CN116067722A - Penetration quality control sample and preparation method thereof - Google Patents
Penetration quality control sample and preparation method thereof Download PDFInfo
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- CN116067722A CN116067722A CN202111269918.2A CN202111269918A CN116067722A CN 116067722 A CN116067722 A CN 116067722A CN 202111269918 A CN202111269918 A CN 202111269918A CN 116067722 A CN116067722 A CN 116067722A
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- 230000035515 penetration Effects 0.000 title claims abstract description 63
- 239000013062 quality control Sample Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title abstract description 10
- 239000000523 sample Substances 0.000 claims abstract description 67
- 239000012188 paraffin wax Substances 0.000 claims abstract description 51
- 239000001993 wax Substances 0.000 claims abstract description 28
- 238000002844 melting Methods 0.000 claims abstract description 26
- 230000008018 melting Effects 0.000 claims abstract description 26
- 239000000654 additive Substances 0.000 claims abstract description 20
- 238000010438 heat treatment Methods 0.000 claims abstract description 19
- 230000000996 additive effect Effects 0.000 claims abstract description 14
- 238000001514 detection method Methods 0.000 claims abstract description 13
- 238000001816 cooling Methods 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 239000003921 oil Substances 0.000 claims description 33
- 238000011049 filling Methods 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 9
- 238000004821 distillation Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 239000010687 lubricating oil Substances 0.000 claims description 5
- 239000002199 base oil Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 239000010779 crude oil Substances 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 5
- 238000003908 quality control method Methods 0.000 abstract description 4
- 238000012360 testing method Methods 0.000 description 15
- 238000012795 verification Methods 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000001681 protective effect Effects 0.000 description 3
- 238000000692 Student's t-test Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 239000012169 petroleum derived wax Substances 0.000 description 2
- 235000019381 petroleum wax Nutrition 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000012353 t test Methods 0.000 description 2
- 239000004169 Hydrogenated Poly-1-Decene Substances 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 239000012164 animal wax Substances 0.000 description 1
- 235000019383 crystalline wax Nutrition 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 238000005495 investment casting Methods 0.000 description 1
- 239000004200 microcrystalline wax Substances 0.000 description 1
- 235000019808 microcrystalline wax Nutrition 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000002304 perfume Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000003209 petroleum derivative Substances 0.000 description 1
- 238000004382 potting Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 229940099259 vaseline Drugs 0.000 description 1
- 239000012178 vegetable wax Substances 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
- 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
-
- 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
- G01N11/00—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties
- G01N11/10—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by moving a body within the material
- G01N11/12—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by moving a body within the material by measuring rising or falling speed of the body; by measuring penetration of wedged gauges
Landscapes
- Physics & Mathematics (AREA)
- 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)
- Lubricants (AREA)
Abstract
The invention discloses a penetration quality control sample and a preparation method thereof. The quality control sample of the invention takes a paraffin sample as a base material, a white oil sample as an additive A and vacuum distillate oil as an additive B; and (3) fully mixing the base material with the additive A and/or the additive B in a heating and melting state, and cooling to obtain a quality control sample. The invention prepares the quality control sample of the penetration degree in the penetration degree detection range (0-25 mm), meets the quality control requirement of the penetration degree detection of wax products, and solves the problems of uniformity and stability of the quality control sample of the penetration degree.
Description
Technical Field
The invention relates to the field of petroleum product detection, in particular to a penetration quality control sample and a preparation method thereof.
Background
The wax products are directly involved in daily production and family life of people, the variety of the wax products is very large, the terminal application market is very active, and the wax products are applied to manufacturing industries such as packaging, electronics, textiles, candles and the like, and are also applied to aspects such as perfume, additives, modifiers and the like. From the viewpoint of the large class of products, wax products are mainly classified into petroleum wax, synthetic wax, animal and vegetable wax, and the like. Petroleum waxes are classified into different varieties according to properties, such as: the oil-containing wax is yellow to black wax removed from petroleum fractions, and the oil content is 3% -50%. Such waxes may be sold after decolorization or by continuing to deoil to produce crude, semi-refined and fully refined paraffins. Microcrystalline wax is mostly derived from the lubricating oil residue fraction obtained after distillation under reduced pressure. The markets of modified paraffin such as chlorinated paraffin, fischer-Tropsch wax and special wax are more complex, and the products are various and miscellaneous. Such as automotive protective waxes for automotive interior cavities and chassis, electronics industry waxes for potting, impregnation and bonding, rubber protective waxes for rubber product additives, high strength film material waxes for precision casting material protective films, and the like.
