CN114573908A - 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
- Publication number
- CN114573908A CN114573908A CN202210337630.2A CN202210337630A CN114573908A CN 114573908 A CN114573908 A CN 114573908A CN 202210337630 A CN202210337630 A CN 202210337630A CN 114573908 A CN114573908 A CN 114573908A
- Authority
- CN
- China
- Prior art keywords
- carbon black
- content
- antioxidant
- plastic
- matrix resin
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000006229 carbon black Substances 0.000 title claims abstract description 104
- 239000000126 substance Substances 0.000 title claims abstract description 31
- 229920003023 plastic Polymers 0.000 title claims abstract description 27
- 239000004033 plastic Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000012360 testing method Methods 0.000 claims abstract description 28
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 27
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 27
- 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 23
- 238000000034 method Methods 0.000 claims abstract description 10
- 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 12
- 238000003801 milling Methods 0.000 claims description 11
- 239000004698 Polyethylene Substances 0.000 claims description 8
- 229920001684 low density polyethylene Polymers 0.000 claims description 8
- 239000004702 low-density polyethylene Substances 0.000 claims description 8
- 239000004594 Masterbatch (MB) Substances 0.000 claims description 7
- -1 polyethylene Polymers 0.000 claims description 7
- PWWSSIYVTQUJQQ-UHFFFAOYSA-N distearyl thiodipropionate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)CCSCCC(=O)OCCCCCCCCCCCCCCCCCC PWWSSIYVTQUJQQ-UHFFFAOYSA-N 0.000 claims description 6
- 238000005259 measurement Methods 0.000 claims description 6
- 239000000155 melt Substances 0.000 claims description 6
- 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 6
- 229920005672 polyolefin resin Polymers 0.000 claims description 6
- 229920000573 polyethylene Polymers 0.000 claims description 5
- 238000003556 assay Methods 0.000 claims 2
- 238000010200 validation analysis Methods 0.000 claims 1
- 238000009841 combustion method Methods 0.000 abstract description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 7
- 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
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 238000012795 verification Methods 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 239000004743 Polypropylene Substances 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229920001155 polypropylene Polymers 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000010998 test method Methods 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
- 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
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification 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
- 238000004321 preservation Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000010421 standard material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000002195 synergetic effect Effects 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
Landscapes
- 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, a preparation method and application thereof. The standard substance 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 content of the carbon black in the standard substance for measuring the content of the plastic carbon black is less than 2 wt%, the relative standard deviation of the test result is less than 10%; when the carbon black content is more than or equal to 2 wt%, the relative standard deviation of the test result is less than 5%, and the method can be used for testing and verifying the common carbon black content and is suitable for self-checking of instruments of a direct combustion method and a TGA method.
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, and a preparation method and application thereof.
Background
Carbon black is widely used in various modified plastics as an excellent colorant and anti-aging agent. The carbon black content is usually measured by a direct combustion method and a TGA (thermal gravimetric analysis) method, but the overall test result fluctuates greatly due to the easy and uneven dispersion of the carbon black. The daily calibration and verification of the two test methods generally only carry out temperature and weight verification, 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 a single verification mode not only has low efficiency, but also cannot effectively feed back real data of the carbon black content. At present, no standard substance with carbon black content is available on the market for checking and verifying comprehensive influence factors, so that a series of standard substances with different gradients of carbon black content need to be designed and manufactured to effectively meet the standard and self-correcting requirements of most products and equipment.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a standard substance for measuring the content of plastic carbon black, 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 present invention provides a standard substance for plastic carbon black content measurement, which comprises a matrix resin, carbon black and an antioxidant, wherein the standard substance 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 accurate and stable, the standard substance with the carbon black content less than 2 wt% 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 2 wt% meets the requirement that the relative standard deviation of the test result is less than 5%, and the standard substance can be used for testing and verifying the carbon black content in common use, and is suitable for self-checking of instruments 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 as the matrix resin and the polyethylene as the matrix resin, the carbon black can be better mixed, so that the carbon black content test result is more accurate and stable.
Preferably, the carbon black is present in the standard in an amount of 0.9 to 32 wt%.
Preferably, the matrix resin is at least one of low density polyethylene and linear low density polyethylene.
