CN107652642A - A kind of polycaprolactone composite material and preparation method thereof - Google Patents

A kind of polycaprolactone composite material and preparation method thereof Download PDF

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Publication number
CN107652642A
CN107652642A CN201710993709.XA CN201710993709A CN107652642A CN 107652642 A CN107652642 A CN 107652642A CN 201710993709 A CN201710993709 A CN 201710993709A CN 107652642 A CN107652642 A CN 107652642A
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temperature
composite material
area
polycaprolactone
parts
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CN201710993709.XA
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Chinese (zh)
Inventor
刘凯
徐志海
孙启林
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Anhui Jianghuai Automobile Group Corp
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Anhui Jianghuai Automobile Group Corp
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Priority to CN201710993709.XA priority Critical patent/CN107652642A/en
Publication of CN107652642A publication Critical patent/CN107652642A/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L67/00Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
    • C08L67/04Polyesters derived from hydroxycarboxylic acids, e.g. lactones
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25Component parts, details or accessories; Auxiliary operations
    • B29C48/92Measuring, controlling or regulating
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00Indexing scheme relating to extrusion moulding
    • B29C2948/92Measuring, controlling or regulating
    • B29C2948/92504Controlled parameter
    • B29C2948/92704Temperature
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/002Physical properties
    • C08K2201/003Additives being defined by their diameter
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/08Stabilised against heat, light or radiation or oxydation

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials For Medical Uses (AREA)

Abstract

It is composed of the following components by weight the present invention relates to a kind of polycaprolactone composite material and preparation method thereof:100 parts of polycaprolactone 80 part, 10 parts of mullite crystal whisker 6 part, 8 parts of nano medical stone 6 part, 0.3 part of compatilizer 0.1 part, 0.5 part of antioxidant 0.1 part.The hardness of wherein mullite crystal whisker is very high, improves the anti-wear performance of polycaprolactone;Nano medical stone has antibiotic property in itself, and it improves the ageing-resistant performance and anti-microbial property of polycaprolactone;The preparation technology of the polycaprolactone composite material of the technical program is simple, has very big promotional value.

