A standard sample for ball pressure temperature detection and preparation method thereof

Abstract

The present invention discloses a standard sample for ball pressure temperature detection, and relates to the technical field of standard samples. The standard sample for ball pressure temperature detection of the present invention comprises the following components in parts by weight: 65-84 parts of PC resin, 1-25 parts of ABS resin, 5-10 parts of polyterephthalate resin, 10-20 parts of filler, 0.1-5 parts of heat-resistant agent, 0.1-3 parts of antioxidant, and 0.5-3 parts of processing aid; the filler is a compound of talcum powder and aluminum titanate; the mass ratio of the talcum powder and aluminum titanate is (1-3): (1-2). The present invention prepares a standard sample for ball pressure temperature detection with good uniformity and stability by selecting the above-mentioned components, which is suitable for industrial application.

Description

Technical Field

[0001] The present invention relates to the technical field of standard samples, and in particular to a standard sample for ball pressure temperature detection and a preparation method thereof. Background Art

[0002] The ball pressure temperature test uses a pressure ball in an oven to evaluate the heat resistance of polymeric materials. It is suitable for non-metallic materials in electrical and electronic products. Under high temperatures, non-metallic materials can melt or soften, reducing their mechanical strength and impacting product quality and safety. Ball pressure temperature testing ensures that products maintain adequate mechanical strength even under high-temperature conditions.

[0003] Standards such as GB / T2099.1-2008 "Plugs and socket-outlets for household and similar purposes - Part 1: General requirements", GB4706.1-2005 "Safety of household and similar electrical appliances - Part 1: General requirements", GB16915.1-2014 "Switches for household and similar fixed electrical installations - Part 1: General requirements", and GB / T5169.21-2017 / IEC 60695-10-2:2014 "Fire hazard testing for electric and electronic products - Part 21: Abnormal hot ball pressure test method" have clear requirements on the heat resistance of products, requiring ball pressure tests and stipulating test methods.

[0004] In order to obtain accurate test results, it is necessary to verify multiple influencing factors such as the oven, pressure ball diameter, load weight, etc. This is time-consuming and requires many verification points, and the calibration results cannot be obtained intuitively. Therefore, it is necessary to develop a standard substance to improve verification efficiency.

[0005] CN108997727A discloses a halogen-free flame-retardant polycarbonate resin composition with high heat ball pressure resistance and its preparation method. The halogen-free flame-retardant polycarbonate composition with high heat ball pressure resistance is prepared by compounding with PPS resin. CN110577728A discloses a polycarbonate composition with high ball pressure resistance and solvent resistance and its preparation method. The composition uses a specific polyester resin in combination with the polycarbonate to impart high pressure resistance and solvent resistance.

[0006] The above patent only pursues high ball pressure temperature, does not involve the uniformity and stability of the product, and is not suitable for ball pressure temperature testing at different temperatures. Summary of the Invention

[0007] The purpose of the present invention is to overcome the shortcomings of the above-mentioned prior art and provide a standard sample for ball pressure temperature detection with good uniformity and stability and a preparation method thereof, and the standard sample can be applicable to ball pressure temperature tests at a variety of different temperatures.

[0008] To achieve the above object, the technical solution adopted by the present invention is:

[0009] A standard sample for ball pressure temperature detection comprises the following components in parts by weight: 65-84 parts of PC resin, 1-25 parts of ABS resin, 5-10 parts of polyterephthalate resin, 10-20 parts of filler, 0.1-5 parts of heat-resistant agent, 0.1-3 parts of antioxidant, and 0.5-3 parts of processing aid; the filler is a compound of talc powder and aluminum titanate; and the mass ratio of the talc powder to the aluminum titanate is (1-3):(1-2).

[0010] PC resin has excellent heat resistance and can remain stable at higher temperatures. By adjusting the proportion of ABS resin, standard materials that meet different temperature requirements can be prepared. For the formulation system described in the present invention, when the amounts of each component meet the above ratios, the standard material has good heat resistance below 75°C. When the mass ratio of PC resin to ABS resin is (80-84): (1-5), the standard material has good thermal stability below 125°C. Adding polyterephthalate resin can improve the processing performance, uniformity, chemical resistance, and stability of the standard sample. Adding an appropriate amount of filler can improve the dimensional stability of the standard sample. Adding heat-resistant agents and antioxidants can improve the stability of the standard sample. PC resin is sensitive to the acidity and alkalinity of fillers. Adding a single filler cannot meet the requirements of the present invention. In addition, the surface flatness of the standard sample must be considered. Adding a compound of talc and aluminum titanate can ensure a low linear expansion coefficient of the standard material and increase its stability.

