CN114034605B - Melt flow rate standard substance and preparation method thereof - Google Patents
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- 239000000126 substance Substances 0.000 title claims abstract description 87
- 238000002360 preparation method Methods 0.000 title abstract description 10
- 239000000155 melt Substances 0.000 claims abstract description 55
- 238000012360 testing method Methods 0.000 claims abstract description 52
- 229920000122 acrylonitrile butadiene styrene Polymers 0.000 claims abstract description 34
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 23
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 23
- 239000004611 light stabiliser Substances 0.000 claims abstract description 20
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 17
- 239000006057 Non-nutritive feed additive Substances 0.000 claims abstract description 12
- 238000001125 extrusion Methods 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 238000012545 processing Methods 0.000 claims description 4
- 229920001577 copolymer Polymers 0.000 claims description 3
- VETPHHXZEJAYOB-UHFFFAOYSA-N 1-n,4-n-dinaphthalen-2-ylbenzene-1,4-diamine Chemical compound C1=CC=CC2=CC(NC=3C=CC(NC=4C=C5C=CC=CC5=CC=4)=CC=3)=CC=C21 VETPHHXZEJAYOB-UHFFFAOYSA-N 0.000 claims description 2
- KGRVJHAUYBGFFP-UHFFFAOYSA-N 2,2'-Methylenebis(4-methyl-6-tert-butylphenol) Chemical compound CC(C)(C)C1=CC(C)=CC(CC=2C(=C(C=C(C)C=2)C(C)(C)C)O)=C1O KGRVJHAUYBGFFP-UHFFFAOYSA-N 0.000 claims description 2
- GHKOFFNLGXMVNJ-UHFFFAOYSA-N Didodecyl thiobispropanoate Chemical compound CCCCCCCCCCCCOC(=O)CCSCCC(=O)OCCCCCCCCCCCC GHKOFFNLGXMVNJ-UHFFFAOYSA-N 0.000 claims description 2
- JKIJEFPNVSHHEI-UHFFFAOYSA-N Phenol, 2,4-bis(1,1-dimethylethyl)-, phosphite (3:1) Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C JKIJEFPNVSHHEI-UHFFFAOYSA-N 0.000 claims description 2
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 claims description 2
- SSDSCDGVMJFTEQ-UHFFFAOYSA-N octadecyl 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)CCC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 SSDSCDGVMJFTEQ-UHFFFAOYSA-N 0.000 claims description 2
- 239000011347 resin Substances 0.000 abstract description 5
- 229920005989 resin Polymers 0.000 abstract description 5
- 238000013112 stability test Methods 0.000 description 20
- 235000006708 antioxidants Nutrition 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 14
- 239000000463 material Substances 0.000 description 14
- 238000003860 storage Methods 0.000 description 6
- 230000007774 longterm Effects 0.000 description 5
- HIDBROSJWZYGSZ-UHFFFAOYSA-N 1-phenylpyrrole-2,5-dione Chemical compound O=C1C=CC(=O)N1C1=CC=CC=C1 HIDBROSJWZYGSZ-UHFFFAOYSA-N 0.000 description 3
- 229920000147 Styrene maleic anhydride Polymers 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- PYSRRFNXTXNWCD-UHFFFAOYSA-N 3-(2-phenylethenyl)furan-2,5-dione Chemical compound O=C1OC(=O)C(C=CC=2C=CC=CC=2)=C1 PYSRRFNXTXNWCD-UHFFFAOYSA-N 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000001746 injection moulding Methods 0.000 description 2
- 238000010525 oxidative degradation reaction Methods 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 238000001134 F-test Methods 0.000 description 1
- 238000000692 Student's t-test Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 238000000556 factor analysis Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000012353 t test Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N11/00—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties
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- 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)
- Processes Of Treating Macromolecular Substances (AREA)
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Abstract
The invention relates to the technical field of standard substance preparation, and discloses a melt flow rate standard substance and a preparation method thereof. The standard substance disclosed by the invention comprises the following components in parts by weight: 30-95 parts of ABS resin, 0.1-1 part of antioxidant, 0.1-1 part of light stabilizer, 5-10 parts of heat resistant agent and 0-0.2 part of processing aid. The preparation method of the standard substance comprises the following steps: mixing and stirring the resin, the antioxidant, the light stabilizer, the heat-resistant agent and the processing aid uniformly; and (5) carrying out melt extrusion, bracing, cooling, granulating and drying to obtain the product. The invention applies the standard substance and the preparation method thereof to the melt flow rate test. The standard substance has excellent uniformity and quality stability, and can be stored for a long time.
