CN107952111A - A kind of bone cement containing cooling agent and preparation method - Google Patents

A kind of bone cement containing cooling agent and preparation method Download PDF

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Publication number
CN107952111A
CN107952111A CN201711210073.3A CN201711210073A CN107952111A CN 107952111 A CN107952111 A CN 107952111A CN 201711210073 A CN201711210073 A CN 201711210073A CN 107952111 A CN107952111 A CN 107952111A
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bone cement
liquid
cooling agent
powder
silver
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李朝阳
崔永顺
夏文飞
吕维加
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Shandong Mingde Biomedical Engineering Co Ltd
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Shandong Mingde Biomedical Engineering Co Ltd
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    • A61L2300/102Metals or metal compounds, e.g. salts such as bicarbonates, carbonates, oxides, zeolites, silicates
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    • A61L2300/40Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
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Abstract

The present invention relates to a kind of bone cement containing cooling agent and preparation method, bone cement to be mainly made of powder and liquid, and wherein powder contains benzoyl peroxide, silver-colored strontium magnesium apatite, polyacrylate, barium sulfate etc., and liquid contains cooling agent.By powder and liquid according to powder liquid mass ratio 1~2.5:1 mixing, is made the bone cement.Cooling agent is introduced in bone cement liquid, with methymethacrylate the Ester exchange endothermic reaction occurs for cooling agent in bone cement solidification process, it is grafted on PMMA strands, due to heat absorption, the heat of MMA polymerisations release is reduced, reduces the maximum temperature of bone cement, and since the addition of cooling agent extends the hardening time of bone cement, the concentration accumulation of heat is further reduced, reduces bone cement maximum temperature.Bone cement produced by the present invention has the characteristics that antibacterial, syringeability are good, while also has good biocompatibility and osteoinductive, can be used for the fixation of a variety of fracture and the filling reparation of bone defect.

