CN108658102A - A kind of raw materials of magnesium oxide and preparation method thereof improving magnesium phosphate cement biocompatibility - Google Patents
A kind of raw materials of magnesium oxide and preparation method thereof improving magnesium phosphate cement biocompatibility Download PDFInfo
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- CN108658102A CN108658102A CN201810489868.0A CN201810489868A CN108658102A CN 108658102 A CN108658102 A CN 108658102A CN 201810489868 A CN201810489868 A CN 201810489868A CN 108658102 A CN108658102 A CN 108658102A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/02—Magnesia
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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
- A61L27/02—Inorganic materials
- A61L27/025—Other specific inorganic materials not covered by A61L27/04 - A61L27/12
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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
- A61L27/02—Inorganic materials
- A61L27/12—Phosphorus-containing materials, e.g. apatite
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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
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B12/00—Cements not provided for in groups C04B7/00 - C04B11/00
- C04B12/02—Phosphate cements
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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
- 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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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Abstract
The present invention provides a kind of preparation methods of magnesium phosphate cement raw materials of magnesium oxide, by magnesia in 1600 ± 1 DEG C of 5 10h of temperature lower calcination, you can.The present invention also provides the raw materials of magnesium oxide being prepared and a kind of magnesium phosphate cements.Raw materials of magnesium oxide is obtained using calcination condition of the present invention, the magnesium phosphate cement cell proliferation rate of preparation is high, high without sensitization of skin reaction, histocompatbility, has good biocompatibility, clinical application good.
Description
Technical field
The invention belongs to biomaterial for medical purpose fields, and in particular to a kind of oxygen improving magnesium phosphate cement biocompatibility
Change magnesium raw material and preparation method thereof.
Background technology
The holder of human body is bone, but it is important also to assume responsibility for load-bearing, protection, hematopoiesis etc. other than the function of holder for bone
Function.Bone itself has certain regeneration and repair ability, but the wound for wound more than 6mm, bone disease (such as infection, bone
Cancer etc.) and geneogenous bone defect, it can not be repaired by the spontaneous repair ability of bone merely, need the treatment of surgical operation
And suitable bone renovating material promotes bone self-healing.Inorganic composition in bone accounts for about the total matter of bone based on calcium phosphorous compound
The 65% of amount, including hydroxyapatite, podolite, unformed calcium phosphate, calcium carbonate, calcium citrate, magnesium phosphate, phosphoric acid
Hydrogen sodium etc., and contain CO3 2-、Cl-、F-、Na+、K+、Mg+Plasma and Sr, Zn etc. are micro-.
The research and development of bone renovating material are always an important topic of orthopaedics, are a work in biomaterial research
The field of jump.Currently, clinically the more biologically active bone renovating material of application is mainly calcium phosphate material
(calcium phosphate cement, CPC), calcium phosphate material has good mechanical property, but calcium-phosphorus ratio is excessively high, leads
Cause its degradation in vivo slowly and no adhesion.In recent years, magnesium phosphate cement (magnesium phosphate cement,
MPC), also known as magnesium-based phosphate bone cement, with its early anti pressured intension is high, setting rate is fast, degradation speed is appropriate, has bonding
Property, and the Mg discharged in MPC degradation processes2+It can promote many good characteristics such as Oesteoblast growth to a certain extent, make it
Aspect is adhesively fixed in unstable fracture treatment and artificial prosthesis to be with a wide range of applications, therefore obtains the extensive pass of people
Note.
Magnesium phosphate cement is a kind of cementitious material made of being mixed with by magnesia, phosphate etc..Wherein, magnesia
Raw material is one of most important components of MPC, is generally made by magnesium hydroxide or basic magnesium carbonate high-temperature calcination.According to calcination temperature
Difference, magnesia obtained be divided into light-burned (900 DEG C or less), reheating (1000 DEG C or more) and melt oxidation magnesium (2800 DEG C with
On).It is generally acknowledged that dead burned magnesia optimum is used for MPC systems, such as：The patent application of 104815352 A of Publication No. CN
A kind of preparation method of the sodium phosphate magnesium base composite material for Bone Defect Repari is disclosed, the raw materials of magnesium oxide calcination condition used is：
10-12h at a temperature of 1200-1400 DEG C, but its raw materials of magnesium oxide prepared can not ensure the biocompatibility of composite material；It is open
Number a kind of preparation method of magnesium phosphate biology gelatine is disclosed for the patent application of 102416197 A of CN, the magnesia used is former
Expect that calcination condition is：3h at a temperature of 1100-1600 DEG C, the MgO activity prepared is uneven, the magnesium phosphate cement of preparation
Same biocompatibility is not ideal enough.
