CN101757685A - Preparation method of medical glass fiber magnesium-containing hydroxyapatite bone cement product - Google Patents
Preparation method of medical glass fiber magnesium-containing hydroxyapatite bone cement product Download PDFInfo
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- CN101757685A CN101757685A CN201010000968A CN201010000968A CN101757685A CN 101757685 A CN101757685 A CN 101757685A CN 201010000968 A CN201010000968 A CN 201010000968A CN 201010000968 A CN201010000968 A CN 201010000968A CN 101757685 A CN101757685 A CN 101757685A
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- glass fiber
- containing hydroxyapatite
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Abstract
The invention relates to a preparation method of a medical glass fiber magnesium-containing hydroxyapatite bone cement product, which comprises the steps of: mixing calcium nitrate, diammonium hydrogen phosphate and urea, adding magnesium phosphate, mixing and stirring, adding magnesium-containing hydroxyapatite prepared by heating into a magnesium oxychloride adhesive, wherein the magnesium oxychloride adhesive is prepared by adding water to dissolve magnesium chloride and magnesium oxide mixture; pasting by using hands to form a prefabricated member; spreading slurry and glass fiber fabrics, flattening and uniformly spreading, brushing the adhesive; spreading a prefabricated external outer skin, and compacting; sealing joints by using a plastic thin film; curing and demoulding; and finishing the product within one day after the demoulding to obtain the bone cement product. Glass fibers in a composite material prepared by the invention are dispersed uniformly, and the magnesium-containing hydroxyapatite is well bonded with a matrix interface, therefore, the medical glass fiber magnesium-contained hydroxyapatite bone cement product is a biological medical composite material with an extremely wide application prospect.
Description
One, technical field:
The present invention relates to a kind of preparation method that magnesium strengthens bone cement product, particularly a kind of preparation method of medical glass fiber magnesium-containing hydroxyapatite bone cement goods of containing.
Two, background technology:
Because reasons such as aged tendency of population, pathological changes, vehicle accident, earthquakes, annual all have a large amount of fracture patients internal fixation operation of need fracturing.Many biomaterials that are prepared from by metal and polymeric material are used for the treatment of orthopaedic disease, but there is significant defective in these materials, as: the mechanical compatibility of metal material and osseous tissue is bad, causes the loosening or dislocation of implant; Produce stress-shielding effect, cause the loose or osteanabrosis of fracture, it is silly to form bone at fracture site, is prone to the secondary fracture; The release of metal ion can cause anaphylaxis; Metal material needs second operation to take out implant; Discharge acidic materials during the polymeric material degrades of present clinical use, cause the non-bacterial inflammatory reaction, and influence the active and propagation of seed cell or somatomedin.Therefore, many research worker are devoted to develop natural polymer and the compound new bio medical material of hydroxyapatite, to satisfy the requirement of the clinical use of orthopaedics.
Hydroxyapatite is an inorganic constituents main in the nature bone, have special bone conductibility, with the good and high moisture resistance of synosteosis, be used to the clinical repair and the reconstruction of sclerous tissues.Nascent hydroapatite particles has very high absorbance and excellent biological compatibility in vivo, not only is widely used in orthopedic bone and transplants, also by the sustained release of drug delivery system.Help degraded and absorbed and stimulate new bone growth in the physiological environment small-medium size, the low-crystallinity of hydroxyapatite means high rate of dissolution, the Ca2+ ion that discharges is absorbed by osseous tissue and regenerates Ca---P inorganic mineral, thereby can promote the generation of osteoblastic adhesion, differentiation and new bone.
Therefore, develop a kind of medical composite glass fiber and contain magnesium enhancing bone cement product,, have great social significance and economic worth to satisfy the clinical instructions for use of orthopaedics.
Three, summary of the invention:
The purpose of this invention is to provide a kind of method for preparing the medical glass fiber magnesium-containing hydroxyapatite bone cement goods, this method can make high-intensity magnesium-containing hydroxyapatite bone fracture internal fixation material---and medical composite glass fiber contains magnesium and strengthens bone cement product.