[0011] Preferably, the melt mass flow rate of the PC resin measured at 300°C and 1.2 kg is 7-20 g / 10 min, and the melt mass flow rate of the ABS resin measured at 220°C and 10 kg is 6-30 g / 10 min. The melt mass flow rate is measured with reference to GB / T 3682.1-2018.

[0012] Further preferably, the PC resin has a melt flow rate of 10-20 g / 10 min at 300°C and 1.2 kg, and the ABS resin has a melt flow rate of 20-30 g / 10 min at 220°C and 10 kg, respectively. These melt flow rates are measured in accordance with GB / T 3682.1-2018. These PC and ABS resins are easy to process, and the prepared standard samples have a sea-island structure, which makes the standard samples more uniform and helps improve their stability. Their excellent appearance further facilitates their application.

[0013] Preferably, the mass ratio of the talc powder to the aluminum titanate is (1-2): 1. The present invention further improves the uniformity and stability of the standard sample by screening the ratio of talc powder to aluminum titanate.

[0014] Preferably, the D50 particle size of the talc is 3-9.3 μm, and the D50 particle size of the aluminum titanate is 1-3.8 μm. Further preferably, the D50 particle size of the talc is 3-4.2 μm, and the D50 particle size of the aluminum titanate is 1-2 μm. Controlling the particle sizes of talc and aluminum titanate within these ranges can fully leverage their effects in reducing shrinkage and linear expansion coefficient.

[0015] Preferably, the poly(terephthalate) resin is at least one of PBT and PET. Adding crystalline polyester resin can reduce the overall viscosity of the material and improve the processing performance and chemical resistance of the standard sample.

[0016] Preferably, the processing aid is at least one of a light stabilizer and a lubricant. The light stabilizer is a hindered amine light stabilizer, a benzotriazole light stabilizer, or a benzophenone light stabilizer. The lubricant is a mixture of white oil and calcium stearate, with the mass ratio of white oil to calcium stearate being 1:(1-2). When the lubricant composition meets the above requirements, the dispersion of the components during processing is improved, which helps improve the uniformity and stability of the product.

[0017] Preferably, the heat-resistant agent is a styrene-maleimide heat-resistant agent; and the antioxidant is a compound of a hindered phenol antioxidant and a phosphite antioxidant.

[0018] Preferably, the standard sample further contains 0.5-3 parts of a colorant, which can make the L value of the standard sample less than 80. The colorant is added to facilitate observation of the indentation diameter and test observation.

[0019] At the same time, the present invention also discloses a method for preparing the standard sample for ball pressure temperature detection, the preparation method comprising the following steps:

[0020] (1) Mixing the components uniformly according to the ratio to obtain a premix;

[0021] (2) The premix is ​​added to a twin-screw extruder, melt-extruded at 230-270° C., drawn into strips, cooled, pelletized, and dried to obtain the standard sample for ball pressure temperature detection.

[0022] Compared to existing technologies, the present invention offers the following advantages: By using PC resin and ABS resin as primary components, a standard sample for ball pressure temperature testing with excellent uniformity and stability is prepared. By adjusting the amount of ABS resin, standard samples suitable for a variety of different temperatures can be prepared. Furthermore, by using a mixture of talc and aluminum titanate as a filler, the present invention significantly improves the uniformity and stability of the standard sample. DETAILED DESCRIPTION

[0023] In order to better illustrate the purpose, technical solutions and advantages of the present invention, the present invention will be further described below in conjunction with specific embodiments.

