CN108570187B - Polypropylene plate for artificial limb orthopedic appliance and preparation method thereof - Google Patents
Polypropylene plate for artificial limb orthopedic appliance and preparation method thereof Download PDFInfo
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- CN108570187B CN108570187B CN201810440527.4A CN201810440527A CN108570187B CN 108570187 B CN108570187 B CN 108570187B CN 201810440527 A CN201810440527 A CN 201810440527A CN 108570187 B CN108570187 B CN 108570187B
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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
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/12—Polypropene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F255/00—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00
- C08F255/02—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00 on to polymers of olefins having two or three carbon atoms
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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
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/14—Copolymers of propene
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Abstract
The invention discloses a polypropylene plate for an artificial limb orthotic, which comprises the following components in parts by weight: 100 parts of polypropylene, 0.01-0.1 part of initiator and 0.1-2.5 parts of cross-linking agent; the crosslinking agent is at least one of 1, 6-hexanediol diacrylate, triallyl isocyanurate, pentaerythritol triacrylate and divinylbenzene. According to the invention, the polypropylene plate for the artificial limb orthosis with remarkably improved anti-sagging performance is efficiently prepared by adopting a specific formula and a one-step extrusion method, and the product is not thinned due to sagging when the plate is used for manufacturing the artificial limb orthosis, so that the mechanical strength of the artificial limb orthosis is ensured, the application range of the polypropylene plate for the artificial limb orthosis can be enlarged, the service cycle of the large artificial limb orthosis for lower limbs is prolonged, and the economic burden of a patient is reduced. Meanwhile, the invention also discloses a preparation method of the polypropylene plate.
Description
Technical Field
The invention relates to a polypropylene plate and a preparation method thereof, in particular to a polypropylene plate for an artificial limb orthopedic appliance and a preparation method thereof.
Background
The polypropylene is non-toxic, odorless and tasteless, is highly favored, is one of the first three general plastics, and has wide sources; in addition, polypropylene is one of the lightest plastics, has excellent mechanical properties, particularly has excellent bending fatigue resistance capable of resisting more than 10-7 times of opening and closing bending, and has the advantage of being unique in the field of artificial limb orthotics, particularly in the field of lower limb orthotics needing long-term wearing and walking. Many current dynamic lower extremity orthoses are made by vacuum forming a sheet of polypropylene that is softened by heating and placed in a plaster mold.
However, since polypropylene is affected by linear structure, the softening point is very close to the melting point, and the sag resistance of polypropylene rapidly decreases and the melt ductility deteriorates after exceeding the melting point. Although the existing polypropylene plate for the artificial limb orthopedic has been produced by selecting polypropylene raw materials with high melt strength, when a larger artificial limb and an orthopedic device are manufactured, the manufacturing is often failed due to sagging and thinning in the process of transferring to a plaster mold from a heater; therefore, although the mechanical property of polyethylene is inferior to that of polypropylene and the polyethylene cannot resist long-term wearing and walking, the polyethylene is still the preferred material for current artificial limb orthotics; this makes the life cycle of large lower limb orthoses shorter, requiring repeated manufacture, and placing a greater economic burden on the patient.
Disclosure of Invention
Based on the above, the invention aims to overcome the defects of the prior art and provide a polypropylene sheet for orthopedic prostheses, which has anti-sagging property, can meet the manufacturing requirements of most artificial limbs and orthoses and has proper melt ductility.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a polypropylene plate for an orthopedic prosthesis comprises the following components in parts by weight: 100 parts of polypropylene, 0.01-0.1 part of initiator and 0.1-2.5 parts of cross-linking agent; the crosslinking agent is at least one of 1, 6-hexanediol diacrylate, triallyl isocyanurate, pentaerythritol triacrylate and divinylbenzene.
The reaction principle of the components in the polypropylene plate for the prosthetic orthopedic appliance is as follows: the initiator can initiate the polypropylene to generate reactive sites, so that the initiator can generate a crosslinking reaction with the crosslinking agent, and the polypropylene is in a rubber state in a molten state to reduce sagging.