Description

A kind of bone cement containing cooling agent and preparation method
Technical field
The present invention relates to a kind of bone cement containing cooling agent and preparation method, belong to bone material field.
Background technology
Polyacrylate bone cement is that it is by powder and liquid two parts at present clinically using a kind of most bone cements Composition.Powder main component is polymethyl methacrylate, and liquid main component is methyl methacrylate monomer.Bone cement can Arbitrary shape is injection moulded and is made, mechanical strength is high, but bone cement also having some limitations property at the same time, as monomer has necessarily Toxicity, developer nonabsorable, biocompatibility be not good enough, cannot absorb degraded after injecting human body, while it is without osteogenic action, It is insecure with synosteosis, easily loosen, and the exothermic reaction in polymerization process may cause nervous function damage etc..
Studies have reported that the curing exotherm of bone cement is reduced by adding modifying agent in bone cement, such as CN1810300A, a kind of micropore bone cement, is mixed by the raw material of following parts by weight:1 part of bone cement, modifying agent 0.2-0.7 Part;Wherein, the modifying agent is mixed by 30 parts by weight of modifying agent solid and water:1 part of modifying agent solid, water 0.5- 0.9 part;The modifying agent solid mixes 30-50 parts of binder by the binder, accelerating agent and pore former of parts by weight, promotes 30-50 parts of agent, 10-30 parts of pore former.The solidification temperature of bone cement separately is reduced by adding beta carotene in bone cement, such as CN105031738A, in bone cement powder and liquid, introduces Hu Luoka elements respectively, when bone cement cures, part Hu Luoka elements Decomposed under the action of BPO and be transformed into vitamin A, vitamin A occurs vinegar exchange reaction with MMA and absorbs heat, and extends consolidating for bone cement Change the time, improve the injection property of bone cement, significantly reduce the heat release of bone cement.
The present invention in bone cement liquid by introducing cooling agent, cooling agent and methacrylic acid in bone cement solidification process The Ester exchange endothermic reaction occurs for formicester, is grafted on PMMA strands, due to heat absorption, reduces the heat that MMA polymerisations discharge Amount, and cooling agent is only introduced in bone cement liquid, optimize bone cement preparation process, and three elements are introduced in bone cement powder Full substituted apatite.
Apatite is the material composition of the inanimate matter of human body hard tissue (bone and tooth), its chemical composition and crystal structure and ridge The mineralogical composition of Vertebrate bone is very close, and doping apatite is to adulterate the displaced type formed after trace element in apatite to consolidate Solution, according to the literature, its biological degradability and biocompatibility can be improved by mixing saamite, or even can be to a certain degree Upper its bone-inducting active of raising, its biocidal property can be increased by mixing silver-colored apatite, its bioactivity etc. can be increased by mixing magnesium apatite. Although having much to the preparation research for adulterating apatite, the research to multi-element doping apatite is less, and particularly three elements are complete The research of substituted apatite has no report.
The present invention uses hydro-thermal method, controls product to precipitate by pH value, and control the temperature, pressure, time of reaction to prepare Silver-colored magnesium saamite, and by its with polyacrylate, barium sulfate etc. are compound prepares bone cement powder, and draw in bone cement liquid Enter cooling agent, reduce the polymerization temperature of bone cement, reduce injury of the bone cement curing exotherm to body, and three elements substitute phosphorus entirely The addition of lime stone improves bioactivity, biocidal property and the osteoinductive of bone cement, and the research to related content of the present invention does not appear in the newspapers Road.
The content of the invention
It is an object of the invention to provide a kind of new bone cement containing cooling agent and preparation method, draw in bone cement powder Enter the silver-colored full substituted apatite of strontium magnesium, and introduce cooling agent in a liquid, reduce the solidification temperature of bone cement, extend the behaviour of bone cement Make the time, obtained bone cement has the characteristics that antibiotic property, injectable, intensity are suitable, while also has good bio-compatible Property and osteoinductive.
Bone cement forms and mass percentage is:
Powder:
Polyacrylate 40%~70%;
Barium sulfate 5%~20%;
Silver-colored magnesium saamite 10~50%;
Benzoyl peroxide 1%~5%;
Liquid:
N, N dimethyl para-totuidine 0.5%~5%;
Hydroquinone 0.05%~2%;
Methyl methacrylate 93~98.5%;
Cooling agent 0.5%~2%.
Polyacrylate can be homopolymer, copolymer or polymer, preferably polymethyl methacrylate.
Cooling agent can be one kind of lycopene, Ubiquinone-50.
Silver-colored magnesium saamite is the doping apatite that silver, magnesium, three element of strontium substitute entirely, using strontium element as base, magnesium, silver element Codope, Ag/ (Ag+Mg+Sr) molar ratio are 1~10:100, Mg/ (Ag+Mg+Sr) molar ratios are 1~30:100, Sr/ (Ag+ Mg+Sr) molar ratio is 60~98:100, (Ag+Mg+Sr)/P molar ratio are 100:60.
The preparation method of bone cement is:
(1) strontium nitrate, magnesium nitrate, silver nitrate solution and the ammonium dibasic phosphate solution of same concentrations, the concentration of solution are configured For 0.05~0.2mol/L;
(2) four kinds of solution are pumped into reaction vessel at the same time, it is respectively 60~98mL/ of strontium nitrate solution to be pumped into speed Min, 1~30mL/min of magnesium nitrate solution, 1~10mL/min of silver nitrate solution, ammonium dibasic phosphate solution 60mL/min, four kinds molten Liquid terminates to be pumped at the same time, and it is 10~30min to be pumped into the time, obtains white emulsion, continues to be uniformly mixed;
(3) ammonium hydroxide is added, has white precipitate gradually to separate out, adjustment pH value is 10~12, continues to be uniformly mixed;