[0024] The ingredients used in the Examples and Comparative Examples are as follows:

[0025] PC1: PC FC3155, Wanhua Chemical (Yantai) Sales Co., Ltd., melt flow rate at 300°C, 1.2 kg: 15 g / 10 min;

[0026] PC2: PC HS100G, Zhejiang Mingri Holding Group Co., Ltd., melt flow rate: 10 g / 10 min at 300°C and 1.2 kg;

[0027] PC3: PC-GT02A, Ningbo Dopoda Polymer Co., Ltd., melt flow rate: 20 g / 10 min at 300 °C and 1.2 kg;

[0028] PC4: PC A1070, Wanhua Chemical (Yantai) Sales Co., Ltd., melt flow rate 7 g / 10 min at 300°C and 1.2 kg;

[0029] ABS1: ABS HP171 C9010, Guangdong Shengchan Petrochemical Co., Ltd., melt mass flow rate measured at 220°C, 10 kg: 24 g / 10 min;

[0030] ABS2: ABS KF-730 (G360), Liaoning Jinfa Technology Co., Ltd., melt mass flow rate measured at 220°C, 10 kg: 20 g / 10 min;

[0031] ABS3: ABS 8391T-Huajin, Liaoning Tongda Chemical Co., Ltd., melt mass flow rate measured at 220°C, 10kg: 30g / 10min;

[0032] ABS4: ABS TH191, produced by PetroChina South China Chemical Sales Branch, with a melt flow rate of 6 g / 10 min at 220°C and 10 kg.

[0033] PBT: PBT CH883, Zhejiang Changhong Biomaterial Co., Ltd.;

[0034] Talc 1: TYT-3000A, Guangzhou Tianyuan Chemical Co., Ltd., D50 particle size 38 μm;

[0035] Talc 2: HTPUItra5L, Liaoning Aihaiyimi Mining Co., Ltd., D50 particle size 3.0 μm;

[0036] Talc 3: TYT-999, Guangzhou Tianyuan Chemical Co., Ltd., D50 particle size 4.2 μm;

[0037] Talc 4: AH-1250N6, Guangxi Longsheng Huamei Talc Development Co., Ltd., D50 particle size 9.0 μm;

[0038] Aluminum titanate 1: aluminum titanate, Wuhan Shuou Technology Co., Ltd., D50 particle size is 1.6 μm;

[0039] Aluminum titanate 2: aluminum titanate, Hubei Nona Technology Co., Ltd., D50 particle size of 1 μm;

[0040] Aluminum titanate 3: aluminum titanate, Zhengzhou Huiju Chemical Co., Ltd., D50 particle size is 2.0 μm;

[0041] Aluminum titanate 4: aluminum titanate, Anhui Zesheng Technology Co., Ltd., D50 particle size 3.8 μm;

[0042] Calcium carbonate: AC-05N, Guangdong Xianglong Technology Co., Ltd., D50 particle size 9.0 μm;

[0043] Glass fiber: ECS301CL-3, Chongqing International Composite Materials Co., Ltd.

[0044] Heat resistant agent: styrene-maleimide heat resistant agent, MS-NB, commercially available;

[0045] Antioxidant: a commercially available mixture of antioxidant 1076 and antioxidant 168 in a mass ratio of 1:1.

[0046] Colorant: CB5093, Dongguan Hanjie Plastic Technology Co., Ltd.

[0047] Lubricant 1: white oil, commercially available;

[0048] Lubricant 2: calcium stearate, commercially available;

[0049] Lubricant 3: zinc stearate, commercially available.

[0050] The heat-resistant agent, antioxidant, colorant, and lubricants 1 to 3 used in the examples and comparative examples are all the same commercially available products, and the above melt mass flow rate is measured with reference to GB / T 3682.1-2018.

[0051] Examples 1 to 8

[0052] The embodiments of the standard sample for ball pressure temperature detection of the present invention, the formulas of Examples 1 to 8 are shown in Table 1, and the preparation method is: the components are uniformly mixed according to the ratio, added to a twin-screw extruder, melt-extruded at 240-270°C, stretched, cooled, pelletized, and dried to obtain the standard sample.

[0053] Comparative Examples 1 to 3

[0054] Comparative Examples 1 to 3 are standard samples for ball pressure temperature detection, the formulations of which are shown in Table 1, and the preparation methods are the same as those of Example 1.

[0055] Table 1 (parts by weight)

[0056]

[0057] Examples 9-11

[0058] The embodiments of the standard sample for ball pressure temperature detection of the present invention, embodiments 9 to 11 are different from embodiment 1 only in that the types of PC resins are different, namely PC2, PC3, and PC4.

[0059] Examples 12 to 14

[0060] In the embodiments of the standard sample for ball pressure temperature detection of the present invention, embodiments 12 to 14 differ from embodiment 1 only in that the types of ABS resin are different, namely ABS2, ABS3, and ABS4.