The preparation method of medical glass fiber magnesium-containing hydroxyapatite bone cement goods of the present invention is characterized in that described bone cement product main material weight proportion is:
Glass fibre 40 ∽ 50 grams; Magnesium-containing hydroxyapatite 1 ∽ 5 grams;
Magnesium oxide 2 ∽ 5 grams; Magnesium chloride 4 ∽ 10 grams;
Water 15 ∽ 25 grams; Additive 2 ∽ 5 grams;
Described magnesium-containing hydroxyapatite preparation method is:
A, with lime nitrate Ca (NO
3)
2, diammonium phosphate (NH
4)
2HPO
4With carbamide CO (NH
2)
22: 3: 5 by volume ∽ of solution mix at 3: 1: 6;
B, magnesium salt is added in the mixed liquor, at 300 ℃ of temperature 100 ∽ reaction 1 ∽ 6 hours down;
C, reaction finish the back natural cooling, pour in the there-necked flask, leave standstill layering;
D, with the supernatant liquid elimination, residue is with flushing with clean water 2 ∽ 4 times, reuse alcohol wash 3 ∽ 5 times, sample;
E, use the alcohol burner heating, drying, after put into Muffle furnace and calcine, the time is 2 ∽ 7 hours;
Behind f, the natural cooling, after the grinding, promptly get magnesium-containing hydroxyapatite.
Acceptable magnesium salt is on the described materia medica: magnesium phosphate Mg
3(PO
4)
2, magnesium nitrate Ma (NO
3)
2Or magnesium carbonate MgCO
3
The preparation method of described chlorine oxygen magnesium adhesive is:
A, magnesium chloride is added water-solubleization, be made into certain density solution;
B, adding magnesium oxide mix and stir, and the time is 10min;
C, add additive in mixed liquor, behind the water reducer, fully stir, the time is 15min;
D, adding chopped strand are made slurry.
Acceptable additive is on the 5 described materia medicas: activated alumina, ferrum oxide, copper oxide, water-soluble polyester resin, polyacrylamide, mineral powder filler; Acceptable chopped strand is on the described materia medica: glass fibre, Plant fiber, sawdust.
The denseness of described slurry is controlled with amount of water.
The preparation method of described composite glass fiber is:
A, be 0.2 ∽ 0.4mm with average thickness, diameter is that the glass fabric of 10 ∽, 13 μ m soaks with 30% sodium peroxide, and is standby in 100 ℃ of dry down backs of 80 ∽;
B, magnesium-containing hydroxyapatite is joined in the chlorine oxygen magnesium adhesive, batching fully stirs, and is standby;
C, exterior skin are made two and half skeleton shape prefabricated components;
D, stuck with paste the internal layer eyelid covering, spread plastic foamboard, pasted firmly,, shakeout, spread equal brush coating at plastic foamboard upper berth slurry, shop glass fabric;
E, then prefabricated exterior skin is spread, compacting, seam crossing is sealed with plastic sheeting;
After f, the curing, open thin film, the demoulding promptly gets medical composite glass fiber and contains magnesium enhancing bone cement product.
Described fiber glass reinforcement is: middle alkali fiber woven roving or grid cloth, high alkali fiber woven roving or grid cloth.
In the described blending process, the remaining slurry of gel can not be joined in the slip of the system of newly mixing.
Solidify under the described room temperature, its temperature is 35 ℃ of 15 ∽, 14 ∽ demouldings after 20 hours, and the goods finishing is finished after the demoulding, is preferably in two days.
Beneficial effect of the present invention is: magnesium-containing hydroxyapatite joins in the chlorine oxygen magnesium adhesive, makes glass fibre woven roving or grid cloth form the build network-like structure, becomes fine and close more, becomes tightr between layer and the layer.Simultaneously, the magnesium-containing hydroxyapatite granule becomes tightr, and size reduces, and can satisfy the clinical instructions for use of fracture internal fixation.
Four, specific embodiment:
Further specify the present invention below in conjunction with specific embodiment.