Preferably, the initiator is at least one of Benzoyl Peroxide (BPO), dicumyl peroxide (DCP), Azobisisobutyronitrile (AIBN). The initiator is selected mainly by considering that the initial reaction temperature of the initiator is lower than the processing temperature of the polypropylene, and the reaction speed of the initiator is matched with the speed of the crosslinking reaction, so that the polypropylene is seriously degraded if the reaction of the initiator is too fast, and the crosslinking reaction is incomplete and the fusion drop of the polypropylene is not obvious if the reaction of the initiator is too slow.
Preferably, the polypropylene is at least one of homo-polypropylene and co-polypropylene, and the melt index of the polypropylene is 1.0-4.0 g/10 min. The polypropylene selected in the invention is the simplest and easily available extrusion grade polypropylene, and the cost is lower, while the prior common artificial limb orthopedic plate is made of the thermoforming grade polypropylene, and the cost is relatively higher (about 50 percent higher than the cost of the polypropylene selected in the invention).
Preferably, the polypropylene plate for the orthopedic prosthesis further comprises an auxiliary agent, and the auxiliary agent is at least one of an antioxidant, a light stabilizer and a slipping agent. The auxiliary agents include but are not limited to antioxidants, light stabilizers and slipping agents, and can be selected conventionally by those skilled in the art according to actual needs.
More preferably, the auxiliary agent comprises an antioxidant, a light stabilizer and a slipping agent, wherein the antioxidant is antioxidant 1010, the light stabilizer is light stabilizer 622, and the slipping agent is ZnSt. The antioxidant includes but is not limited to antioxidant 1010, the light stabilizer includes but is not limited to light stabilizer 622, and the slip agent is ZnSt, and the ordinary choice can be made by those skilled in the art according to actual needs.
Meanwhile, the invention also discloses a preparation method of the polypropylene plate for the prosthetic orthopedic appliance, which comprises the following steps:
uniformly mixing polypropylene, an initiator, a cross-linking agent and an auxiliary agent to obtain a mixture, adding the mixture into a screw extruder with the length-diameter ratio of 10-35, and performing extrusion molding to obtain the polypropylene plate for the artificial limb orthotic.
The screw extruder can be a single screw extruder, a double screw extruder or a multi-screw extruder, the screw can be divided into a feeding section, a melting section, a reaction section and an extrusion section, wherein an exhaust port connected with a vacuum pump with the vacuum degree of not less than 0.08MPa is arranged at the extrusion section.
Preferably, the screw extruder comprises a feeding section, a melting section, a reaction section and an extrusion section, wherein the temperature of the feeding section is 150-170 ℃, the temperature of the melting section is 180-210 ℃, the temperature of the reaction section is 180-210 ℃, the temperature of the extrusion section is 190-230 ℃, the rotating speed of the screw is 30-100 r/min, and the vacuum degree is 0.08 MPa.
The initiator initiates the polypropylene to generate a crosslinking reaction and simultaneously can cause the polypropylene to be degraded to destroy the mechanical property of the polypropylene, so the processing technology is controlled, mainly the processing temperature and the retention time of the material at the processing temperature; the processing conditions can reduce the degradation degree of the polypropylene to the maximum extent, and simultaneously improve the efficiency of the crosslinking reaction, so that the sag of the polypropylene is obviously reduced.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, the polypropylene plate for the artificial limb orthosis with remarkably improved anti-sagging performance is efficiently prepared by adopting a specific formula and a one-step extrusion method, and the product is not thinned due to sagging when the plate is used for manufacturing the artificial limb orthosis, so that the mechanical strength of the artificial limb orthosis is ensured, the application range of the polypropylene plate for the artificial limb orthosis can be enlarged, the service cycle of the large artificial limb orthosis for lower limbs is prolonged, and the economic burden of a patient is reduced.
