CN111117081A - Dynamic fully-vulcanized thermoplastic polyolefin elastomer and preparation method thereof - Google Patents
Dynamic fully-vulcanized thermoplastic polyolefin elastomer and preparation method thereof Download PDFInfo
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- 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
- C08L23/16—Elastomeric ethene-propene or ethene-propene-diene copolymers, e.g. EPR and EPDM rubbers
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- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
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- C08K2003/265—Calcium, strontium or barium carbonate
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- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- C08L2207/04—Thermoplastic elastomer
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Abstract
The invention relates to a dynamic fully-vulcanized thermoplastic polyolefin elastomer, which is prepared from the following raw materials in parts by weight: 75 parts by weight of EPDM 3092E; 10-12 parts by weight of PP-F401; 15-17 parts by weight of PP-K7726; 24-26 parts by weight of CaCO3(ii) a 1 part by weight of small materials; the weight part of the white oil is adjusted according to the hardness; the small material comprises a vulcanizing agent, an initiator, a vulcanization accelerator, a light stabilizer, a heat stabilizer, a lubricant and silicone master batches. Its strength, elasticity, heat resistance and compression resistanceThe long-term deformability is greatly improved, meanwhile, the fatigue resistance, the chemical resistance and the processing stability are obviously improved, and the rubber-plastic blending ratio can be changed in a larger range, so that the material has a larger adjustment margin on the performance. The blending technology of dynamic vulcanization is a breakthrough of TPV production technology. The method is not only suitable for TPV with EPDM/PP composition, but also suitable for various other rubber-plastic blending systems.
Description
[ technical field ] A method for producing a semiconductor device
The invention relates to the technical field of chemical industry, in particular to a dynamic fully-vulcanized thermoplastic polyolefin elastomer and a preparation method thereof.
[ background of the invention ]
Thermoplastic elastomer (TPE for short) is a high polymer material which has the characteristics of both rubber and thermoplastic plastics, has high rubber elasticity at normal temperature and can be plasticized and molded at high temperature, and is the third generation rubber following natural rubber and synthetic rubber.
At present, the types of thermoplastic elastomers have almost related to all fields of synthetic rubber, and have been developed into eight major types, such as styrene-type TPE (SBS, SIS, etc.), polyolefin-type TPE (tpo), diene-type TPE (TPB, TPI), polyvinyl chloride-type TPE (TPVC, TCPE), polyurethane-type TPE (tpu), polyester-type TPE (tpee), polyamide-type TPE (tpa), and organic fluorine-type TPE (tpf). The first four types of materials are general materials, the yield is over 85 percent, the styrene thermoplastic elastomer accounts for half of the materials, but the TPO is the fastest-developed product.
Thermoplastic polyolefin elastomer (TPO) is an elastomer material composed of two components, rubber and polyolefin. Typical rubber components are ethylene propylene rubber (EPDM), Nitrile Butadiene Rubber (NBR) and butyl rubber (IIR); the polyolefin components mainly comprise PP, PE, ethylene-vinyl acetate copolymer resin (EVA) and the like.
The major methods for producing TPO In the world currently include three processes, namely, mechanical blending (CompunedTPO), reactor synthesis (In-situ TPO) and dynamic full vulcanization (dynamic Vulcanization).
The mechanical blending method is the earliest developed production process with the most mature technology, and ethylene propylene rubber and polypropylene are blended by a double-screw extruder; the reactor synthesis method is a newly developed production process, firstly introducing propylene to generate homopolymerized propylene in a reactor, and then introducing ethylene and propylene to generate an ethylene-propylene copolymer; dynamic full-cure is a process whereby fully vulcanized rubber particles are uniformly dispersed in a continuous matrix of polyolefin thermoplastic material by a dynamic vulcanization and blending process. The rubber component content of the thermoplastic polyolefin elastomer produced by a mechanical blending method and a reactor synthesis method is lower than 50 percent, and the thermoplastic polyolefin elastomer can only be used as high-impact polypropylene in the fields of automobiles (bumpers), household appliances and the like; the thermoplastic polyolefin elastomer (TPV) produced by the dynamic full vulcanization method has the rubber component content of 60-70 percent, has the comprehensive performance equivalent to ethylene propylene vulcanized rubber, and can partially replace the ethylene propylene diene vulcanized rubber to be used for manufacturing various rubber products such as automobile accessories, building materials, electronic and electrical products, industrial products, consumer goods and the like. However, the thermoplastic polyolefin elastomer produced by the dynamic full vulcanization method can also show different properties according to different formulas and preparation processes. At present, the domestic TPV production is only maintained at a middle-low level, and the scientific research and production level needs to be improved.
