[0019] Preferably, the impurities in step (1) are filtered with a 0.5 um nylon filter.

[0020] Preferably, the weight ratio of PPO polyphenyl ether resin to solvent in step (1) is 1:1-2.

[0021] Preferably, the stirring speed in step (2) is 800-1000 rpm, and the time is 1-3 h.

[0022] Preferably, the impurities in step (2) are filtered with a 0.5 um nylon filter.

[0023] Preferably, the weight ratio of dicyandiamide to solvent in step (2) is 1:4-10.

[0024] Preferably, the stirring speed in step (3) is 800-1000 rpm, and the time is 1-3 h.

[0025] Preferably, the impurities in step (3) are filtered with a 0.5 um nylon filter.

[0026] Preferably, in step (4), the filtered impurities are sucked into a tin paper box with a pipette, repeatedly washed with a solvent, and then dried in a vacuum oven at 105°C.

[0027] Compared with the prior art, the present application has the following advantages:

[0028] 1. The detection method of the present application is easy and simple to operate, realizes effective detection of the influence of impurities of electronic grade solid resin on glue mixing, fills the gap in quality control, strengthens the quality control of raw materials, enhances the rigor of detection, improves the timeliness of glue mixing, ensures the stability of the quality of raw material resin, effectively improves the detection capability of the detection department, and protects the strictness of the formula.

[0029] 2. The application scheme is implemented and verified by adjusting glue. The occurrence probability of adjusting glue impurity filtration is reduced, the manual repeated work is reduced, the economic loss is avoided from the source, the production cost is reduced; at the same time, the delivery delay caused by the damage of glue impurity circulation filtration is avoided, the product quality verification time is accelerated, the customer satisfaction is improved, and the product competitive advantage in the market is improved;

[0030] 3. The method for filtering the production in the field production is simulated, the production is effectively restored at the minimum cost, the viscosity and concentration of the glue system are increased by using dicyandiamide as a tackifier and an indicator to improve the aggregation of fine particle impurities and deepen the color of the impurities, so that the impurities are observed and detected conveniently, the detection method is effective and scientific, the quality risk of the raw material impurities mixed into the glue system is prevented in advance. BRIEF DESCRIPTION OF DRAWINGS

[0031] Figure 1 Table 3 is the filtration and filtration impurity diagram of double material group 1 (left A right B);

[0032] Figure 2 Table 3 is the filtration and filtration impurity diagram of double material group 2 (left A right B);

[0033] Figure 3 Table 3 is the filtration and filtration impurity diagram of double material group 3 (left A right B);

[0034] Figure 4 Table 3 is the filtration and filtration impurity diagram of double material group 4 (left A right B). DETAILED DESCRIPTION

[0035] The application will be described in detail below in combination with the drawings and specific examples. The following examples are implemented on the premise of the technical scheme of the application, and detailed implementation modes and specific operation processes are given, but the protection scope of the application is not limited to the following examples.

[0036] A method for testing impurities of electronic-grade solid polyphenyl ether resin, comprising the following steps:

[0037] (1) Prepare the following components and weight parts:

[0038] PPO polyphenyl ether resin 30-100 parts;

[0039] Dicyandiamide 1-30 parts;

[0040] Solvent 100-300 parts;

[0041] (2) The electronic-grade PPO polyphenyl ether resin is added to a 1000ml clean container bottle, clean solvent is slowly added thereto, and ordinary stirring (rotation speed 800-1000 rpm) is started to pretreat the electronic-grade solid resin for 1-3h;

[0042] (3) The dissolved PPO polyphenyl ether resin solution is visually observed to be fully dissolved, and the system impurities are filtered with a 0.5 um nylon filter screen;

[0043] (4) Electronic grade dicyandiamide is added to a 1000 ml clean container bottle, clean solvent is slowly added thereto, and ordinary stirring is started (800-1000 rpm) for 1-3 h of pretreatment;

[0044] (5) The dissolved dicyandiamide solution is visually observed to be fully dissolved, and the system impurities are filtered with a 0.5 um nylon filter screen;

[0045] (6) The filtered dicyandiamide solution is slowly poured into the PPO polyphenyl ether resin solution container bottle, and ordinary stirring is started (800-1000 rpm) for 1-3 h of mixing treatment of the electronic grade resin mixed solution;

[0046] (7) The completely mixed solution is filtered with a 0.5 um nylon filter screen, the filter impurities are sucked into a tin paper box with a pipette, repeatedly washed with solvent, dried in a vacuum oven at 105°C, and observed under a microscope.

[0047] DETAILED DESCRIPTION

[0048] Example 1

[0049] A method for testing electronic grade solid polyphenyl ether resin impurities, comprising the following steps:

[0050] 1. Electronic grade dicyandiamide is added to clean solvent according to the amount (material group 1-5, the relationship between the number of impurities and the sample is observed) and fully dissolved, and filtered with a 0.5 um nylon filter screen to try to exclude or reduce the influence of impurities on the experiment. The results are shown in Table 1.

[0051] Table 1

[0052]

[0053] 2. PPO polyphenyl ether resin is added to clean solvent according to a certain amount (material group 1-4) and fully dissolved, and filtered with a 0.5 um nylon filter screen, combined with the current quality inspection operation method, and the on-site judgment standard is used to observe whether the impurities are over standard. The results are shown in Table 2.