Therefore, magnesia preparation process is improved, it is excellent, no cytotoxicity to obtain good biocompatibility, degradation property
The material of bone cement containing magnesium is bone renovating material field technology personnel's urgent problem to be solved.
Invention content
The object of the present invention is to provide a kind of activated magnesia, the magnesium phosphate cement that it is prepared is made to have good biology
Compatibility and physicochemical property.
The present invention provides a kind of preparation methods of magnesium phosphate cement raw materials of magnesium oxide, by magnesia 1600 ± 1
DEG C temperature lower calcination 5-10h, you can.
Wherein, the specific method is as follows：
(1) magnesia is taken, is warming up to 1600 ± 1 DEG C, keeps the temperature 5h；
(2) it is cooled to room temperature, magnesia is taken out and crushes, sieving must calcine the raw materials of magnesium oxide 1 of 5h；
(3) by the raw materials of magnesium oxide 1 of step (2), it is warming up to 1600 ± 1 DEG C again, keeps the temperature 5h, then crushes, be sieved, obtain
Calcine the raw materials of magnesium oxide 2 of 10h.
Wherein, the rate of the heating is 10 ± 2 DEG C/min；
When the cooling, initial rate of temperature fall is 10 ± 2 DEG C/min, and after being down to 500 DEG C, rate of temperature fall is adjusted to 2 ± 1
℃/min。
Wherein, the sieving was 300 mesh sieve.
Wherein, the magnesia is medical grade magnesia.
The present invention also provides the raw materials of magnesium oxide that above-mentioned preparation method obtains.
The present invention also provides purposes of the above-mentioned raw materials of magnesium oxide in preparing magnesium phosphate cement.
The present invention also provides a kind of magnesium phosphate cements, by the preparation of magnesia, phosphate, sugar, calcium salt and solidify liquid
At the magnesia is above-mentioned raw materials of magnesium oxide.
Wherein, the raw material that the powder is matched by following weight is prepared：2~4 parts of raw materials of magnesium oxide, potassium phosphate 2~4
Part, 0.1~1 part of sucrose, 0.1~1 part of hydroxyapatite；
The solidify liquid is the phosphoric acid solution that mass fraction is 15%.
The present invention also provides purposes of the above-mentioned magnesium phosphate cement in preparing bone renovating material.
It is generally believed that with the raising of calcination temperature, the extension of calcination time, magnesia body surface area smaller obtained,
Hydration activity is lower, and the magnesium phosphate cement performance prepared may be more excellent.
Inventor long-term experiment research in find, the bio-compatible of raw materials of magnesium oxide calcine technology and magnesium phosphate cement
Property it is closely related, when use calcine technology of the present invention, i.e., magnesia is first calcined to 5h at a certain temperature, then blocking by being sintered
Magnesia calcines 5h after pulverizing, the raw materials of magnesium oxide of acquisition is used to prepare MPC, may make MPC good physical properties, bio-compatible
Property is good；On this basis, change calcination temperature, time, then the MPC biocompatibilities that prepared by raw materials of magnesium oxide are poor, uncomfortable
In clinical application.
Obviously, the above according to the present invention is not being departed from according to the ordinary technical knowledge and customary means of this field
Under the premise of the above-mentioned basic fundamental thought of the present invention, the modification, replacement or change of other diversified forms can also be made.
The specific implementation mode of form by the following examples remakes further specifically the above of the present invention
It is bright.But the range that this should not be interpreted as to the above-mentioned theme of the present invention is only limitted to example below.It is all to be based on the above of the present invention
The technology realized all belongs to the scope of the present invention.
Description of the drawings
Fig. 1 is bone tissue slice map：A, b, c, d are control sample, and e, f, g, h are MPC of the present invention, and wherein a, e are implantation 1
Week；B, f is implantation 4 weeks；C, g is implantation 12 weeks；D, h is implantation 26 weeks.