Preferably, the melt mass flow rate of the matrix resin is 1.5 to 2.5g/10 min. The melt mass flow rate of the matrix resin was measured according to GB/T3682.1-2018 using a 2.16kg weight and at a temperature of 190 ℃.
The polyethylene can be selected from at least one of high density polyethylene, medium density polyethylene, low density polyethylene and linear low density polyethylene. Compared with high/medium density polyethylene, low density polyethylene and linear low density polyethylene, the crystallinity is lower, the melt fluidity is better, and the PE resin is easier to be uniformly mixed with carbon black, so that the PE resin is preferably at least one of low density polyethylene and linear low density polyethylene, so that the carbon black content result measured by a direct combustion method and a TGA method is more accurate and stable. Compared with low-density polyethylene, linear low-density polyethylene has a higher melting point and better heat resistance, and is not easy to pyrolyze and age in the production process, so that the PE resin is further preferably linear low-density polyethylene, and the result of the carbon black content 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/cm3。
Preferably, 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 carbon black is added in the form of the carbon black master batch, so that the dispersibility of the carbon black in the matrix resin is better, and the test result of the content of the carbon black is more accurate and stable.
Preferably, the polyolefin resin carrier and the matrix resin are the same in type, and the weight content of the carbon black in the carbon black master batch is 45-47%.
Preferably, the antioxidant comprises a main antioxidant and an auxiliary antioxidant, the main antioxidant is an antioxidant 1076, the auxiliary antioxidant is an antioxidant DSTDP, and the weight ratio of the antioxidant 1076 to the antioxidant DSTDP is 1: 1-3.
The antioxidant selection comprises a main antioxidant and a secondary antioxidant. Wherein, the primary antioxidant can be at least one of phenolic antioxidant, aromatic amine antioxidant and the like, and the secondary antioxidant can be at least one of phosphite antioxidant, thioester antioxidant and the like. The inventor finds that the antioxidant 1076 and the antioxidant DSTDP are reasonably compounded to generate a synergistic antioxidation effect, so that a carbon black content test result is more accurate and stable.
In a second aspect, the invention provides a preparation method of the standard for determining the content of the plastic carbon black, which comprises the following steps: and uniformly mixing the matrix resin and the carbon black or the matrix resin, the carbon black and the antioxidant, banburying, and then milling to obtain the standard substance for measuring the content of the plastic carbon black.
The product obtained after open milling can be directly used for testing and verifying the content of the carbon black, and can also be further subjected to tabletting treatment and then used for testing and verifying the content of the carbon black.
Preferably, the banburying temperature is 170-200 ℃, the banburying time is 15-30 min, the open mixing temperature is 200-220 ℃, and the open mixing time is 10-20 min. Compared with the temperature and/or time of internal mixing and/or open milling which are outside the range, the temperature and time of internal mixing and open milling which are selected within the range can enable the test result of the carbon black content of the obtained standard substance to be more accurate.
In a third aspect, the invention provides application of the standard substance for measuring the content of the plastic carbon black in testing and verifying the content of the carbon black.
Compared with the prior art, the invention has the beneficial effects that: the standard substance for measuring the content of the plastic carbon black meets the requirements that the relative standard deviation of the test result of the content of the carbon black is less than 10% when the content of the carbon black is less than 2 wt% and the relative standard deviation of the test result of the content of the carbon black is less than 5% when the content of the carbon black is more than or equal to 2 wt%, has low cost, can be used for the test and verification of the content of the common carbon black, and is suitable for the instrument self-checking of a direct combustion method and a TGA method and the like.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples. It will be understood by those skilled in the art that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The reagents, methods and equipment adopted by the invention are conventional in the technical field if no special description is given.