[0061] Examples 15 to 17

[0062] The embodiments of the standard sample for ball pressure temperature detection of the present invention, embodiments 15 to 17 are different from embodiment 1 only in that the types of talcum powder are different, namely talcum powder 2, talcum powder 3, and talcum powder 4.

[0063] Examples 18 to 20

[0064] The embodiments of the standard sample for ball pressure temperature detection of the present invention, embodiments 18 to 20 differ from embodiment 1 only in the types of aluminum titanate, namely aluminum titanate 2, aluminum titanate 3, and aluminum titanate 4.

[0065] Ball pressure temperature tests were performed on the standard samples for ball pressure temperature detection described in the examples and comparative examples. The tests were performed in ovens at 125°C and 75°C, respectively, with reference to GB / T5169.21-2017 / IEC 60695-10-2:2014 "Fire hazard testing for electrical and electronic products - Part 21: Abnormal hot ball pressure test method". The test results are shown in Table 2.

[0066] Table 2

[0067]

[0068]

[0069] Current requirements for ball pressure temperature generally require an indentation diameter of less than 2 mm at either 125°C or 75°C. The test results above demonstrate that the standard sample for ball pressure temperature testing described in Example 1 is suitable for ball pressure temperature testing at 75°C, and the standard samples for ball pressure temperature testing described in Examples 2-3 are suitable for ball pressure temperature testing at both 125°C and 75°C. All examples and comparative examples can meet the requirements for ball pressure temperature testing under at least one of these temperature conditions.

[0070] The standard samples for ball pressure temperature detection described in the embodiments and comparative examples were tested for uniformity. Except for the test conditions of Examples 2 to 3 being 125°C, the test conditions of other embodiments and comparative examples were 75°C. With reference to CNAS-GL003-2018 "Guidelines for the Evaluation of Uniformity and Stability of Proficiency Testing Samples", a single-factor analysis of variance was used to test the uniformity between samples. Ten groups of prepared samples were randomly selected, each group having two standard samples. The standard samples were conditioned in a constant temperature and humidity chamber at (23±2)°C & (50±5)%RH for 24 hours and then tested. The test results are shown in Table 3. The critical value F of uniformity of each product is 0.05(9,10) =3.02, if the statistical value F<F 0.05(9,10) =3.02, it is considered that there is no significant difference between the groups and within the group, which means that the sample is uniform, and the smaller the value, the more uniform the product. If F≥F 0.05(9,10) =3.02, it means that the product is not uniform enough.

[0071] Table 3

[0072]

[0073]

[0074] The stability test was conducted on the standard samples for ball pressure temperature detection described in the examples and comparative examples. Except for the test conditions of Examples 2 to 3 being 125°C, the test conditions of the other examples and comparative examples were 75°C. With reference to CNAS-GL003 "Guidelines for the Evaluation of Uniformity and Stability of Capability Testing Samples", the stability of the samples was tested by using the consistency between the two average values ​​in the t-test method. The uniformity test data was taken as one of the average values, and 10 groups of samples were randomly selected from the samples that were sealed and stored for 6 months. Two samples were tested in each group. The standard samples were adjusted in a constant temperature and humidity chamber at (23±2)°C & (50±5)%RH for 24 hours and then tested. The average value of the test data was taken as another average value. The test results are shown in Table 4. The critical value of stability t 0.05(38) =1.686, if the statistical value t<t 0.05(38) , there is no significant difference between the average values, and the sample stability is good.

[0075] Table 4

[0076] project t-value Example 1 0.05 Example 2 0.44(125℃) Example 3 0.52(125℃) Example 4 0.69 Example 5 0.20 Example 6 0.42 Example 7 0.88 Example 8 0.95 Example 9 0.23 Example 10 0.18 Example 11 1.10 Example 12 0.66 Example 13 0.56 Example 14 1.32 Example 15 0.59 Example 16 0.56 Example 17 1.56 Example 18 0.54 Example 19 0.24 Example 20 1.67 Comparative Example 1 1.96 Comparative Example 2 1.82 Comparative Example 3 1.75

[0077] As shown in Tables 3 to 4, the F values ​​of the standard samples for ball pressure temperature detection in Examples 1 to 20 are all less than F 0.05(9,10) , t values ​​are all less than t 0.05(38) , with good uniformity and stability, suitable as a standard substance for ball pressure temperature detection.