Drawings
FIG. 1 is a diagram of a device for testing the sagging resistance of a plate according to the present invention;
wherein, the test sample plate is 1, 15cm multiplied by 10cm multiplied by 4 mm; 2. a jig for fixing the sample plate; 3. a sample support frame.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to the accompanying drawings and specific embodiments.
Example 1
In an embodiment of the polypropylene sheet for orthopedic prosthesis of the present invention, the polypropylene sheet for orthopedic prosthesis of the present embodiment is prepared by the following preparation method:
100 parts by weight of polypropylene (MFR: 3.0g/10 min); 0.02 parts by weight of an initiator dicumyl peroxide; 0.4 parts by weight of a crosslinking agent divinylbenzene; 0.3 part by weight of an antioxidant; 0.2 parts by weight of a light stabilizer; 0.1 part by weight of slipping agent is mixed evenly. Then adding the mixture into a double-screw extruder with the length-diameter ratio of 33 and the diameter of a screw rod of 50mm, setting the temperature of the extruder from a feeding port to a machine head at 170 ℃, 200 ℃, 200 ℃, 180 ℃, 190 ℃, 190 ℃, 100r/min of the rotation speed of the screw rod and 0.08MPa of the vacuum degree of an exhaust port, and extruding the mixture into a plate with the thickness of 4 mm.
Example 2
In an embodiment of the polypropylene sheet for orthopedic prosthesis of the present invention, the polypropylene sheet for orthopedic prosthesis of the present embodiment is prepared by the following preparation method:
100 parts by weight of polypropylene (MFR: 2.0g/10 min); 0.03 parts by weight of an initiator dicumyl peroxide; 0.2 parts by weight of a crosslinking agent divinylbenzene; 1.0 part by weight of triallyl isocyanurate; 0.3 part by weight of an antioxidant; 0.2 parts by weight of a light stabilizer; 0.1 part by weight of slipping agent is mixed evenly. Then adding the mixture into a double-screw extruder with the length-diameter ratio of 35 and the diameter of a screw rod of 65mm, setting the temperature of the extruder from a feeding port to a machine head at 160 ℃, 190 ℃, 190 ℃, 190 ℃, 190 ℃, 190 ℃, 50r/min of the rotation speed of the screw rod, and 0.08MPa of the vacuum degree of an exhaust port, and extruding the mixture into a plate with the thickness of 4 mm.
Example 3
In an embodiment of the polypropylene sheet for orthopedic prosthesis of the present invention, the polypropylene sheet for orthopedic prosthesis of the present embodiment is prepared by the following preparation method:
100 parts by weight of polypropylene (MFR ═ 1.0g/10 min); 0.05 part by weight of an initiator dicumyl peroxide; 1.2 parts by weight of a crosslinker triallyl isocyanurate; 0.3 part by weight of an antioxidant; 0.2 parts by weight of a light stabilizer; 0.1 part by weight of slipping agent is mixed evenly. Then adding the mixture into a single-screw extruder with the length-diameter ratio of 20 and the screw diameter of 120mm, setting the temperature of the extruder from a feeding port to a machine head at 160 ℃, 200 ℃, 200 ℃, 210 ℃, the rotating speed of the screw at 30r/min and the vacuum degree of an exhaust port at 0.08MPa, and extruding the mixture into a plate with the thickness of 4 mm.
Example 4
In an embodiment of the polypropylene sheet for orthopedic prosthesis of the present invention, the polypropylene sheet for orthopedic prosthesis of the present embodiment is prepared by the following preparation method:
100 parts by weight of polypropylene (MFR 4.0g/10 min); 0.1 part by weight of an initiator benzoyl peroxide; 2.5 parts by weight of a crosslinking agent 1, 6-hexanediol diacrylate; 0.3 part by weight of an antioxidant; 0.2 parts by weight of a light stabilizer; 0.1 part by weight of slipping agent is mixed evenly. Then adding the mixture into a single-screw extruder with the length-diameter ratio of 10 and the screw diameter of 120mm, setting the temperature of the extruder from a feeding port to a machine head at 150 ℃, 180 ℃, 180 ℃, 230 ℃, the rotating speed of the screw at 40r/min and the vacuum degree of an exhaust port at 0.08MPa, and extruding the mixture into a plate with the thickness of 4 mm.
