CN108218291A - A kind of preparation method for the bioceramic material for adulterating dicalcium silicate nano powder - Google Patents
A kind of preparation method for the bioceramic material for adulterating dicalcium silicate nano powder Download PDFInfo
- Publication number
- CN108218291A CN108218291A CN201810106677.1A CN201810106677A CN108218291A CN 108218291 A CN108218291 A CN 108218291A CN 201810106677 A CN201810106677 A CN 201810106677A CN 108218291 A CN108218291 A CN 108218291A
- Authority
- CN
- China
- Prior art keywords
- parts
- nano powder
- dicalcium silicate
- silicate nano
- doping
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
Classifications
-
- 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
- C04B26/00—Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
- C04B26/02—Macromolecular compounds
- C04B26/04—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B26/045—Polyalkenes
-
- 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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00008—Obtaining or using nanotechnology related materials
-
- 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
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Materials For Medical Uses (AREA)
Abstract
The invention discloses a kind of preparation methods for the bioceramic material for adulterating dicalcium silicate nano powder, the technique is by thiodipropionic acid dilauryl cinnamic acid ester, sodium tetraborate, methyl triacetoxysilane etc. carries out compressive reaction, add the organic components of lubricant and antifoaming agent making material, then ball-milling technology is utilized by aluminium hydroxide ceramic powder, clay, carbon black, polyethylene wax, the mixture of raw material such as spodumene are ground, it is dry, activation, cross screening and choosing, prepare ceramic masterbatch, above-mentioned organic components and ceramic masterbatch are further subjected to progressive sintering step by step, finally it is granulated using twin-screw extrusion technology, vacuum dehydration, plastotype, high pressure steam sterilization and etc. be prepared doping dicalcium silicate nano powder bioceramic material.The bioceramic material of doping dicalcium silicate nano powder being prepared, safe and non-toxic, the high resistance to compression of intensity can carry out biodegradation, have preferable application prospect.
Description
Technical field
The present invention relates to this technical fields of material, are related specifically to a kind of bioceramic for adulterating dicalcium silicate nano powder
The preparation method of material.
Background technology
It is well known that calcium silicates (monocalcium silicate CS, dicalcium silicate C2S and tricalcium silicate C3S) can be with water when being mixed with water
It closes, and solidifies and harden by precipitating gelatinous calcium silicate hydrate (Ca-Si-H2O glue) (C-S-H), with common baud
Blue cement (OPC) is similar.Point out that hydroxyapatite core can be formed and be given birth on the calcium silicate particle of hydration in disclosed document
It is long, therefore the calcium silicates being hydrated is the potential candidate biomaterial of hard tissue repair.Equally, Ni et al. also studied " skeletonization
External comparison of the cell-like cell to the reaction of calcium silicates and tricalcium phosphate cement ".The result shows that calcium silicate cements are raw
Object is compatible and bioactivity, therefore is suitable as new bone reparing biological material.By dicalcium silicate nanometer in the present invention
Powder is added in the preparation of bioceramic, not only increases the hardness and intensity of bioceramic, while also improve bioceramic
The biocompatibility of material imparts the new performance characteristic of bioceramic so that the doping dicalcium silicate nano powder being prepared
Bioceramic material, safe and non-toxic, the high resistance to compression of intensity can carry out biodegradation, have preferable application prospect.
Invention content
In order to solve the above technical problems, the invention discloses a kind of bioceramic materials for adulterating dicalcium silicate nano powder
Preparation method, the technique is by thiodipropionic acid dilauryl cinnamic acid ester, sodium tetraborate, methyl triacetoxysilane, lignin sulfonic acid
Sodium, dicalcium silicate nano powder, zinc stearate, orange osmanthus acid barium etc. carry out compressive reaction, add lubricant and antifoaming agent making material
Organic components, then using ball-milling technology by raw material such as aluminium hydroxide ceramic powder, clay, carbon black, polyethylene wax, spodumenes
Mixture is ground, dries, activating, crossing screening and choosing, prepares ceramic masterbatch, further by above-mentioned organic components and ceramic masterbatch
Carry out progressive sintering step by step, be finally granulated using twin-screw extrusion technology, vacuum dehydration, plastotype, high pressure steam sterilization etc.