Penetration refers to the depth of penetration of a standard needle into a sample under specified test conditions, and the hardness of the wax is characterized by the penetration, so that the penetration is an important performance index of the wax in industrial application, and the processing and the use of the wax are affected. The yield of the wax products in China is high, the import and export trade ratio is large, the variety and the richness of the products are high, and new requirements and challenges are provided for the detection of the penetration of the current wax products. And in paraffin modification production and research, penetration is an important index for measuring product quality, and the penetration detection is more complicated and difficult. The detection method for wax products mainly comprises American society for testing and materials ASTM D1321, german national standard DIN 51579, and the current detection method for paraffin penetration in China GB/T4985. The principle of the method is similar, after the heated sample is melted, the heated sample is poured into a former to be cooled in the air under the control condition, then the temperature of the sample is controlled to be the test temperature in a water bath, and a standard needle of a needle penetrometer is penetrated into the sample under the specified weight.
The main influencing factors of the penetration of wax products are carbon distribution and oil content. The smaller the carbon number of the carbon distribution composition, the higher the oil content, the larger the penetration, and the worse the stability of wax products along with the increase of the oil content, the oil precipitation phenomenon can also occur in a special high penetration sample, the penetration is obviously influenced, and the research and the application of the penetration quality control sample are restricted by the sample preparation and the stability. At present, the method is limited by oil precipitation of a sample with higher penetration, the stability is poor, and no penetration quality control sample for detecting the penetration of wax products is available in China.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a penetration quality control sample and a preparation method thereof, which meet the penetration detection quality control requirement of wax products.
The penetration quality control sample of the invention takes the quality of the quality control sample as a reference and comprises the following components: 60% -100% of paraffin components, 0% -20% of additives A and 0% -20% of additives B;
the paraffin component can be one or more of semi-refined paraffin, full-refined paraffin, industrial paraffin and crude paraffin; preferably a semi-refined paraffin sample;
the additive A is one or more of light white oil, industrial white oil or lubricating oil base oil; the white oil sample is industrial white oil;
the additive B is vacuum distillate oil of paraffin-based crude oil, and the vacuum distillate oil is one or more of any fractions within the distillation range of 350-550 ℃;
the preparation method of the penetration quality control sample comprises the following steps: and uniformly mixing the paraffin components, the additive A and the additive B in a heating mode, and then filling the mixture into a sample container for cooling and solidifying to obtain the penetration quality control sample.
In the method of the invention, the heating conditions are as follows: the heating temperature is generally higher than the melting point of paraffin wax, preferably 10-17 ℃ above the melting point, not higher than 95 ℃, preferably 40-60 minutes; after the components are completely melted, the heating temperature is maintained and stirring is sufficient, preferably at a speed of 50 to 1000 rpm, more preferably at a speed of 200 to 300 rpm, and for a period of preferably 10 to 20 minutes.
The penetration range of the penetration quality control sample is 0-25nm, and the penetration full detection range requirement can be met.
At present, for paraffin sample preparation, the penetration is increased mainly by adding white oil or lubricating oil base oil, but when the proportion of the white oil or the lubricating oil base oil added into paraffin is large, obvious oil separation phenomenon exists, and the penetration cannot be effectively increased. The vacuum distillate oil, or vaseline, is added to the paraffin, so that the penetration is not increased as expected, but the penetration is reduced, and the vacuum distillate oil is not added in the paraffin preparation process industry. The invention provides that the white oil and the vacuum distillate are mixed and added, and has very good effects: on one hand, the addition of the vacuum distillate well stabilizes the paraffin sample added with the white oil, greatly improves the addition amount of the white oil and widens the penetration quality control sample range; on the other hand, on the premise of adding white oil, the addition of the vacuum distillate does not cause abnormal decrease in penetration result. The invention provides a penetration quality control sample and a preparation method thereof, which meet the penetration quality control requirement of wax products, solve the problems of uniformity and stability of the penetration quality control sample, and prepare the penetration quality control sample within the penetration detection range (0-25 mm).
Detailed Description
The following detailed description of specific embodiments of the invention is, but it should be understood that the invention is not limited to specific embodiments. In order to achieve the aim of the invention, the quality control sample for verifying penetration has good uniformity and stability.
Example 1
350g of semi-refined paraffin wax are prepared and placed in a beaker which has been cleaned and dried.
100g of technical white oil was added, 50g of vacuum distillate (distillation range from 350 to 550 ℃ C.) was added, and the sample was melted at 15 ℃ above the melting point of semi-refined paraffin.
After the sample was completely melted, the heating temperature was maintained, the sample was sufficiently stirred at 300 rpm for 15 minutes.