Description
Technical Field
The invention relates to the technical field of standard substance preparation, in particular to a melt flow rate standard substance and a preparation method thereof.
Background
Melt flow rate (including melt mass flow rate and melt finger volume flow rate) refers to the extrusion rate of a molten resin through a die of a specified length and inside diameter under specified temperature, load and piston position conditions. The melt flow rate is used for describing the mobility of plastic materials in the injection molding process, and has important guiding significance for ensuring the quality of thermoplastic plastics and products thereof and for confirming and adjusting the process in the injection molding production process.
When using melt flow rate test equipment, equipment level, equipment temperature, die state, cartridge cleanliness, etc., all affect the test results, and standard substances are now commonly used to calibrate the state of instruments and devices, verify the accuracy of the test operation. According to the inquiry of a national standard substance resource sharing platform, the existing commercial melt flow rate standard substance is only three types of PE material (applicable to 190 ℃), PS material (applicable to 200 ℃) and PP material (applicable to 230 ℃), and the standard substance material and the temperature are single in solidification.
The measurement of the melt flow rate is a process of melting a sample by heating. In some engineering plastics, the melt flow rate is typically higher than 230 ℃ to be sufficiently melted, such as 250 ℃ for PBT materials, 280 ℃ for PA materials, and 300 ℃ for PC materials. However, the standard substance with high temperature (230-300 ℃) is not applicable to the market at present, and the main reason is that the accuracy of the test result cannot be ensured when the existing standard substance is used for testing the high-temperature melt flow rate, for example, PBT, PA, PC material is very sensitive to humidity and is easy to absorb water and degrade, the fluctuation of the test result of a melt finger is large, and the standard substance cannot meet the stability requirement; if PE and PP materials are higher than 250 ℃, oxidative degradation can occur, so that the polymer main chain is broken from the weak bond in the middle, the molecular weight is reduced, the state becomes sticky, the melt index is enlarged, and the melt index test repeatability is poor.
Therefore, development of a melt flow rate standard substance suitable for high temperature is needed to enrich the variety of the standard substance.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a melt flow rate standard substance and a preparation method thereof, so as to overcome the technical defect that the standard substance only has three temperature points of 190 ℃, 200 ℃ and 230 ℃ in the prior art, and the standard substance is applicable to high temperature (230-300 ℃).
In order to solve the technical problems, in a first aspect, the invention provides a melt flow rate standard substance, which comprises the following components in parts by weight:
30-95 parts of ABS resin, 0.1-1 part of antioxidant, 0.1-1 part of light stabilizer, 5-10 parts of heat resistant agent and 0-0.2 part of processing aid. The mass flow rate of the melt of the ABS resin is 5-40 g/10min (220 ℃ and 10 kg). The mass flow rate of the melt is detected under the condition of 220 ℃/10kg according to the standard GB/T3682.1; the heat resistant agent is a repeating unit derived from a material comprising N-phenylmaleimide, styrene and maleic anhydride.
The invention selects ABS resin with the melt mass flow rate of 5-40 g/10min as matrix resin, is easy to process, and is easy to be oxidized and degraded when the temperature is higher than 250 ℃ compared with PP and PE resins, and the decomposition temperature of the ABS resin is higher than 350 ℃ in air atmosphere, thus being applicable to high-temperature melt flow rate test. The ABS resin is modified, an antioxidant is added to inhibit ageing and degradation of the ABS resin, and a light stabilizer and a heat-resistant agent are added to improve weather resistance and heat resistance, so that the ABS resin can be stably used at high temperature and can be stored for a long time, and in long-term storage for 6 months, the melt flow rate test result in a standard substance is still stable and is similar to the first test result.
