CN114573908B - Standard substance for measuring content of plastic carbon black, and preparation method and application thereof - Google Patents
Standard substance for measuring content of plastic carbon black, and preparation method and application thereof Download PDFInfo
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- 239000006229 carbon black Substances 0.000 title claims abstract description 100
- 239000000126 substance Substances 0.000 title claims abstract description 29
- 229920003023 plastic Polymers 0.000 title claims abstract description 24
- 239000004033 plastic Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 31
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 31
- 238000012360 testing method Methods 0.000 claims abstract description 29
- 229920005989 resin Polymers 0.000 claims abstract description 26
- 239000011347 resin Substances 0.000 claims abstract description 26
- 239000011159 matrix material Substances 0.000 claims abstract description 24
- 238000012795 verification Methods 0.000 claims abstract description 9
- 229920000092 linear low density polyethylene Polymers 0.000 claims description 15
- 239000004707 linear low-density polyethylene Substances 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 14
- 229920001684 low density polyethylene Polymers 0.000 claims description 8
- 239000004702 low-density polyethylene Substances 0.000 claims description 8
- 238000003801 milling Methods 0.000 claims description 8
- 239000004698 Polyethylene Substances 0.000 claims description 7
- -1 polyethylene Polymers 0.000 claims description 7
- 229920005672 polyolefin resin Polymers 0.000 claims description 7
- 239000004594 Masterbatch (MB) Substances 0.000 claims description 6
- PWWSSIYVTQUJQQ-UHFFFAOYSA-N distearyl thiodipropionate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)CCSCCC(=O)OCCCCCCCCCCCCCCCCCC PWWSSIYVTQUJQQ-UHFFFAOYSA-N 0.000 claims description 6
- SSDSCDGVMJFTEQ-UHFFFAOYSA-N octadecyl 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical group CCCCCCCCCCCCCCCCCCOC(=O)CCC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 SSDSCDGVMJFTEQ-UHFFFAOYSA-N 0.000 claims description 6
- 239000000155 melt Substances 0.000 claims description 5
- 229920000573 polyethylene Polymers 0.000 claims description 5
- 238000000034 method Methods 0.000 abstract description 10
- 238000009841 combustion method Methods 0.000 abstract description 7
- 238000010438 heat treatment Methods 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 238000002411 thermogravimetry Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 229920001903 high density polyethylene Polymers 0.000 description 4
- 239000004700 high-density polyethylene Substances 0.000 description 4
- 229920001179 medium density polyethylene Polymers 0.000 description 4
- 239000004701 medium-density polyethylene Substances 0.000 description 4
- 239000012528 membrane Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 238000000197 pyrolysis Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 239000004743 Polypropylene Substances 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 229920001155 polypropylene Polymers 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- BLDFSDCBQJUWFG-UHFFFAOYSA-N 2-(methylamino)-1,2-diphenylethanol Chemical compound C=1C=CC=CC=1C(NC)C(O)C1=CC=CC=C1 BLDFSDCBQJUWFG-UHFFFAOYSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 150000004982 aromatic amines Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 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
- 239000002530 phenolic antioxidant Substances 0.000 description 1
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 150000007970 thio esters Chemical class 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/08—Copolymers of ethene
- C08L23/0807—Copolymers of ethene with unsaturated hydrocarbons only containing more than three carbon atoms
- C08L23/0815—Copolymers of ethene with aliphatic 1-olefins
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/06—Polyethene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/12—Polypropene
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/06—Properties of polyethylene
- C08L2207/066—LDPE (radical process)
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N2001/2893—Preparing calibration standards
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a standard substance for measuring the content of plastic carbon black, and a preparation method and application thereof. The standard for measuring the content of the plastic carbon black comprises the following components in parts by weight: 60-100 parts of matrix resin, 0.9-32 parts of carbon black and 0-1 part of antioxidant. When the carbon black content in the standard substance for measuring the content of the plastic carbon black is less than 2 weight percent, the relative standard deviation of the test result is less than 10 percent; when the carbon black content is more than or equal to 2wt%, the relative standard deviation of the test result is less than 5%, and the method can be used for the test verification of the common carbon black content, and is suitable for the self-calibration check of instruments of a direct combustion method and a TGA method, and the like.