Embodiment 1:
1) took by weighing lime nitrate Ca (NO in 2: 3: 5 by volume
3)
2, diammonium phosphate (NH
4)
2HPO
4With carbamide CO (NH
2)
2, after the mixing, add 2 parts magnesium phosphate with volume ratio, stir 10min, form the hydroxyapatite precursor solution, react 6 hours after-filtration down for 260 ℃ in temperature, put into Muffle furnace to calcine, the time is 6 hours, behind the natural cooling, after the grinding, promptly get magnesium-containing hydroxyapatite;
2) 5 gram magnesium chlorides are added 20 water-solubleization of gram, be made into certain density solution, add 2 gram magnesium oxide again, after mixing stirring 10min, add the water-soluble polyester resin of 0.6 gram, behind the water reducer, fully stir 15min, add short glass fiber at last, make chlorine oxygen magnesium adhesive;
3) magnesium-containing hydroxyapatite 3 grams are joined in the 30 gram chlorine oxygen magnesium adhesives, batching fully stirs, and is standby;
4) exterior skin is made two and half skeleton shape prefabricated components, has stuck with paste the internal layer eyelid covering, spreads plastic foamboard, paste firmly,, shakeout, spread equal brush coating at plastic foamboard upper berth slurry, shop glass fabric, then prefabricated exterior skin is spread, compacting, seam crossing is sealed with plastic sheeting, solidifies.
5) under the room temperature, temperature is solidified down at 25 ℃, the demoulding after 19 hours, and the goods finishing is finished in two days after the demoulding, promptly gets medical composite glass fiber and contains magnesium enhancing bone cement product.
Embodiment 2:
1) took by weighing lime nitrate Ca (NO in 3: 3: 4 by volume
3)
2, diammonium phosphate (NH
4)
2HPO
4With carbamide CO (NH
2)
2, after the mixing, add 3 parts magnesium carbonate with volume ratio, stir 10min, form the hydroxyapatite precursor solution, react 6.5 hours after-filtration down for 280 ℃ in temperature, put into Muffle furnace to calcine, the time is 7 hours, behind the natural cooling, after the grinding, promptly get magnesium-containing hydroxyapatite;
2) 6 gram magnesium chlorides are added 20 water-solubleization of gram, be made into certain density solution, add 2 gram magnesium oxide again, after mixing stirring 10min, add the water-soluble polyester resin and the 0.2 gram mineral powder filler of 0.5 gram, behind the water reducer, fully stir 20min, add short glass fiber at last, make chlorine oxygen magnesium adhesive;
3) magnesium-containing hydroxyapatite 4 grams are joined in the 30 gram chlorine oxygen magnesium adhesives, batching fully stirs, and is standby;
4) exterior skin is made two and half skeleton shape prefabricated components, has stuck with paste the internal layer eyelid covering, spreads plastic foamboard, paste firmly,, shakeout, spread equal brush coating at plastic foamboard upper berth slurry, shop glass fabric, then prefabricated exterior skin is spread, compacting, seam crossing is sealed with plastic sheeting, solidifies.
5) heat down, temperature is solidified down at 70 ℃, the demoulding after 10 hours, and the goods finishing is finished in the demoulding one day after, promptly gets medical composite glass fiber and contains magnesium enhancing bone cement product.
Embodiment 3:
1) took by weighing lime nitrate Ca (NO in 3: 1: 6 by volume
3)
2, diammonium phosphate (NH
4)
2HPO
4With carbamide CO (NH
2)
2, after the mixing, add 3 parts magnesium phosphate with volume ratio, stir 10min, form the hydroxyapatite precursor solution, react 6 hours after-filtration down for 300 ℃ in temperature, put into Muffle furnace to calcine, the time is 7 hours, behind the natural cooling, after the grinding, promptly get magnesium-containing hydroxyapatite;
2) 7 gram magnesium chlorides are added 20 water-solubleization of gram, be made into certain density solution, add 2 gram magnesium oxide again, after mixing stirring 10min, add the polyacrylamide of 0.4 gram, behind the water reducer, fully stir 20min, add short glass fiber at last, make chlorine oxygen magnesium adhesive;
3) magnesium-containing hydroxyapatite 4 grams are joined in the 30 gram chlorine oxygen magnesium adhesives, batching fully stirs, and is standby;
4) exterior skin is made two and half skeleton shape prefabricated components, has stuck with paste the internal layer eyelid covering, spreads plastic foamboard, paste firmly,, shakeout, spread equal brush coating at plastic foamboard upper berth slurry, shop glass fabric, then prefabricated exterior skin is spread, compacting, seam crossing is sealed with plastic sheeting, solidifies.