Description

A kind of polycaprolactone composite material and preparation method thereof
Technical field
The invention belongs to technical field of polymer materials, particularly relates to a kind of polycaprolactone composite material and its preparation side Method.
Background technology
Polycaprolactone is a kind of engineering plastics of high comprehensive performance, and its good stability of the dimension, insulating properties is good, oil resistant, into Type processing characteristics is relatively good, but its is wear-resisting, anti-microbial property is general, special at some which greatly limits polycaprolactone composite material Application on different Material Field.
How to improve the performance of polycaprolactone be this area always in the problem of exploration, applicant by a variety of effort, In terms of the anti-wear performance and anti-microbial property of polycaprolactone is improved, larger progress is obtained.
The content of the invention
It is an object of the invention to provide a kind of polycaprolactone composite material and preparation method thereof, to solve in the prior art, The problem of anti-wear performance and not high anti-microbial property of polycaprolactone.
The present invention is achieved by the following technical solutions:
A kind of polycaprolactone composite material, it is composed of the following components by weight:
The polycaprolactone is linear polycaprolactone.
A diameter of 50-70nm of the mullite crystal whisker.
The nano medical stone particle diameter is 20-30 μm.
The compatilizer is SEBS-g-MAH.
The antioxidant is three (2,4- di-t-butyls) phenyl-phosphites, four [β-(3,5- di-tert-butyl-hydroxy phenyls) Propionic acid] one kind or more in pentaerythritol ester or 1,3,5- trimethyls -2,4,6- (3,5- di-t-butyl -4- hydroxyphenylmethyls) benzene Kind.
A kind of preparation method of polycaprolactone composite material, comprises the following steps:
(1) weigh 80 parts -100 parts polycaprolactone, 6 parts -10 parts of mullite crystal whisker, 6 parts -8 parts of nano medical stone, 0.1 part -0.3 part of SEBS-g-MAH, 0.1 part -0.5 part of antioxidant, it is mixed and stirred for uniformly, obtaining compound;
(2) the compound extruding pelletization that will be obtained in step (1), that is, obtain polycaprolactone composite material.
The step (2) is specially:
The compound obtained in step (1) is put into extruding pelletization in the hopper of double screw extruder, wherein, it is described double Screw extruder includes six humidity provinces sequentially arranged, 80~120 DEG C of area's temperature, two 160~200 DEG C of area's temperature, 3rd area 160~200 DEG C of temperature, four 160~200 DEG C of area's temperature, five 160~200 DEG C of area's temperature, six 160~200 DEG C of area's temperature, head 160~200 DEG C of temperature, 200~280r/min of screw speed.
The beneficial effects of the invention are as follows:
1st, the hardness of mullite crystal whisker is very high, improves the anti-wear performance of polycaprolactone.
2nd, nano medical stone has antibiotic property in itself, and it improves the ageing-resistant performance and anti-microbial property of polycaprolactone.
3rd, the preparation technology of the polycaprolactone composite material of the technical program is simple, has very big promotional value.
Embodiment
Describe technical scheme in detail by the following examples, following embodiment be only it is exemplary, only Explanation and illustration technical scheme can be used for, and be not to be construed as the limitation to technical solution of the present invention.
Raw material used is as follows in each embodiment of the technical program:
Polycaprolactone (model 6800), Sweden's Paasche support;Mullite crystal whisker, Yangquan spark Xin Yuan founding materialses factory;Nanometer Medical stone, the day nano biological Science and Technology Ltd. in Tianjin sea;SEBS-g-MAH, the sub- match plasticizing Co., Ltd in Suzhou;Antioxidant (model Irganox168, Irganox1010, Irganox1330), Switzerland's Ciba.
Tester used in the technical program is as follows:
ZSK30 type double screw extruders, German W&P companies;JL-1000 type tensile testing machines, the wide just experiment instrument in Guangzhou Device company produces;HTL900-T-5B type injection (mo(u)lding) machines, the production of Hai Tai plastics machineries Co., Ltd;XCJ-500 type shock-testings Machine, the production of Chengde testing machine factory;QT-1196 type tester for elongation, Dongguan City Gao Tai detecting instruments Co., Ltd;QD-GJS- B12K type homogenizers, Beijing perseverance Order instrument and meter Co., Ltd.
The technical program provides a kind of polycaprolactone composite material, composed of the following components by weight:
The polycaprolactone is linear polycaprolactone.
A diameter of 50-70nm of the mullite crystal whisker.
The nano medical stone particle diameter is 20-30 μm.
The compatilizer is SEBS-g-MAH.
The antioxidant is three (2,4- di-t-butyls) phenyl-phosphites (Irganox168), four [β-(bis- tertiary fourths of 3,5- Base -4- hydroxy phenyls) propionic acid] pentaerythritol ester (Irganox1010) or 1,3,5- trimethyls -2,4,6- (3,5- di-t-butyls - 4- hydroxyphenylmethyls) one or more in benzene (Irganox1330).
A kind of preparation method of polycaprolactone composite material, comprises the following steps:
(1) weigh 80 parts -100 parts polycaprolactone, 6 parts -10 parts of mullite crystal whisker, 6 parts -8 parts of nano medical stone, 0.1 part -0.3 part of SEBS-g-MAH, 0.1 part -0.5 part of antioxidant, it is mixed and stirred for uniformly, obtaining compound;
(2) the compound extruding pelletization that will be obtained in step (1), that is, obtain polycaprolactone composite material.
The step (2) is specially:
The compound obtained in step (1) is put into extruding pelletization in the hopper of double screw extruder, wherein, it is described double Screw extruder includes six humidity provinces sequentially arranged, 80~120 DEG C of area's temperature, two 160~200 DEG C of area's temperature, 3rd area 160~200 DEG C of temperature, four 160~200 DEG C of area's temperature, five 160~200 DEG C of area's temperature, six 160~200 DEG C of area's temperature, head 160~200 DEG C of temperature, 200~280r/min of screw speed.
Embodiment 1
(1) weigh 80 parts of polycaprolactones, 6 parts of mullite crystal whiskers, 6 parts of nano medical stones, 0.1 part of SEBS-g-MAH, 0.1 part Irganox1010, it is mixed and stirred for uniformly, obtaining compound;
(2) the compound extruding pelletization that will be obtained in step (1), that is, obtain polycaprolactone composite material P1.
Wherein each area's temperature of double screw extruder and screw speed are respectively:One 80 DEG C of area's temperature, two 160 DEG C of area's temperature, Three 160 DEG C of area's temperature, four 160 DEG C of area's temperature, five 160 DEG C of area's temperature, six 160 DEG C of area's temperature, 160 DEG C of head temperature, screw rod turn Fast 200r/min.
Embodiment 2
(1) 100 parts of polycaprolactones, 10 parts of mullite crystal whiskers, 8 parts of nano medical stones, 0.3 part of SEBS-g-MAH, 0.1 are weighed Part Irganox168,0.2 part of Irganox1010,0.2 part of Irganox1330, it is mixed and stirred for uniformly, obtaining compound;
(2) the compound extruding pelletization that will be obtained in step (1), that is, obtain polycaprolactone composite material P2.
Wherein each area's temperature of double screw extruder and screw speed are respectively:One 120 DEG C of area's temperature, two 200 DEG C of area's temperature, Three 200 DEG C of area's temperature, four 200 DEG C of area's temperature, five 200 DEG C of area's temperature, six 200 DEG C of area's temperature, 200 DEG C of head temperature, screw rod turn Fast 280r/min.
Embodiment 3
(1) weigh 90 parts of polycaprolactones, 8 parts of mullite crystal whiskers, 7 parts of nano medical stones, 0.2 part of SEBS-g-MAH, 0.1 part Irganox168,0.2 part of Irganox1010, it is mixed and stirred for uniformly, obtaining compound;
(2) the compound extruding pelletization that will be obtained in step (1), that is, obtain polycaprolactone composite material P3.
Wherein each area's temperature of double screw extruder and screw speed are respectively:One 100 DEG C of area's temperature, two 180 DEG C of area's temperature, Three 180 DEG C of area's temperature, four 180 DEG C of area's temperature, five 180 DEG C of area's temperature, six 180 DEG C of area's temperature, 180 DEG C of head temperature;Screw rod turns Fast 240r/min.
Embodiment 4
(1) weigh 85 parts of polycaprolactones, 7 parts of mullite crystal whiskers, 8 parts of nano medical stones, 0.3 part of SEBS-g-MAH, 0.1 part Irganox168,0.1 part of Irganox1330, it is mixed and stirred for uniformly, obtaining compound;
(2) the compound extruding pelletization that will be obtained in step (1), that is, obtain polycaprolactone composite material P4.
Wherein each area's temperature of double screw extruder and screw speed are respectively:One 110 DEG C of area's temperature, two 195 DEG C of area's temperature, Three 195 DEG C of area's temperature, four 195 DEG C of area's temperature, five 195 DEG C of area's temperature, six 195 DEG C of area's temperature, 195 DEG C of head temperature;Screw rod turns Fast 245r/min.
Embodiment 5
(1) weigh 95 parts of polycaprolactones, 7 parts of mullite crystal whiskers, 7 parts of nano medical stones, 0.2 part of SEBS-g-MAH, 0.1 part Irganox168,0.3 part of Irganox1330, it is mixed and stirred for uniformly, obtaining compound;
(2) the compound extruding pelletization that will be obtained in step (1), that is, obtain polycaprolactone composite material P5.
Wherein each area's temperature of double screw extruder and screw speed are respectively:One 115 DEG C of area's temperature, two 185 DEG C of area's temperature, Three 185 DEG C of area's temperature, four 185 DEG C of area's temperature, five 185 DEG C of area's temperature, six 185 DEG C of area's temperature, 185 DEG C of head temperature;Screw rod turns Fast 265r/min.
Comparative example 1
(1) 85 parts of polycaprolactones, 0.1 part of Irganox168,0.3 part of Irganox1330 are weighed, is mixed and stirred for uniformly, Obtain compound;
(2) the compound extruding pelletization that will be obtained in step (1), that is, obtain polycaprolactone composite material D1.
Wherein each area's temperature of double screw extruder and screw speed are respectively:One 100 DEG C of area's temperature, two 175 DEG C of area's temperature, Three 175 DEG C of area's temperature, four 175 DEG C of area's temperature, five 175 DEG C of area's temperature, six 175 DEG C of area's temperature, 175 DEG C of head temperature;Screw rod turns Fast 255r/min.
Performance test:
Polycaprolactone composite material prepared by above-described embodiment 1-5 and comparative example 1 is made into batten with injection machine to test, surveyed Try data such as following table:
1 each embodiment of table and the test of comparative example properties of product
As can be seen from the above table, compared with comparative example 1, anti-wear performance, anti-microbial property have different degrees of embodiment 1-5 Improve, this extends the application field of polycaprolactone composite material, disclosure satisfy that the fields such as IT, communication, electronics, automobile to engineering The requirement of part.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with A variety of changes, modification can be carried out to these embodiments, replace without departing from the principles and spirit of the present invention by understanding And deformation, the scope of the present invention are extremely equally limited by appended claims.