[0054] Table 2

[0055]

[0056] 3. Test with two-component resin system

[0057] A method for testing impurities of electronic grade solid polyphenyl ether resin, the components and ingredients are shown in Table 3. Among them, the electronic grade PPO polyphenyl ether resin is polyphenyl ether (A / B is different company of PPO produced respectively, A is the standard sample, supplier Shabik, B is the experimental sample, supplier Kolon), another electronic grade dicyandiamide supplier is Ningxia Darong, and the solvent is butanone.

[0058] (1) The electronic grade PPO polyphenyl ether resin was added to a 1000ml clean container bottle, and clean solvent was slowly added thereto, and ordinary stirring (900rpm) was started to pretreat the electronic grade solid resin for 2h;

[0059] (2) The dissolved resin was visually observed to be fully dissolved, and the system impurities were repeatedly filtered with a 0.5um nylon filter screen;

[0060] (3) The electronic grade dicyandiamide was added to a 1000ml clean container bottle, and clean solvent was slowly added thereto, and ordinary stirring (900rpm) was started to pretreat it for 2h;

[0061] (4) The dissolved dicyandiamide was visually observed to be fully dissolved, and the system impurities were repeatedly filtered with a 0.5um nylon filter screen;

[0062] (5) The filtered and dissolved dicyandiamide was slowly poured into the PPO polyphenyl ether resin solution container bottle, and ordinary stirring (900rpm) was started to mix the electronic grade resin mixed solution for 2h;

[0063] (6) The completely mixed solution was filtered with a 0.5um nylon filter screen, and the filter impurities were sucked into a tin paper box with a pipette and repeatedly washed with solvent, then dried in a vacuum oven at 105℃, and observed under a microscope; the results are shown in Table 3.

[0064] Table 3

[0065]

[0066] Conclusion analysis:

[0067] 1. The dicyandiamide impurities are black particle impurities, which can be fully filtered in repeated filtration to ensure that the experimental factors are not affected by external resin carrying impurities.

[0068] 2. The PPO polyphenyl ether resin (abnormal batch) cannot be completely filtered out in the case of shear or pump pressure due to the interference of impurity morphology, small particle size (15-800um) or low viscosity of glue, and can easily penetrate into the glue through the filter screen hole. In the static state, some impurities that have not been completely filtered out can still be found.

[0069] 3. Through the two-component resin system test method, test verification part of different component material ratio unreasonable easy to cause experimental distortion (such as table 3: double material group 1~2), unable to simulate the real scene, reference to simulate the scene material similar proportion can quickly and easily detect abnormal material impurity, further verify the effectiveness of the method, give the subsequent glue quality guarantee, improve the production capacity of the scene, strengthen the quality supervision, consolidate the quality defense line, also to achieve the customer's certification time limit, full meet the terminal PCB each verification.

[0070] The above description of the embodiments is to facilitate those of ordinary skill in the art to understand and use the application. Those skilled in the art can obviously make various modifications to these embodiments, and apply the general principles described herein to other embodiments without having to go through creative labor. Therefore, the present application is not limited to the above embodiments, and any improvements and modifications made by those skilled in the art without departing from the scope of the present application should be within the scope of protection of the present application.

Claims

1. A method of testing an electronic grade solid polyphenylene ether resin for impurities, characterized by, Using glue, the glue includes the following parts by weight components: PPO polyphenyl ether resin 30~100 parts; Dicyandiamide 1~30 parts; Solvent 100~300 parts; The PPO polyphenyl ether resin and dicyandiamide are both electronic grade; The solvent is selected from one or more of acetone, butanone, cyclohexanone; The glue includes PPO polyphenyl ether resin 70~100 parts; The method for testing the impurities of electronic grade solid polyphenyl ether resin comprises the following steps: (1) PPO polyphenyl ether resin is dissolved in a solvent after stirring and filtered to obtain a PPO polyphenyl ether resin solution; (2) Dicyandiamide is dissolved in a solvent after stirring and filtered to obtain a dicyandiamide solution; (3) The dicyandiamide solution is added to the PPO polyphenyl ether resin solution, stirred and mixed, and then filtered; (4) The filtered impurities are washed with a solvent and dried, and then observed under a microscope; The stirring speed of step (1) is 800~1000 rpm, the time is 1~3 h, and the impurities are filtered with a 0.5 um nylon filter screen; The stirring speed of step (2) is 800~1000 rpm, the time is 1~3 h, and the impurities are filtered with a 0.5 um nylon filter screen; The stirring speed of step (3) is 800~1000 rpm, the time is 1~3 h, and the impurities are filtered with a 0.5 um nylon filter screen.

2. The method for testing impurities in electronic-grade solid polyphenylene ether resin according to claim 1, characterized in that, The PPO polyphenyl ether resin has a molecular weight Mn of 2200~2600 g / mol and a dissolution viscosity of 200~300 mpa·s.

3. The method for testing impurities in electronic-grade solid polyphenylene ether resin according to claim 1, characterized in that, The PPO polyphenyl ether resin is a common low-hydroxyl PPO polyphenyl ether resin.

4. The method for testing impurities in electronic-grade solid polyphenylene ether resin according to claim 1, characterized in that, In step (4), the filtered impurities are sucked into a tin paper box and repeatedly washed with a solvent, and then dried in a vacuum oven at 105℃.

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