The heat resistant agent is simultaneously introduced with benzene rings, five-membered rings and N-phenylmaleimide (NPMI), and is embedded into a macromolecular chain of a melt flow rate standard substance, the benzene rings on the N substituent groups can increase the space resistance (such as internal rotation resistance of the macromolecular chain) of the movement of the macromolecular chain, the heat resistance can be improved while good processability and fluidity are ensured, the standard substance is stable at high temperature (such as 350 ℃ is ensured not to be decomposed), the compatibility with ABS resin is good, and the aim of improving the uniformity and the stability of the melt flow rate standard substance in a synergic way with other components is fulfilled.
As a preferred embodiment of the melt flow rate standard substance, the invention comprises the following components in parts by weight: 90-93 parts of ABS resin, 0.1-0.4 part of antioxidant, 0.2-0.5 part of light stabilizer, 5-6 parts of heat resistant agent and 0.1-0.2 part of processing aid.
As a preferred embodiment of the melt flow rate standard substance of the present invention, the ABS resin comprises at least one ABS resin of different melt mass flow rates. When a plurality of ABS resins with different melt mass flow rates are used for mixing, the melt flow rate standard substances with different standard values can be flexibly prepared by adjusting the proportion of the ABS resins with different melt mass flow rates, and the fixed value range is wider.
As a preferable embodiment of the melt flow rate standard substance, the antioxidant is at least one of antioxidant 1010, antioxidant 168, antioxidant 1076, antioxidant 2246, antioxidant 626, antioxidant DNP, antioxidant DLTP and antioxidant TNP. The antioxidant is added to prevent thermal oxidative degradation in the process of processing or testing ABS resin, and also can prevent obvious natural aging of standard substances in the daily storage process.
As a preferred embodiment of the melt flow rate standard substance according to the present invention, the light stabilizer is at least one of UV326, UV329, UV770, UV3853, light stabilizer 961, light stabilizer 744. The light stabilizer can shield or absorb the energy of ultraviolet rays, so that the service life of the standard substance is prolonged.
As a preferred embodiment of the melt flow rate standard substance according to the present invention, the heat-resistant agent is a styrene-N-phenylmaleimide-maleic anhydride copolymer (S-NPMI-MAH).
As a preferable embodiment of the melt flow rate standard substance according to the present invention, the processing aid is at least one of 10# white oil, 5# white oil, 7# white oil, and 15# white oil.
In a second aspect, the present invention provides a method for preparing a melt flow rate standard substance, comprising the steps of:
(1) Mixing and stirring the ABS resin, the antioxidant, the light stabilizer, the heat-resistant agent and the processing aid; preferably, the stirring speed is 100-200 r/min, and the stirring time is 2-4 min;
(2) And (5) carrying out melt extrusion, bracing, cooling, granulating and drying to obtain the product.
As a preferred embodiment of the method for producing a melt flow rate standard substance according to the present invention, the processing conditions of the melt extrusion are as follows: vacuum is controlled to be minus 0.06 to minus 0.08MPa, the rotating speed of the host machine is 400 to 500r/min, the feeding amount is controlled to be 400 to 500kg/h, and the temperature of each interval is controlled as follows: the first area temperature is 100+/-10 ℃, the second area temperature is 200+/-10 ℃, the third area temperature is 200+/-10 ℃, the fourth area temperature is 200+/-10 ℃, the fifth area temperature is 200+/-10 ℃, the sixth area temperature is 200+/-10 ℃, the seventh area temperature is 200+/-10 ℃, the eighth area temperature is 200+/-10 ℃, and the ninth area temperature is 200+/-10 ℃.
In a third aspect, the present invention applies the melt flow rate standard to melt flow rate testing.
Compared with the prior art, the invention has the beneficial effects that:
1. the melt flow rate standard substance overcomes the defect of the lack of the high-temperature (230-300 ℃) standard substance in the prior art, can be used as the standard substance to check the state of equipment at high temperature, and improves the accuracy of the checking test.
2. The melt flow rate standard substance can realize melt flow rate constant value under different load weights within the temperature range of 220 ℃ to 300 ℃ by using the same standard substance, has wider applicable temperature range, and saves the fund investment for separately purchasing the standard substance under different temperatures.