Description
Technical Field
The invention belongs to the field of plastics, and relates to a standard substance for measuring the content of plastic carbon black, a preparation method and application thereof.
Background
Carbon black is widely used as an excellent colorant and anti-aging agent in various modified plastics. The carbon black content is usually tested by a direct combustion method and a TGA (thermal gravimetric analysis) method, but the overall test result greatly fluctuates due to the fact that the carbon black is easily dispersed unevenly. The daily calibration check of the two test methods is generally only performed by temperature and weight check, and the test of the carbon black content is influenced by various aspects such as test temperature, atmosphere, flow, environment, instrument state and the like, and the single check mode is low in efficiency and cannot effectively feed back the real data of the carbon black content. At present, no standard substance with carbon black content is used for checking and verifying comprehensive influence factors, so that a series of standard substances with carbon black content with different gradients are required to be designed and manufactured to effectively meet the standard matching and self-correcting requirements of most products and equipment.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a standard substance for measuring the content of plastic carbon black, and a preparation method and application thereof, so as to meet the standard and self-calibration requirements of most products and equipment.
In order to achieve the above object, in a first aspect, the invention provides a standard for determining the content of plastic carbon black, which comprises a matrix resin, carbon black and an antioxidant, wherein the standard comprises the following components in parts by weight: 60-100 parts of matrix resin, 0.9-32 parts of carbon black and 0-1 part of antioxidant.
The standard substance takes polyolefin resin as matrix resin, and carbon black and antioxidant with specific dosage are added, so that the determination result of the carbon black content is ensured to be accurate and stable, the standard substance with the carbon black content less than 2wt% meets the requirement that the relative standard deviation of the test result is less than 10% and the standard substance with the carbon black content more than or equal to 2wt% meets the relative standard deviation of the test result is less than 5%, the standard substance can be used for the test verification of the common carbon black content, and is suitable for the instrument self-calibration verification of a direct combustion method and a TGA method, and the like. Preferably, the matrix resin is polyethylene. Compared with the polyolefin resin such as polypropylene and the like which is used as matrix resin and polyethylene which is used as matrix resin, the carbon black can be better mixed with the carbon black, so that the carbon black content test result is accurate and has higher stability.
Preferably, the carbon black is present in the standard in an amount of 0.9 to 32wt%.
Preferably, the matrix resin is at least one of low density polyethylene and linear low density polyethylene.
Preferably, the matrix resin has a melt mass flow rate of 1.5-2.5g/10min. The melt mass flow rate of the matrix resin was measured according to GB/T3682.1-2018 using a weight of 2.16kg and at a temperature of 190 ℃.
The polyethylene may be at least one selected from high density polyethylene, medium density polyethylene, low density polyethylene, and linear low density polyethylene. The PE resin is preferably at least one of low-density polyethylene and linear low-density polyethylene to make the carbon black content result measured by the direct combustion method and the TGA method more accurate and stable, because the low-density polyethylene and the linear low-density polyethylene have lower crystallinity, better melt fluidity and more uniform mixing with carbon black than the high/medium-density polyethylene. Compared with low-density polyethylene, the linear low-density polyethylene has higher melting point, better heat resistance and less possibility of pyrolysis and aging in the production process, so that the PE resin is more preferably the linear low-density polyethylene, so that the carbon black content result measured by a direct combustion method is more accurate and stable. The density of the linear low density polyethylene is not particularly limited; in some embodiments, the linear low density polyethylene has a density of 0.913 to 0.930g/cm 3 。
Preferably, the carbon black is added in the form of a carbon black masterbatch comprising carbon black and a polyolefin resin carrier. The carbon black is added in the form of carbon black master batch, so that the dispersibility of the carbon black in matrix resin is better, and the carbon black content test result is more accurate and stable.