And (5) standing at a melting temperature, and filling the sample into a clean sample bottle after standing, and cooling and solidifying. Penetration value was 18.7mm as measured according to GB/T4985.
Example 2
350g of semi-refined paraffin wax are prepared and placed in a beaker which has been cleaned and dried.
50g of white oil was added, 100g of vacuum distillate (distillation range from 350 to 450 ℃ C.) was added, and the sample was melted at 17 ℃ above the melting point of the semi-refined paraffin.
After the sample was completely melted, the heating temperature was maintained, the sample was sufficiently stirred at 400 rpm for 10 minutes.
And (5) standing at a melting temperature, and filling the sample into a clean sample bottle after standing, and cooling and solidifying. Penetration value was 16.2mm according to GB/T4985.
Example 3
400g of semi-refined paraffin wax are prepared and placed in a beaker which has been cleaned and dried.
100g of white oil was added, 100g of vacuum distillate (distillation range of 350-400 ℃ C.) was added, and the sample was melted at a temperature 10 ℃ above the melting point of the semi-refined paraffin.
After the sample was completely melted, the heating temperature was maintained, the sample was sufficiently stirred at 100 rpm for 25 minutes.
And (5) standing at a melting temperature, and filling the sample into a clean sample bottle after standing, and cooling and solidifying. Penetration value was 21.3mm according to GB/T4985.
Example 4
450g of semi-refined paraffin wax was prepared and placed in a beaker which had been cleaned and dried.
25g of light white oil was added, and the sample was melted at a temperature higher than the melting point of the semi-refined paraffin wax and at a temperature 15℃higher than the melting point of the semi-refined paraffin wax.
After the sample was completely melted, the heating temperature was maintained, and the sample was sufficiently stirred at a rotational speed of 300 rpm. Stirring time was 15 minutes.
And (5) standing at a melting temperature, and filling the sample into a clean sample bottle after standing, and cooling and solidifying. The penetration value was 9.6mm according to GB/T4985.
Example 5
350g of semi-refined paraffin wax are prepared and placed in a beaker which has been cleaned and dried.
100g of technical white oil was added, 50g of vacuum distillate (distillation range 400-550 ℃ C.) was added, and the sample was melted at 15 ℃ above the melting point of semi-refined paraffin.
After the sample was completely melted, the heating temperature was maintained, and the sample was sufficiently stirred at a rotational speed of 300 rpm. Stirring time was 15 minutes.
And (5) standing at a melting temperature, and filling the sample into a clean sample bottle after standing, and cooling and solidifying. Penetration value was 17.2mm according to GB/T4985.
Example 6
350g of semi-refined paraffin wax are prepared and placed in a beaker which has been cleaned and dried.
Adding 50g of white oil, adding 100g of vacuum distillate (distillation range of 400-460 ℃) and melting the sample under the condition that the semi-refined paraffin is higher than the melting point temperature,
the sample was melted at a temperature 15 ℃ above the melting point of the semi-refined paraffin wax.
After the sample was completely melted, the heating temperature was maintained, and the sample was sufficiently stirred at a rotational speed of 300 rpm. Stirring time was 15 minutes.
And (5) standing at a melting temperature, and filling the sample into a clean sample bottle after standing, and cooling and solidifying. The penetration value was 15.3mm according to GB/T4985.
Example 7
450g of fully refined paraffin wax was prepared and placed in a beaker which had been cleaned and dried.
25g of light white oil is added, the sample is melted under the condition that the semi-refined paraffin is higher than the melting point temperature,
the sample was melted at a temperature 15 ℃ above the melting point of the semi-refined paraffin wax.
After the sample was completely melted, the heating temperature was maintained, and the sample was sufficiently stirred at a rotational speed of 300 rpm. Stirring time was 15 minutes.
And (5) standing at a melting temperature, and filling the sample into a clean sample bottle after standing, and cooling and solidifying. Penetration value was 8.8mm according to GB/T4985.
Example 8
460g of coarse crystalline wax was prepared and placed in a beaker which had been cleaned and dried.
40g of light white oil is added, the sample is melted under the condition that the semi-refined paraffin is higher than the melting point temperature,
the sample was melted at a temperature 15 ℃ above the melting point of the semi-refined paraffin wax.
After the sample was completely melted, the heating temperature was maintained, and the sample was sufficiently stirred at a rotational speed of 300 rpm. Stirring time was 15 minutes.
And (5) standing at a melting temperature, and filling the sample into a clean sample bottle after standing, and cooling and solidifying. Penetration value was 7.4mm according to GB/T4985.