3. When a plurality of ABS resins are used for mixing, the melt flow rate standard substance with different standard values can be flexibly prepared by adjusting the proportion of the ABS resins with different melt flow rates, and a wider fixed value range can be realized.
4. The melt flow rate standard substance has excellent uniformity and stability, the melt flow rate test results of a plurality of samples are very similar in a plurality of sampling tests, and in long-term storage for 6 months, the melt flow rate test result in the standard substance is still stable and is similar to the first test result.
5. The preparation method of the melt flow rate standard substance is simple, has low production cost and is beneficial to popularization and application.
Detailed Description
The following describes the embodiments of the present invention in further detail with reference to examples. The following examples are illustrative of the invention and are not intended to limit the scope of the invention.
In the description of the present invention, it should be understood that the apparatus or device referred to is a conventional apparatus or device unless otherwise indicated; all the materials or compounds are commercially available conventional test materials or compounds unless otherwise specified; the methods involved, unless otherwise specified, are all conventional methods.
The raw materials used in the following examples and comparative examples are described below, but are not limited to these materials:
ABS resin 1, china petrochemical industry sales Co., ltd, brand ABS 3504, melt mass flow rate of 5g/10min;
ABS resin 2, china petrochemical industry sales Co., ltd, brand ABS 8391, melt mass flow rate of 25g/10min;
ABS resin 3, china petrochemical industry sales Co., ltd, brand ABS 8391B, melt mass flow rate of 40g/10min;
ABS resin 4, china petrochemical industry sales Co., ltd, brand ABS 8391G, melt mass flow rate of 50G/10min;
the melt mass flow rate of the ABS resin is detected under the condition of 220 ℃/10kg according to the standard GB/T3682.1.
Antioxidant, commercially available, brand 1010;
antioxidant, commercially available, brand 168;
light stabilizers, commercially available under the trade designation UV770;
styrene-N-phenylmaleimide-maleic anhydride copolymer, japanese electric chemistry, brand MS-NB;
styrene-maleic anhydride copolymer, polyscope, SZ23110;
processing aids, commercially available, 10# white oil.
Examples 1 to 5:
according to the formula of Table 1, the resin, the antioxidant, the light stabilizer, the heat-resistant agent and the processing aid are put into a high-speed mixer to be uniformly stirred at the stirring speed of 100-200 r/min for 2-4 min. And (3) carrying out melt extrusion by using a 40:1 length-diameter ratio double screw extruder, bracing, cooling, granulating, then placing the granules in a vacuum drying oven at 80-100 ℃ for drying for 3-6 hours, cooling, and then sub-packaging in sealed bags, wherein each bag is 50g, thus obtaining the standard substance.
The processing conditions of the extruder melt extrusion are as follows: vacuum is controlled at-0.06 to-0.08 MPa, the rotation speed of the host machine is 400-500 r/min, the feeding amount is controlled at 400-500 kg/h, and the temperature of each interval is controlled as follows: the first area temperature is 100+/-10 ℃, the second area temperature is 200+/-10 ℃, the third area temperature is 200+/-10 ℃, the fourth area temperature is 200+/-10 ℃, the fifth area temperature is 200+/-10 ℃, the sixth area temperature is 200+/-10 ℃, the seventh area temperature is 200+/-10 ℃, the eighth area temperature is 200+/-10 ℃, and the ninth area temperature is 200+/-10 ℃.
Table 1 examples and comparative examples melt flow rate standards component contents (parts by weight)
The standard substances prepared in the above examples and comparative examples were sequentially subjected to uniformity and stability test, and specific test methods and test results are as follows:
(1) And (3) uniformity test: among the standard substance samples that were packaged, 10 groups of samples (1 bag per group) were randomly extracted for uniformity verification. The melt mass flow rate test was carried out on each group of samples, respectively, and each group of samples was repeated 2 times, using a melt flow rate tester, according to the test conditions in Table 1 and the requirements of the A method in the Standard GB/T3682.1, section 1. Determination of melt Mass Flow Rate (MFR) and melt volume flow Rate (MVR) of plastics. The test results were analyzed by single factor analysis of variance (F-test) and if the F-number was less than the specified limit, it was shown that there was no significant difference between the samples and the samples, and the samples were uniform.