Claims (8)

1. a kind of polycaprolactone composite material, it is characterised in that composed of the following components by weight:
2. polycaprolactone composite material according to claim 1, it is characterised in that the polycaprolactone gathers in oneself to be linear Ester.
3. polycaprolactone composite material according to claim 1, it is characterised in that the mullite crystal whisker it is a diameter of 50-70nm。
4. polycaprolactone composite material according to claim 1, it is characterised in that the nano medical stone particle diameter is 20- 30μm。
5. polycaprolactone composite material according to claim 1, it is characterised in that the compatilizer is SEBS-g-MAH.
6. polycaprolactone composite material according to claim 1, it is characterised in that the antioxidant is three (2,4- bis- uncles Butyl) phenyl-phosphite, four [β-(3,5- di-tert-butyl-hydroxy phenyls) propionic acid] pentaerythritol esters or 1,3,5- trimethyls- One or more in 2,4,6- (3,5- di-t-butyl -4- hydroxyphenylmethyls) benzene.
7. a kind of preparation method of polycaprolactone composite material, it is characterised in that comprise the following steps:
(1) weigh 80 parts -100 parts polycaprolactone, 6 parts -10 parts of mullite crystal whisker, 6 parts -8 parts of nano medical stone, 0.1 The SEBS-g-MAH, 0.1 part -0.5 part of antioxidant of -0.3 part of part, it is mixed and stirred for uniformly, obtaining compound;
(2) the compound extruding pelletization that will be obtained in step (1), that is, obtain polycaprolactone composite material.
8. the preparation method of polycaprolactone composite material according to claim 7, it is characterised in that step (2) tool Body is:
The compound obtained in step (1) is put into extruding pelletization in the hopper of double screw extruder, wherein, the twin-screw Extruder includes six humidity provinces sequentially arranged, 80~120 DEG C of area's temperature, two 160~200 DEG C of area's temperature, three area's temperature 160~200 DEG C, four 160~200 DEG C of area's temperature, five 160~200 DEG C of area's temperature, six 160~200 DEG C of area's temperature, head temperature 160~200 DEG C, 200~280r/min of screw speed.
CN201710993709.XA 2017-10-23 2017-10-23 A kind of polycaprolactone composite material and preparation method thereof Pending CN107652642A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103113731A (en) * 2013-02-20 2013-05-22 合肥杰事杰新材料股份有限公司 Kaolin-modified polycaprolactone composite material and preparation method thereof
CN103525047A (en) * 2013-09-05 2014-01-22 新疆科蓝双谊医疗科技股份有限公司 Antibacterial low-temperature thermoplastic material for orthopedics department and radiotherapy

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103113731A (en) * 2013-02-20 2013-05-22 合肥杰事杰新材料股份有限公司 Kaolin-modified polycaprolactone composite material and preparation method thereof
CN103525047A (en) * 2013-09-05 2014-01-22 新疆科蓝双谊医疗科技股份有限公司 Antibacterial low-temperature thermoplastic material for orthopedics department and radiotherapy

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