The bioceramic material of doping dicalcium silicate nano powder is prepared in step.The life of doping dicalcium silicate nano powder being prepared
Object ceramic material, safe and non-toxic, the high resistance to compression of intensity, can carry out biodegradation, have preferable application prospect.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of preparation method for the bioceramic material for adulterating dicalcium silicate nano powder, includes the following steps:
(1) by 1-5 parts of thiodipropionic acid dilauryl cinnamic acid ester, 4-10 parts of sodium tetraborate, methyl triacetoxysilane 2-6
1-4 parts of part, 4-9 parts of sodium lignin sulfonate, 4-9 parts of dicalcium silicate nano powder, 1-3 parts of zinc stearate, orange osmanthus acid barium mixed injections
Compressive reaction is carried out in Muffle furnace, reaction temperature is 105 DEG C, and pressure is set as 8MPa, then sustained response 5h adds in lubricant
1-3 parts, 1-2 parts of antifoaming agent, persistently stir 50min, and reduction of blood pressure in high-speed to normal pressure is kept the temperature spare;
(2) by 20-25 parts of aluminium oxide ceramics powder, 15-20 parts of clay, 5-10 parts of carbon black, 2-5 parts of polyethylene wax, spodumene
5-10 parts of mixing, ball milling 20-24 hours is then continuous drying at a temperature of 70-80 DEG C in electric vacunm drying case, is completely dried
It is sieved in inert gas flow afterwards, sealing is spare;
(3) three-step approach sintering will be carried out in the reactant of step (1) and the sieving of step (2) injection vacuum sintering furnace,
First step sintering keeps the temperature 30min, second step is sintered with 5 DEG C/min's with the heating rate of 10 DEG C/min to 100-110 DEG C of heat preservation
Heating rate is warming up to 130-135 DEG C, keeps the temperature 30min, and third step sintering keeps the temperature 12-18h controlled at 150-160 DEG C;
(4) the reaction paste injection double screw extruder in step (3) is squeezed, obtains masterbatch;
(5) by the masterbatch in step (4) through vacuum dehydration, plastotype, high pressure steam sterilization, 65 DEG C of dryings, pack up into
Product.
Preferably, the lubricant in the step (1) is ethylene glycol, polyethylene glycol, silicone oil, one kind in glycerine or several
Kind.
Preferably, the antifoaming agent in the step (1) is octadecyl alcolol stearate and triethanolamine stearate mass ratio 1:1
Mixed liquor.
Preferably, the inert gas in the step (2) is argon gas.
Preferably, the mesh size of crossing in the step (2) is 7000 mesh.
Preferably, in the step (4) double-screw extruder screw temperature be 180-200 DEG C, rotating speed for 500-700 turn/
Minute.
Preferably, to be increased to 450mmHg in 1min, dewatering time is the vacuum meter parameter in the step (5)
90sec。
Preferably, the high pressure steam sterilization parameter in the step (5) is pressure 103.4kPa, and 121.3 DEG C of temperature sterilizes
Time is 20min.
Compared with prior art, the present invention advantage is:
(1) preparation method of the bioceramic material of doping dicalcium silicate nano powder of the invention is by thiodipropionic acid dilauryl
Cinnamic acid ester, sodium tetraborate, methyl triacetoxysilane, sodium lignin sulfonate, dicalcium silicate nano powder, zinc stearate, orange osmanthus
Sour barium etc. carries out compressive reaction, adds the organic components of lubricant and antifoaming agent making material, then using ball-milling technology by hydrogen
The mixture of raw material such as aluminium oxide ceramics powder, clay, carbon black, polyethylene wax, spodumene are ground, dry, activating, crossing and sieve
Choosing prepares ceramic masterbatch, and above-mentioned organic components and ceramic masterbatch further are carried out progressive sintering step by step, finally utilize twin-screw
Extruding technology is granulated, vacuum dehydration, plastotype, high pressure steam sterilization and etc. doping dicalcium silicate nano powder is prepared
Bioceramic material.The bioceramic material of doping dicalcium silicate nano powder being prepared, safe and non-toxic, intensity highly resistance
Pressure, can carry out biodegradation, have preferable application prospect.