(2) Stability test: after the prepared standard substance is sealed and stored at room temperature in a dark place for 6 months, 6 groups of samples are randomly extracted from the standard substance, and each group of samples is subjected to melt mass flow rate test by using a melt flow rate tester according to the test conditions of table 1 and the requirements of the method A in the test 1 part of the standard method for measuring the melt Mass Flow Rate (MFR) and the melt volume flow rate (MVR) of the standard GB/T3682.1, and each group of samples is repeatedly tested for 2 times. And analyzing the test result by a t-test method, and if the t value is smaller than a specified limit value, proving that the standard substance has no significant change.
The results of the uniformity test of the standard substance of example 1 are shown in Table 2, and the results of the stability test are shown in Table 3.
TABLE 2 example 1 Standard substance uniformity test results
TABLE 3 example 1 results of stability test of standard substances
The results of the uniformity test of the standard substance of example 2 are shown in Table 4, and the results of the stability test are shown in Table 5.
TABLE 4 example 2 Standard substance uniformity test results
TABLE 5 example 2 Standard substance stability test results
Example 3 the results of the uniformity test of the standard substance are shown in table 6, and the results of the stability test are shown in table 7.
TABLE 6 example 3 Standard substance uniformity test results
TABLE 7 example 3 results of stability test of standard substances
The results of the uniformity test of the standard substance of example 4 are shown in Table 8, and the results of the stability test are shown in Table 9.
TABLE 8 results of Standard substance uniformity test for example 4
TABLE 9 results of Standard substance stability test of example 4
Example 5 the results of the uniformity test of the standard substance are shown in table 10, and the results of the stability test are shown in table 11.
TABLE 10 results of Standard substance uniformity test of example 5
TABLE 11 example 5 Standard substance stability test results
The results of the uniformity test of the standard substance of example 6 are shown in Table 12, and the results of the stability test are shown in Table 13.
TABLE 12 results of Standard substance uniformity test for EXAMPLE 6
TABLE 13 results of Standard substance stability test
The results of the uniformity test of the standard substance of comparative example 1 are shown in Table 14, and the results of the stability test are shown in Table 15.
TABLE 14 results of comparative example 1 Standard substance uniformity test
TABLE 15 stability test results of comparative example 1 Standard substance
The results of the uniformity test of the standard substance of comparative example 2 are shown in Table 16, and the results of the stability test are shown in Table 17.
TABLE 16 comparative example 2 Standard substance uniformity test results
Table 17 comparative example 2 results of stability test of standard substance
The results of the examples and comparative examples for the uniformity and stability test are summarized in Table 18.
Table 18 summary of the results of the uniformity and stability test of the standard substance
| Numerical value | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | Comparative example 1 | Comparative example 2 | Limit value |
| F value | 0.33 | 0.88 | 1.28 | 1.67 | 1.62 | 1.97 | 3.14 | 3.98 | 3.02 |
| t value | 0.67 | 1.84 | 1.64 | 1.72 | 1.83 | 0.45 | 3.30 | 2.64 | 2.04 |
According to the test results of tables 2 to 13 and 18, the standard substance of each embodiment of the invention has excellent uniformity and stability when being tested at 220 ℃, 230 ℃, 260 ℃ and 300 ℃, the test results of melt flow rates of a plurality of samples are very close to each other through sampling and testing for multiple times, the F value is less than or equal to 3.02, the test results of melt flow rates in the standard substance are still stable in long-term storage for 6 months, the t value is less than or equal to 2.04, and the stability of the standard substance is good.
According to the test results of tables 14, 15 and 18, the heat-resistant agent in comparative example 1 is styrene-maleic anhydride copolymer (SMA), the F value is greater than 3.02, the t value is greater than 2.04 in long-term storage for 6 months, the uniformity and stability are poor, and when the temperature exceeds 280 ℃, the product is easy to degrade and cannot meet the requirement of high-temperature standard samples.