The raw material sources used in the examples and comparative examples are as follows:
linear low density polyethylene 1: LLDPE 7042, China petrochemical, density 0.920g/cm3Melt flow rate (190 ℃, 2.16 Kg): 2g/10 min;
linear low density polyethylene 2: m500026, Saber, density 0.922g/cm3Melt flow rate (190 ℃, 2.16 Kg): 2.8g/10 min;
linear low density polyethylene 3: 2021D, Dow, U.S. density of 0.918g/cm3Melt flow rate (190 ℃, 2.16 Kg): 1.2g/10 min;
high density polyethylene: HDPE 8008, Mount-mountain petrochemical, density 0.957g/cm3；
Medium density polyethylene: MDPE MM2002, China petrochemical, density 0.931g/cm3；
Low density polyethylene: LDPE LD450, China petrochemical, density of 0.921g/cm3；
Polypropylene: EP300M, Mediterranean Shell, Density 0.904g/cm3；
Carbon black master batch: 2772, Kabot chemical industry, the weight content of carbon black is 45% -47%;
antioxidant 1076: the same materials were commercially available in other examples and comparative examples;
antioxidant DSTDP: the same materials were 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 and the preparation conditions of the standard substance for measuring the content of plastic carbon black are shown in table 1, and the preparation method comprises the following steps: (1) uniformly mixing the raw materials to obtain a premixed sample; (2) heating a torque rheometer (an internal mixing module) to 200 ℃, keeping the temperature and stabilizing for 10min, pouring the premixed sample into the torque rheometer, and keeping the temperature and mixing for 20min according to the required sample preparation conditions; (3) taking out the sample after banburying, putting the sample into an open mill with the preset temperature of 200 ℃, and carrying out open milling for 10min under the condition of heat preservation; (4) taking out the open-milled sample, preparing a film at the pressure of 15MPa by using a tabletting machine and a film die with the thickness of 2mm, wherein the tabletting temperature is 200 ℃, the pressure maintaining time is 5min, taking out the film, and cutting or crushing and granulating the film to obtain the sample with the size of 5mm by 5 mm.
TABLE 1
Standard substance test method:
testing conditions by a direct combustion method: weighing about 1g of a dried combustion boat, recording the weight A of the sample to be accurate to 0.0001g, heating to 350 ℃ within 10min, heating to 450 ℃ within 10min, continuously heating to 10min to 600 ℃ by using a carbon black content tester in the atmosphere of nitrogen (the volume concentration is 99.99%, and the volume concentration is 1.5L/min), keeping the temperature at 600 ℃ for 10min, continuously ventilating, taking out 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 to an oxygen atmosphere (volume concentration is 99.5%, 1.5L/min; dry air atmosphere can also be adopted), heating to 600 ℃, keeping at 600 ℃ for 20min, taking out after cooling, cooling in a dryer for 30min, weighing, and recording the decomposition weight C;
calculating the content of carbon black: carbon black content ═ 100% by weight [ (pyrolysis weight B-decomposition weight C)/sample weight a ];
each standard sample was tested 5 times.
② TGA method test conditions: introducing dry nitrogen without oxygen at a flow rate of 50mL/min, introducing the gas for 5-10min before the test starts to ensure that the furnace is in an oxygen-free atmosphere, heating to 850 ℃ at a temperature rise rate of 20 ℃/min, switching the nitrogen into dry air (volume concentration: 80% nitrogen and 20% oxygen) after the temperature reaches 850 ℃, wherein the flow rate is 50mL/min, and then burning the carbon black, and heating to 950 ℃ at a temperature rise rate of 20 ℃/min. The weight loss in the stage of 850-950 ℃ is the carbon black content.
Each standard sample was tested 5 times.
The results of the above tests are shown in Table 2.
TABLE 2
As can be seen from the examples 1 to 13 in Table 2, the data measured in the examples of the present invention can obtain stable data according to different formulation components and contents, and when the carbon black content is less than 2%, the relative standard deviation is less than 10%; when the content of the carbon black is more than 2 percent, the relative standard deviation is less than 5 percent, the fluctuation of the sample is small, and the test is stable. As can be seen from comparative example 1, when the carbon black content exceeded 32 wt%, the relative standard deviation exceeded 5%, and the sample fluctuation was large. The invention covers the standard substance range of 0.9 wt% to 32 wt% 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 different types of polyolefin resin substrates, and stable samples can be obtained. Example 3 a more stable sample was obtained using linear low density polyethylene. Example 3 has better uniformity and smaller data fluctuation compared with examples 8, 9 and 10, and the stability of the sample can be better ensured by preferably using linear low density polyethylene as the resin matrix.
