CN114381074B - Standard substance with glass transition temperature lower than 100 ℃ and preparation method thereof - Google Patents
Standard substance with glass transition temperature lower than 100 ℃ and preparation method thereof Download PDFInfo
- Publication number
- CN114381074B CN114381074B CN202111625224.8A CN202111625224A CN114381074B CN 114381074 B CN114381074 B CN 114381074B CN 202111625224 A CN202111625224 A CN 202111625224A CN 114381074 B CN114381074 B CN 114381074B
- Authority
- CN
- China
- Prior art keywords
- glass transition
- transition temperature
- standard substance
- plasticizer
- stabilizer
- 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.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/04—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08L27/06—Homopolymers or copolymers of vinyl chloride
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
- C08K5/098—Metal salts of carboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/10—Esters; Ether-esters
- C08K5/12—Esters; Ether-esters of cyclic polycarboxylic acids
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/20—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Physics & Mathematics (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Investigating Or Analyzing Materials Using Thermal Means (AREA)
Abstract
The invention discloses a standard substance with a glass transition temperature lower than 100 ℃ and a preparation method thereof, belonging to the field of preparation of a standard substance. The glass transition temperature of the product can be adjusted according to actual requirements, the temperature range covers a low temperature range of-40-76 ℃, the performance is stable, and the storage and the transportation are convenient; the standard substance product has uniform and stable test result, and is suitable for being used as a standard sample for monitoring, detecting or calibrating a low glass transition temperature object. The invention also discloses a preparation method and application of the product.
Description
Technical Field
The invention relates to the field of preparation of a standard substance, in particular to a standard substance with a glass transition temperature lower than 100 ℃ and a preparation method thereof.
Background
The differential scanning calorimeter is used as important equipment for thermal analysis test, the temperature accuracy is an important equipment index, the accurate monitoring and the output of the test temperature of the instrument are the basic assurance of the test result of a sample, the existing calibration method adopts standard metal for testing, and the separate monitoring is carried out through different standard metal single-point monitoring temperatures. In practical testing, there are many test samples with melting points and glass transition temperatures lower than 100 ℃ at room temperature, and if the temperature of the temperature section cannot be monitored accurately, the accuracy of the test result cannot be ensured.
At present, several metals of gallium (Ga), indium (In), tin (Sn), lead (Pb) and zinc (Zn) are used as standard metals In the calibration specification JJG-936, and the equipment automatically selects the metals to be calibrated according to the needs. The melting point of the metal gallium (Ga) is 29.76 ℃ which is only slightly higher than the room temperature by 5-6 ℃, so that the metal gallium (Ga) can be easily melted off directly in use in summer at a higher temperature, the transition from solid state to liquid state can not be completed in an instrument, the metal is easily oxidized in the air to form an oxide film, and the oxide film can be continuously melted and solidified in storage; in addition, gallium can infiltrate the glass, so that the glass container is not suitable for storage. Therefore, gallium (Ga) is seldom selected during the calibration of the device, and the calibration starts from indium (In), but the melting point of indium is as high as 156.51 ℃, so that the indium is difficult to be used for the temperature monitoring calibration below 100 ℃.
The literature DSC calibration method of a differential scanning calorimeter refers to the calibration of biphenyl at a temperature below 100 ℃, wherein the melting point of biphenyl is 69.26 ℃ (non-glass temperature), and the melting heat is 120.4J/g, which meets the temperature requirement standard. However, biphenyl is a low-toxicity substance, has irritation to human, and the vapor can stimulate eyes, nose, trachea and the like, causes symptoms such as inappetence, vomiting and the like, and can damage the nervous system and digestive system of the human body to a certain extent. In addition, biphenyl is flammable, and has combustion danger when meeting high temperature, open fire or oxidant, so special storage is needed, and the biphenyl is complicated to process and can cause potential safety hazard.
CN112745568A provides a polymer-based melting temperature standard substance applied to DSC equipment calibration, where the standard substance has multiple melting temperatures, and compared with the existing metal standard substance, the standard substance has a heat flow change more similar to that of a polymer to be measured in the melting process, so that the melting temperature of the polymer can be measured more accurately. However, this solution does not address the polymer standard in the low temperature range (below 100 ℃) and the standard is measured by the melting point, not the glass transition temperature.