[0078] Comparative Examples 1 and 2 did not use the filler described in the present invention, and the uniformity and stability of the samples were significantly inferior to those of the present invention. The contents of PC resin and ABS resin in Comparative Example 3 were not within the range defined by the present invention, and similarly, a standard substance suitable for ball pressure temperature detection could not be prepared.

[0079] By comparing the test results of Example 1 and Example 4, it can be found that for the system of the present invention, the lubricant is preferably a compound of white oil and calcium stearate.

[0080] By comparing the test results of Example 1 with those of Examples 5 to 8, it can be found that the mass ratio of talc powder to aluminum titanate is preferably (1-2):1.

[0081] Comparing the test results of Example 1 with those of Examples 9 to 11, it can be found that the melt flow rate of the PC resin is preferably 10 to 20 g / 10 min. Comparing the test results of Example 1 with those of Examples 12 to 14, it can be found that the melt flow rate of the ABS resin is preferably 20 to 30 g / 10 min.

[0082] Comparing the test results of Example 1 with those of Examples 15 to 17, it can be found that the D50 particle size of talc is preferably 3.0-4.2 μm. Comparing the test results of Example 1 with those of Examples 18 to 20, it can be found that the D50 particle size of aluminum titanate is preferably 1-2 μm.

[0083] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and are not intended to limit the scope of protection of the present invention. Although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art should understand that the technical solutions of the present invention may be modified or replaced by equivalents without departing from the essence and scope of the technical solutions of the present invention.

Claims

1. A standard sample for ball pressure temperature detection, characterized in that: The invention comprises the following ingredients in parts by weight: 65-84 parts of PC resin, 1-25 parts of ABS resin, 5-10 parts of polyterephthalate resin, 10-20 parts of filler, 0.1-5 parts of heat-resistant agent, 0.1-3 parts of antioxidant, and 0.5-3 parts of processing aid; the filler is a compound of talc powder and aluminum titanate; and the mass ratio of the talc powder to the aluminum titanate is (1-3):(1-2).

2. The standard sample for ball pressure temperature detection according to claim 1, wherein: The melt mass flow rate of the PC resin measured at 300° C. and 1.2 kg is 7-20 g / 10 min, and the melt mass flow rate of the ABS resin measured at 220° C. and 10 kg is 6-30 g / 10 min. The melt mass flow rate is measured with reference to GB / T 3682.1-2018.

3. The standard sample for ball pressure temperature detection according to claim 2, wherein: The melt mass flow rate of the PC resin measured at 300° C. and 1.2 kg is 10-20 g / 10 min, and the melt mass flow rate of the ABS resin measured at 220° C. and 10 kg is 20-30 g / 10 min. The melt mass flow rate is measured with reference to GB / T 3682.1-2018.

4. The standard sample for ball pressure temperature detection according to claim 1, wherein: The mass ratio of the talc powder to the aluminum titanate is (1-2):

1.

5. The standard sample for ball pressure temperature detection according to claim 1, wherein: The D50 particle size of the talc powder is 3-9.3 μm, and the D50 particle size of the aluminum titanate is 1-3.8 μm.

6. The standard sample for ball pressure temperature detection according to claim 1, wherein: The D50 particle size of the talc powder is 3-4.2 μm, and the D50 particle size of the aluminum titanate is 1-2 μm.

7. The standard sample for ball pressure temperature detection according to claim 1, wherein: The poly(terephthalate) resin is at least one of PBT and PET; the processing aid is at least one of a light stabilizer and a lubricant; the light stabilizer is a hindered amine light stabilizer, a benzotriazole light stabilizer, or a benzophenone light stabilizer; and the lubricant is a compound of white oil and calcium stearate, wherein the mass ratio of the white oil to calcium stearate is 1:(1-2).

8. The standard sample for ball pressure temperature detection according to claim 1, wherein: The heat-resistant agent is a styrene-maleimide heat-resistant agent; and the antioxidant is a compound of a hindered phenol antioxidant and a phosphite antioxidant.

9. The standard sample for ball pressure temperature detection according to claim 1, wherein: It also contains 0.5-3 parts of colorant.

10. A method for preparing a standard sample for ball pressure temperature detection according to any one of claims 1 to 9, characterized in that: The steps include: (1) Mixing the components uniformly according to the ratio to obtain a premix; (2) adding the premix into a twin-screw extruder for melt extrusion, stranding, cooling, pelletizing, and drying to obtain the standard sample for ball pressure temperature detection.

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