From examples 3 and 12-13, it is known that the stability of the sample can be further ensured by using polyethylene as the resin matrix when the melt mass flow rate (190 ℃, 2.16Kg) is 1.5-2.5g/10 min.
Combining the carbon black content characteristic, when the carbon black content of the sample is lower than 2%, the mean value fluctuation of the sample is less than +/-10%; when the content of the carbon black is more than 2 percent, the average value fluctuation is less than +/-5 percent. The fixed value ranges of the standard substances of the carbon black content in the examples 1-7 are as follows:
example 1: carbon black content (0.91 + -0.10) wt%;
example 2: carbon black content (2.30. + -. 0.12 wt%);
example 3: carbon black content (4.60. + -. 0.23) wt%;
example 4: carbon black content (6.90. + -. 0.35) wt%;
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 samples were left for 12 months at room temperature, the test data were as follows:
TABLE 3
As can be seen from Table 3, since the sample has pure components, the change of the content of the main component does not occur in the normal temperature environment, after the sample is placed for 12 months at normal temperature, the data test is still stable in a fixed value range, 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, the composition of which is the same as example 3, and the preparation method is the same as example 3 except that the banburying and open milling conditions are different. Examples 14 to 23 the mixing and milling conditions are given in Table 4.
TABLE 4
The carbon black content of the standard materials of examples 14 to 23 was measured by the direct combustion method and the TGA method as described above, and the results are shown in Table 5.
TABLE 5
From the embodiment 3 and the embodiments 14 to 23, it can be seen that when the banburying temperature is 170 to 200 ℃, the banburying time is 15 to 30min, the open milling temperature is 200 to 220 ℃, and the open milling time is 10 to 20min, the test result of the carbon black content is more stable and accurate than that when the banburying and/or open milling process conditions are outside the range.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
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.
2. The plastic carbon black assay standard of claim 1, wherein the carbon black is present in the standard in an amount of 0.9 to 32 weight percent.
3. The plastic carbon black content measurement standard of claim 1, wherein the matrix resin is polyethylene.
4. The plastic carbon black content measurement standard according to claim 2, wherein the matrix resin is at least one of low density polyethylene and linear low density polyethylene.
5. The plastic carbon black content measurement standard according to claim 3, wherein the matrix resin has a melt mass flow rate of 1.5 to 2.5g/10 min; the melt mass flow rate of the matrix resin was measured according to GB/T3682.1-2018 using a 2.16kg weight and at a temperature of 190 ℃.
6. The plastic carbon black content measurement standard according to claim 1, wherein 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.
7. The standard substance for measuring the content of the plastic carbon black in claim 1, wherein the antioxidant comprises a main antioxidant 1076 and an auxiliary antioxidant DSTDP, and the weight ratio of the antioxidant 1076 to the antioxidant DSTDP is 1: 1-3.
8. The method for preparing a standard substance for measuring the content of plastic carbon black according to any one of claims 1 to 7, comprising the following steps: and uniformly mixing the matrix resin and the carbon black or the matrix resin, the carbon black and the antioxidant, banburying, and then milling to obtain the standard substance for measuring the content of the plastic carbon black.
9. The preparation method according to claim 8, wherein the banburying temperature is 170-200 ℃, the banburying time is 15-30 min, the open mixing temperature is 200-220 ℃, and the open mixing time is 10-20 min.