(4) white precipitate is separated from liquid, white precipitate is transferred in the barrier box containing micron openings, control isolation For box on liquid upper strata, liquid just immersion precipitation, is 150~250 DEG C in temperature, pressure reacts 4 under conditions of being 0.4~2MPa ~24h, cleaning, drying, last 500~1000 DEG C, sinter 3~12h, cooling, grinding obtain 5~200 μm of silver-colored magnesium strontium phosphorus ash Stone.
(5) silver-colored magnesium saamite is uniformly mixed with polyacrylate, benzoyl peroxide, barium sulfate, obtains bone cement Powder, by N, N dimethyl para-totuidine, hydroquinone, methyl methacrylate, cooling agent are uniformly mixed, and obtain bone cement liquid Body;
(6) according to powder liquid mass ratio 1~2.5:1 is uniformly mixed powder and liquid, is expelled to required position and completes to repair.
Continue to be uniformly mixed described in above-mentioned steps (2), (3), preferably incorporation time is 5~60min.
The advantage of the invention is that:Introduce cooling agent in bone cement liquid, cooling agent and first in bone cement solidification process The Ester exchange endothermic reaction occurs for base methacrylate, is grafted on PMMA strands, due to heat absorption, reduces MMA polymerisations The heat of release, reduces the maximum temperature of bone cement, and since the addition of cooling agent extends the hardening time of bone cement, more The concentration accumulation of heat is reduce further, reduces bone cement maximum temperature.And introducing, there is antibiotic property, bioactivity and bone to lure The full substituted apatite of three elements for the property led.
Calcium constituent is all replaced with strontium, magnesium, silver element in the preparation process of apatite, is formed using strontium element as base, magnesium, The problem of silver-colored magnesium saamite of silver element doping, solves using calcium constituent as base, the more difficult doping of the element of larger ionic radius, Strontium, silver element ionic radius are big, and magnesium elements ionic radius is small, and using strontium element as base, silver, magnesium elements easily lift doping content, make The apatite of standby highly doped amount.Silver-colored magnesium saamite and polyacrylate be compound to prepare bone cement, the addition of silver-colored magnesium saamite, Since strontium has partial development effect, the use of barium sulfate developer is reduced, improves the biocompatibility and biology of bone cement Activity, silver-colored magnesium saamite discharge a variety of needed by human body trace elements at the same time, and silver sustained release degraded assigns bone cement good antibacterial Effect, obvious bacteriostasis is respectively provided with to Gram-negative bacteria and gram-positive bacteria;The sustained release degraded of strontium improves bone water Biocompatibility, the bone-inducting active of mud, the sustained release degraded of magnesium improve bone density and anti-brittleness, reduce bone-loss and fracture Incidence, and play the role of analgesic, alleviate the psychological pressure of patient.The filling of fixation, bone defect available for a variety of fracture.
Brief description of the drawings
Fig. 1:Bone cement solidification temperature curve comparison figure;
Fig. 2:The compression strength figure of the bone cement containing cooling agent.
Embodiment
Present disclosure is described in further detail with reference to embodiment, but embodiments of the present invention are unlimited In this.
Bone cement and preparation method are as follows:
(1) strontium nitrate, magnesium nitrate, silver nitrate solution and the ammonium dibasic phosphate solution of 0.05~0.2mol/L is configured,
(2) four kinds of solution are pumped into reaction vessel at the same time, it is respectively 60~98mL/ of strontium nitrate solution to be pumped into speed Min, 1~30mL/min of magnesium nitrate solution, 1~10mL/min of silver nitrate solution, ammonium dibasic phosphate solution 60mL/min, four kinds molten Liquid terminates to be pumped at the same time, and it is 10~30min to be pumped into the time, obtains white emulsion, continues to be uniformly mixed, incorporation time for 5~ 60min;
(3) ammonium hydroxide is added, has white precipitate gradually to separate out, adjustment pH value is 10~12, continues to be uniformly mixed, incorporation time For 5~60min;
(4) white precipitate is separated from liquid, white precipitate is transferred in the barrier box containing micron openings, control isolation For box on liquid upper strata, liquid just immersion precipitation, is 150~250 DEG C in temperature, pressure reacts 4 under conditions of being 0.4~2MPa ~24h, cleaning, drying, last 500~1000 DEG C, sinter 3~12h, cooling, grinding obtain 5~200 μm of silver-colored magnesium strontium phosphorus ash Stone.
(5) by 10~50% silver-colored magnesium saamite and 40%~70% polymethyl methacrylate, 1%~5% Benzoyl peroxide, 5%~20% barium sulfate are uniformly mixed, and obtain bone cement powder, by 0.5%~5% N, N dimethyl Para-totuidine, 0.05%~2% hydroquinone, 93~98.5% methyl methacrylate, 0.5%~2% cooling agent It is uniformly mixed, obtains bone cement liquid;
(6) according to powder liquid mass ratio 1~2.5:1, bone cement powder is added in bone cement liquid and is uniformly mixed, there is 4 The injection time of~10min, is expelled to required position and completes to repair.
Embodiment 1
Powder contains 70% polymethyl methacrylate, 18% barium sulfate, 10% silver-colored magnesium saamite, 2% mistake Benzoyl Oxide;Liquid contains 2% N, N dimethyl para-totuidine, 1% hydroquinone, 1% lycopene, 96% Methyl methacrylate.
Bone cement preparation method is as follows:
(1) strontium nitrate, magnesium nitrate, silver nitrate solution and the ammonium dibasic phosphate solution of 0.05mol/L is configured,
(2) four kinds of solution are pumped into reaction vessel at the same time, it is respectively strontium nitrate solution 98mL/min to be pumped into speed, nitre Sour magnesium solution 1mL/min, silver nitrate solution 1mL/min, ammonium dibasic phosphate solution 60mL/min, four kinds of solution terminate to pump at the same time Enter, it is 10min to be pumped into the time, obtains white emulsion, continues to be uniformly mixed, incorporation time 60min;