[ summary of the invention ]
In order to solve the above problems, an object of the present invention is to provide a dynamically fully-vulcanized thermoplastic polyolefin elastomer having high heat resistance, a large compression set resistance, and further improved material properties, and a method for producing the same.
In order to achieve the purpose, the invention adopts the technical scheme that:
a dynamically fully vulcanized thermoplastic polyolefin elastomer is prepared by the following raw materials:
75 parts by weight of EPDM 3092E;
10-12 parts by weight of PP-F401;
15-17 parts by weight of PP-K7726;
24-26 parts by weight of CaCO3;
1 part by weight of small materials;
the weight part of the white oil is adjusted according to the hardness;
the small material comprises a vulcanizing agent, an initiator, a vulcanization accelerator, a light stabilizer, a heat stabilizer, a lubricant and silicone master batches.
The dynamically fully vulcanized thermoplastic polyolefin elastomer in the present invention is further configured as: the small materials comprise the following components in percentage by weight:
1-1.5 parts by weight of a vulcanizing agent;
0.1 part by weight of an initiator;
1-1.5 parts by weight of a vulcanization accelerator;
0.1 to 0.3 parts by weight of a light stabilizer;
0.1-0.2 parts by weight of a heat stabilizer;
0.1-0.2 parts by weight of a slip agent;
1.0-3.0 parts by weight of silicone master batch.
A process for preparing a dynamically fully vulcanized thermoplastic polyolefin elastomer comprising the steps of:
(1) EPDM3092E, PP-F401, PP-K7726 and CaCO in the raw material as defined in claim 1 or 23Sequentially adding into a stirring pan, stirring, kneading for 1-2min after adding EPDM3092E, kneading for 1-2min after adding PP-F401 and PP-K7726, and kneading for CaCO3Kneading for 1-2min after the materials are put into the reactor, and then discharging;
(2) putting the stirred materials into a 95 machine, and granulating to form an intermediate;
(3) and secondly batching by using a kneading pot: feeding the intermediate into a kneading pot, adding the small material as described in claim 1 or 2 while kneading, and kneading for 0.5min after the addition is completed;
(4) and putting the prepared materials for the second time into a 65-machine for granulation, wherein a TPV special type is selected for a screw structure of the 65-machine, and white oil is added in the granulation process to adjust the hardness of the materials.
Compared with the prior art, the invention has the following beneficial effects: the TPV prepared by the dynamic fully-vulcanized thermoplastic polyolefin elastomer and the preparation method thereof is the EPDM particles which are completely crosslinked in a phase state and are dispersed in a PP matrix. This is a system that differs greatly in composition, structure and mechanical blending processes and reactor synthesis processes. In TPV, the rubber component is fully crosslinked, so that the strength, elasticity, heat resistance and compression permanent deformation resistance of the material are greatly improved compared with the former two methods, meanwhile, the fatigue resistance, chemical resistance and processing stability are obviously improved, and the rubber-plastic blending ratio can be changed in a larger range, so that the material has a larger adjustment range in performance. The blending technology of dynamic vulcanization is a breakthrough of TPV production technology. The method is not only suitable for TPV with EPDM/PP composition, but also suitable for various other rubber-plastic blending systems.
