CN116084054A - Polypropylene medical monofilament with high knotting strength and preparation method thereof - Google Patents
Polypropylene medical monofilament with high knotting strength and preparation method thereof Download PDFInfo
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- CN116084054A CN116084054A CN202211646427.XA CN202211646427A CN116084054A CN 116084054 A CN116084054 A CN 116084054A CN 202211646427 A CN202211646427 A CN 202211646427A CN 116084054 A CN116084054 A CN 116084054A
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- -1 Polypropylene Polymers 0.000 title claims abstract description 199
- 239000004743 Polypropylene Substances 0.000 title claims abstract description 193
- 229920001155 polypropylene Polymers 0.000 title claims abstract description 193
- 238000002360 preparation method Methods 0.000 title abstract description 10
- 239000011347 resin Substances 0.000 claims abstract description 134
- 229920005989 resin Polymers 0.000 claims abstract description 134
- 229920013716 polyethylene resin Polymers 0.000 claims abstract description 67
- 229920002943 EPDM rubber Polymers 0.000 claims abstract description 50
- 238000000034 method Methods 0.000 claims abstract description 43
- 238000001816 cooling Methods 0.000 claims description 64
- 239000000843 powder Substances 0.000 claims description 54
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 32
- 230000001678 irradiating effect Effects 0.000 claims description 32
- 239000002994 raw material Substances 0.000 claims description 25
- 229920001684 low density polyethylene Polymers 0.000 claims description 24
- 239000004702 low-density polyethylene Substances 0.000 claims description 24
- 238000009998 heat setting Methods 0.000 claims description 19
- 239000008187 granular material Substances 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 16
- 229910052757 nitrogen Inorganic materials 0.000 claims description 16
- 239000002245 particle Substances 0.000 claims description 16
- 238000010298 pulverizing process Methods 0.000 claims description 16
- 238000012216 screening Methods 0.000 claims description 16
- 150000001993 dienes Chemical class 0.000 claims description 10
- 238000005096 rolling process Methods 0.000 claims description 10
- 238000007599 discharging Methods 0.000 claims description 9
- 238000005469 granulation Methods 0.000 claims description 9
- 230000003179 granulation Effects 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 229920000092 linear low density polyethylene Polymers 0.000 claims description 7
- 239000004707 linear low-density polyethylene Substances 0.000 claims description 7
- 238000007710 freezing Methods 0.000 claims description 4
- 230000008014 freezing Effects 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 12
- 238000006243 chemical reaction Methods 0.000 abstract description 8
- 125000000864 peroxy group Chemical group O(O*)* 0.000 abstract description 8
- 239000004698 Polyethylene Substances 0.000 abstract description 6
- 239000000654 additive Substances 0.000 abstract description 6
- 229920000573 polyethylene Polymers 0.000 abstract description 6
- 239000003607 modifier Substances 0.000 abstract description 4
- 230000008569 process Effects 0.000 description 14
- 238000012360 testing method Methods 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 8
- 239000000835 fiber Substances 0.000 description 6
- 238000000465 moulding Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- 229920000181 Ethylene propylene rubber Polymers 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229920000098 polyolefin Polymers 0.000 description 2
- 238000009864 tensile test Methods 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 206010061592 cardiac fibrillation Diseases 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002600 fibrillogenic effect Effects 0.000 description 1
- 238000002513 implantation Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 229920002725 thermoplastic elastomer Polymers 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 230000002087 whitening effect Effects 0.000 description 1
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/06—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyolefin as constituent
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/28—Treatment by wave energy or particle radiation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/04—Homopolymers or copolymers of ethene
- C08J2323/06—Polyethene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/04—Homopolymers or copolymers of ethene
- C08J2323/08—Copolymers of ethene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/10—Homopolymers or copolymers of propene
- C08J2323/12—Polypropene
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Abstract
The application discloses a medical polypropylene monofilament with high knotting strength and a preparation method thereof, wherein the monofilament comprises the following components: 70-90 parts by weight of polypropylene resin; 5-15 parts by weight of pre-irradiation polyethylene resin; 5-15 parts by weight of pre-irradiation polypropylene resin; 3-8 parts by weight of ethylene propylene diene monomer rubber; and the sum of the weight parts of the polypropylene resin, the pre-irradiation polyethylene resin, the pre-irradiation polypropylene resin and the ethylene propylene diene monomer is 100. The preparation method comprises the steps of introducing peroxy groups into macromolecular chains of polyethylene resin and polypropylene resin in a pre-irradiation mode, and decomposing the peroxy groups at high temperature to generate free radicals through banburying, so as to initiate the reaction among pre-irradiation polypropylene, pre-irradiation polyethylene and ethylene propylene diene monomer, thereby preparing the polypropylene grafted modifier. The method does not introduce additives, ensures the cleanness of materials and meets the medical requirements.
Description
Technical Field
The invention relates to the field of monofilaments in general, in particular to a medical polypropylene monofilament with high knotting strength and a preparation method thereof.