(2) the bioceramic material raw material of doping dicalcium silicate nano powder of the invention is easy to get, is simple for process, suitable for advising greatly
Mould industrialization is used, highly practical.
Specific embodiment
The technical solution of invention is described in detail with reference to specific embodiment.
Embodiment 1
(1) by 1 part of thiodipropionic acid dilauryl cinnamic acid ester, 4 parts of sodium tetraborate, 2 parts of methyl triacetoxysilane, lignin
It carries out pressurizeing in 1 part of 4 parts of sodium sulfonate, 4 parts of dicalcium silicate nano powder, 1 part of zinc stearate, orange osmanthus acid barium mixed injection Muffle furnace anti-
Should, reaction temperature is 105 DEG C, and pressure is set as 8MPa, sustained response 5h, then adds in 1 part of ethylene glycol, 1 part of antifoaming agent, is continued
50min is stirred, reduction of blood pressure in high-speed to normal pressure, heat preservation is spare, and wherein antifoaming agent is octadecyl alcolol stearate and triethanolamine stearate
Mass ratio 1:1 mixed liquor;
(2) by 5 parts of 20 parts of aluminium oxide ceramics powder, 15 parts of clay, 5 parts of carbon black, 2 parts of polyethylene wax, spodumene mixing, ball milling
It is 20 hours, then continuous drying at a temperature of 70-80 DEG C in electric vacunm drying case, mistake in an argon stream after being completely dried
Sieve, it is 7000 mesh to cross mesh size, and sealing is spare;
(3) three-step approach sintering will be carried out in the reactant of step (1) and the sieving of step (2) injection vacuum sintering furnace,
First step sintering keeps the temperature 30min, second step is sintered with 5 DEG C/min's with the heating rate of 10 DEG C/min to 100-110 DEG C of heat preservation
Heating rate is warming up to 130-135 DEG C, keeps the temperature 30min, and third step sintering keeps the temperature 12h controlled at 150-160 DEG C;
(4) the reaction paste injection double screw extruder in step (3) is squeezed, double-screw extruder screw temperature is
180 DEG C, rotating speed is 500 revs/min, obtains masterbatch;
(5) by the masterbatch in step (4) through vacuum dehydration, plastotype, high pressure steam sterilization, 65 DEG C of dryings, pack up into
Product, wherein vacuum meter parameter are pressure to be increased to 450mmHg, dewatering time 90sec, high pressure steam sterilization parameter in 1min
103.4kPa, 121.3 DEG C of temperature, sterilization time 20min.
The performance test results of the bioceramic material of doping dicalcium silicate nano powder obtained are as shown in table 1.
Embodiment 2
(1) by 2 parts of thiodipropionic acid dilauryl cinnamic acid ester, 6 parts of sodium tetraborate, 3 parts of methyl triacetoxysilane, lignin
It carries out pressurizeing in 2 parts of 5 parts of sodium sulfonate, 6 parts of dicalcium silicate nano powder, 1 part of zinc stearate, orange osmanthus acid barium mixed injection Muffle furnaces anti-
Should, reaction temperature is 105 DEG C, and pressure is set as 8MPa, sustained response 5h, then adds in 2 parts of polyethylene glycol, 1 part of antifoaming agent, holds
Continuous stirring 50min, reduction of blood pressure in high-speed to normal pressure, heat preservation is spare, and wherein antifoaming agent is three ethyl alcohol of octadecyl alcolol stearate and stearic acid
Amine mass ratio 1:1 mixed liquor;
(2) by 6 parts of 22 parts of aluminium oxide ceramics powder, 16 parts of clay, 7 parts of carbon black, 3 parts of polyethylene wax, spodumene mixing, ball milling
It is 21 hours, then continuous drying at a temperature of 70-80 DEG C in electric vacunm drying case, mistake in an argon stream after being completely dried
Sieve, it is 7000 mesh to cross mesh size, and sealing is spare;
(3) three-step approach sintering will be carried out in the reactant of step (1) and the sieving of step (2) injection vacuum sintering furnace,
First step sintering keeps the temperature 30min, second step is sintered with 5 DEG C/min's with the heating rate of 10 DEG C/min to 100-110 DEG C of heat preservation
Heating rate is warming up to 130-135 DEG C, keeps the temperature 30min, and third step sintering keeps the temperature 14h controlled at 150-160 DEG C;
(4) the reaction paste injection double screw extruder in step (3) is squeezed, double-screw extruder screw temperature is
180 DEG C, rotating speed is 600 revs/min, obtains masterbatch;
(5) by the masterbatch in step (4) through vacuum dehydration, plastotype, high pressure steam sterilization, 65 DEG C of dryings, pack up into
Product, wherein vacuum meter parameter are pressure to be increased to 450mmHg, dewatering time 90sec, high pressure steam sterilization parameter in 1min
103.4kPa, 121.3 DEG C of temperature, sterilization time 20min.