CN111198202a discloses a preparation method of a standard substance: taking cobalt foil with purity of more than 99% as a raw material, analyzing and confirming the components and the content of the raw material, and purifying the raw material by adopting a vacuum distillation method according to different boiling points and saturated vapor pressures of the components; performing uniformity primary detection of a specific magnitude on the purified raw materials, and screening out raw materials with uniform Curie temperature as candidate standard substances; and carrying out uniformity test, stability test, magnitude determination and uncertainty analysis on the candidate standard substances according to the metering requirements, and if the uniformity, stability and uncertainty meet the requirements, the magnitude is accurate and stable, and the standard substances accord with the metering characteristics, namely the cobalt curie point standard substances. However, the calibration temperature of cobalt foil 1116 ℃ is not applicable to the low temperature section as well; and the curie point is selected, and the glass transition temperature is not related.
Disclosure of Invention
Based on the defects existing in the prior art, the invention aims to provide a standard substance with the glass transition temperature lower than 100 ℃, the glass transition temperature of the product can be adjusted according to actual requirements, the temperature range covers a low temperature range of-40-76 ℃, the performance is stable, and the storage and the transportation are convenient; the standard substance product has uniform and stable test result, and is suitable for being used as a standard sample for monitoring, detecting or calibrating a low glass transition temperature object.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the standard substance with the glass transition temperature lower than 100 ℃ comprises the following components in parts by weight:
100 parts of PVC resin, 0.1 to 60 parts of plasticizer, 0.1 to 2 parts of lubricant and 0.1 to 4.5 parts of stabilizer;
the polymerization degree of the PVC resin is 1250-2600 according to GB/T5761-2018 test.
The glass transition temperature of the PVC resin is below 100 ℃, and according to actual requirements, the interaction force among PVC resin molecules can be effectively reduced by adding the plasticizer, the mobility of the PVC resin is improved, and the crystallinity of the PVC resin is reduced, so that the glass transition temperature of the PVC resin is changed, and the glass transition temperature of the PVC resin can cover a low-temperature range of-40-76 ℃.
Meanwhile, the inventor finds that the polymerization degree of the PVC resin is also in important connection with the performance of a final product, if the polymerization degree of the PVC resin is too low, the absorption capacity of a plasticizer is limited, the selectable range of the glass transition temperature of the product is narrowed, and if the plasticizer with the same addition amount is added, the product is likely to generate an oil-out phenomenon, the plasticizer content cannot be confirmed and can be directly emitted on the surface of a sample, the possibility of being polluted is increased, the instability in test application is enhanced, and the deviation of parallel test results is larger; if the polymerization degree of the PVC is too high, the density of the product is possibly reduced, the volatility is improved, the plasticizing time of the product on a plasticator is prolonged, the decomposition amount of the PVC resin in the process is increased, the decomposition amount of the PVC resin cannot be accurately evaluated, the instability of the result of the product when the PVC resin is applied to a test is further caused, the uniformity of the product is also not guaranteed, and if too much lubricant and stabilizer are added to guarantee the stability of the product, the content of the PVC resin matrix is possibly reduced, so that the stability and uniformity of the product are difficult to guarantee; according to the results of experiments conducted by the inventor, the PVC resin with the polymerization degree of 1250-2600 is used as a matrix to prepare the product with the best effect.
Preferably, the plasticizer is any one of p-benzene plasticizer, o-benzene plasticizer, polyester plasticizer, epoxy plasticizer, citrate plasticizer, vegetable oil based plasticizer, halogenated polyether fatty acid ester and adipic acid di (2-ethylhexyl) ester;
more preferably, the plasticizer is an o-benzene plasticizer;
more preferably, the plasticizer is dioctyl phthalate (DOP).