Background
The polypropylene monofilament has the advantages of biological inertia, low cost and convenient processing and forming, and is widely applied to medical implantation materials such as surgical suture lines, medical patches and the like. However, the polypropylene resin has higher isotacticity, easy crystallization and easy fibrillation in the monofilament forming process, so that the polypropylene monofilament has the defects of high rigidity, insufficient toughness, easy stress whitening in the bending process, low knotting strength and the like. The raw material polypropylene resin is blended with toughening materials such as low-density polyethylene, ethylene propylene rubber, thermoplastic elastomer and the like, so that the toughness of the polypropylene monofilament can be effectively improved, and the comprehensive performance of the monofilament can be improved. However, on one hand, the polypropylene resin is incompatible with other toughening materials, and the interfacial bonding force is low; on the other hand, the raw materials prepared by direct blending are difficult to ensure uniform dispersion, so that the monofilament structure is not uniform, and the product performance is not stable. The compatibilization technology can effectively improve the interaction force of the polypropylene resin and the toughening material, ensure the uniformity of raw materials, and improve the performance of the monofilament and the stability of the product.
The polypropylene compatibilizer is generally divided into physical compatibilizer and chemical compatibilizer, wherein the physical compatibilizer realizes multicomponent compatibilizer by adding a third component compatibilizer, and the method has a certain effect on improving the compatibility of the polymer, but has limited improvement effect, and the product stability is difficult to control because the addition amount of the compatibilizer is small. The chemical compatibilization is to covalently bond the molecular chain of the polypropylene resin with the molecular chain of other toughening materials through chemical reaction, so that the interfacial compatibility between the polypropylene resin and the toughening materials is improved. In addition, as the molecular chain of the toughening material is covalently connected with the molecular chain of the polypropylene, the dispersion phase of the toughening resin is smaller, the uniformity of the system is higher, and the performance and stability of the product are improved.
However, polypropylene resin and toughening material are mainly polyolefin materials, generally show chemical reaction inertia, and can realize chemical compatibilization by adding auxiliary additives such as initiator and the like. Typically such additives are rendered biologically toxic and thus materials prepared by such methods are difficult to apply in the biomedical field. Therefore, how to realize chemical compatibilization on polyolefin under clean conditions, so as to prepare polypropylene medical monofilaments with high knotting strength and stable performance is a difficult problem to be solved urgently.
Disclosure of Invention
In view of the foregoing drawbacks or shortcomings of the prior art, it would be desirable to provide a high knot strength polypropylene medical monofilament and a method of making the same.
In a first aspect, a medical polypropylene monofilament with high knotting strength is provided, and the medical polypropylene monofilament comprises the following components:
70-90 parts by weight of polypropylene resin;
5-15 parts by weight of pre-irradiation polyethylene resin;
5-15 parts by weight of pre-irradiation polypropylene resin;
3-8 parts by weight of ethylene propylene diene monomer rubber;
and the sum of the weight parts of the polypropylene resin, the pre-irradiation polyethylene resin, the pre-irradiation polypropylene resin and the ethylene propylene diene monomer is 100.
In a second aspect, the preparation method of the high knotting strength polypropylene medical monofilament comprises the following steps:
step one: adding polyethylene resin granules into an ultralow temperature pulverizer, cooling by liquid nitrogen, reducing the temperature to-150 ℃, pulverizing and screening at low temperature to obtain polyethylene resin powder with the particle size lower than 10 meshes, and pre-irradiating the polyethylene resin powder to obtain pre-irradiated polyethylene resin;
step two: adding polypropylene resin granules into an ultralow temperature pulverizer, cooling by liquid nitrogen, reducing the temperature to-50 ℃, pulverizing and screening at low temperature to obtain polypropylene resin powder with the particle size lower than 10 meshes, and pre-irradiating the polypropylene resin powder to obtain pre-irradiated polypropylene resin;
step three: adding the pre-irradiated polyethylene resin and the pre-irradiated polypropylene resin into an internal mixer according to the proportion, banburying for 10-15 minutes at 190 ℃, discharging, cooling and granulating to obtain a polypropylene-polyethylene-ethylene propylene diene monomer graft;
step four: adding the polypropylene-polyethylene-ethylene propylene diene monomer rubber graft and polypropylene resin into a high-speed mixer according to a proportion, uniformly stirring, extruding and granulating at 120-190 ℃ by using a co-rotating double-screw extruder, and carrying out traction and cooling granulation to obtain a high knotting strength polypropylene medical monofilament raw material;
step five: and extruding the high knotting strength medical polypropylene monofilament raw material by a single screw extruder at 280 ℃/290 ℃/290 ℃ to form, cooling, stretching, heat setting and rolling to obtain the high knotting strength medical polypropylene monofilament.
The beneficial effects of the invention are that:
1. the preparation method comprises the steps of introducing peroxy groups into macromolecular chains of polyethylene resin and polypropylene resin in a pre-irradiation mode, and decomposing the peroxy groups at high temperature to generate free radicals through banburying, so as to initiate the reaction among pre-irradiation polypropylene, pre-irradiation polyethylene and ethylene propylene diene monomer, thereby preparing the polypropylene grafted modifier. The method has the advantages that no additive is introduced, the material cleanness is ensured, and the medical requirements are met;
2. because the polyethylene resin and the ethylene propylene diene monomer molecular chain are grafted with the polypropylene long chain, the compatibility with the polypropylene matrix resin is improved, and raw materials with uniform components can be prepared, so that the prepared polypropylene medical monofilament product has stable performance and high knotting strength.