The performance test results of the bioceramic material of doping dicalcium silicate nano powder obtained are as shown in table 1.
Embodiment 3
(1) by 4 parts of thiodipropionic acid dilauryl cinnamic acid ester, 8 parts of sodium tetraborate, 5 parts of methyl triacetoxysilane, lignin
It carries out pressurizeing in 3 parts of 8 parts of sodium sulfonate, 7 parts of dicalcium silicate nano powder, 2 parts of zinc stearate, orange osmanthus acid barium mixed injection Muffle furnaces anti-
Should, reaction temperature is 105 DEG C, and pressure is set as 8MPa, sustained response 5h, then adds in 2 parts of silicone oil, 1 part of antifoaming agent, persistently stirs
50min is mixed, reduction of blood pressure in high-speed to normal pressure, heat preservation is spare, and wherein antifoaming agent is octadecyl alcolol stearate and triethanolamine stearate matter
Measure ratio 1:1 mixed liquor;
(2) by 9 parts of 24 parts of aluminium oxide ceramics powder, 18 parts of clay, 9 parts of carbon black, 4 parts of polyethylene wax, spodumene mixing, ball milling
It is 23 hours, then continuous drying at a temperature of 70-80 DEG C in electric vacunm drying case, mistake in an argon stream after being completely dried
Sieve, it is 7000 mesh to cross mesh size, and sealing is spare;
(3) three-step approach sintering will be carried out in the reactant of step (1) and the sieving of step (2) injection vacuum sintering furnace,
First step sintering keeps the temperature 30min, second step is sintered with 5 DEG C/min's with the heating rate of 10 DEG C/min to 100-110 DEG C of heat preservation
Heating rate is warming up to 130-135 DEG C, keeps the temperature 30min, and third step sintering keeps the temperature 16h controlled at 150-160 DEG C;
(4) the reaction paste injection double screw extruder in step (3) is squeezed, double-screw extruder screw temperature is
190 DEG C, rotating speed is 600 revs/min, obtains masterbatch;
(5) by the masterbatch in step (4) through vacuum dehydration, plastotype, high pressure steam sterilization, 65 DEG C of dryings, pack up into
Product, wherein vacuum meter parameter are pressure to be increased to 450mmHg, dewatering time 90sec, high pressure steam sterilization parameter in 1min
103.4kPa, 121.3 DEG C of temperature, sterilization time 20min.
The performance test results of the bioceramic material of doping dicalcium silicate nano powder obtained are as shown in table 1.