5) heat down, temperature is solidified down at 60 ℃, the demoulding after 12 hours, and the goods finishing is finished in the demoulding one day after, promptly gets medical composite glass fiber and contains magnesium enhancing bone cement product.
Attention: in the blending process, the remaining slurry of gel can not be joined in the slip of the system of newly mixing.
Claims (10)
1. the preparation method of medical glass fiber magnesium-containing hydroxyapatite bone cement goods is characterized in that described bone cement product main material weight proportion is:
Glass fibre 40 ∽ 50 grams; Magnesium-containing hydroxyapatite 1 ∽ 5 grams;
Magnesium oxide 2 ∽ 5 grams; Magnesium chloride 4 ∽ 10 grams;
Water 15 ∽ 25 grams; Additive 2 ∽ 5 grams;
2. the preparation method of medical glass fiber magnesium-containing hydroxyapatite bone cement goods according to claim 1 is characterized in that described magnesium-containing hydroxyapatite preparation method is:
A, with lime nitrate Ca (NO
3)
2, diammonium phosphate (NH
4)
2HPO
4With carbamide CO (NH
2)
22: 3: 5 by volume ∽ of solution mix at 3: 1: 6;
B, magnesium salt is added in the mixed liquor, at 300 ℃ of temperature 100 ∽ reaction 1 ∽ 6 hours down;
C, reaction finish the back natural cooling, pour in the there-necked flask, leave standstill layering;
D, with the supernatant liquid elimination, residue is with flushing with clean water 2 ∽ 4 times, reuse alcohol wash 3 ∽ 5 times, sample;
E, use the alcohol burner heating, drying, after put into Muffle furnace and calcine, the time is 2 ∽ 7 hours;
Behind f, the natural cooling, after the grinding, promptly get magnesium-containing hydroxyapatite.
3. the preparation method of medical glass fiber magnesium-containing hydroxyapatite bone cement goods according to claim 1 and 2 is characterized in that acceptable magnesium salt is on the described materia medica: magnesium phosphate Mg
3(PO
4)
2, magnesium nitrate Ma (NO
3)
2Or magnesium carbonate MgCO
3
4. the preparation method of medical glass fiber magnesium-containing hydroxyapatite bone cement goods according to claim 1 is characterized in that the preparation method of described chlorine oxygen magnesium adhesive is:
A, magnesium chloride is added water-solubleization, be made into certain density solution;
B, adding magnesium oxide mix and stir, and the time is 10min;
C, add additive in mixed liquor, behind the water reducer, fully stir, the time is 15min:
D, adding chopped strand are made slurry.
5. according to the preparation method of claim 1 or 4 described medical glass fiber magnesium-containing hydroxyapatite bone cement goods, it is characterized in that acceptable additive is on the described materia medica: activated alumina, ferrum oxide, copper oxide, water-soluble polyester resin, polyacrylamide, mineral powder filler; Acceptable chopped strand is on the described materia medica: glass fibre, Plant fiber, sawdust.
6. according to the preparation method of claim 1 or 4 described medical glass fiber magnesium-containing hydroxyapatite bone cement goods, it is characterized in that the denseness of described slurry is controlled with amount of water.
7. the preparation method of medical glass fiber magnesium-containing hydroxyapatite bone cement goods according to claim 1 is characterized in that the preparation method of described composite glass fiber is:
A, be 0.2 ∽ 0.4mm with average thickness, diameter is that the glass fabric of 10 ∽, 13 μ m soaks with 30% sodium peroxide, and is standby in 100 ℃ of dry down backs of 80 ∽;
B, magnesium-containing hydroxyapatite is joined in the chlorine oxygen magnesium adhesive, batching fully stirs, and is standby;
C, exterior skin are made two and half skeleton shape prefabricated components;
D, stuck with paste the internal layer eyelid covering, spread plastic foamboard, pasted firmly,, shakeout, spread equal brush coating at plastic foamboard upper berth slurry, shop glass fabric;
E, then prefabricated exterior skin is spread, compacting, seam crossing is sealed with plastic sheeting;
After f, the curing, open thin film, the demoulding promptly gets medical composite glass fiber and contains magnesium enhancing bone cement product.