Drawings
Other features, objects and advantages of the present application will become more apparent upon reading of the detailed description of non-limiting embodiments, made with reference to the following drawings, in which:
fig. 1 is a flowchart of a method for preparing a high knot strength polypropylene medical monofilament in this example.
Detailed Description
The present application is described in further detail below with reference to the drawings and examples. It is to be understood that the specific embodiments described herein are merely illustrative of the invention and are not limiting of the invention. It should be noted that, for convenience of description, only the portions related to the invention are shown in the drawings.
It should be noted that, in the case of no conflict, the embodiments and features in the embodiments may be combined with each other. The present application will be described in detail below with reference to the accompanying drawings in conjunction with embodiments.
The embodiment provides a medical polypropylene monofilament with high knotting strength, which comprises the following components:
70-90 parts by weight of polypropylene resin;
5-15 parts by weight of pre-irradiation polyethylene resin;
5-15 parts by weight of pre-irradiation polypropylene resin;
3-8 parts by weight of ethylene propylene diene monomer rubber;
and the sum of the weight parts of the polypropylene resin, the pre-irradiation polyethylene resin, the pre-irradiation polypropylene resin and the ethylene propylene diene monomer is 100.
In the embodiment, the toughness of the polypropylene resin can be effectively improved by blending the polypropylene resin with the low-density polyethylene resin, the ethylene propylene rubber resin and other polymers with flexible molecular chains, so that the knotting strength of the polypropylene monofilament is improved; and the polypropylene resin and other polymers are not compatible, the obtained monofilament raw materials are uneven, the stability of the monofilament performance is seriously affected, and the pre-irradiated polyethylene resin and the pre-irradiated polypropylene resin are used for generating reaction with ethylene propylene diene monomer rubber to prepare the polypropylene grafted modifier.
Further, the pre-irradiation polyethylene resin is prepared by the following method:
freezing and crushing granular polyethylene resin to obtain polyethylene resin powder,
the method comprises the steps of pre-irradiating polyethylene resin powder in an air atmosphere by using 60Co or an electron accelerator as an irradiation source, wherein the pre-irradiation dose range is 10-40kGy.
In the embodiment, the polyethylene resin is formed into powder, then certain pre-irradiation is carried out, peroxy groups are introduced into a macromolecular chain of the polyethylene resin in a pre-irradiation mode, and in the subsequent banburying process, the peroxy groups are decomposed at high temperature to generate free radicals, so that the reaction between the pre-irradiation polyethylene and ethylene propylene diene monomer is initiated.
Further, the pre-irradiation polypropylene resin is prepared by the following method:
freezing and crushing granular polypropylene resin to obtain polyethylene resin powder,
the method comprises the steps of pre-irradiating polypropylene resin powder in an air atmosphere by using 60Co or an electron accelerator as an irradiation source, wherein the pre-irradiation dose range is 5-15kGy.
In the embodiment, the polypropylene resin is formed into powder, then certain pre-irradiation is carried out, peroxy groups are introduced into a polypropylene resin macromolecular chain in a pre-irradiation mode, and in the subsequent banburying process, the peroxy groups are decomposed at high temperature to generate free radicals, so that the reaction between the pre-irradiation polypropylene and ethylene propylene diene monomer is initiated, and the polypropylene grafted modifier is prepared through the reaction between the pre-irradiation polypropylene, the pre-irradiation polyethylene and ethylene propylene diene monomer.
Further, the polyethylene resin is one or two of low density polyethylene and linear low density polyethylene;
the polypropylene is isotactic polypropylene, and the isotacticity is more than 97%;
the mass percentage content of diene components in the ethylene propylene diene monomer is 5-8%.
The polypropylene resin, the polyethylene resin and the ethylene propylene diene monomer rubber adopted in the embodiment are all of medical grade and are used for preparing medical monofilaments; and as the polypropylene long chain is grafted on the polyethylene resin and the ethylene propylene diene monomer molecular chain, the compatibility with the polypropylene matrix resin is improved, and raw materials with uniform components can be prepared, so that the prepared polypropylene medical monofilament product has stable performance and high knotting strength.
Referring to fig. 1, the embodiment also provides a method for preparing a medical polypropylene monofilament with high knotting strength, which comprises the following steps:
step one: adding polyethylene resin granules into an ultralow temperature pulverizer, cooling by liquid nitrogen, reducing the temperature to-150 ℃, pulverizing and screening at low temperature to obtain polyethylene resin powder with the particle size lower than 10 meshes, and pre-irradiating the polyethylene resin powder to obtain pre-irradiated polyethylene resin;
step two: adding polypropylene resin granules into an ultralow temperature pulverizer, cooling by liquid nitrogen, reducing the temperature to-50 ℃, pulverizing and screening at low temperature to obtain polypropylene resin powder with the particle size lower than 10 meshes, and pre-irradiating the polypropylene resin powder to obtain pre-irradiated polypropylene resin;
step three: adding the pre-irradiated polyethylene resin and the pre-irradiated polypropylene resin into an internal mixer according to the proportion, banburying for 10-15 minutes at 190 ℃, discharging, cooling and granulating to obtain a polypropylene-polyethylene-ethylene propylene diene monomer graft;
step four: adding the polypropylene-polyethylene-ethylene propylene diene monomer rubber graft and polypropylene resin into a high-speed mixer according to a proportion, uniformly stirring, extruding and granulating at 120-190 ℃ by using a co-rotating double-screw extruder, and carrying out traction and cooling granulation to obtain a high knotting strength polypropylene medical monofilament raw material;
step five: and extruding the high knotting strength medical polypropylene monofilament raw material by a single screw extruder at 280 ℃/290 ℃/290 ℃ to form, cooling, stretching, heat setting and rolling to obtain the high knotting strength medical polypropylene monofilament.