(3) ammonium hydroxide is added, has white precipitate gradually to separate out, adjustment pH value is 10, continues to be uniformly mixed, incorporation time is 5min;
(4) white precipitate is separated from liquid, white precipitate is transferred in the barrier box containing micron openings, control isolation For box on liquid upper strata, liquid just immersion precipitation, is 150 DEG C in temperature, and pressure reacts 8h under conditions of being 1.35MPa, cleaning, It is dry, last 500 DEG C, 12h is sintered, cooling, grinding obtain 5~200 μm of silver-colored magnesium saamite.
(5) by 10% silver-colored magnesium saamite and 70% polymethyl methacrylate, 2% benzoyl peroxide, 18% barium sulfate is uniformly mixed, and obtains bone cement powder, by 2% N, N dimethyl para-totuidine, and 1% hydroquinone, 1% lycopene, 97% methyl methacrylate are uniformly mixed, and obtain bone cement liquid;
(6) according to powder liquid mass ratio 2.5:1 by bone cement powder be added in bone cement liquid be uniformly mixed, have 8min's Injection time, is expelled to required position and completes to repair.
According to the solidification temperature of the requirement test bone cement of YY0459 standards, test curve is as shown in Fig. 1-b, maximum temperature For 65.4 DEG C, it is 15.5min that maximum temperature, which corresponds to the time, shown in Fig. 1-a, to be 91 DEG C without cooling agent maximum temperature, and highest It is 10.8min that temperature, which corresponds to the time,.
Bone cement is expelled in sampling die, the sample that a diameter of 6.0mm length is 12mm is obtained after curing.Omnipotent Intensity test is carried out on mechanics tester, as shown in attached drawing 2-D, obtained sample compression strength is 79.1MPa.
Embodiment 2
Powder contains 40% polymethyl methacrylate, 8% barium sulfate, 50% silver-colored magnesium saamite, 2% peroxide Change benzoyl;Liquid contains 2% N, N dimethyl para-totuidine, 1% hydroquinone, 1% Ubiquinone-50,96% methyl Methyl acrylate.
Bone cement preparation method is as follows:
(1) saamite prepared using embodiment 1;
(2) by 50% silver-colored magnesium saamite and 40% polymethyl methacrylate, 2% benzoyl peroxide, 8% Barium sulfate be uniformly mixed, obtain bone cement powder, by 2% N, N dimethyl para-totuidine, 1% hydroquinone, 1% Ubiquinone-50,97% methyl methacrylate are uniformly mixed, and obtain bone cement liquid;
(3) according to powder liquid mass ratio 2.5:1 by bone cement powder be added in bone cement liquid be uniformly mixed, have 6min's Injection time, is expelled to required position and completes to repair.
According to YY0459 standards requirement test bone cement solidification temperature, test curve as shown in fig 1-c, maximum temperature For 69.5 DEG C, it is 13min that maximum temperature, which corresponds to the time,.
Bone cement is expelled in sampling die, the sample that a diameter of 6.0mm length is 12mm is obtained after curing.Omnipotent Intensity test is carried out on mechanics tester, as shown in attached drawing 2-E, obtained sample compression strength is 75.3MPa.
Embodiment 3
Powder contains 60% polymethyl methacrylate, 10% barium sulfate, 28% silver-colored magnesium saamite, 2% mistake Benzoyl Oxide;Liquid contains 4% N, N dimethyl para-totuidine, 1% hydroquinone, 2% lycopene, 93% Methyl methacrylate.
Bone cement preparation method is as follows:
(1) strontium nitrate, magnesium nitrate, silver nitrate solution and the ammonium dibasic phosphate solution of 0.2mol/L is configured,
(2) four kinds of solution are pumped into reaction vessel at the same time, it is respectively strontium nitrate solution 89mL/min to be pumped into speed, nitre Sour magnesium solution 10mL/min, silver nitrate solution 1mL/min, ammonium dibasic phosphate solution 60mL/min, four kinds of solution terminate to pump at the same time Enter, it is 30min to be pumped into the time, obtains white emulsion, continues to be uniformly mixed, incorporation time 5min;
(3) ammonium hydroxide is added, has white precipitate gradually to separate out, adjustment pH value is 12, continues to be uniformly mixed, incorporation time is 60min;
(4) white precipitate is separated from liquid, white precipitate is transferred in the barrier box containing micron openings, control isolation For box on liquid upper strata, liquid just immersion precipitation, is 200 DEG C in temperature, and pressure reacts 12h under conditions of being 1.5MPa, cleaning, It is dry, last 1000 DEG C, 4h is sintered, cooling, grinding obtain 5~200 μm of silver-colored magnesium saamite.
(5) by 28% silver-colored magnesium saamite and 60% polymethyl methacrylate, 2% benzoyl peroxide, 10% barium sulfate is uniformly mixed, and obtains bone cement powder, by 4% N, N dimethyl para-totuidine, and 1% hydroquinone, 2% lycopene, 93% methyl methacrylate are uniformly mixed, and obtain bone cement liquid;
(6) according to powder liquid mass ratio 2:Bone cement powder is added in bone cement liquid and is uniformly mixed by 1, there is the note of 9min The time is penetrated, required position is expelled to and completes to repair.
Bone cement is expelled in sampling die, the sample that a diameter of 6.0mm length is 12mm is obtained after curing.Omnipotent Intensity test is carried out on mechanics tester, as shown in attached drawing 2-F, obtained sample compression strength is 72.2MPa.
Embodiment 4
Powder contains 70% polymethyl methacrylate, 14% barium sulfate, 15% silver-colored magnesium saamite, 1% mistake Benzoyl Oxide;Liquid contains 3% N, N dimethyl para-totuidine, 1% hydroquinone, 0.5% lycopene, 95.5% methyl methacrylate.
Bone cement preparation method is as follows:
(1) saamite prepared using embodiment 3;
(2) by 15% silver-colored magnesium saamite and 70% polymethyl methacrylate, 1% benzoyl peroxide, 14% barium sulfate is uniformly mixed, and obtains bone cement powder, by 3% N, N dimethyl para-totuidine, and 1% hydroquinone, 0.5% lycopene, 95.5% methyl methacrylate are uniformly mixed, and obtain bone cement liquid;
(3) according to powder liquid mass ratio 2:Bone cement powder is added in bone cement liquid and is uniformly mixed by 1, there is the note of 6min The time is penetrated, required position is expelled to and completes to repair.
Bone cement is expelled in sampling die, the sample that a diameter of 6.0mm length is 12mm is obtained after curing.Omnipotent Intensity test is carried out on mechanics tester, as shown in attached drawing 2-G, obtained sample compression strength is 82.8MPa.