Experiments of the inventor show that the introduction of different plasticizers not only affects the glass transition temperature of the prepared standard substance, but also causes differences in substance uniformity and stability, and the mixing of different types of plasticizers can lead to drastic reduction in uniformity and stability of a product, so that a single pure type plasticizer is preferably used as a component; among the numerous plasticizer classes, the standard substance prepared with p-phthalic plasticizer DOP is optimal in terms of substance uniformity and stability.
Preferably, the polymerization degree of the PVC resin is more than or equal to 2000, and the standard substance with the glass transition temperature lower than 100 ℃ comprises the following components in parts by weight: 100 parts of PVC resin, 50-60 parts of plasticizer, 0.8-1.2 parts of lubricant and 4-4.5 parts of stabilizer.
As described above, the increase of the polymerization degree of the PVC resin leads to the improvement of the decomposition rate of the prepared standard substance product in the process of processing plastication, and the inventor experiments find that after adopting the PVC resin with the polymerization degree of 2000-2600 as a matrix and simultaneously adjusting the content of other components of the formula, particularly the content of the lubricant and the stabilizer, the uniformity and the stability of the obtained substance product are better than those of the product prepared by the PVC resin with the low polymerization degree.
On the other hand, the lubricant and the stabilizer are only used as the inhibiting components of decomposition phenomena in the PVC resin processing process, and further continuous addition of the lubricant and the stabilizer has limited improvement on the performance of the product, and on the contrary, the raw material waste is caused.
Preferably, the plasticizer absorption of the PVC resin is more than or equal to 24g per 100g, and the plasticizer absorption of the PVC resin is tested according to the GB/T3400-2002 standard.
The plasticizer absorption amount of the PVC resin greatly determines the types and the addition amount ranges of the available plasticizers and has certain relation with the polymerization degree, if the plasticizer absorption amount of the PVC resin is insufficient, the PVC resin can only select low-content plasticizers for matching in the specific polymerization degree range, so that the adjustable range of the glass transition temperature of a product standard substance is greatly shortened, and if more plasticizers are added, the obtained product possibly has an oil-out phenomenon.
Preferably, the stabilizer is at least one of methyl tin stabilizer, calcium-zinc composite stabilizer, stearic acid stabilizer, tribasic lead sulfate stabilizer and dibasic lead phosphite stabilizer;
more preferably, the stabilizer is a calcium-zinc compound stabilizer.
The stabilizer can effectively relieve the thermal decomposition effect of the PVC resin, and can also timely absorb hydrogen chloride generated by dechlorination of the PVC resin; wherein, the calcium-zinc compound stabilizer has the best effect, and the stabilizer also has a certain lubrication effect.
Preferably, the lubricant is at least one of polyethylene glycol type lubricant, stearic acid, magnesium stearate, fatty acid complex ester type lubricant and fatty alcohol carboxylic acid type lubricant;
more preferably, the lubricant is a polydiethanol-based lubricant.
The lubricant can prevent the PVC resin matrix from adhering to the charging barrel in the process of processing and injection molding, and can effectively inhibit the friction heating phenomenon between materials and prevent the thermal degradation phenomenon of the PVC resin; among them, the preferred polydiethanol lubricant is PEG-4000 which has the best lubrication effect, and the melting point is only 27 ℃, thus being more beneficial to preparing the standard substance with low glass transition temperature.
Another object of the present invention is to provide a method for preparing the standard substance having a glass transition temperature lower than 100 ℃, comprising the steps of:
(1) Uniformly mixing PVC resin, plasticizer, stabilizer and lubricant according to a proportion, and putting the mixture into a double-roller plasticator for mixing and plasticizing to obtain a plasticizing material;
(2) And placing the plasticizing material into a hydraulic press, preheating, pressing and cooling, and obtaining the standard substance with the glass transition temperature lower than 100 ℃ after press molding.
The preparation method of the PVC matrix atomization standard substance has simple operation steps and can realize industrial mass production.
Preferably, the temperature during the mixing in the step (1) is 60-80 ℃ and the time is 5-10 min;
preferably, the rate of mixing plasticization in the step (1) is 25-35 rpm;
preferably, the temperature during the preheating treatment in the step (2) is 160-170 ℃.
It is still another object of the present invention to provide the application of the standard substance with glass transition temperature lower than 100 ℃ in low glass transition temperature sample detection and result verification monitoring, detection instrument accuracy monitoring and calibration.
Compared with the existing standard substance, the standard substance with the glass transition temperature lower than 100 ℃ is easier to store and transport, is convenient to weigh and take, and can be used as a standard sample for detecting a glass transition temperature sample with the glass transition temperature lower than 100 ℃ or used for monitoring and calibrating the accuracy of a low temperature zone of detection equipment; the product has strong stability, safety and environmental protection, low environmental requirement during test use, and no special treatment is needed after use; the product has wide application range, and fills the blank of the polymer type standard substance applicable to the glass transition temperature lower than 100 ℃ in the prior art.
The invention has the beneficial effects that the invention provides the standard substance with the glass transition temperature lower than 100 ℃, the glass transition temperature of the product can be adjusted according to actual requirements, the temperature range covers a low temperature range of-40-76 ℃, the performance is stable, and the storage and the transportation are convenient; the standard substance product has uniform and stable test result, and is suitable for being used as a standard sample for monitoring, detecting or calibrating a low glass transition temperature object. The invention also provides a preparation method and application of the product.
Detailed Description
The present invention will be further described with reference to specific examples and comparative examples for better illustrating the objects, technical solutions and advantages of the present invention, and the object of the present invention is to be understood in detail, not to limit the present invention. All other embodiments, which can be made by those skilled in the art without the inventive effort, are intended to be within the scope of the present invention. The experimental reagents and instruments designed in the practice and comparative examples of the present invention are common reagents and instruments unless otherwise specified.
The information for the raw materials used in each example and comparative example is as follows:
PVC resin 1: PVCS-70M, a product produced by Ningbo Co., ltd, a polymerization degree of 1500, and a plasticizer absorption of 100g resin of more than or equal to 24g;
PVC resin 2: PVCS-85, a product produced by Ningbo Co., ltd, a polymerization degree of 2500, and a plasticizer absorption of 100g resin of more than or equal to 24g;
PVC resin 3: PVC S-65, a product produced by Ningbo Co., ltd, a degree of polymerization of 1000, and a plasticizer absorption of 100g resin of < 24g;
PVC resin 4: PVC S-90, a product produced by Ningbo industries, inc., has a degree of polymerization of 3200, and 100g of resin has a plasticizer absorption of more than or equal to 30g;
plasticizer 1: DOP, a o-benzene plasticizer, available from Tokyo chemical industries Co., ltd;
plasticizer 2: DPHP: o-benzene plasticizers available from weibian plasticizer limited, guangzhou;
plasticizer 3: TOTM, a polyester plasticizer available from Jia Australia Zhejiang environmental technologies Co., ltd;
lubricant 1: HONEOL PEG-4000 available from Jinchangsheng technologies, inc. of Guangzhou;
lubricant 2: commercial magnesium stearate;
stabilizer 1: the calcium-zinc composite stabilizer PKD 9051CZ is purchased from Dai Yikai Mi Sen chemical industry products Co., ltd;
stabilizer 2: methyl tin is commercially available.
Examples 1 to 12
In the embodiment of the standard substance with the glass transition temperature lower than 100 ℃, the preparation method of the product comprises the following steps:
(1) Adding PVC resin, plasticizer, stabilizer and lubricant into a high-speed mixer according to the proportion, mixing for 5-10 min at 60-80 ℃ until uniform, and then placing into a double-roll plasticator for mixing and plasticizing at the speed of 25-35 rpm to obtain a plasticizing material;
(2) Placing the plasticizing material into a hydraulic press, preheating, pressing and cooling, and obtaining the standard substance with the glass transition temperature lower than 100 ℃ after press molding; the temperature during the preheating treatment is 160-170 ℃.
The proportions of the raw materials used in each example are shown in Table 1.
Comparative examples 1 to 3
The products of comparative examples 1 to 3 differ from those of examples 1 to 12 only in the formulation or ratio of the component raw materials, the ratio of the raw materials being shown in Table 1.
TABLE 1
Effect example
In order to verify the glass transition temperature range of the standard substance with the glass transition temperature lower than 100 ℃ obtained in the embodiment of the invention, the products obtained in each embodiment and the comparative example are tested by DSC differential scanning calorimetry, and reference is made to ISO 11357-2:2020 test method is as follows:
(1) Weighing 5 mg-20 mg of standard substance to be tested as a test sample;
(2) Taking a differential scanning calorimeter as a testing instrument, taking two identical special testing sample dishes, taking one special testing sample dish as a sample dish and the other special testing sample dish as a reference dish, placing a testing sample in the sample dish, placing the sample dish into a sample holder of the differential scanning calorimeter by using tweezers, and covering an instrument protective cover;
(3) After nitrogen is introduced into a differential scanning calorimeter to be cleaned for 5min in advance, heating is started at a rate of 10K/min to a temperature which is about 30 ℃ higher than the glass transition termination temperature (Tefm) (heat history is eliminated) and then the temperature is kept constant for 5min;
(4) Cooling to about 50 ℃ below the intended glass transition temperature (Tefc) at a rate of 10K/min and then maintaining the temperature for 5min;
(5) The temperature was raised to the same temperature a second time at a rate of 10K/min.
(6) Cooling the instrument to room temperature, taking out the sample dish, checking whether the sample dish is deformed, whether the sample overflows, whether the quality of the sample dish is lost, opening the sample dish for inspection and the like;
(7) A DSC differential thermal test curve is derived and drawn, and the glass transition temperature T of the test sample is obtained by fitting g The method comprises the steps of carrying out a first treatment on the surface of the The results of each test are shown in Table 2.
TABLE 2
As can be seen from Table 2, the glass transition temperatures of the standard substances obtained in the examples of the present invention are all lower than 100 ℃, the temperature interval is large, and the application range is wide.
Based on the test, 12 samples with the same mass are randomly extracted from the products of the example and the comparative example respectively, and each sample is tested twice in parallel, and the uniformity verification is adopted according to the test data result "F value calculation of each product is carried out by a single-factor analysis of variance method, and the reference standard is CNAS-GL003-2018. Uniformity critical value F of each product according to the degree of freedom and the significance level 0.05(11,12) =2.72, if the statistic F < F 0.05(11,12) =2.72, then no significant difference between the same lot of each product is considered, i.e. the sample is homogeneous, if the F value is not less than the critical value F 0.05(11,12) =2.72, the product uniformity is insufficient, and the test results are shown in table 3.
TABLE 3 Table 3
As can be seen from the table, the standard substances obtained in each example below the glass transition temperature of 100℃have F values less than the critical value F 0.05(11,12) The products obtained in examples 7 and 8 have good uniformity, in which the polymerization degree of the PVC resin used in the products obtained in examples 3 and 4 is higher than 2000, and in order to ensure that the products do not significantly decompose during subsequent processing, a part of the stabilizer and the lubricant are additionally added, and the uniformity of the obtained product is higher than the products obtained in examples 4 and 5 by merely increasing the polymerization degree of the PVC resin or by additionally reinforcing the stabilizer or the lubricant alone, whereas it is difficult to maintain the uniformity of the product even if the excess stabilizer and the lubricant are added when the polymerization degree of the PVC resin is too high, as is known from the product of comparative example 3.
Based on the results, the stability of each example and comparative example product was evaluated by using an independent sample t-test method, and the reference standard is CNAS-GL003-2018. If the relation between the statistic t of a certain product and the significance level a and the degree of freedom f (f=n1+n2-2) is t < ta (f), the characteristic magnitude of the product is considered to have no significance change and high stability; otherwise, the characteristic value of the standard substance is considered to have changed significantly. The time interval of the test and inspection process is 0 month, 1 month, 3 months and 6 months, 6 samples of each group of products are randomly extracted at each time point, each sample is measured for 2 times in parallel, t value counted by test data is calculated, and the stability critical value t of each product is calculated 0.05(11) If t<t 0.05(11) The content value of the sample is not changed obviously, and the prepared standard substance is stable. The statistical value t is obtained by the following formula:
in order to ensure the accuracy of the average value and the standard deviation, n is more than or equal to 6;
if t<A critical value t with a degree of freedom of significance level a (typically a=0.05) of n-1 a(n-1) There was no significant difference between the average and standard/reference values, and the test and record results for each product are shown in table 4 below.
TABLE 4 Table 4
Calculated, critical value t a(11) The t values of the products of examples are less than the critical value =1.796, indicating good stability of the products, and similar to the results in table 3, the products obtained in examples 7 and 8, using PVC resins with a degree of polymerization > 2000 as component, are also better in stability than the corresponding products of examples 3 and 4, after adding additional lubricants and stabilizers.
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 (11)
1. The standard substance with the glass transition temperature lower than 100 ℃ is characterized by comprising the following components in parts by weight:
100 parts of PVC resin, 0.1-60 parts of plasticizer, 0.1-2 parts of lubricant and 0.1-4.5 parts of stabilizer;
the polymerization degree of the PVC resin is 1250-2600, and the plasticizer absorption amount of each 100g of the PVC resin is more than or equal to 24g; the plasticizer is any one of p-benzene plasticizer, o-benzene plasticizer, polyester plasticizer, epoxy plasticizer, citrate plasticizer, vegetable oil-based plasticizer, halogenated polyether fatty acid ester and adipic acid di (2-ethylhexyl) ester.
2. The standard substance having a glass transition temperature of less than 100 ℃ according to claim 1, wherein the plasticizer is a o-benzene plasticizer.
3. The standard substance with the glass transition temperature lower than 100 ℃ according to claim 1, wherein the polymerization degree of the PVC resin is more than or equal to 2000, and the standard substance with the glass transition temperature lower than 100 ℃ comprises the following components in parts by weight: 100 parts of PVC resin, 50-60 parts of plasticizer, 0.8-1.2 parts of lubricant and 4-4.5 parts of stabilizer.
4. The standard substance having a glass transition temperature of less than 100 ℃ according to claim 1, wherein the stabilizer is at least one of a methyl tin stabilizer, a calcium zinc compound stabilizer, a stearic acid stabilizer, a tribasic lead sulfate stabilizer, and a dibasic lead phosphite stabilizer.
5. The standard substance having a glass transition temperature of less than 100 ℃ according to claim 4, wherein the stabilizer is a calcium-zinc based composite stabilizer.
6. The standard substance having a glass transition temperature of less than 100 ℃ according to claim 1, wherein the lubricant is at least one of polyethylene glycol-based lubricant, stearic acid, magnesium stearate, fatty acid complex ester-based lubricant, and fatty alcohol carboxylic acid-based lubricant.
7. The standard substance having a glass transition temperature of less than 100 ℃ according to claim 6, wherein the lubricant is a polydiethanol-based lubricant.
8. The method for preparing a standard substance having a glass transition temperature of less than 100 ℃ according to any one of claims 1 to 7, comprising the steps of:
(1) Uniformly mixing PVC resin, plasticizer, stabilizer and lubricant according to a proportion, and putting the mixture into a double-roller plasticator for mixing and plasticizing to obtain a plasticizing material;
(2) And placing the plasticizing material into a hydraulic press, preheating, pressing and cooling, and obtaining the standard substance with the glass transition temperature lower than 100 ℃ after press molding.
9. The method for preparing a standard substance having a glass transition temperature lower than 100 ℃ as claimed in claim 8, wherein the temperature at the time of mixing in the step (1) is 60 to 80 ℃ for 5 to 10 minutes; the rate of mixing and plasticizing is 25-35 rpm.
10. The method for producing a glass transition temperature-lower than 100℃standard substance according to claim 8, wherein the temperature at the time of the preheating treatment in the step (2) is 160 to 170 ℃.
11. The use of the standard substance with a glass transition temperature lower than 100 ℃ according to any one of claims 1-7 in low glass transition temperature sample detection and result verification monitoring, detection instrument accuracy monitoring and calibration.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111625224.8A CN114381074B (en) | 2021-12-27 | 2021-12-27 | Standard substance with glass transition temperature lower than 100 ℃ and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111625224.8A CN114381074B (en) | 2021-12-27 | 2021-12-27 | Standard substance with glass transition temperature lower than 100 ℃ and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114381074A CN114381074A (en) | 2022-04-22 |
| CN114381074B true CN114381074B (en) | 2023-07-18 |
Family
ID=81196975
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111625224.8A Active CN114381074B (en) | 2021-12-27 | 2021-12-27 | Standard substance with glass transition temperature lower than 100 ℃ and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114381074B (en) |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105802055A (en) * | 2012-12-13 | 2016-07-27 | 苏州亨利通信材料有限公司 | Flame-retardant cable material for automotive wires |
| CN103289003B (en) * | 2013-05-23 | 2016-03-09 | 吴江市风尚鞋厂 | A kind of HPVC resin material and preparation method thereof |
| CN106519500A (en) * | 2016-11-09 | 2017-03-22 | 广东省汕头市质量计量监督检测所 | Standard substance for phthalic acid ester plasticizer measurement and preparation method of standard substance |
| KR20210087396A (en) * | 2020-01-02 | 2021-07-12 | 엘에스전선 주식회사 | Resin composition for sheath of cable having an excellent high-temperature and long-term oil resistance |
-
2021
- 2021-12-27 CN CN202111625224.8A patent/CN114381074B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN114381074A (en) | 2022-04-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Ahn et al. | Characterization and properties of LDPE film with gallic‐acid‐based oxygen scavenging system useful as a functional packaging material | |
| JP2019112640A (en) | Composition based on poly(arylene ether ketone) having improved properties | |
| WO2017088692A1 (en) | Reinforced flame resistant glass fiber pbt compound and preparation method thereof | |
| JP2984881B2 (en) | Stabilizer for plastic materials | |
| CN109021515B (en) | Polylactic acid 3D printing material and preparation method thereof | |
| DE102007033970A1 (en) | Use of tempered polyvinyl alcohols as stabilizer additive of PVC | |
| WO2017113283A1 (en) | Self-formaldehyde-scavenging heat-resistant abs material and preparation method therefor | |
| DE102007033971A1 (en) | Use of carboxyl-containing polyvinyl alcohols as stabilizer additive of PVC | |
| WO2012069285A1 (en) | Diisononyl terephthalate (dint) as softener for thermoplastic applications | |
| CN114381074B (en) | Standard substance with glass transition temperature lower than 100 ℃ and preparation method thereof | |
| CN106519500A (en) | Standard substance for phthalic acid ester plasticizer measurement and preparation method of standard substance | |
| WO2020107389A1 (en) | Anti-aging pvc composition, preparation method therefor and use thereof | |
| US4388410A (en) | Method to determine carbon black content | |
| DE102007026166A1 (en) | Thermoplastic shaping of polyvinyl alcohol for manufacturing granulates, foil, fibers or coating for use in pharmaceutical or cosmetic applications, involves accomplishing shaping in absence of extrusion additive | |
| BR112012015377B1 (en) | PROCESS FOR EXTRUDING A COMPOSITION | |
| US10759924B2 (en) | Surface-coated acetylacetone metal salt and method for producing same | |
| CN113429635A (en) | High-starch-content film-grade full-biodegradable masterbatch and preparation method thereof | |
| EP0081144A2 (en) | Heat-shapable sheet-like semi-finished products of fibre-reinforced polyethylene terephthalate | |
| TW272987B (en) | ||
| CN112341734A (en) | Environment-friendly nitrogen-containing organic zinc PVC heat stabilizer for transparent products and preparation method thereof | |
| JP2001040217A (en) | Stabilizer lubricant solid composition for chlorine- containing resin and chlorine-containing resin composition containing the same | |
| CN114196139B (en) | PVC matrix atomization standard substance and preparation method thereof | |
| CN105542407A (en) | Glass fiber reinforced PBT composition and preparation method and application thereof | |
| EP3904451A1 (en) | Polyvinylidene fluoride resin composition and molded body | |
| CN108395649A (en) | A kind of thermoplastic agent |
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 |