The preparation method provided by the embodiment can obtain the polypropylene medical monofilament with high knotting strength, the knotting strength of the prepared monofilament reaches 2.9-6.7cN/dtex, and other additives are not introduced, so that the preparation method can be more applied to the field of medical monofilaments.
Further, the step of pre-irradiating the polyethylene resin powder to obtain a pre-irradiated polyethylene resin comprises the steps of:
using 60Co as an irradiation source, and pre-irradiating polyethylene resin powder by using gamma rays in an air atmosphere, wherein the pre-irradiation dose range is 10-40kGy, so as to obtain pre-irradiated polyethylene resin;
or adopting an electron accelerator as an irradiation source, and pre-irradiating polyethylene resin powder by using beta rays under the air atmosphere, wherein the pre-irradiation dose range is 10-40kGy, so as to obtain pre-irradiated polyethylene resin;
the step of pre-irradiating the polypropylene resin powder to obtain pre-irradiated polypropylene resin comprises the following steps:
using 60Co as an irradiation source, and pre-irradiating the polypropylene resin powder by using gamma rays in an air atmosphere, wherein the pre-irradiation dose range is 5-15kGy, so as to obtain pre-irradiated polypropylene resin;
or adopting an electron accelerator as an irradiation source, and pre-irradiating the polypropylene resin powder by using beta rays in an air atmosphere, wherein the pre-irradiation dose range is 5-15kGy, so as to obtain the pre-irradiated polypropylene resin.
The steps show the mode of preparing the pre-irradiated polyethylene resin and the pre-irradiated polypropylene resin, and the irradiation mode of radioactivity or the irradiation mode of an electron accelerator can be adopted.
Further, the weight ratio of the polypropylene resin, the pre-irradiation polyethylene resin, the pre-irradiation polypropylene resin and the ethylene propylene diene monomer in the third step and the fourth step is (70-90): (5-15): (5-15): (3-8).
Further, the polyethylene resin is one or two of low density polyethylene and linear low density polyethylene;
the polypropylene is isotactic polypropylene, and the isotacticity is more than 97%;
the mass percentage content of diene components in the ethylene propylene diene monomer is 5-8%.
The polypropylene resin, the polyethylene resin and the ethylene propylene diene monomer rubber adopted in the embodiment are all of medical grade and are used for preparing medical monofilaments; and as the polypropylene long chain is grafted on the polyethylene resin and the ethylene propylene diene monomer molecular chain, the compatibility with the polypropylene matrix resin is improved, and raw materials with uniform components can be prepared, so that the prepared polypropylene medical monofilament product has stable performance and high knotting strength.
In the fifth step, the cooling method is water cooling, the cooling temperature is 12 ℃, the stretching method is secondary stretching, the primary stretching ratio is 4, the secondary stretching ratio is 1.2, and the heat setting temperature is 160 ℃.
In the fifth step, the diameter of the medical polypropylene monofilament with high knotting strength is 0.05-0.3mm.
Five examples and five comparative examples are given below, and monofilament breaking strength, linear density of monofilament, knotting strength test of monofilament of examples and comparative examples were performed according to the above-described method:
example 1
Step one: adding the low-density polyethylene resin granules into an ultralow temperature pulverizer, cooling by using liquid nitrogen, reducing the temperature to-150 ℃, and pulverizing and screening at low temperature to obtain low-density polyethylene resin powder with the particle size of less than 10 meshes. Using 60Co as an irradiation source, and pre-irradiating the low-density polyethylene resin powder by using gamma rays in an air atmosphere, wherein the pre-irradiation dose is 10kGy, so as to obtain pre-irradiated low-density polyethylene resin;
step two: adding the polypropylene resin granules into an ultralow temperature pulverizer, cooling by liquid nitrogen, reducing the temperature to-50 ℃, and pulverizing and screening at low temperature to obtain polypropylene resin powder with the particle size lower than 10 meshes. Using 60Co as an irradiation source, and pre-irradiating the polypropylene resin powder by using gamma rays under the air atmosphere, wherein the pre-irradiation dose is 5kGy, so as to obtain pre-irradiated polypropylene resin;
step three: and (3) adding the pre-irradiated low-density polyethylene resin prepared in the first step and the pre-irradiated polypropylene resin prepared in the second step into an internal mixer according to the mass ratio of 5:5:3, banburying for 15 minutes at 190 ℃, discharging, cooling and granulating to obtain the polypropylene-polyethylene-ethylene propylene diene monomer rubber graft, wherein the mass percentage of diene components in the ethylene propylene diene monomer rubber is 5%.