TPV effectively overcomes the fatal weakness of the conventional TPO product, namely the defects of heat resistance, compression deformation resistance and the like, and the material performance is further improved and is far better than that of thermoplastic resin. The compression deformation can be controlled below 40 percent, the use temperature can reach 100-120 ℃, and rubber products which require not strict compression deformation and low use temperature can completely replace rubber; for rubber products with strict environmental protection requirements, no toxicity and sanitation, the rubber products are not TPV Mohs.
[ detailed description ] embodiments
The dynamic fully vulcanized thermoplastic polyolefin elastomer and the preparation method thereof according to the present invention will be described in further detail by way of specific examples.
The disclosure may be understood more readily by reference to the following detailed description of preferred embodiments of the invention and the examples included therein. In the following specification and claims, reference will be made to a number of terms which shall be defined to have the following meanings. When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or as a range of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when a range of "1 to 5" is disclosed, the described range should be interpreted to include the ranges "1 to 4," "1 to 3," "1-2 and 4-5," "1-3 and 5," and the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.
A dynamically fully vulcanized thermoplastic polyolefin elastomer is prepared by the following raw materials:
75 parts by weight of EPDM 3092E;
10-12 parts by weight of PP-F401;
15-17 parts by weight of PP-K7726;
24-26 parts by weight of CaCO3;
1 part by weight of small materials;
the weight part of the white oil is adjusted according to the hardness;
the small material comprises a vulcanizing agent, an initiator, a vulcanization accelerator, a light stabilizer, a heat stabilizer, a lubricant and silicone master batches.
The small materials comprise the following components in percentage by weight:
1-1.5 parts by weight of a vulcanizing agent;
0.1 part by weight of an initiator;
1-1.5 parts by weight of a vulcanization accelerator;
0.1 to 0.3 parts by weight of a light stabilizer;
0.1-0.2 parts by weight of a heat stabilizer;
0.1-0.2 parts by weight of a slip agent;
1.0-3.0 parts by weight of silicone master batch.
A process for preparing a dynamically fully vulcanized thermoplastic polyolefin elastomer comprising the steps of:
(1) EPDM3092E, PP-F401, PP-K7726 and CaCO in the raw material as defined in claim 1 or 23Sequentially adding into a stirring pan, stirring, kneading for 1-2min after adding EPDM3092E, kneading for 1-2min after adding PP-F401 and PP-K7726, and kneading for CaCO3Kneading for 1-2min after the materials are put into the reactor, and then discharging;
(2) putting the stirred materials into a 95 machine, and granulating to form an intermediate;
(3) and secondly batching by using a kneading pot: feeding the intermediate into a kneading pot, adding the small material as described in claim 1 or 2 while kneading, and kneading for 0.5min after the addition is completed;
(4) and putting the prepared materials for the second time into a 65-machine for granulation, wherein a TPV special type is selected for a screw structure of the 65-machine, and white oil is added in the granulation process to adjust the hardness of the materials.
And (3) separating water from the granulated water-containing particles by a particle drier, removing water on the surfaces of the particles by hot air, removing chips by a separating screen, conveying the particles to a particle storage bin by an air conveyor, simultaneously introducing hot air for drying, and dedusting tail gas discharged by drying and air conveying to reach the standard and discharge. The dried granular materials are weighed by a hopper scale from a storage bin, then are packaged into a multilayer composite paper bag coated with a damp-proof and water-proof coating material by a bagging machine, and are conveyed to a tray of a tray lifter after passing through a bag sewing machine, a shaping conveyor, a metal detector and a printer, and then finished products of 1 ton per tray are conveyed to a finished product warehouse by a forklift.
The EPDM3092E is ethylene propylene diene monomer. PP-F401 and PP-K7726 are polypropylene with different labels. White oil is a mixture of refined liquid hydrocarbons obtained from petroleum, mainly a mixture of saturated naphthenic and paraffinic hydrocarbons, and is obtained by atmospheric and reduced pressure fractionation, solvent extraction and dewaxing, and hydrorefining of crude oil. The white oil is mainly used as a lubricant to improve the compatibility of two phases. The white oil is not particularly limited in this application and is commercially available. Preferably a white oil according to standard Q/MSH 32-2009.