Embodiment 4
(1) by 5 parts of thiodipropionic acid dilauryl cinnamic acid ester, 10 parts of sodium tetraborate, 6 parts of methyl triacetoxysilane, wooden
It pressurizes in 4 parts of plain 9 parts of sodium sulfonate, 9 parts of dicalcium silicate nano powder, 3 parts of zinc stearate, orange osmanthus acid barium mixed injection Muffle furnaces
Reaction, reaction temperature are 105 DEG C, and pressure is set as 8MPa, sustained response 5h, then add in 3 parts of glycerine, 2 parts of antifoaming agent, hold
Continuous stirring 50min, reduction of blood pressure in high-speed to normal pressure, heat preservation is spare, and wherein antifoaming agent is three ethyl alcohol of octadecyl alcolol stearate and stearic acid
Amine mass ratio 1:1 mixed liquor;
(2) 225 parts of aluminium oxide ceramics powder, 20 parts of clay, 10 parts of carbon black, 5 parts of polyethylene wax, 10 parts of spodumene are mixed,
Ball milling 24 hours, it is then continuous drying at a temperature of 70-80 DEG C in electric vacunm drying case, after being completely dried in an argon stream
Sieving, it is 7000 mesh to cross mesh size, and sealing is spare;
(3) three-step approach sintering will be carried out in the reactant of step (1) and the sieving of step (2) injection vacuum sintering furnace,
First step sintering keeps the temperature 30min, second step is sintered with 5 DEG C/min's with the heating rate of 10 DEG C/min to 100-110 DEG C of heat preservation
Heating rate is warming up to 130-135 DEG C, keeps the temperature 30min, and third step sintering keeps the temperature 18h controlled at 150-160 DEG C;
(4) the reaction paste injection double screw extruder in step (3) is squeezed, double-screw extruder screw temperature is
200 DEG C, rotating speed is 700 revs/min, obtains masterbatch;
(5) by the masterbatch in step (4) through vacuum dehydration, plastotype, high pressure steam sterilization, 65 DEG C of dryings, pack up into
Product, wherein vacuum meter parameter are pressure to be increased to 450mmHg, dewatering time 90sec, high pressure steam sterilization parameter in 1min
103.4kPa, 121.3 DEG C of temperature, sterilization time 20min.
The performance test results of the bioceramic material of doping dicalcium silicate nano powder obtained are as shown in table 1.
Comparative example 1
(1) by 1 part of thiodipropionic acid dilauryl cinnamic acid ester, 4 parts of sodium tetraborate, 2 parts of methyl triacetoxysilane, lignin
It carries out pressurizeing in 1 part of 4 parts of sodium sulfonate, 4 parts of dicalcium silicate nano powder, 1 part of zinc stearate, orange osmanthus acid barium mixed injection Muffle furnace anti-
Should, reaction temperature is 105 DEG C, and pressure is set as 8MPa, sustained response 5h, then adds in 1 part of ethylene glycol, 1 part of antifoaming agent, is continued
50min is stirred, reduction of blood pressure in high-speed to normal pressure, heat preservation is spare, and wherein antifoaming agent is octadecyl alcolol stearate and triethanolamine stearate
Mass ratio 1:1 mixed liquor;
(2) by 5 parts of 20 parts of aluminium oxide ceramics powder, 15 parts of clay, 5 parts of carbon black, 2 parts of polyethylene wax, spodumene mixing, ball milling
It is 20 hours, then continuous drying at a temperature of 70-80 DEG C in electric vacunm drying case, mistake in an argon stream after being completely dried
Sieve, it is 7000 mesh to cross mesh size, and sealing is spare;
(3) three-step approach sintering will be carried out in the reactant of step (1) and the sieving of step (2) injection vacuum sintering furnace,
First step sintering keeps the temperature 30min, second step is sintered with 5 DEG C/min's with the heating rate of 10 DEG C/min to 100-110 DEG C of heat preservation
Heating rate is warming up to 130-135 DEG C, keeps the temperature 30min, and third step sintering keeps the temperature 12h controlled at 150-160 DEG C;
(4) the reaction paste injection double screw extruder in step (3) is squeezed, double-screw extruder screw temperature is
180 DEG C, rotating speed is 500 revs/min, obtains masterbatch;
(5) by the masterbatch in step (4) through vacuum dehydration, plastotype, high pressure steam sterilization, 65 DEG C of dryings, pack up into
Product, wherein vacuum meter parameter are pressure to be increased to 450mmHg, dewatering time 90sec, high pressure steam sterilization parameter in 1min
103.4kPa, 121.3 DEG C of temperature, sterilization time 20min.
The performance test results of the bioceramic material of doping dicalcium silicate nano powder obtained are as shown in table 1.