Step four: and (3) adding the polypropylene resin and the polypropylene-polyethylene-ethylene propylene diene monomer rubber graft obtained in the step (III) into a high-speed mixer according to the mass ratio of 87:13, uniformly stirring, extruding and granulating at 120-190 ℃ by using a co-rotating double-screw extruder, and carrying out traction and cooling granulation to obtain the medical polypropylene monofilament raw material with high knotting strength.
Step five: extruding and molding the high knotting strength polypropylene medical monofilament raw material obtained in the step four by a single screw extruder under the condition of (280 ℃/290 ℃/290 ℃), cooling, stretching, heat setting and rolling to obtain the high knotting strength polypropylene medical monofilament with the diameter of 0.20mm, wherein the specific process adopts a water cooling mode, the cooling temperature is 12 ℃, the stretching method is secondary stretching, the primary stretching ratio is 4, the secondary stretching ratio is 1.2, and the heat setting temperature is 160 ℃.
Example two
Step one: adding the linear low-density polyethylene resin granules into an ultralow temperature pulverizer, cooling by using liquid nitrogen, reducing the temperature to-150 ℃, and pulverizing and screening at low temperature to obtain linear polyethylene resin powder with the particle size of less than 10 meshes. Using an electron accelerator as an irradiation source, and pre-irradiating linear polyethylene resin powder with beta rays under the air atmosphere, wherein the pre-irradiation dose is 40kGy, so as to obtain pre-irradiated linear low-density polyethylene resin;
step two: adding the polypropylene resin granules into an ultralow temperature pulverizer, cooling by liquid nitrogen, reducing the temperature to-50 ℃, and pulverizing and screening at low temperature to obtain polypropylene resin powder with the particle size lower than 10 meshes. Using an electron accelerator as an irradiation source, and pre-irradiating polypropylene resin powder with beta rays under the air atmosphere, wherein the pre-irradiation dose is 15kGy, so as to obtain pre-irradiated polypropylene resin;
step three: and (3) adding the pre-irradiated linear low-density polyethylene resin prepared in the first step and the pre-irradiated polypropylene resin prepared in the second step into an internal mixer according to the mass ratio of 15:10:5, banburying for 10 minutes at 190 ℃, discharging, cooling and granulating to obtain a polypropylene-polyethylene-ethylene propylene diene monomer graft, wherein the mass percentage of diene components in the ethylene propylene diene monomer is 8%.
Step four: and (3) adding the polypropylene resin and the polypropylene-polyethylene-ethylene propylene diene monomer rubber graft obtained in the step (III) into a high-speed mixer according to the mass ratio of 70:30, uniformly stirring, extruding and granulating at 120-190 ℃ by using a co-rotating double-screw extruder, and carrying out traction and cooling granulation to obtain the medical polypropylene monofilament raw material with high knotting strength.
Step five: extruding and molding the high knotting strength polypropylene medical monofilament raw material obtained in the step four by a single screw extruder under the condition of (280 ℃/290 ℃/290 ℃), cooling, stretching, heat setting and rolling to obtain the high knotting strength polypropylene medical monofilament with the diameter of 0.20mm, wherein the specific process adopts a water cooling mode, the cooling temperature is 12 ℃, the stretching method is secondary stretching, the primary stretching ratio is 4, the secondary stretching ratio is 1.2, and the heat setting temperature is 160 ℃.
Example III
Step one: adding the low-density polyethylene resin granules into an ultralow temperature pulverizer, cooling by using liquid nitrogen, reducing the temperature to-150 ℃, and pulverizing and screening at low temperature to obtain low-density polyethylene resin powder with the particle size of less than 10 meshes. Using 60Co as an irradiation source, and pre-irradiating the low-density polyethylene resin powder by using gamma rays in an air atmosphere, wherein the pre-irradiation dose is 20kGy, so as to obtain pre-irradiated low-density polyethylene resin;
step two: adding the polypropylene resin granules into an ultralow temperature pulverizer, cooling by liquid nitrogen, reducing the temperature to-50 ℃, and pulverizing and screening at low temperature to obtain polypropylene resin powder with the particle size lower than 10 meshes. Using 60Co as an irradiation source, and pre-irradiating the polypropylene resin powder by using gamma rays under the air atmosphere, wherein the pre-irradiation dose is 10kGy, so as to obtain pre-irradiated polypropylene resin;
step three: and (3) adding the pre-irradiated polyethylene resin prepared in the first step and the pre-irradiated polypropylene resin prepared in the second step into an internal mixer according to the mass ratio of 7:5:8, banburying the mixture at 190 ℃ for 12 minutes, and discharging, cooling and granulating the mixture to obtain a polypropylene-polyethylene-ethylene propylene diene monomer graft, wherein the mass percentage of diene components in the ethylene propylene diene monomer is 5%.
Step four: and (3) adding the polypropylene resin and the polypropylene-polyethylene-ethylene propylene diene monomer rubber graft obtained in the step (III) into a high-speed mixer according to the mass ratio of 80:20, uniformly stirring, extruding and granulating at 120-190 ℃ by using a co-rotating double-screw extruder, and carrying out traction and cooling granulation to obtain the medical polypropylene monofilament raw material with high knotting strength.