Specific implementation mode
It is described further below with embodiment, but the present invention is not limited to these embodiments.
The experiment reagent and instrument that the present invention uses are as follows：
Medical grade MgO is purchased from Xingtai metallurgy Mei Ye Co., Ltds, KH2PO4Purchased from Hunan Jiudian Pharmaceutical Co., Ltd,
Hydroxyapatite is provided by Sichuan University's biomaterial Engineering Research Center.Remaining reagent is purchased from Chengdu section dragon chemical reagent
Factory.1700 DEG C of accurate case type experiment electric stoves (Shanghai hard iron crystalline substance SXL-1700), biochemical cultivation case (KXB-250A analyses in Shanghai section), planet
Formula ball milling instrument (Retsch-PM400).
1 magnesia forging technology of embodiment
1, the raw materials of magnesium oxide of calcining 5h is obtained
MgO is put into the crucible of base diameter 10cm high 10cm, crucible is then put into high-temperature experiment electric stove (Shanghai hard iron
It is brilliant).Electric furnace heats up 0 DEG C -1600 DEG C, and heating rate is 10 ± 2 DEG C/min, and heat up total time-consuming 160min.
Electric furnace keeps the temperature 5h at 1600 ± 1 DEG C.
Carry out 1600 DEG C -500 DEG C of cooling, rate of temperature fall is 10 ± 2 DEG C/min, and when 500 DEG C of furnace temperature, electric furnace starts journey
Sequence cools down, and rate of temperature fall is 2 ± 1 DEG C/min.
When electric furnace is cooled to room temperature, blocking MgO will be sintered and taken out, pulverized with mortar, ground by planetary type ball-milling instrument
Grind 1h (300r/min suspends 5s per 30s).
MgO after milling obtains the MgO raw materials 1 of 1600 DEG C of heat preservation 5h by nylon mesh (300 mesh) sieving, and grain size is less than 45
μm。
2, the raw materials of magnesium oxide of calcining 10h is obtained
MgO (raw materials of magnesium oxide of calcining 5h) of the grain size less than 45 μm that sieving obtains is calcined into 5h again, grind,
300 mesh nylon mesh are crossed, the MgO raw materials of calcining 10h are obtained.
Embodiment 2 prepares magnesium phosphate cement
Prepare powder：2~4g of raw materials of magnesium oxide, the potassium phosphate 2~4g, HA for the calcining 5h or 10h that Example 1 obtains
(hydroxyapatite) 0.1~1g, sucrose 0.1~1g mixing, it is spare using 25KGy irradiation sterilizations；
Prepare solidify liquid (15% phosphoric acid solution)：By phosphatase 11 5g, sodium dihydrogen phosphate 5-6g, sodium chloride 1-2g, pure water
77-79g is mixed, spare with 121 DEG C of high pressure sterilizations 30 minutes；
Powder and solidify liquid are sufficiently stirred into slurry with 0.2-0.4ml/g, solidification both magnesium phosphate cement of the present invention.
Beneficial effects of the present invention are illustrated below by way of test example：
The Study on Biocompatibility of the different magnesium phosphate cements of test example 1
Raw materials of magnesium oxide is prepared by different calcination conditions first, it is as follows respectively：
Contrast groups (1 sample of number)：It, specifically will doctor with reference to the preparation of the magnesium phosphates biology gelatine such as Li Junming and performance characterization
1300 DEG C of calcining 3h are carried out with grade MgO with chamber type electric resistance furnace (SRJX-4-13), utilize planetary ball mill (QM-3SP2) ball milling
It is crushed to average grain diameter and is less than 10 μm.
2 sample of number：According to 1 method of embodiment, the calcining 5h raw materials of magnesium oxide of acquisition.
3 sample of number：According to 1 method of embodiment, the calcining 10h raw materials of magnesium oxide of acquisition.
4 sample of number：It is the raw materials of magnesium oxide that 15h is calcined at 1600 DEG C, preparation method is as follows：Take present invention calcining 10h
MgO (1 method of embodiment), according to method in the embodiment of the present invention 1, again after heating calcining 5h, 300 mesh nylon are crossed in grinding
Sieve, you can.