8. according to the preparation method of claim 1 or 7 described medical glass fiber magnesium-containing hydroxyapatite bone cement goods, it is characterized in that described fiber glass reinforcement is: middle alkali fiber woven roving or grid cloth, high alkali fiber woven roving or grid cloth.
9. according to the preparation method of claim 1 or 7 described medical glass fiber magnesium-containing hydroxyapatite bone cement goods, it is characterized in that in the described blending process, the remaining slurry of gel can not be joined in the slip of the system of newly mixing.
10. according to the preparation method of claim 1 or 7 described medical glass fiber magnesium-containing hydroxyapatite bone cement goods, it is characterized in that solidifying under the described room temperature, its temperature is 35 ℃ of 15 ∽, 14 ∽ demouldings after 20 hours, the goods finishing is finished after the demoulding, is preferably in two days.
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|---|---|---|---|
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|---|---|---|---|
| CN201010000968A CN101757685A (en) | 2010-01-22 | 2010-01-22 | Preparation method of medical glass fiber magnesium-containing hydroxyapatite bone cement product |
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ID=42489167
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104013539A (en) * | 2014-03-20 | 2014-09-03 | 胡方 | Preparation method of bone repair toothpaste agent inducing gene expression |
| CN104591679A (en) * | 2015-01-31 | 2015-05-06 | 河南理工大学 | Modified magnesium oxychloride bone cement as well as preparation method and application thereof |
| CN111417606A (en) * | 2017-09-18 | 2020-07-14 | 南洋理工大学 | Cementitious composition, cement-based structure, and method of forming same |
| CN115181499A (en) * | 2022-07-26 | 2022-10-14 | 北京林业大学 | Water-resistant, high-adhesion and flame-retardant magnesium oxychloride inorganic adhesive as well as preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1562390A (en) * | 2004-03-17 | 2005-01-12 | 武汉理工大学 | Method for preparing artificial head bones made from composite material and for modifying surface |
| CN101491700A (en) * | 2009-03-03 | 2009-07-29 | 陕西科技大学 | Preparation method of carbon nano-tube reinforced magnesium-containing hydroxylapatite bone-cement composite material |
-
2010
- 2010-01-22 CN CN201010000968A patent/CN101757685A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1562390A (en) * | 2004-03-17 | 2005-01-12 | 武汉理工大学 | Method for preparing artificial head bones made from composite material and for modifying surface |
| CN101491700A (en) * | 2009-03-03 | 2009-07-29 | 陕西科技大学 | Preparation method of carbon nano-tube reinforced magnesium-containing hydroxylapatite bone-cement composite material |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104013539A (en) * | 2014-03-20 | 2014-09-03 | 胡方 | Preparation method of bone repair toothpaste agent inducing gene expression |
| CN104013539B (en) * | 2014-03-20 | 2016-07-06 | 胡方 | A kind of preparation method of the Bone Defect Repari toothpaste unguentum with inducible gene expression |
| CN104591679A (en) * | 2015-01-31 | 2015-05-06 | 河南理工大学 | Modified magnesium oxychloride bone cement as well as preparation method and application thereof |
| CN111417606A (en) * | 2017-09-18 | 2020-07-14 | 南洋理工大学 | Cementitious composition, cement-based structure, and method of forming same |
| CN115181499A (en) * | 2022-07-26 | 2022-10-14 | 北京林业大学 | Water-resistant, high-adhesion and flame-retardant magnesium oxychloride inorganic adhesive as well as preparation method and application thereof |
| CN115181499B (en) * | 2022-07-26 | 2023-05-26 | 北京林业大学 | Waterproof high-cementing-performance flame-retardant magnesium oxychloride inorganic adhesive and preparation method and application thereof |
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Application publication date: 20100630 |