Claims (5)

1. a kind of bone cement containing cooling agent, it is characterised in that composition and mass percentage are:
Powder:
Polymethyl methacrylate 40%~70%;
Barium sulfate 5%~20%;
Silver-colored magnesium saamite 10~50%;
Benzoyl peroxide 1%~5%;
Liquid:
N, N dimethyl para-totuidine 0.5%~5%;
Hydroquinone 0.05%~2%;
Methyl methacrylate 93~98.5%;
Cooling agent 0.5%~2%.
2. bone cement as claimed in claim 1, it is characterised in that cooling agent is one kind of lycopene or Ubiquinone-50.
3. bone cement as claimed in claim 1, it is characterised in that in silver-colored magnesium saamite, Ag/ (Ag+Mg+Sr) molar ratio is 1~10:100, Mg/ (Ag+Mg+Sr) molar ratios are 1~30:100, Sr/ (Ag+Mg+Sr) molar ratios are 60~98:100, (Ag+ Mg+Sr)/P molar ratios are 100:60.
4. the preparation method of bone cement as claimed in claim 1, it is characterised in that step is as follows:
(1) silver nitrate, magnesium nitrate, strontium nitrate solution and the ammonium dibasic phosphate solution of same concentrations are configured, the concentration of solution is 0.05~0.2mol/L;
(2) four kinds of solution are pumped into reaction vessel at the same time, it is respectively 60~98mL/min of strontium nitrate solution to be pumped into speed, nitre Sour 1~30mL/min of magnesium solution, 1~10mL/min of silver nitrate solution, ammonium dibasic phosphate solution 60mL/min, four kinds of solution are at the same time End is pumped into, and it is 10~30min to be pumped into the time, obtains white emulsion, continues to be uniformly mixed;
(3) ammonium hydroxide is added, has white precipitate gradually to separate out, adjustment pH value is 10~12, continues to be uniformly mixed;
(4) white precipitate is separated from liquid, white precipitate is transferred in the barrier box containing micron openings, control barrier box exists Liquid upper strata, liquid just immersion precipitation, is 150~250 DEG C in temperature, reaction 4 under conditions of pressure is 0.4~2MPa~ 24h, cleaning, drying, last 500~1000 DEG C, sinter 3~12h, cooling, grinding obtain 5~200 μm of silver-colored magnesium saamite.
(5) silver-colored magnesium saamite is uniformly mixed with polyacrylate, benzoyl peroxide, barium sulfate, obtains bone cement powder, By N, N dimethyl para-totuidine, hydroquinone, methyl methacrylate, cooling agent are uniformly mixed, and obtain bone cement liquid;
(6) according to powder liquid mass ratio 1~2.5:1 is uniformly mixed powder and liquid, is expelled to required position and completes to repair.
5. method as claimed in claim 4, it is characterised in that continue to be uniformly mixed described in step (2), (3), during mixing Between be 5~60min.
CN201711210073.3A 2017-11-27 2017-11-27 A kind of bone cement containing cooling agent and preparation method Pending CN107952111A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109091701A (en) * 2018-09-27 2018-12-28 中国科学院上海硅酸盐研究所 A kind of organic bone cement of low temperature and preparation method thereof
CN109316627A (en) * 2018-10-26 2019-02-12 中国医学科学院北京协和医院 A kind of novel artificial bone material and its preparation method and application
CN109331226A (en) * 2018-10-26 2019-02-15 中国医学科学院北京协和医院 A kind of modified mineralized collagen artificial bone and its preparation method and application
CN111905150A (en) * 2020-08-10 2020-11-10 中国人民解放军总医院第一医学中心 Bone cement with color development function