Each experiment is as follows：
1, cell in vitro poison is tested
Magnesia in order to compare different temperatures calcining prepares it influence of bone-cement biological compatibility, is compared
Experiment is tested using cell in vitro poison to verify biocompatibility, and cell proliferation rate is higher, and biocompatibility is better.
Experimental method：
By 2~4g of magnesia (being respectively the raw materials of magnesium oxide that different calcination temperatures obtain), potassium phosphate 2~4g, HA (hydroxyl
Apatite) 0.1~1g, 0.1~1g of sucrose is mixed, spare using 25KGy irradiation sterilizations.Solidify liquid (15% phosphoric acid solution：
Mixed by phosphatase 11 5g sodium dihydrogen phosphate 5-6g sodium chloride 1-2g pure water 77-79g) with 121 DEG C of high pressure sterilizations 30 minutes, then
Powder and solidify liquid are sufficiently stirred into magnesium phosphate slurry (slurry i.e. before magnesium phosphate cement solidification) with 0.2-0.4ml/g,
Then slurry is filled into syringe, is injected into the RPMI1640 cell culture fluids for being preinstalled with 1ml and (is noted by 0.2g/ml
Enter), it (is extracted with RPMI1640 cell culture fluids) after 37 DEG C of extractions for 24 hours and takes 929 cells of supernatant culture NCTC clone, profit
Cell proliferative conditions are detected with the method for CCK8, the specific standard by GB/T16886.5-2003 executes.
Cell proliferation rate is as shown in table 1.
The cell proliferation rate of 1 each sample of table
| Sample number into spectrum | Calcination temperature (DEG C) | Calcination time (h) | Cell proliferation rate |
| 1 | 1300 | 3 | 85.63±1.63 |
| 2 | 1600 | 5 | 91.77±1.82 |
| 3 | 1600 | 10 | 104.76±2.50 |
| 4 | 1600 | 15 | 74.72±2.02 |
As shown in Table 1, in a certain range with magnesia calcination temperature, the increase of time, the biology of the MPC prepared
Compatibility also opposite enhancing, but upon calcination between reach certain value after, the MPC that is prepared with the increase of calcination time, magnesia
Biocompatibility reduce.
Wherein, the cell proliferation rate highest of the MPC prepared with the magnesia obtained when 1600 DEG C of heat preservation 10h of calcination temperature,
Illustrate that biocompatibility is best, and then biocompatibility is poor under other calcination conditions.
2, sensitization of skin is tested
Compare the sensitization of skin reaction of the bone cement of the magnesia preparation of different temperatures calcining, positive control with animal model
2.4- dinitrofluorobenzene is selected to be configured to the olive oil solution of a concentration of 40ml/L.
According to GB/T 16886.10, bone cement, which needs to extract, obtains leaching liquor, and leaching liquor is cooked Skin sensitization.
Experimental method：The extraction of sample, using double extractions, polar solvent selects physiological saline, nonpolarity molten for this experiment
Sesame oil is selected in agent.Each sample is prepared into slurry by preceding method, is filled into syringe, the pole for being preinstalled with 1ml is injected into
Property or nonpolar solvent in (by 0.2g/ml inject), 37 DEG C extraction for 24 hours after, take supernatant spare.
25 healthy rabbits are selected, are divided into 5 groups：I.e.：Polar solvent extracts embodiment, and nonpolar solvent extracts embodiment,
Polar solvent extraction contrast groups, nonpolar solvent extraction contrast groups, positive control (SDS that i.e. GB/T 16886.10 is mentioned) group,
Every group 5." embodiment " the i.e. MPC slurries of 3 sample preparation of number；" contrast groups " the i.e. MPC of 1 sample preparation of number
Slurry.
Bilateral spinal dorsal body setae is removed before experiment.Leaching liquor is dripped on the absorbability gauze of 2.5x2.5cm sizes, every piece
Gauze drips 0.5ml, and gauze is spread on a rabbit back both sides, and per the point of side 2, every rabbit applies 4 points, then fixed with bandage altogether
4h.Then 1h after removal applying patch, for 24 hours, 48h, 72h record each contact site situation.
Dermoreaction scores and stimulates classification to be executed with reference to GB/T16886.10-2003 Plays.
Experimental result is as shown in table 2.