According to the test results of tables 16, 17 and 18, the ABS resin of comparative example 2 had a melt mass flow rate of 50g/10min at 220℃under 10kg, an F value of more than 3.02, a t value of more than 2.04 in long-term storage for 6 months, poor uniformity and stability, and uniformity and stability at 300℃under 2.16kg test conditions did not meet the limiting requirements. In summary, the standard substance of the embodiment of the invention adopts the ABS resin with the melt mass flow rate of 5-40 g/10min, has good quality stability, and lays a foundation for the uniformity and stability of the standard substance. The anti-oxidant, the light stabilizer and the heat-resistant agent are added to ensure that the anti-oxidant, the light stabilizer and the heat-resistant agent are stable at high temperature and can be stored for a long time.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted equally without departing from the spirit and scope of the technical solution of the present invention.
Claims (9)
1. The melt flow rate standard substance is characterized by comprising the following components in parts by weight: 30-93 parts of ABS resin, 0.1-1 part of antioxidant, 0.1-1 part of light stabilizer, 5-10 parts of heat resistant agent and 0-0.2 part of processing aid;
the mass flow rate of the melt of the ABS resin is 5-40 g/10min; the mass flow rate of the melt is detected under the condition of 220 ℃/10kg according to the standard GB/T3682.1;
the heat-resistant agent is a styrene-N-phenylmaleimide-maleic anhydride copolymer.
2. The melt flow rate standard substance according to claim 1, wherein the antioxidant is 0.1 to 0.4 part, the light stabilizer is 0.2 to 0.5 part, the heat resistant agent is 5 to 6 parts, and the processing aid is 0.1 to 0.2 part.
3. The melt flow rate standard according to claim 1 or 2, characterized in that the ABS resin comprises at least one ABS resin of different melt mass flow rate.
4. The melt flow rate standard according to claim 1 or 2, wherein the antioxidant is at least one of antioxidant 1010, antioxidant 168, antioxidant 1076, antioxidant 2246, antioxidant 626, antioxidant DNP, antioxidant DLTP, antioxidant TNP.
5. The melt flow rate standard according to claim 1 or 2, wherein the light stabilizer is at least one of UV326, UV329, UV770, UV3853, light stabilizer 961, light stabilizer 744.
6. The melt flow rate standard according to claim 1 or 2, wherein the processing aid is at least one of 10# white oil, 5# white oil, 7# white oil, 15# white oil.
7. The method for producing a melt flow rate standard substance according to any one of claims 1 to 6, comprising the steps of:
(1) Mixing and stirring the ABS resin, the antioxidant, the light stabilizer, the heat-resistant agent and the processing aid;
(2) And (5) carrying out melt extrusion, bracing, cooling, granulating and drying to obtain the product.
8. The method according to claim 7, wherein the processing conditions of the melt extrusion are: vacuum is controlled to be-0.06 to-0.08 MPa, the rotating speed of a host machine is 400-500 r/min, the feeding amount is controlled to be 400-500 kg/h, and the temperature of each interval is controlled as follows: the first area temperature is 100+/-10 ℃, the second area temperature is 200+/-10 ℃, the third area temperature is 200+/-10 ℃, the fourth area temperature is 200+/-10 ℃, the fifth area temperature is 200+/-10 ℃, the sixth area temperature is 200+/-10 ℃, the seventh area temperature is 200+/-10 ℃, the eighth area temperature is 200+/-10 ℃, and the ninth area temperature is 200+/-10 ℃.
9. Use of a standard according to any one of claims 1 to 6 in a melt flow rate test.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202111262144.0A CN114034605B (en) | 2021-10-28 | 2021-10-28 | Melt flow rate standard substance and preparation method thereof |
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| CN114621535B (en) * | 2022-03-31 | 2023-11-21 | 国高材高分子材料产业创新中心有限公司 | ABS (Acrylonitrile butadiene styrene) substrate standard sample and preparation method and application thereof |
| CN114634666B (en) * | 2022-03-31 | 2023-11-10 | 国高材高分子材料产业创新中心有限公司 | Standard substance for measuring plastic melt flow rate and preparation method and application thereof |
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