Preferably, the polyolefin resin carrier and the matrix resin are the same in kind, and the carbon black masterbatch contains 45-47% by weight of carbon black.
Preferably, the antioxidant comprises a main antioxidant and an auxiliary antioxidant, wherein the main antioxidant is antioxidant 1076, the auxiliary antioxidant is antioxidant DSTDP, and the weight ratio of the antioxidant 1076 to the antioxidant DSTDP is 1:1-3.
The antioxidant comprises a main antioxidant and an auxiliary antioxidant. Wherein the main antioxidant can be selected from at least one of phenolic antioxidant, aromatic amine antioxidant, etc., and the auxiliary antioxidant can be selected from at least one of phosphite antioxidant, thioester antioxidant, etc. The inventor finds that reasonable compounding of the antioxidant 1076 and the antioxidant DSTDP can produce synergistic antioxidation, so that the carbon black content test result is more accurate and stable.
In a second aspect, the invention provides a method for preparing the standard for determining the content of plastic carbon black, which comprises the following steps: and mixing matrix resin and carbon black or matrix resin, carbon black and antioxidant uniformly, banburying, and carrying out open milling to obtain the standard substance for measuring the content of the plastic carbon black.
The product obtained after open mill can be directly used for carbon black content test verification, and can also be further subjected to tabletting treatment and then used for carbon black content test verification.
Preferably, the banburying temperature is 170-200 ℃, the banburying time is 15-30 min, the open milling temperature is 200-220 ℃ and the open milling time is 10-20 min. The temperature and/or time of the internal mixing and/or the open mixing are/is out of the range, and the temperature and time of the internal mixing and the open mixing are selected to be in the range, so that the carbon black content test result of the obtained standard substance is more accurate.
In a third aspect, the invention provides an application of the standard for determining the content of carbon black in plastic in carbon black content test verification.
Compared with the prior art, the invention has the beneficial effects that: the standard substance for measuring the content of the carbon black in the plastic meets the requirements that the relative standard deviation of the carbon black content test result is less than 10 percent when the carbon black content is less than 2 weight percent and the relative standard deviation of the carbon black content test result is less than 5 percent when the carbon black content is more than or equal to 2 weight percent, has low cost, can be used for the test verification of the commonly used carbon black content, and is suitable for the self-calibration verification of instruments of a direct combustion method and a TGA method and the like.
Detailed Description
For a better description of the objects, technical solutions and advantages of the present invention, the present invention will be further described with reference to the following specific examples. It will be appreciated by persons skilled in the art that the specific embodiments described herein are for purposes of illustration only and are not intended to be limiting.
The reagents, methods and apparatus employed in the present invention, unless otherwise specified, are all conventional in the art.
The sources of the raw materials used in each of the examples and comparative examples are as follows:
linear low density polyethylene 1: LLDPE 7042, china petrochemical, density of 0.920g/cm 3 Melt flow rate (190 ℃,2.16 Kg): 2g/10min;
linear low density polyethylene 2: m500026, saint, density of 0.922g/cm 3 Melt flow rate (190 ℃,2.16 Kg): 2.8g/10min;
linear low density polyethylene 3:2021D, dow, USA, density 0.918g/cm 3 Melt flow rate (190 ℃,2.16 Kg): 1.2g/10min;
high density polyethylene: HDPE 8008, dushan mountain petrochemical, density 0.957g/cm 3 ；
Medium density polyethylene: MDPE MM2002, china petrochemical industry, density of 0.931g/cm 3 ；
Low density polyethylene: LDPE LD450, china petrochemical industry, density of 0.921g/cm 3 ；
Polypropylene: EP300M, medium sea Shell, density 0.904g/cm 3 ；
Carbon black master batch: 2772, cabo chemical industry, wherein the weight content of the carbon black is 45% -47%;
antioxidant 1076: commercially available, the same species as in the other examples and comparative examples;
antioxidant DSTDP: the same substances are commercially available in other examples and comparative examples.