2 each sample stimulate the reaction situation of table counts
| Sample | Mean score | Reaction type |
| Polar solvent extracts embodiment | 0 | Nothing |
| Nonpolar solvent extracts embodiment | 0.2 | It is extremely slight |
| Polar solvent extracts contrast groups | 0.3 | It is extremely slight |
| Nonpolar solvent extracts contrast groups | 0.4 | Slightly |
| Positive control | 5 | Severe |
As known from Table 2, when preparing magnesium phosphate cement leaching liquor using raw materials of magnesium oxide, polarity and nonpolar solvent
It uses, the leaching liquor of preparation is weaker to the sensitivity response of family's rabbit skin, the extraction especially prepared with raw materials of magnesium oxide of the present invention
Liquid, almost without sensitivity response.
3, rabbit bone condyle implantation experiment
Compare inventive samples (i.e. the MPC of 3 sample preparation of number) and commercial like product (self-curing phosphorus with animal model
Sour calcium bone cement CPC is purchased from Shanghai Ruibang Biological Material Co., Ltd.) inflammatory reaction after bone implantation, situation of degrading and new
Raw bone-shaped condition.
Experimental method：(1) animal prepares：26 healthy new zealand white rabbits are selected, are raised under same rearing conditions
After 10 days, every White Rabbit rabbit weight is in 3-4kg.(2) sample preparation：The sample injection of slurry shape is entered into internal diameter 6mm, long 10mm
Pp plastic tubes in, taken out after sample half solidifies and obtain 6mm × 10mm cylindrical sample blocks.(3) it is implanted into：Every New Zealand
White Rabbit uses the sodium intravenous anesthesia of amobarbital.At the bone condyle of two leg of rabbit respectively with surgical drill punch to obtain 6mm ×
The bone defect of 10mm, will be in inventive samples and control CPC implantation bone defects.Left side is inventive samples, and right side is control sample
Product.Postoperative continuous three days intramuscular injection penicillin prevents from infecting and observing every White Rabbit body temperature and implant site verification situation.
6 White Rabbits are put to death after being implanted into 1 week, 4 weeks, 12 weeks, 26 weeks respectively, implantation is put to death 2 White Rabbits after 2 weeks, taken
Material, 10% formalin are fixed, paraffin embedding, conventional section, and hematoxylin eosin staining does tissue-estimating with light microscope.
Histological evaluation executes according to standard specified in GB/T16886.6-1997.Establishing criteria, from inflammation, material degradation and surrounding
Tissue reflection carries out histological observation.
Experimental result：(1) the postoperative 1st, 2,3 day, each implant site had slight redness, control group redness degree slightly heavy.Body
It slightly decreases again, other indexs are normal；Postoperative 3rd week, each implant site redness disappeared, and weight is gradually increasing, other indexs
Normally.
(2) inflammation：Material is implanted into 1 week, and polarity inflammation is presented in implantation point, it is seen that neutrophil cell, eosinophil,
It is the most apparent with control sample；Inflammatory reaction weakens after 2 weeks；There is a small amount of lymphocytic infiltration after 4 weeks, is in chronic inflammation.12 weeks
The inflammation of inventive samples disappears substantially afterwards, but control sample is still in chronic inflammation, until the inflammation ability of 26 weeks control samples
It is basic to disappear.
(3) degradation situation：1 week present invention and control material are without significant change, since the 4th week, sample of the present invention after implantation
Product and control sample all start to degrade, but the degradation rate of inventive samples is significantly faster than that control material, inventive samples are dropping
New bone is also being grown while solution, and the rate of new bone growth is suitable with degradation rate (as shown in Figure 1).
As it can be seen that the magnesium phosphate cement prepared using the method for the present invention, has good histocompatbility after bone implantation.
Therefore, raw materials of magnesium oxide is obtained using calcination condition of the present invention, the magnesium phosphate cement cell proliferation rate of preparation is high,
No sensitization of skin reaction, histocompatbility are high, have good biocompatibility, clinical application good.
Claims (10)
1. a kind of preparation method of magnesium phosphate cement raw materials of magnesium oxide, it is characterised in that：By magnesia in 1600 ± 1 DEG C of temperature
Degree is lower to calcine 5-10h, you can.