Example 9
And verifying uniformity and stability of the quality control sample. According to the method provided by the invention, the quality control sample with the full detection range (0-25 nmm) is prepared, the quality control requirement of the penetration detection of wax products is met, and the uniformity and stability of the penetration quality control sample are verified.
And (3) carrying out uniformity verification, namely according to CNAS-GL003:2018 'ability verification sample uniformity and stability evaluation guide', verifying sample uniformity verification, preparing 10 different samples, dividing the samples, randomly selecting 10 samples (marked as F1-F10) of each test sample, repeating the test for 2 times, and measuring penetration results. F test values were calculated by means of the sum of squares between samples, the mean square between samples, the sum of squares within samples, and the mean square within samples, see table 1. The test was found to be 3.02 at a 0.05 significant level F threshold F0.05 (9, 10). As can be seen from Table 2, the samples S1-S10 all have calculated F values less than the critical value, i.e., the precision test sample is uniform.
TABLE 1 test sample F test values
According to CNAS-GL003:2018, ability verification sample uniformity and stability evaluation guide, stability verification is carried out, after the good uniformity of the samples is determined, 6 samples after 10 test samples are separated are selected, and penetration results are measured at intervals of 30 days. The t-test values were calculated from the mean values measured in the uniformity test, the standard deviation and the mean values measured in the stability test, the standard deviation (table 2). The test can be checked that the critical value t0.05 (10) of the significant level t of 0.05 is 2.228, and the calculated t values of the samples S1-S10 are all smaller than the critical value, namely the precision test sample is stable.
Table 2 test sample t-test values
Claims (10)
1. A penetration quality control sample, characterized by: based on the quality of the quality control sample, the method comprises the following components: 60% -100% of paraffin components, 0% -20% of additives A and 0% -20% of additives B; the paraffin components are one or more of semi-refined paraffin, fully refined paraffin, industrial paraffin and crude paraffin; the additive A is one or more of light white oil, industrial white oil or lubricating oil base oil; the additive B is vacuum distillate of paraffin-based crude oil.
2. The quality control sample of claim 1, wherein: the additive B is one or more of any fractions in the distillation range of 350-550 ℃ of the vacuum distillate of the paraffin-based crude oil.
3. The quality control sample of claim 1, wherein: the paraffin component is semi-refined paraffin.
4. The quality control sample of claim 1, wherein: additive A is industrial white oil.
5. A method for preparing the penetration quality control sample according to any one of claims 1 to 4, comprising the following steps: and uniformly mixing the paraffin components, the additive A and the additive B in a heating mode, and then filling the mixture into a sample container for cooling and solidifying to obtain the penetration quality control sample.
6. The method according to claim 5, wherein: the heating conditions are as follows: the heating temperature is higher than the melting point of paraffin, and after each component is completely melted, the heating temperature is maintained, and the mixture is fully stirred.
7. The method according to claim 6, wherein: the stirring speed is 50-1000 rpm, and the stirring time is preferably 10-20 min.
8. The method according to claim 5, wherein: the heating temperature is 10-17 ℃ above the melting point and is not higher than 95 ℃, and the heating time is 40-60 minutes.
9. A penetration quality control sample according to any one of claims 1 to 4 having a penetration in the range of 0 to 25nm.
10. Use of a penetration quality control sample according to any one of claims 1 to 4 in the penetration detection of wax products.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111269918.2A CN116067722A (en) | 2021-10-29 | 2021-10-29 | Penetration quality control sample and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111269918.2A CN116067722A (en) | 2021-10-29 | 2021-10-29 | Penetration quality control sample and preparation method thereof |
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| Publication Number | Publication Date |
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| CN116067722A true CN116067722A (en) | 2023-05-05 |
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| CN202111269918.2A Pending CN116067722A (en) | 2021-10-29 | 2021-10-29 | Penetration quality control sample and preparation method thereof |
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2021
- 2021-10-29 CN CN202111269918.2A patent/CN116067722A/en active Pending
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Effective date of registration: 20240205 Address after: 100728 No. 22 North Main Street, Chaoyang District, Beijing, Chaoyangmen Applicant after: CHINA PETROLEUM & CHEMICAL Corp. Country or region after: China Applicant after: Sinopec (Dalian) Petrochemical Research Institute Co.,Ltd. Address before: 100728 No. 22 North Main Street, Chaoyang District, Beijing, Chaoyangmen Applicant before: CHINA PETROLEUM & CHEMICAL Corp. Country or region before: China Applicant before: DALIAN RESEARCH INSTITUTE OF PETROLEUM AND PETROCHEMICALS, SINOPEC Corp. |
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