The detection shows that the specifications and indexes of the prepared product are as follows:
item | 6420AN | 7320AN | 8020AN | 8720AN | 4010DN | 5010DN |
Hardness (Shao) | 64A | 73A | 80A | 87A | 40D | 50D |
Specific gravity of | 0.97 | 0.98 | 0.97 | 0.96 | 0.95 | 0.94 |
Tensile Strength (MPa) | 6.9 | 8.3 | 11.0 | 15.9 | 19.0 | 27.6 |
Elongation at Break (%) | 400 | 375 | 450 | 530 | 600 | 600 |
Modulus of 100% (Mpa) | 2.3 | 3.2 | 4.8 | 6.9 | 8.6 | 10.0 |
Permanent set (%) | 10 | 14 | 20 | 33 | 48 | 61 |
Compression set (%) | 30 | 34 | 39 | 36 | 44 | 47 |
Brittleness temperature (. degree.C.) | -60 | -63 | -63 | -61 | -57 | -34 |
The above-mentioned embodiments are merely illustrative of the principles and effects of the present invention, and some embodiments may be used, not restrictive; it should be noted that, for those skilled in the art, various changes and modifications can be made without departing from the inventive concept of the present invention, and these changes and modifications belong to the protection scope of the present invention.
Claims (3)
1. A dynamically fully vulcanized thermoplastic polyolefin elastomer characterized by: the preparation raw materials comprise:
75 parts by weight of EPDM 3092E;
10-12 parts by weight of PP-F401;
15-17 parts by weight of PP-K7726;
24-26 parts by weight of CaCO3;
1 part by weight of small materials;
the weight part of the white oil is adjusted according to the hardness;
the small material comprises a vulcanizing agent, an initiator, a vulcanization accelerator, a light stabilizer, a heat stabilizer, a lubricant and silicone master batches.
2. The dynamically fully vulcanized thermoplastic polyolefin elastomer according to claim 1, wherein: the small materials comprise the following components in percentage by weight:
1-1.5 parts by weight of a vulcanizing agent;
0.1 part by weight of an initiator;
1-1.5 parts by weight of a vulcanization accelerator;
0.1 to 0.3 parts by weight of a light stabilizer;
0.1-0.2 parts by weight of a heat stabilizer;
0.1-0.2 parts by weight of a slip agent;
1.0-3.0 parts by weight of silicone master batch.
3. A process for preparing a dynamically fully vulcanized thermoplastic polyolefin elastomer, characterized in that: the method comprises the following steps:
(1) EPDM3092E, PP-F401, PP-K7726 and CaCO in the raw material as defined in claim 1 or 23Sequentially adding into a stirring pan, stirring, kneading for 1-2min after adding EPDM3092E, kneading for 1-2min after adding PP-F401 and PP-K7726, and kneading for CaCO3Kneading for 1-2min after the materials are put into the reactor, and then discharging;
(2) putting the stirred materials into a 95 machine, and granulating to form an intermediate;
(3) and secondly batching by using a kneading pot: feeding the intermediate into a kneading pot, adding the small material as described in claim 1 or 2 while kneading, and kneading for 0.5min after the addition is completed;
(4) and putting the prepared materials for the second time into a 65-machine for granulation, wherein a TPV special type is selected for a screw structure of the 65-machine, and white oil is added in the granulation process to adjust the hardness of the materials.
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Cited By (1)
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CN112606498A (en) * | 2020-12-26 | 2021-04-06 | 北京宇阳泽丽防水材料有限责任公司 | Bondable TPO waterproof coiled material, and preparation method and application thereof |
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Cited By (2)
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CN112606498A (en) * | 2020-12-26 | 2021-04-06 | 北京宇阳泽丽防水材料有限责任公司 | Bondable TPO waterproof coiled material, and preparation method and application thereof |
CN112606498B (en) * | 2020-12-26 | 2023-09-22 | 河北宇阳泽丽防水材料有限公司 | Bondable TPO waterproof coiled material, preparation method and application thereof |
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