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105031738A (en) * 2015-09-09 2015-11-11 山东明德生物医学工程有限公司 Weak-exothermic bone cement and preparation method and application
CN105107021A (en) * 2015-09-09 2015-12-02 天津大学 Injectable antibacterial bone cement and preparation method and application thereof
CN105439110A (en) * 2015-11-12 2016-03-30 中国科学院金属研究所 Sr and Mg doped amorphous apatite material and crystalline apatite material
CN106075587A (en) * 2016-06-07 2016-11-09 山东明德生物医学工程有限公司 Polynary codope bone cement and preparation method

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105031738A (en) * 2015-09-09 2015-11-11 山东明德生物医学工程有限公司 Weak-exothermic bone cement and preparation method and application
CN105107021A (en) * 2015-09-09 2015-12-02 天津大学 Injectable antibacterial bone cement and preparation method and application thereof
CN105439110A (en) * 2015-11-12 2016-03-30 中国科学院金属研究所 Sr and Mg doped amorphous apatite material and crystalline apatite material
CN106075587A (en) * 2016-06-07 2016-11-09 山东明德生物医学工程有限公司 Polynary codope bone cement and preparation method

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
林英光: "溶胶-凝胶结合超临界流体干燥法制备纳米掺锶羟基磷灰石的研究", 《高校化学工程学报》 *
薛淼: "《口腔生物材料学》", 30 September 2006, 上海世界图书出版公司 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109091701A (en) * 2018-09-27 2018-12-28 中国科学院上海硅酸盐研究所 A kind of organic bone cement of low temperature and preparation method thereof
CN109316627A (en) * 2018-10-26 2019-02-12 中国医学科学院北京协和医院 A kind of novel artificial bone material and its preparation method and application
CN109331226A (en) * 2018-10-26 2019-02-15 中国医学科学院北京协和医院 A kind of modified mineralized collagen artificial bone and its preparation method and application
CN111905150A (en) * 2020-08-10 2020-11-10 中国人民解放军总医院第一医学中心 Bone cement with color development function

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