CN107875449A - A kind of preparation method of nano composite material - Google Patents
A kind of preparation method of nano composite material Download PDFInfo
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- CN107875449A CN107875449A CN201710994500.5A CN201710994500A CN107875449A CN 107875449 A CN107875449 A CN 107875449A CN 201710994500 A CN201710994500 A CN 201710994500A CN 107875449 A CN107875449 A CN 107875449A
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- preparation
- composite material
- nano composite
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/40—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material
- A61L27/42—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material having an inorganic matrix
- A61L27/425—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material having an inorganic matrix of phosphorus containing material, e.g. apatite
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/40—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material
- A61L27/44—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material having a macromolecular matrix
- A61L27/46—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material having a macromolecular matrix with phosphorus-containing inorganic fillers
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2430/00—Materials or treatment for tissue regeneration
- A61L2430/02—Materials or treatment for tissue regeneration for reconstruction of bones; weight-bearing implants
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- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Oral & Maxillofacial Surgery (AREA)
- Transplantation (AREA)
- Materials Engineering (AREA)
- Engineering & Computer Science (AREA)
- Dermatology (AREA)
- Medicinal Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Composite Materials (AREA)
- Epidemiology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Colloid Chemistry (AREA)
Abstract
A kind of preparation method of nano composite material, belongs to field of material preparation.Comprise the following steps：By four water-calcium nitrate and diammonium hydrogen phosphate wiring solution-forming, surfactant is added, in the presence of being stirred vigorously, is precipitated after making stable system, obtains white gum sediment, and be washed with deionized, filtered and calcined after being dried in vacuo, ground after cooling standby；Take dried powder to be placed in the concentrated sulfuric acid, mixture of ice and water is poured into after being stirred at room temperature, lasting stirring；Sonicated, heating stirring is scrubbed, after drying, is made after ball milling.Pass through the improvement to conventional preparation techniques, so that prepared nano composite material has preferably dispersiveness and heat endurance, with bigger specific surface area and more preferable bioactivity, the preparation method condition of nano composite material of the present invention is simple, it is easily operated, and preparation process is very fast, cost is saved, suitable for popularization and application.
Description
Technical field
The invention belongs to field of material preparation, more particularly to a kind of preparation method of nano composite material.
Background technology
With the fast development of modern science and technology, various medical technology also obtain fast renewal, and some new materials are used
Medical recovery.It is a kind of conventional nontoxic nonreactive prototype that hydroxyapatite (HA) molecular formula, which is, have bioactivity and
The ceramic material of biocompatibility.Its surface has polarity, can produce stronger adhesion with body tissue, while have again very
Excellent bone conductivity, had a wide range of applications in bone tissue reparation and bone tissue alternative aspect.But HA itself be difficult to be molded, it is necessary to
With some other Material cladding especially with macromolecule is compound can just prepare bone renovating material.Traditional PEEK/HA composite woods
Material is prepared using the methods of in-situ polymerization, melt blending mostly.Because skeleton shape is different, and all it is by complexity
Curved surface is formed, and can not accomplish accurately to customize by traditional manufacturing process.
The content of the invention
A kind of present invention seek to address that above mentioned problem, there is provided preparation method of nano composite material.
A kind of preparation method of nano composite material, it is characterised in that comprise the following steps：
（1）Four water-calcium nitrate and diammonium hydrogen phosphate are configured to solution, calcium-phosphorus ratio 1.67, add the poly- second two of surfactant
Alcohol -2000, in the presence of being stirred vigorously, pH value are adjusted to 13 with ammoniacal liquor, is precipitated after making stable system, obtains white gum precipitation
Thing, precipitation is aged, and pH value is washed with deionized to 7, after filtering and being dried in vacuo, be placed in Muffle furnace and calcine, cool down
After grind it is standby；
（2）Take the dried PEEK powder of 2g to be placed in the 100mL concentrated sulfuric acids, be stirred at room temperature, the solution after the completion of reaction is poured into
In mixture of ice and water, continue stirring until faint yellow gelatinous precipitate and all separate out, it is about 7 to be washed with deionized to pH values, is filtered
After be drying to obtain SPEEK；
（3）HA powder and PEEK powder are dispersed in SPEEK DMF solution respectively, are ultrasonically treated 1h,
DMF is removed under heating stirring, high temperature, product is scrubbed, after drying, is made after the h of ball milling 12.
A kind of preparation method of nano composite material of the present invention, it is characterised in that the step（1）Described in sink
The shallow lake time is 1h.
A kind of preparation method of nano composite material of the present invention, it is characterised in that the step（1）Described in it is old
The change time is 20h.
A kind of preparation method of nano composite material of the present invention, it is characterised in that the step（1）Described in horse
Not the temperature of stove is 1000 DEG C.
A kind of preparation method of nano composite material of the present invention, it is characterised in that the step（3）Described in plus
Hot temperature is 120 DEG C, mixing time 24h.
A kind of preparation method of nano composite material of the present invention, passes through the improvement to conventional preparation techniques so that
Prepared nano composite material has preferably dispersiveness and heat endurance, has bigger specific surface area and preferably biology is living
Property, the preparation method condition of nano composite material of the present invention is simple, easily operated, and preparation process is very fast, saves
Cost, suitable for popularization and application.