Example 5
In an embodiment of the polypropylene sheet for orthopedic prosthesis of the present invention, the polypropylene sheet for orthopedic prosthesis of the present embodiment is prepared by the following preparation method:
100 parts by weight of polypropylene (MFR ═ 1.0g/10 min); 0.01 part by weight of an initiator azobisisobutyronitrile; 0.1 part by weight of a crosslinking agent pentaerythritol triacrylate; 0.3 part by weight of an antioxidant; 0.2 parts by weight of a light stabilizer; 0.1 part by weight of slipping agent is mixed evenly. Then adding the mixture into a single-screw extruder with the length-diameter ratio of 25 and the screw diameter of 120mm, setting the temperature of the extruder from a feed inlet to a machine head at 160 ℃, 210 ℃, 210 ℃, the screw rotation speed of 80r/min and the vacuum degree of an exhaust port at 0.08MPa, and extruding the mixture into a plate with the thickness of 4 mm.
Comparative example 1
100 parts by weight of polypropylene (special high melt strength polypropylene MFR for thermoforming is 0.8g/10min) with the trademark of HP300E, and 0.3 part by weight of antioxidant; 0.2 parts by weight of a light stabilizer; 0.1 part by weight of slipping agent is mixed evenly. Then adding the mixture into a double-screw extruder with the length-diameter ratio of 33 and the diameter of a screw rod of 50mm, setting the temperature of the extruder from a feeding port to a machine head at 170 ℃, 200 ℃, 200 ℃, 180 ℃, 180 ℃, 170 ℃, the rotating speed of the screw rod at 100r/min and the vacuum degree of an exhaust port at 0.08MPa, and extruding the mixture into a plate with the thickness of 4 mm.
Comparative example 2
100 parts by weight of polypropylene (special high melt strength polypropylene MFR for thermoforming is 0.8g/10min) with the trademark of HP300E, and 0.3 part by weight of antioxidant; 0.2 parts by weight of a light stabilizer; 0.1 part by weight of slipping agent is mixed evenly. Then adding the mixture into a double-screw extruder with the length-diameter ratio of 35 and the diameter of a screw rod of 65mm, setting the temperature of the extruder from a feeding port to a machine head at 160 ℃, 190 ℃, 190 ℃, 190 ℃, 170 ℃, the rotating speed of the screw rod at 50r/min and the vacuum degree of an exhaust port at 0.08MPa, and extruding the mixture into a plate with the thickness of 4 mm.
Comparative example 3
100 parts by weight of polypropylene (special high melt strength polypropylene MFR for thermoforming is 0.8g/10min) with the trademark of HP300E, and 0.3 part by weight of antioxidant; 0.2 parts by weight of a light stabilizer; 0.1 part by weight of slipping agent is mixed evenly. Then adding the mixture into a single-screw extruder with the length-diameter ratio of 20 and the screw diameter of 120mm, setting the temperature of the extruder from a feeding port to a machine head at 160 ℃, 200 ℃, 200 ℃, 180 ℃, the rotating speed of the screw at 40r/min and the vacuum degree of an exhaust port at 0.08MPa, and extruding the mixture into a plate with the thickness of 4 mm.
The polypropylene sheets obtained in examples 1 to 5 and comparative examples 1 to 3 were subjected to melt index and sag test, and the test results are shown in table 1:
melt index (MFR) was measured according to ASTM D1238, 230 ℃ C., 2.16 Kg.
The plate sag resistance test used the apparatus shown in figure 1, where 1 is a 15cm x 10cm x 4mm test panel, 2 is the fixture used to hold the panel, 3 is a sample support frame having a width of 10cm and a height of 15cm, and two parallel side panels are spaced 12cm apart. During testing, the sample is fixed according to the mode in the figure and then placed in an environment with the temperature of 170 ℃, the temperature is preserved for more than 15min, and after the sample is completely melted, the sagging amplitude of the lowest point of the sample is measured.
Table 1 shows the test results of the polypropylene sheets prepared according to the present invention
As can be seen from Table 1, the polypropylene sheets obtained in the present application have significantly lower melt index and lower sag than those of the comparative examples.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (6)
1. The polypropylene plate for the artificial limb orthopedic appliance is characterized by comprising the following components in parts by weight: 100 parts of polypropylene, 0.01-0.1 part of initiator and 0.1-2.5 parts of cross-linking agent; the polypropylene is at least one of homo-polypropylene and co-polypropylene, and the melt index of the polypropylene is 1.0-4.0 g/10 min; the crosslinking agent is triallyl isocyanurate and divinylbenzene.
2. A polypropylene sheet for an orthopaedic prosthesis according to claim 1, wherein the initiator is at least one of benzoyl peroxide, dicumyl peroxide, azobisisobutyronitrile.
3. A polypropylene sheet for an orthopedic prosthesis according to any of claims 1 to 2, further comprising an auxiliary agent, wherein the auxiliary agent is at least one of an antioxidant, a light stabilizer and a slip agent.
4. A polypropylene sheet for an orthopedic prosthesis according to claim 3, wherein the auxiliary agent comprises an antioxidant, a light stabilizer and a slip agent, wherein the antioxidant is antioxidant 1010, the light stabilizer is light stabilizer 622 and the slip agent is ZnSt.
5. A method of making a polypropylene sheet for an orthopaedic prosthesis according to any one of claims 1 to 4, the method comprising:
uniformly mixing polypropylene, an initiator, a cross-linking agent and an auxiliary agent to obtain a mixture, adding the mixture into a screw extruder with the length-diameter ratio of 10-35, and performing extrusion molding to obtain the polypropylene plate for the artificial limb orthotic.
6. The method for preparing a polypropylene plate for an orthopedic prosthesis according to claim 5, wherein the screw extruder comprises a feeding section, a melting section, a reaction section and an extrusion section, the temperature of the feeding section is 150 to 170 ℃, the temperature of the melting section is 180 to 210 ℃, the temperature of the reaction section is 180 to 210 ℃, the temperature of the extrusion section is 190 to 230 ℃, the rotation speed of the screw is 30 to 100r/min, and the vacuum degree is 0.08 MPa.
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| CN1869119A (en) * | 2005-05-27 | 2006-11-29 | 青岛大学 | Preparation method of partly cross-linked dystectic strength polypropylene |
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| WO2006057361A1 (en) * | 2004-11-25 | 2006-06-01 | Mitsui Chemicals, Inc. | Propylene resin composition and use thereof |
| CN106715551B (en) * | 2014-09-30 | 2020-03-13 | 积水化学工业株式会社 | Crosslinked polyolefin foam |
| CN107216545A (en) * | 2017-05-24 | 2017-09-29 | 广东圆融新材料有限公司 | A kind of dynamic crosslinking PP/PE intermingling materials for characteristic of turning white with low-density high-impact proof stress and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1869119A (en) * | 2005-05-27 | 2006-11-29 | 青岛大学 | Preparation method of partly cross-linked dystectic strength polypropylene |
| CN101376683A (en) * | 2008-10-07 | 2009-03-04 | 中国科学院长春应用化学研究所 | Preparation of high melt strength polypropylene |
| CN102558449A (en) * | 2011-12-13 | 2012-07-11 | 金发科技股份有限公司 | High-melt-strength polypropylene material, and preparation method and application thereof |
| CN105504170A (en) * | 2014-09-22 | 2016-04-20 | 中国石化扬子石油化工有限公司 | High melt strength polypropylene preparation method |
| RU2014153836A (en) * | 2014-12-30 | 2016-07-20 | Публичное акционерное общество "СИБУР Холдинг" | HIGH MELT POLYPROPYLENE COMPOSITION AND METHOD FOR PRODUCING IT |
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