Examples 1 to 13
Examples 1 to 13 respectively provide a standard substance for measuring the content of plastic carbon black, the composition of the standard substance for measuring the content of plastic carbon black and the preparation conditions thereof are shown in Table 1, and the preparation method comprises the following steps: (1) uniformly mixing all the raw materials to obtain a premixed sample; (2) Heating a torque rheometer (banburying module) to 200 ℃, keeping the temperature and stabilizing for 10min, pouring a premixed sample into the torque rheometer, and keeping the temperature and banburying for 20min according to required sample preparation conditions; (3) Taking out the sample after banburying is finished, putting the sample into an open mill with the preset temperature of 200 ℃, and preserving heat for 10min; (4) Taking out the open-mixed sample, preparing a membrane at 15MPa by using a tabletting machine and a membrane die with the thickness of 2mm, tabletting at 200 ℃ for 5min, taking out the membrane, and cutting or crushing and granulating the membrane to obtain a sample with the size of 5mm x 5 mm.
TABLE 1
The standard substance testing method comprises the following steps:
(1) direct combustion test conditions: weighing about 1g of a sample by using a dried combustion boat, recording the weight A of the sample to be accurate to 0.0001g, heating to 350 ℃ in a nitrogen (volume concentration is 99.99 percent, and 1.5L/min) atmosphere for 10min, then heating to 450 ℃ for 10min, continuously heating to 600 ℃ for 10min, maintaining the temperature at 600 ℃ for 10min, continuously ventilating, taking out the sample after cooling, weighing after cooling for 30min in a dryer, and recording the pyrolysis weight B.
Putting the sample into the instrument again, switching the instrument into an oxygen atmosphere (volume concentration is 99.5%,1.5L/min; a dry air atmosphere can also be adopted), heating to 600 ℃, keeping at 600 ℃ for 20min, taking out after cooling, weighing after cooling for 30min in a dryer, and recording the decomposition weight C;
calculating the carbon black content: carbon black content = [ (pyrolysis weight B-decomposition weight C)/sample weight a ] ×100%;
each standard sample was tested 5 times.
(2) TGA test conditions: introducing dry nitrogen without oxygen at a flow rate of 50mL/min, introducing air for 5-10min before the start of test to ensure that the furnace is in an oxygen-free atmosphere, heating to 850 ℃ at a heating rate of 20 ℃/min, switching the nitrogen into dry air (volume concentration: 80% nitrogen and 20% oxygen) after the temperature reaches 850 ℃, and burning carbon black at a flow rate of 50mL/min, and heating to 950 ℃ at a heating rate of 20 ℃/min. The weight loss at 850-950 ℃ is the carbon black content.
Each standard sample was tested 5 times.
The results of the above test are shown in Table 2.
TABLE 2
As can be seen from examples 1 to 13 in Table 2, the data obtained in the examples of the present invention can be obtained as stable data according to the composition and content of the formulation, and the relative standard deviation is less than 10% when the carbon black content is less than 2%; when the content of the carbon black is more than 2%, the relative standard deviation is less than 5%, the fluctuation of the sample is small, and the test is stable. As is clear from comparative example 1, when the carbon black content exceeds 32% by weight, the relative standard deviation exceeds 5%, and the sample fluctuation is large. The invention covers the standard substance range of 0.9wt% to 32wt% of carbon black content, and has wide applicability.
As is clear from examples 3, 8, 9, 10 and 11, the present invention is applicable to various types of polyolefin resin substrates, and stable samples can be obtained. Example 3 a more stable sample was obtained by selecting a linear low density polyethylene. Example 3 has better uniformity and less data fluctuation than examples 8, 9 and 10, and the preferred linear low density polyethylene as the resin matrix can ensure the stability of the sample.
As is clear from examples 3 and examples 12 to 13, the stability of the sample can be further ensured by using polyethylene as a resin matrix at a melt mass flow rate (190 ℃ C., 2.16 Kg) of 1.5 to 2.5g/10min.