10. Use of the plastic carbon black assay standard of any one of claims 1 to 7 in carbon black content test validation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210337630.2A CN114573908B (en) | 2022-03-31 | 2022-03-31 | Standard substance for measuring content of plastic carbon black, and preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210337630.2A CN114573908B (en) | 2022-03-31 | 2022-03-31 | Standard substance for measuring content of plastic carbon black, and preparation method and application thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114573908A true CN114573908A (en) | 2022-06-03 |
| CN114573908B CN114573908B (en) | 2023-11-21 |
Family
ID=81779365
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210337630.2A Active CN114573908B (en) | 2022-03-31 | 2022-03-31 | Standard substance for measuring content of plastic carbon black, and preparation method and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114573908B (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN103289174A (en) * | 2013-06-24 | 2013-09-11 | 金发科技股份有限公司 | Highly-universal carbon black master-batches, preparation system apparatus and preparation method thereof |
| CN103645116A (en) * | 2013-12-18 | 2014-03-19 | 成都菲斯特化工有限公司 | Determination method for content of carbon black |
| CN104861278A (en) * | 2015-04-21 | 2015-08-26 | 安徽埃克森科技集团有限公司 | Communication cable special-purposed cable sheath material and preparation method thereof |
| CN106336562A (en) * | 2016-08-21 | 2017-01-18 | 江苏上上电缆集团有限公司 | Flame retardant polyethylene cable material and preparation method thereof |
| CN107200897A (en) * | 2016-03-17 | 2017-09-26 | 中国石化扬子石油化工有限公司 | Black masterbatch for high-density polyethylene geomembrane |
-
2022
- 2022-03-31 CN CN202210337630.2A patent/CN114573908B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN103289174A (en) * | 2013-06-24 | 2013-09-11 | 金发科技股份有限公司 | Highly-universal carbon black master-batches, preparation system apparatus and preparation method thereof |
| CN103645116A (en) * | 2013-12-18 | 2014-03-19 | 成都菲斯特化工有限公司 | Determination method for content of carbon black |
| CN104861278A (en) * | 2015-04-21 | 2015-08-26 | 安徽埃克森科技集团有限公司 | Communication cable special-purposed cable sheath material and preparation method thereof |
| CN107200897A (en) * | 2016-03-17 | 2017-09-26 | 中国石化扬子石油化工有限公司 | Black masterbatch for high-density polyethylene geomembrane |
| CN106336562A (en) * | 2016-08-21 | 2017-01-18 | 江苏上上电缆集团有限公司 | Flame retardant polyethylene cable material and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 刘西文 编著, 文化发展出版社 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114573908B (en) | 2023-11-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101302300B (en) | Antifog crystal film and preparation thereof | |
| CN102924762B (en) | Sulfur pre-dispersing mother rubber particle tread rubber and preparation method thereof | |
| CN102504404B (en) | Low-glossiness extinction haze distribution controllable biaxially-oriented polypropylene (BOPP) film | |
| CN112029256A (en) | Color master batch and preparation method thereof | |
| CN108314820A (en) | Stretched film and preparation method thereof | |
| CN110628107B (en) | Film opening agent, modified ethylene propylene rubber film and composition for forming same | |
| CN114573908B (en) | Standard substance for measuring content of plastic carbon black, and preparation method and application thereof | |
| CN111089843A (en) | Method for detecting application performance of plastic system titanium dioxide | |
| CN109553842A (en) | Composition for preparing linear low density polyethylene film and preparation method thereof | |
| Schmid et al. | Mechanical and barrier properties of thermoplastic whey protein isolate/ethylene vinyl acetate blends | |
| CN114112937A (en) | Method for detecting decoloring force of titanium dioxide in HIPS (high impact polystyrene) resin system | |
| CN109553872A (en) | A kind of composite material and preparation method and application of plastic penholder | |
| CN108192220A (en) | It is a kind of for polypropylene material of expansion tank and preparation method thereof | |
| BR112019005889B1 (en) | POLYETHYLENE COMPOSITION AND INJECTION MOLDED ARTICLE | |
| CN111995813A (en) | Polyethylene composite material and preparation method and application thereof | |
| US3060149A (en) | Stabilized polymer compositions | |
| CN111171450A (en) | High-impact-resistance and high-load-bearing polypropylene composite material, and preparation method and application thereof | |
| CN109738364B (en) | Method for detecting dispersibility of carbon black | |
| CN114634666B (en) | Standard substance for measuring plastic melt flow rate and preparation method and application thereof | |
| CN102854158B (en) | A kind of method of Fast Measurement phytase heat resistance | |
| CN111057297A (en) | Environment-friendly oxygen index standard substance and preparation method thereof | |
| CN114524991B (en) | Ash standard substance of PP base material, its preparation method and application | |
| Deshmukh et al. | Polymer‐and wax‐based monoconcentrate predispersed pigments in the colouring of plastics | |
| CN105647046A (en) | Preparation method of phenolic-antioxidant-containing positive control substance of food contact plastics | |
| CN110577788A (en) | Powder coating for food contact and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |