CN112745577B - Rotary rheometer standard substance for high-molecular polymer and preparation method and application thereof - Google Patents
Rotary rheometer standard substance for high-molecular polymer and preparation method and application thereof Download PDFInfo
- Publication number
- CN112745577B CN112745577B CN202011628818.XA CN202011628818A CN112745577B CN 112745577 B CN112745577 B CN 112745577B CN 202011628818 A CN202011628818 A CN 202011628818A CN 112745577 B CN112745577 B CN 112745577B
- Authority
- CN
- China
- Prior art keywords
- high molecular
- standard substance
- rotational rheometer
- antioxidant
- viscosity
- 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
- 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
- G01N11/00—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties
-
- 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
- G01N11/14—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by moving a body within the material by using rotary bodies, e.g. vane
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- 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
- G01N2011/0006—Calibrating, controlling or cleaning viscometers
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention provides a rotational rheometer standard substance for a high molecular polymer, and a preparation method and application thereof. The rotational rheometer standard substance for the high molecular polymer comprises the following components in parts by weight: polypropylene resin: 93.3-96.5 parts; viscosity stabilizer: 3-5 parts; hindered phenol antioxidant: 0.1-0.4 part; phosphite ester antioxidant: 0.1-0.4 part; ultraviolet absorber: 0.1-0.4 part; lubricant: 0.1 to 0.5 portion. The standard substance of the rotational rheometer for the high molecular polymer, which is prepared by the invention, has small viscosity change within the temperature range of 190-230 ℃, can calibrate the rotational rheometer within the temperature range of more than 190 ℃, and improves the detection precision of the instrument on the high molecular polymer.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a rotational rheometer standard substance for a high polymer, and a preparation method and application thereof.
Background
The viscosity is characterized by the degree of deformation resistance of the fluid and is an important rheological property parameter of the fluid. The magnitude of the viscosity depends primarily on the fluid itself and secondarily on external factors such as temperature, pressure, shear rate and the length of time over which the shearing action takes place. Fluids can be classified as newtonian and non-newtonian according to whether viscosity is related to shear rate at the time of measurement. The viscosity of the non-newtonian fluid changes with the change of the shear rate, and the non-newtonian fluid needs to pay attention to rheological property parameters such as storage modulus, loss modulus loss angle and the like when the viscosity is tested, and is generally analyzed by a rotational rheometer.
The use of the standard ISO 6721-2010 in the rotational rheometer mentions that the rheometer should be periodically calibrated, and the rheometers on the market have various brands and models and large performance differences, so that the complete calibration of the rheometer with the non-Newtonian fluid standard substance is required. At present, no calibration standard specially used for the rotational rheometer exists in China, and the calibration standard is known by referring to the JJG 1002-2005 rotational viscometer calibration standard, and calibration parameters of the viscometer mainly have instrument repeatability and stability and all need to be tested by using certified standard substances. At present, the domestic viscosity standard substance is mainly solution type Newtonian fluid (the viscosity constant value temperature is 20 ℃). Van Wanjie et al developed four melt non-Newtonian fluid standard substances with different nominal values by using polydimethylsiloxane as a raw material, and the test temperature was 50 ℃. The internationally issued standard substances for calibrating the rotational rheometer are SRM 2490 and SRM 2491, and the application range of the two substances is 0-50 ℃; the temperature range of the polymer melt viscosity test is generally between 120 and 320 ℃.
Therefore, it is desirable to develop a standard substance with different viscosity values in a higher temperature range.
Disclosure of Invention
The invention aims to overcome the defect that the difference between the calibration temperature of the non-Newtonian fluid viscosity standard substance for the rotational rheometer in the prior art and the test temperature of the viscosity of the high molecular polymer is larger, and provides the rotational rheometer standard substance for the high molecular polymer. The standard substance of the rotational rheometer for the high molecular polymer, which is prepared by the invention, has small viscosity change within the temperature range of 190-230 ℃, can calibrate the rotational rheometer within the temperature range of more than 190 ℃, and improves the detection precision of the instrument on the high molecular polymer.
The invention also aims to provide a preparation method of the standard substance for the rotational rheometer for the high molecular polymer.
The invention also aims to provide the application of the rotary rheometer standard substance for the high-molecular polymer in calibrating the rotary rheometer.
In order to achieve the purpose, the invention adopts the following technical scheme:
a rotational rheometer standard substance for high molecular polymers comprises the following components in parts by weight:
the inventor of the invention discovers through a large number of experimental studies that PP (polypropylene) has good heat resistance, aging resistance, high mechanical strength and long-term stability, is suitable for preparing a melt viscosity standard substance, and can improve the initial viscosity value of the material by adding a viscosity stabilizer into the polypropylene standard substance, so that the degradation of the material is reduced in the processing process; meanwhile, the viscosity stabilizer is cooperated with an antioxidant and a light stabilizer, so that the viscosity change range of the standard substance in the detection temperature range of the high molecular polymer is small, the stability of the viscosity can be kept in a wider temperature range, the reproducibility is good, and the calibration of an instrument and the detection of the viscosity of the polymer are facilitated.
Preferably, the rotational rheometer standard substance for the high molecular polymer comprises the following components in parts by weight:
preferably, the viscosity stabilizer is a 2-ethylhexanoate-based viscosity stabilizer.
Further preferably, the viscosity stabilizer is potassium 2-ethylhexanoate.
Preferably, the ultraviolet absorber is one or a combination of several of hindered amine light stabilizer and benzotriazole light stabilizer.
Preferably, the lubricant is one or a combination of more of an EBS lubricant, a stearate lubricant and an ester lubricant.
The preparation method of the rotational rheometer standard substance for the high molecular polymer is characterized by comprising the following steps:
uniformly mixing polypropylene resin, hindered phenol antioxidant, phosphite antioxidant, ultraviolet absorbent, lubricant and viscosity stabilizer, and then extruding and injection molding to obtain the rotational rheometer standard substance for the high molecular polymer.
Preferably, the temperature of the extrusion is 190-210 ℃.
Preferably, the extrusion may be performed using a twin screw extruder.
Preferably, the parameters of the twin-screw extruder are: the rotating speed of the screw is 350-450 r/min; the length-diameter ratio of the screw is 40-48: 1.
The application of the standard substance of the rotational rheometer for the high molecular polymer in calibrating the rotational rheometer is also within the protection scope of the invention.
Preferably, the temperature range of the calibration is 190-230 ℃.
Compared with the prior art, the invention has the following beneficial effects:
the viscosity stabilizer is added into the polypropylene standard substance, so that the initial viscosity value of the material can be improved, and the degradation of the material is reduced in the processing process; meanwhile, the viscosity stabilizer is cooperated with an antioxidant and a light stabilizer, so that the viscosity change range of the standard substance in the detection temperature range of the high molecular polymer is small, the stability of the viscosity can be kept in a wider temperature range, the reproducibility is good, and the calibration of an instrument and the detection of the viscosity of the polymer are facilitated. The standard substance of the rotational rheometer for the high molecular polymer, which is prepared by the invention, has small viscosity change within the temperature range of 190-230 ℃, can calibrate the rotational rheometer within the temperature range of more than 200 ℃, and improves the detection precision of the instrument on the high molecular polymer.
Detailed Description
The present invention is further illustrated by the following specific examples, which are not intended to limit the invention in any way. Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated. Unless otherwise indicated, reagents and materials used in the present invention are commercially available.
The embodiment of the invention adopts the following raw materials:
polypropylene resin: k9015, available from Yangzi petrochemical company, Inc.;
polyamide resin: PA66, HY2800A, available from Jiangsu Haiyang chemical fibers, Inc.;
viscosity stabilizer: 2-Ethyl hexanoate POTASSIUM, 15% POTASSIUM HEX-CEM, available from OMG, USA;
antioxidant 1010 available from basf (china) ltd;
antioxidant 168: purchased from basf (china) ltd;
ultraviolet absorber: hindered amine light stabilizer, CHIMASSORB 944FDL, available from basf (china) ltd;
lubricant: EBS, KAOWAX EB-G, purchased from Japan flower King.
Examples 1 to 6
According to the formulation in table 1, the rotational rheometer standard for high molecular polymers was prepared as follows:
adding polypropylene resin, hindered phenol antioxidant 1010, phosphite antioxidant 168, ultraviolet absorbent, lubricant and viscosity stabilizer into a high-speed mixer, uniformly mixing, and extruding in a double-screw extruder, wherein the temperature of the double-screw extruder is 190-210 ℃, the rotating speed of a screw is 350-450 r/min, and the length-diameter ratio of the screw is 40: 1.
TABLE 1 content of each component (parts by weight) of the rotational rheometer standard for high molecular polymers in the example in the calibration rotational rheometer
| Examples | 1 | 2 | 3 | 4 | 5 |
| Polypropylene resin | 93.3 | 94 | 94.4 | 95.5 | 96.5 |
| Viscosity stabilizer | 5 | 5 | 4.5 | 3.5 | 3 |
| Antioxidant 1010 | 0.4 | 0.4 | 0.3 | 0.2 | 0.1 |
| Antioxidant 168 | 0.4 | 0.4 | 0.2 | 0.3 | 0.1 |
| Ultraviolet absorber | 0.4 | 0.1 | 0.2 | 0.3 | 0.2 |
| Lubricant agent | 0.5 | 0.1 | 0.4 | 0.2 | 0.1 |
Comparative example 1
This comparative example is compared with example 4, except that the polypropylene resin was replaced with a polyamide resin.
Comparative example 2
This comparative example is different from example 4 in that no viscosity stabilizer is added.
The performance of the standard substance for a rotational rheometer for a high molecular polymer prepared in the above examples and comparative examples was tested, and the specific test items and test methods were as follows:
and (3) viscosity testing:
1. sample preparation: preparing a polypropylene sheet into a wafer with the diameter of 25mm and the thickness of 2nm by using an engraving machine;
2. and (3) testing: and (3) carrying out steady-state frequency scanning and dynamic frequency scanning on the polypropylene wafer by using a rotary rheometer, wherein the frequency range is 0.01-250 rad/s, the test temperature is 190 ℃, the stabilization time is 60s, and the diameter of the clamp is 25 mm. And recording the intersection point of the viscosity, the storage modulus and the loss modulus of the sample.
The test results are shown in table 2, table 2 and table 3.
Table 2 results of viscosity test of samples prepared in examples and comparative examples
| Viscosity (Pa.s) | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Comparative example 2 |
| 190℃ | 3058 | 3115 | 3026 | 2973 | 2883 | 2834 |
| 210℃ | 2874 | 2912 | 2783 | 2720 | 2623 | 2267 |
| 230℃ | 2702 | 2723 | 2561 | 2488 | 2387 | 1768 |
Table 2
| Viscosity (Pa.s) | Comparative example 1 |
| 270℃ | 626 |
| 290℃ | 532 |
| 310℃ | 441 |
TABLE 3 results of viscosity (190 ℃) measurements at different storage times for samples prepared in examples and comparative examples
| Viscosity (Pa.s) | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Comparative example 1 | Comparative example 2 |
| Day 0 | 3058 | 3115 | 3026 | 2973 | 2883 | 626 | 2834 |
| 1 day | 3055 | 3117 | 3027 | 2976 | 2886 | 607 | 2823 |
| 1 month | 3063 | 3110 | 3020 | 2965 | 2878 | 576 | 2796 |
| 3 months old | 3065 | 3121 | 3017 | 2960 | 2865 | 518 | 2734 |
The data results in tables 1 to 3 show that the rotational rheometer standard substance for the high molecular polymer prepared in each embodiment of the invention has viscosity reduced by about 6% to 13% when the viscosity test temperature is increased by 20 ℃, the viscosity change is small within 3 months of storage life, and the change rate is within +/-1%; comparative example 1 since the polyamide resin is used, when the viscosity test temperature is increased by 20 ℃, the viscosity is reduced by about 17%, and the viscosity of the standard substance is reduced by more than 15% within 3 months of storage life, which affects the calibration result; in comparative example 2, since no viscosity stabilizer is added, when the viscosity testing temperature is increased by 20 ℃, the viscosity is reduced by about 20-22%, the viscosity change is small within 3 months of storage life, and the change rate is about 3%.
The above-mentioned embodiments, objects, technical solutions and advantages of the present invention are further described in detail, it should be understood that the above-mentioned embodiments are only examples of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (7)
1. A rotational rheometer standard substance for high molecular polymers is characterized by comprising the following components in parts by weight:
polypropylene resin: 93.3-96.5 parts;
viscosity stabilizer: 3-5 parts;
hindered phenol antioxidant: 0.1-0.4 part;
phosphite ester antioxidant: 0.1-0.4 part;
ultraviolet absorber: 0.1-0.4 part;
lubricant: 0.1-0.5 part;
the polypropylene resin is K9015, the viscosity stabilizer is potassium 2-ethyl hexanoate, the hindered phenol antioxidant is antioxidant 1010, and the phosphite antioxidant is antioxidant 168; the ultraviolet absorber is CHIMASSORB 944FDL which is a hindered amine light stabilizer.
2. The rotational rheometer standard material for high molecular polymers according to claim 1, comprising the following components in parts by weight:
polypropylene resin: 94-95.5 parts;
viscosity stabilizer: 3.5-4.5 parts;
hindered phenol antioxidant: 0.2-0.3 part;
phosphite ester antioxidant: 0.2-0.3 part;
ultraviolet absorber: 0.2-0.3 part;
lubricant: 0.2 to 0.4 portion.
3. The rotational rheometer standard substance according to claim 1, wherein the lubricant is one or a combination of EBS lubricant, stearate lubricant, and ester lubricant.
4. The method for preparing a rotational rheometer standard substance for a high molecular polymer according to any one of claims 1 to 3, comprising the steps of:
uniformly mixing polypropylene resin, hindered phenol antioxidant, phosphite antioxidant, ultraviolet absorbent, lubricant and viscosity stabilizer, and then extruding and injection molding to obtain the standard substance of the rotational rheometer for the high molecular polymer.
5. The method for preparing the rotational rheometer standard substance for high molecular polymers according to claim 4, wherein the extrusion temperature is 190 to 210 ℃.
6. Use of a rotary rheometer standard according to any one of claims 1 to 3 for high molecular weight polymers in calibrating a rotary rheometer.
7. The use of a rotational rheometer standard according to claim 6 for calibrating a rotational rheometer, wherein the calibration temperature is in the range of 190-230 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011628818.XA CN112745577B (en) | 2020-12-30 | 2020-12-30 | Rotary rheometer standard substance for high-molecular polymer and preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011628818.XA CN112745577B (en) | 2020-12-30 | 2020-12-30 | Rotary rheometer standard substance for high-molecular polymer and preparation method and application thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112745577A CN112745577A (en) | 2021-05-04 |
| CN112745577B true CN112745577B (en) | 2022-08-30 |
Family
ID=75650731
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011628818.XA Active CN112745577B (en) | 2020-12-30 | 2020-12-30 | Rotary rheometer standard substance for high-molecular polymer and preparation method and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112745577B (en) |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103344476B (en) * | 2013-05-31 | 2016-01-20 | 中国计量科学研究院 | Non-newtonian fluid viscosity standard substance and preparation method thereof |
| KR102344135B1 (en) * | 2015-06-30 | 2021-12-29 | 스미토모 긴조쿠 고잔 가부시키가이샤 | Heat ray shielding film, transparent substrate with heat ray shielding, automobile, building material, dispersion, mixed composition, dispersion preparation method, dispersion liquid, dispersion liquid preparation method |
| CN105088862A (en) * | 2015-08-13 | 2015-11-25 | 合肥龙发包装有限公司 | Surface sizing agent improving water resistance of paperboard |
| CN105504490A (en) * | 2015-12-22 | 2016-04-20 | 成都新柯力化工科技有限公司 | Method for preparing ecological plastic |
-
2020
- 2020-12-30 CN CN202011628818.XA patent/CN112745577B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN112745577A (en) | 2021-05-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Stange et al. | Rheological behavior of blends from a linear and a long-chain branched polypropylene | |
| US11453776B2 (en) | Polylactic acid 3D printing material and preparation method thereof | |
| CN112745577B (en) | Rotary rheometer standard substance for high-molecular polymer and preparation method and application thereof | |
| CN114034605B (en) | Melt flow rate standard substance and preparation method thereof | |
| EP3757152A1 (en) | Controlled rheology modified mixed-plastic polyethylene blend | |
| Rettler et al. | Water uptake of poly (2-N-alkyl-2-oxazoline) s: influence of crystallinity and hydrogen-bonding on the mechanical properties | |
| Ayoub et al. | Effect of plasticizers and polymer blends for processing softwood kraft lignin as carbon fiber precursors | |
| DK201700367A1 (en) | A hydrophilic polymer material | |
| Dooher et al. | Environmental stress cracking of polymers: Case studies from industry (ABS and LDPE) | |
| Arakawa et al. | Enhancement of melt elasticity for poly (3‐hydroxybutyrate‐co‐3‐hydroxyvalerate) by addition of weak gel | |
| Timoteo et al. | Stress cracking and photodegradation behavior of polycarbonate. The combination of two major causes of polymer failure | |
| AU2019100615A4 (en) | Polylactic acid 3D printing material and preparation method thereof | |
| Parisi et al. | Alternative Use of the Sentmanat Extensional Rheometer to Investigate the Rheological Behavior of Industrial Rubbers at very Large Deformations | |
| CN114605737B (en) | PP (Polypropylene) base standard sample for detecting bending performance and preparation method thereof | |
| KR20230026891A (en) | Evaluation method for degaradability of polyemr | |
| CN111234456A (en) | Anti-aging and mildew-proof polyether-ether-ketone material and preparation method thereof | |
| Kang et al. | Extrusion coating performances of iPP/LDPE blends | |
| Xian-Wu et al. | The effect of polypropylene/polyamide 66 blending modification on melt strength and rheologic behaviors of polypropylene | |
| CN114605750B (en) | Plastic Vicat softening temperature standard sample and preparation method thereof | |
| CN114773732B (en) | Standard sample for notch impact strength detection and preparation method thereof | |
| Zoller et al. | Extensional viscosity measurements and characterization of poly (vinyl chloride‐co‐vinyl acetate) plastisols and foams | |
| Plog et al. | Investigation of Pharmaceutical Hot-Melts via Simultaneous Rheometry and Polarization Microscopy | |
| KR102602710B1 (en) | Thermoplastic molding composition and automobile parts comprising molded article of the same | |
| CN117247629A (en) | PP (polypropylene) base standard sample for detecting ball indentation hardness and preparation method thereof | |
| Ferreira et al. | Homogeneous poly (L‐lactic acid)/chitosan blended films |
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 |