When the carbon black content of the sample is required to be lower than 2 percent by combining the carbon black content characteristics, the average fluctuation of the sample is less than +/-10 percent; when the content of the carbon black is more than 2%, the mean fluctuation is less than +/-5%. Examples 1 to 7 carbon black content standard substance constant value ranges are:
example 1: carbon black content (0.91.+ -. 0.10% by weight);
example 2: carbon black content (2.30.+ -. 0.12% by weight);
example 3: carbon black content (4.60.+ -. 0.23 wt.%;
example 4: carbon black content (6.90.+ -. 0.35% by weight);
example 5: carbon black content (9.20.+ -. 0.46 wt.%;
example 6: carbon black content (22.50.+ -. 1.10 wt.%;
example 7: carbon black content (30.40.+ -. 1.50 wt%).
As shown in table 3, after the standard substance sample was left for 12 months in the normal temperature environment, the test data were as follows:
TABLE 3 Table 3
As shown in Table 3, the sample components are pure, the content of the main component is not changed in the normal temperature environment, the data test is still stable within the fixed value range after the sample is placed for 12 months at normal temperature, the relative standard deviation of the sample is less than 5%, the sample deviation is small, and the repeatability is good.
Examples 14 to 23 each provide a plastic carbon black content measurement standard substance having the same composition as in example 3, and the preparation method is the same as in example 3 except that the conditions of banburying and open milling are different. The banburying and open milling conditions of examples 14 to 23 are shown in Table 4.
TABLE 4 Table 4
The carbon black contents of the standard substances of examples 14 to 23 were measured according to the direct combustion method and the TGA method described above, and the results are shown in Table 5.
TABLE 5
As is clear from examples 3 and 14-23, when the internal mixing temperature is 170-200 ℃, the internal mixing time is 15-30 min, the open mixing temperature is 200-220 ℃ and the open mixing time is 10-20 min, the carbon black content test result is more stable and accurate than when the internal mixing and/or open mixing process conditions are out of the range.
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 (5)
1. The standard substance for measuring the content of the plastic carbon black is characterized by comprising the following components in parts by weight: 60-100 parts of matrix resin, 0.9-32 parts of carbon black and 0-1 part of antioxidant; the weight percentage of the carbon black in the standard substance is 0.9-32wt%; the matrix resin is polyethylene; the carbon black is added in the form of carbon black master batch, and the carbon black master batch comprises carbon black and a polyolefin resin carrier; the polyolefin resin carrier and the matrix resin are the same in kind;
the preparation method of the standard substance for measuring the content of the plastic carbon black comprises the following steps: mixing matrix resin and carbon black or matrix resin, carbon black and antioxidant uniformly, banburying, and then open milling to obtain a standard substance for measuring the content of the plastic carbon black; wherein the banburying temperature is 170-200 ℃, the banburying time is 15-30 min, the open milling temperature is 200-220 ℃, and the open milling time is 10-20 min.
2. The standard for determining the content of carbon black in plastic according to claim 1, wherein the matrix resin is at least one of low density polyethylene and linear low density polyethylene.
3. The standard for determining the content of plastic carbon black according to claim 2, wherein the melt mass flow rate of the matrix resin is 1.5-2.5g/10 min; the melt mass flow rate of the matrix resin was measured according to GB/T3682.1-2018 using a weight of 2.16kg and at a temperature of 190 ℃.
4. The standard for determining the content of the plastic carbon black according to claim 1, wherein the antioxidant comprises a main antioxidant and an auxiliary antioxidant, the main antioxidant is antioxidant 1076, the auxiliary antioxidant is antioxidant DSTDP, and the weight ratio of the antioxidant 1076 to the antioxidant DSTDP is 1:1-3.
5. The use of the standard for determining the content of plastic carbon black according to any one of claims 1 to 4 in carbon black content test verification.
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Citations (7)
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|---|---|---|---|---|
| US5656686A (en) * | 1994-06-28 | 1997-08-12 | Hoechst Aktiengesellschaft | Polyethylene molding compositions |
| CN101967241A (en) * | 2009-07-27 | 2011-02-09 | 中国石油天然气股份有限公司 | Carbon black composition blending material and preparation method thereof |
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