Step five: extruding and molding the high knotting strength polypropylene medical monofilament raw material obtained in the step four by a single screw extruder under the condition of (280 ℃/290 ℃/290 ℃), cooling, stretching, heat setting and rolling to obtain the high knotting strength polypropylene medical monofilament with the diameter of 0.20mm, wherein the specific process adopts a water cooling mode, the cooling temperature is 12 ℃, the stretching method is secondary stretching, the primary stretching ratio is 4, the secondary stretching ratio is 1.2, and the heat setting temperature is 160 ℃.
Example IV
Step one: adding the low-density polyethylene resin granules into an ultralow temperature pulverizer, cooling by using liquid nitrogen, reducing the temperature to-150 ℃, and pulverizing and screening at low temperature to obtain low-density polyethylene resin powder with the particle size of less than 10 meshes. Using 60Co as an irradiation source, and pre-irradiating the low-density polyethylene resin powder by using gamma rays in an air atmosphere, wherein the pre-irradiation dose is 20kGy, so as to obtain pre-irradiated low-density polyethylene resin;
step two: adding the polypropylene resin granules into an ultralow temperature pulverizer, cooling by liquid nitrogen, reducing the temperature to-50 ℃, and pulverizing and screening at low temperature to obtain polypropylene resin powder with the particle size lower than 10 meshes. Using an electron accelerator as an irradiation source, and pre-irradiating polypropylene resin powder with beta rays under the air atmosphere, wherein the pre-irradiation dose is 10kGy, so as to obtain pre-irradiated polypropylene resin;
step three: and (3) adding the pre-irradiated polyethylene resin prepared in the first step and the pre-irradiated polypropylene resin prepared in the second step into an internal mixer according to the mass ratio of 7:5:8, banburying for 10 minutes at 190 ℃, discharging, cooling and granulating to obtain a polypropylene-polyethylene-ethylene propylene diene monomer graft, wherein the mass percentage of diene components in the ethylene propylene diene monomer is 5%.
Step four: and (3) adding the polypropylene resin and the polypropylene-polyethylene-ethylene propylene diene monomer rubber graft obtained in the step (III) into a high-speed mixer according to the mass ratio of 80:20, uniformly stirring, extruding and granulating at 120-190 ℃ by using a co-rotating double-screw extruder, and carrying out traction and cooling granulation to obtain the medical polypropylene monofilament raw material with high knotting strength.
Step five: extruding and molding the high knotting strength polypropylene medical monofilament raw material obtained in the step four by a single screw extruder under the condition of (280 ℃/290 ℃/290 ℃), cooling, stretching, heat setting and rolling to obtain the high knotting strength polypropylene medical monofilament with the diameter of 0.06mm, wherein the specific process is to adopt a water cooling mode, the cooling temperature is 12 ℃, the stretching method is secondary stretching, the primary stretching ratio is 4, the secondary stretching ratio is 1.2, and the heat setting temperature is 160 ℃.
Example five
Step one: adding the low-density polyethylene resin granules into an ultralow temperature pulverizer, cooling by using liquid nitrogen, reducing the temperature to-150 ℃, and pulverizing and screening at low temperature to obtain low-density polyethylene resin powder with the particle size of less than 10 meshes. Using 60Co as an irradiation source, and pre-irradiating the low-density polyethylene resin powder by using gamma rays in an air atmosphere, wherein the pre-irradiation dose is 20kGy, so as to obtain pre-irradiated low-density polyethylene resin;
step two: adding the polypropylene resin granules into an ultralow temperature pulverizer, cooling by liquid nitrogen, reducing the temperature to-50 ℃, and pulverizing and screening at low temperature to obtain polypropylene resin powder with the particle size lower than 10 meshes. Using an electron accelerator as an irradiation source, and pre-irradiating polypropylene resin powder with beta rays under the air atmosphere, wherein the pre-irradiation dose is 10kGy, so as to obtain pre-irradiated polypropylene resin;
step three: and (3) adding the pre-irradiated polyethylene resin prepared in the first step and the pre-irradiated polypropylene resin prepared in the second step into an internal mixer according to the mass ratio of 7:5:8, banburying for 5 minutes at 190 ℃, discharging, cooling and granulating to obtain a polypropylene-polyethylene-ethylene propylene diene monomer graft, wherein the mass percentage of diene components in the ethylene propylene diene monomer is 5%.
Step four: and (3) adding the polypropylene resin and the polypropylene-polyethylene-ethylene propylene diene monomer rubber graft obtained in the step (III) into a high-speed mixer according to the mass ratio of 80:20, uniformly stirring, extruding and granulating at 120-190 ℃ by using a co-rotating double-screw extruder, and carrying out traction and cooling granulation to obtain the medical polypropylene monofilament raw material with high knotting strength.
Step five: extruding and molding the high knotting strength polypropylene medical monofilament raw material obtained in the step four by a single screw extruder under the condition of (280 ℃/290 ℃/290 ℃), cooling, stretching, heat setting and rolling to obtain the high knotting strength polypropylene medical monofilament with the diameter of 0.28mm, wherein the specific process adopts a water cooling mode, the cooling temperature is 12 ℃, the stretching method is secondary stretching, the primary stretching ratio is 4, the secondary stretching ratio is 1.2, and the heat setting temperature is 160 ℃.
Comparative example one:
and extruding and molding the polypropylene resin by a single screw extruder at the temperature of 280 ℃/290 ℃/290 ℃, cooling, stretching, heat setting and rolling to obtain the medical polypropylene monofilament with the diameter of 0.20mm, wherein the specific process adopts a water cooling mode, the cooling temperature is 12 ℃, the stretching method is secondary stretching, the primary stretching ratio is 4, the secondary stretching ratio is 1.2, and the heat setting temperature is 160 ℃.
Comparative example two:
step one: adding low-density polyethylene resin, polypropylene resin and ethylene propylene diene monomer into an internal mixer according to the mass ratio of 5:5:3, banburying for 5 minutes at 190 ℃, discharging, cooling and granulating to obtain a polypropylene-polyethylene-ethylene propylene diene monomer blend, wherein the mass percentage of diene components in the ethylene propylene diene monomer is 5%.
Step two: and (3) adding the polypropylene resin and the polypropylene-polyethylene-ethylene propylene diene monomer rubber blend obtained in the step (II) into a high-speed mixer according to the mass ratio of 87:13, uniformly stirring, extruding and granulating at 120-190 ℃ by using a co-rotating double-screw extruder, and carrying out traction and cooling granulation to obtain the polypropylene medical monofilament raw material.
Step three: extruding the medical polypropylene monofilament raw material obtained in the second step by a single screw extruder at 280 ℃/290 ℃/290 ℃ to form, cooling, stretching, heat setting and rolling to obtain the medical polypropylene monofilament with the diameter of 0.20mm, wherein the specific process is that a water cooling mode is adopted, the cooling temperature is 12 ℃, the stretching method is secondary stretching, the primary stretching ratio is 4, the secondary stretching ratio is 1.2, and the heat setting temperature is 160 ℃.
Comparative example three:
compared with the first embodiment, the pre-irradiation polyethylene in the first step has a pre-irradiation dose of 5kGy, the pre-irradiation polypropylene has a pre-irradiation dose of 3kGy, and other process conditions are the same as the first embodiment.
Comparative example four:
in comparison with example one, the pre-irradiation of polyethylene in step one was performed at a pre-irradiation dose of 50kGy, the pre-irradiation of polypropylene was performed at a pre-irradiation dose of 30kGy, and the other process conditions were the same as in example one.
Comparative example five:
in comparison with example one, the banburying time in step three was 3 minutes, and the other process conditions were the same as in example one.
Wherein, the test results of examples one to five, comparative examples one to five are shown in the following table,
wherein, breaking strength test of monofilament: according to GB/T14344-2008 standard of chemical fiber filament tensile property test method, the strong test experiment is carried out under the conditions that the ambient temperature is 20+/-2 ℃ and the relative humidity is (65+/-2)%, a desktop computer strong tensile test instrument is adopted for testing, the average value is obtained after five times of testing, the clamping distance is (500+/-1.0) mm, and the tensile speed is 50cm/min.
Linear density testing of monofilaments: testing according to GB/T14343-2008 standard of chemical fiber filament yarn Density test method
The knotting strength test method of the monofilament comprises the following steps: if a filament is loaded in a bent state, it breaks more easily than if it is straightened, because the breaking occurs through a high degree of elongation of the surface layer of the fiber. This reflects the size of the brittleness of the filaments. Physical properties such as brittleness of the fiber can be estimated from the percentage of breaking strength measured when the filament is in a knotted state to the linear strength of the fiber. The test environment condition is that the temperature is 20+/-2 ℃, the relative humidity is (65+/-2)% and the strong test is carried out by adopting a desktop computer type strong tensile test instrument, the average value is obtained after five times of testing, the clamping distance is (500+/-1.0) mm, the clamped fiber is knotted at the middle of an upper clamp and a lower clamp, the tensile speed is 50cm/min, and the measured data is the knotting strength.
Firstly, other additives are not required to be introduced in the preparation process of the monofilament, so that the monofilament is more suitable for the medical field, and according to the table, the monofilament has good knotting strength and stable performance.
The foregoing description is only of the preferred embodiments of the present application and is presented as a description of the principles of the technology being utilized. It will be appreciated by persons skilled in the art that the scope of the invention referred to in this application is not limited to the specific combinations of features described above, but it is intended to cover other embodiments in which any combination of features described above or equivalents thereof is possible without departing from the spirit of the invention. Such as the above-described features and technical features having similar functions (but not limited to) disclosed in the present application are replaced with each other.
Claims (10)
1. The medical polypropylene monofilament with high knotting strength is characterized by comprising the following components:
70-90 parts by weight of polypropylene resin;
5-15 parts by weight of pre-irradiation polyethylene resin;
5-15 parts by weight of pre-irradiation polypropylene resin;
3-8 parts by weight of ethylene propylene diene monomer rubber;
and the sum of the weight parts of the polypropylene resin, the pre-irradiation polyethylene resin, the pre-irradiation polypropylene resin and the ethylene propylene diene monomer is 100.
2. The high knot strength polypropylene medical monofilament of claim 1, wherein the pre-irradiated polyethylene resin is prepared by the following method:
freezing and crushing granular polyethylene resin to obtain polyethylene resin powder,
the method comprises the steps of pre-irradiating polyethylene resin powder in an air atmosphere by using 60Co or an electron accelerator as an irradiation source, wherein the pre-irradiation dose range is 10-40kGy.
3. The high knot strength polypropylene medical monofilament of claim 1, wherein the pre-irradiated polypropylene resin is prepared by the following method:
freezing and crushing granular polypropylene resin to obtain polyethylene resin powder,
the method comprises the steps of pre-irradiating polypropylene resin powder in an air atmosphere by using 60Co or an electron accelerator as an irradiation source, wherein the pre-irradiation dose range is 5-15kGy.
4. The high knot strength polypropylene medical monofilament of claim 1, wherein the polyethylene resin is one or both of low density polyethylene and linear low density polyethylene;
the polypropylene is isotactic polypropylene, and the isotacticity is more than 97%;
the mass percentage content of diene components in the ethylene propylene diene monomer is 5-8%.
5. A method for preparing the medical high knot strength polypropylene monofilament according to any one of claims 1 to 4, comprising the steps of:
step one: adding polyethylene resin granules into an ultralow temperature pulverizer, cooling by liquid nitrogen, reducing the temperature to-150 ℃, pulverizing and screening at low temperature to obtain polyethylene resin powder with the particle size lower than 10 meshes, and pre-irradiating the polyethylene resin powder to obtain pre-irradiated polyethylene resin;
step two: adding polypropylene resin granules into an ultralow temperature pulverizer, cooling by liquid nitrogen, reducing the temperature to-50 ℃, pulverizing and screening at low temperature to obtain polypropylene resin powder with the particle size lower than 10 meshes, and pre-irradiating the polypropylene resin powder to obtain pre-irradiated polypropylene resin;
step three: adding the pre-irradiated polyethylene resin and the pre-irradiated polypropylene resin into an internal mixer according to the proportion, banburying for 10-15 minutes at 190 ℃, discharging, cooling and granulating to obtain a polypropylene-polyethylene-ethylene propylene diene monomer graft;
step four: adding the polypropylene-polyethylene-ethylene propylene diene monomer rubber graft and polypropylene resin into a high-speed mixer according to a proportion, uniformly stirring, extruding and granulating at 120-190 ℃ by using a co-rotating double-screw extruder, and carrying out traction and cooling granulation to obtain a high knotting strength polypropylene medical monofilament raw material;
step five: and extruding the high knotting strength medical polypropylene monofilament raw material by a single screw extruder at 280 ℃/290 ℃/290 ℃ to form, cooling, stretching, heat setting and rolling to obtain the high knotting strength medical polypropylene monofilament.
6. The method for preparing a medical monofilament of polypropylene with high knotting strength according to claim 5, wherein the step of pre-irradiating the polyethylene resin powder to obtain a pre-irradiated polyethylene resin comprises the steps of:
using 60Co as an irradiation source, and pre-irradiating polyethylene resin powder by using gamma rays in an air atmosphere, wherein the pre-irradiation dose range is 10-40kGy, so as to obtain pre-irradiated polyethylene resin;
or adopting an electron accelerator as an irradiation source, and pre-irradiating polyethylene resin powder by using beta rays under the air atmosphere, wherein the pre-irradiation dose range is 10-40kGy, so as to obtain pre-irradiated polyethylene resin;
the step of pre-irradiating the polypropylene resin powder to obtain pre-irradiated polypropylene resin comprises the following steps:
using 60Co as an irradiation source, and pre-irradiating the polypropylene resin powder by using gamma rays in an air atmosphere, wherein the pre-irradiation dose range is 5-15kGy, so as to obtain pre-irradiated polypropylene resin;
or adopting an electron accelerator as an irradiation source, and pre-irradiating the polypropylene resin powder by using beta rays in an air atmosphere, wherein the pre-irradiation dose range is 5-15kGy, so as to obtain the pre-irradiated polypropylene resin.
7. The method for preparing the medical polypropylene monofilament with high knotting strength according to claim 5, wherein the weight ratio of the polypropylene resin to the pre-irradiated polyethylene resin to the pre-irradiated polypropylene resin to the ethylene propylene diene monomer rubber in the third step and the fourth step is (70-90): (5-15): (5-15): (3-8).
8. The method for preparing a medical monofilament of high knotting strength polypropylene according to claim 5, wherein the polyethylene resin is one or both of low density polyethylene and linear low density polyethylene;
the polypropylene is isotactic polypropylene, and the isotacticity is more than 97%;
the mass percentage content of diene components in the ethylene propylene diene monomer is 5-8%.
9. The method for preparing medical polypropylene monofilaments with high knot strength according to claim 5, wherein in the fifth step, the cooling method is water cooling, the cooling temperature is 12 ℃, the stretching method is secondary stretching, the primary stretching ratio is 4, the secondary stretching ratio is 1.2, and the heat setting temperature is 160 ℃.
10. The method for producing a high knot strength polypropylene medical monofilament according to claim 5, wherein in the fifth step, the diameter of the high knot strength polypropylene medical monofilament is 0.05-0.3mm.
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