Embodiment
A kind of preparation method of nano composite material, comprises the following steps：
（1）Four water-calcium nitrate and diammonium hydrogen phosphate are configured to solution, calcium-phosphorus ratio 1.67, add the poly- second two of surfactant
Alcohol -2000, in the presence of being stirred vigorously, pH value are adjusted to 13 with ammoniacal liquor, is precipitated after making stable system, obtains white gum precipitation
Thing, precipitation is aged, and pH value is washed with deionized to 7, after filtering and being dried in vacuo, be placed in Muffle furnace and calcine, cool down
After grind it is standby；
（2）Take the dried PEEK powder of 2g to be placed in the 100mL concentrated sulfuric acids, be stirred at room temperature, the solution after the completion of reaction is poured into
In mixture of ice and water, continue stirring until faint yellow gelatinous precipitate and all separate out, it is about 7 to be washed with deionized to pH values, is filtered
After be drying to obtain SPEEK；
（3）HA powder and PEEK powder are dispersed in SPEEK DMF solution respectively, are ultrasonically treated 1h,
DMF is removed under heating stirring, high temperature, product is scrubbed, after drying, is made after ball milling 12h.
A kind of preparation method of nano composite material of the present invention, the step（1）Described in the sedimentation time be 1h.
The step（1）Described in digestion time be 20h.The step（1）Described in Muffle furnace temperature be 1000 DEG C.The step
（3）Described in heating-up temperature be 120 DEG C, mixing time 24h.Reaction between PEEK and the concentrated sulfuric acid belongs to reversible reaction, and with
The progress of reaction, reaction product water can produce the effect of dilution to the sulfonating agent concentrated sulfuric acid, therefore sulfonation speed reduces.In DMF
Solubility is not high, the SPEEK reacted through 60h, the crosslinking and degraded of polymer is produced because sulfonation time is long, simultaneously because sulphur
Acidic group is continuously increased, and the steric hindrance that sulfonate radical enters back into sulfonation position constantly increases so that the sulfonation speed in system slows down.
Bulking agent SPEEK is surface-treated to nano HA, using on SPEEK strands-reaction between SO3H groups and nano HA
Strengthen HA and PEEK interface adhesions, while bulking agent is dispersed between PEEK/HA boundary, plays emulsification, so as to drop
Low phase interface can, and then play and make dispersion particle miniaturization and equally distributed effect.The cavitation effect of ultrasonic wave simultaneously,
In solution macromolecular chain can be made to substantially improve the dispersal behavior of inorganic filler.In SLS forming processes, composite powder is easy
Acted on by factors such as heat, oxygen, be easily caused flavescence and mechanical properties decrease.It is modified and super by bulking agent SPEEK surface
After sound, ball-milling treatment, the powder has preferably dispersiveness and heat endurance.
Claims (5)
1. a kind of preparation method of nano composite material, it is characterised in that comprise the following steps：
(1) four water-calcium nitrate and diammonium hydrogen phosphate are configured to solution, calcium-phosphorus ratio 1.67, add the poly- second two of surfactant
Alcohol -2000, in the presence of being stirred vigorously, pH value are adjusted to 13 with ammoniacal liquor, is precipitated after making stable system, obtains white gum precipitation
Thing, precipitation is aged, and pH value is washed with deionized to 7, after filtering and being dried in vacuo, be placed in Muffle furnace and calcine, cool down
After grind it is standby；
(2) take the dried PEEK powder of 2g to be placed in the 100mL concentrated sulfuric acids, be stirred at room temperature, the solution after the completion of reaction is poured into
In mixture of ice and water, continue stirring until faint yellow gelatinous precipitate and all separate out, it is about 7 to be washed with deionized to pH values, is filtered
After be drying to obtain SPEEK；
(3) HA powder and PEEK powder are dispersed in SPEEK DMF solution respectively, are ultrasonically treated 1h,
DMF is removed under heating stirring, high temperature, product is scrubbed, after drying, is made after the h of ball milling 12.
A kind of 2. preparation method of nano composite material as claimed in claim 1, it is characterised in that the step（1）Described in
Sedimentation time is 1h.
A kind of 3. preparation method of nano composite material as claimed in claim 1, it is characterised in that the step（1）Described in
Digestion time is 20h.
A kind of 4. preparation method of nano composite material as claimed in claim 1, it is characterised in that the step（1）Described in
The temperature of Muffle furnace is 1000 DEG C.
A kind of 5. preparation method of nano composite material as claimed in claim 1, it is characterised in that the step（3）Described in
Heating-up temperature is 120 DEG C, mixing time 24h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710994500.5A CN107875449A (en) | 2017-10-23 | 2017-10-23 | A kind of preparation method of nano composite material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710994500.5A CN107875449A (en) | 2017-10-23 | 2017-10-23 | A kind of preparation method of nano composite material |
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| Publication Number | Publication Date |
|---|---|
| CN107875449A true CN107875449A (en) | 2018-04-06 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201710994500.5A Withdrawn CN107875449A (en) | 2017-10-23 | 2017-10-23 | A kind of preparation method of nano composite material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113024993A (en) * | 2021-03-24 | 2021-06-25 | 广州机械科学研究院有限公司 | Polyether-ether-ketone composite material and preparation method and application thereof |
-
2017
- 2017-10-23 CN CN201710994500.5A patent/CN107875449A/en not_active Withdrawn
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113024993A (en) * | 2021-03-24 | 2021-06-25 | 广州机械科学研究院有限公司 | Polyether-ether-ketone composite material and preparation method and application thereof |
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Application publication date: 20180406 |