2. the preparation method of raw materials of magnesium oxide according to claim 1, it is characterised in that：The specific method is as follows：
(1) magnesia is taken, is warming up to 1600 ± 1 DEG C, keeps the temperature 5h；
(2) it is cooled to room temperature, magnesia is taken out and crushes, sieving must calcine the raw materials of magnesium oxide 1 of 5h；
(3) by the raw materials of magnesium oxide 1 of step (2), it is warming up to 1600 ± 1 DEG C again, keeps the temperature 5h, then crushes, be sieved, must calcine
The raw materials of magnesium oxide 2 of 10h.
3. the preparation method of raw materials of magnesium oxide according to claim 2, it is characterised in that：
The rate of the heating is 10 ± 2 DEG C/min；
When the cooling, initial rate of temperature fall be 10 ± 2 DEG C/min, after being down to 500 DEG C, rate of temperature fall be adjusted to 2 ± 1 DEG C/
min。
4. the preparation method of raw materials of magnesium oxide according to claim 2, it is characterised in that：The sieving was 300 mesh sieve.
5. according to the preparation method of raw materials of magnesium oxide described in claim 1-4 any one, it is characterised in that：The magnesia is
Medical grade magnesia.
6. the raw materials of magnesium oxide that claim 1-5 any one preparation methods obtain.
7. purposes of the raw materials of magnesium oxide described in claim 6 in preparing magnesium phosphate cement.
8. a kind of magnesium phosphate cement is prepared by magnesia, phosphate, sugar, calcium salt and solidify liquid, it is characterised in that：Institute
It is the raw materials of magnesium oxide described in claim 6 to state magnesia.
9. magnesium phosphate cement according to claim 8, it is characterised in that：
The raw material that the powder is matched by following weight is prepared：2~4 parts of raw materials of magnesium oxide, 2~4 parts of potassium phosphate, sucrose
0.1~1 part, 0.1~1 part of hydroxyapatite；
The solidify liquid is the phosphoric acid solution that mass fraction is 15%.
10. purposes of the magnesium phosphate cement of claim 8 or 9 in preparing bone renovating material.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111888521A (en) * | 2020-06-11 | 2020-11-06 | 上海蕴邦生物科技有限公司 | Bone repair material and preparation method thereof |
| CN113209369A (en) * | 2021-04-29 | 2021-08-06 | 西安理工大学 | Preparation method of high-porosity magnesium phosphate bone cement composite porous scaffold |
| CN114053476A (en) * | 2021-11-30 | 2022-02-18 | 西华师范大学 | Antibacterial magnesium phosphate bone cement and preparation method and application thereof |
| CN115444967A (en) * | 2022-08-08 | 2022-12-09 | 武汉理工大学 | Bioactive hard tissue adhesive and preparation method and application thereof |
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| CN1683607A (en) * | 2004-04-14 | 2005-10-19 | 上海祯吉电子新材料有限公司 | Process for producing high temperature super conductivity material magnesium oxide single crystal and preparing device |
| CN102515576A (en) * | 2011-12-05 | 2012-06-27 | 苏州达普生物技术有限公司 | Magnesium oxide for magnesium phosphate concrete, preparation method of magnesium oxide and magnesium phosphate concrete |
| CN105329922A (en) * | 2015-12-15 | 2016-02-17 | 营口镁质材料研究院有限公司 | Preparation method of magnesium oxide crystal powder |
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| CN111888521A (en) * | 2020-06-11 | 2020-11-06 | 上海蕴邦生物科技有限公司 | Bone repair material and preparation method thereof |
| CN113209369A (en) * | 2021-04-29 | 2021-08-06 | 西安理工大学 | Preparation method of high-porosity magnesium phosphate bone cement composite porous scaffold |
| CN114053476A (en) * | 2021-11-30 | 2022-02-18 | 西华师范大学 | Antibacterial magnesium phosphate bone cement and preparation method and application thereof |
| CN114053476B (en) * | 2021-11-30 | 2022-11-25 | 西华师范大学 | Antibacterial magnesium phosphate bone cement and preparation method and application thereof |
| CN115444967A (en) * | 2022-08-08 | 2022-12-09 | 武汉理工大学 | Bioactive hard tissue adhesive and preparation method and application thereof |
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