Comparative example 2
(1) by 5 parts of thiodipropionic acid dilauryl cinnamic acid ester, 10 parts of sodium tetraborate, 6 parts of methyl triacetoxysilane, wooden
It pressurizes in 4 parts of plain 9 parts of sodium sulfonate, 9 parts of dicalcium silicate nano powder, 3 parts of zinc stearate, orange osmanthus acid barium mixed injection Muffle furnaces
Reaction, reaction temperature are 105 DEG C, and pressure is set as 8MPa, sustained response 5h, then add in 3 parts of glycerine, 2 parts of antifoaming agent, hold
Continuous stirring 50min, reduction of blood pressure in high-speed to normal pressure, heat preservation is spare, and wherein antifoaming agent is three ethyl alcohol of octadecyl alcolol stearate and stearic acid
Amine mass ratio 1:1 mixed liquor;
(2) 225 parts of aluminium oxide ceramics powder, 20 parts of clay, 10 parts of carbon black, 5 parts of polyethylene wax, 10 parts of spodumene are mixed,
Ball milling 24 hours, it is then continuous drying at a temperature of 70-80 DEG C in electric vacunm drying case, after being completely dried in an argon stream
Sieving, it is 7000 mesh to cross mesh size, and sealing is spare;
(3) three-step approach sintering will be carried out in the reactant of step (1) and the sieving of step (2) injection vacuum sintering furnace,
First step sintering keeps the temperature 30min, second step is sintered with 5 DEG C/min's with the heating rate of 10 DEG C/min to 100-110 DEG C of heat preservation
Heating rate is warming up to 130-135 DEG C, keeps the temperature 30min, and third step sintering keeps the temperature 18h controlled at 150-160 DEG C;
(4) the reaction paste injection double screw extruder in step (3) is squeezed, double-screw extruder screw temperature is
200 DEG C, rotating speed is 700 revs/min, obtains masterbatch;
(5) by the masterbatch in step (4) through vacuum dehydration, plastotype, high pressure steam sterilization, 65 DEG C of dryings, pack up into
Product, wherein vacuum meter parameter are pressure to be increased to 450mmHg, dewatering time 90sec, high pressure steam sterilization parameter in 1min
103.4kPa, 121.3 DEG C of temperature, sterilization time 20min.
The performance test results of the bioceramic material of doping dicalcium silicate nano powder obtained are as shown in table 1.
By the bioceramic material of the doping dicalcium silicate nano powder obtained of embodiment 1-4 and comparative example 1-2 respectively into
Row bending strength, compression strength, degradation rate, Acute systemic toxicity test (animal) this several performance tests.
Table 1
The preparation method of the bioceramic material of the doping dicalcium silicate nano powder of the present invention is by thiodipropionic acid dilauryl osmanthus
Acid esters, sodium tetraborate, methyl triacetoxysilane, sodium lignin sulfonate, dicalcium silicate nano powder, zinc stearate, orange osmanthus acid
Barium etc. carries out compressive reaction, adds the organic components of lubricant and antifoaming agent making material, then using ball-milling technology by hydrogen-oxygen
Change the mixture of raw material such as aluminium ceramic powder, clay, carbon black, polyethylene wax, spodumene be ground, dry, activating, crossing and sieve
Choosing prepares ceramic masterbatch, and above-mentioned organic components and ceramic masterbatch further are carried out progressive sintering step by step, finally utilize twin-screw
Extruding technology is granulated, vacuum dehydration, plastotype, high pressure steam sterilization and etc. doping dicalcium silicate nano powder is prepared
Bioceramic material.The bioceramic material of doping dicalcium silicate nano powder being prepared, safe and non-toxic, intensity highly resistance
Pressure, can carry out biodegradation, have preferable application prospect.The bioceramic material of the doping dicalcium silicate nano powder of the present invention
Raw material is easy to get, is simple for process, is used suitable for heavy industrialization, highly practical.
The foregoing is merely the embodiment of the present invention, are not intended to limit the scope of the invention, every to utilize this hair
The equivalent structure or equivalent flow shift that bright description is made directly or indirectly is used in other relevant technology necks
Domain is included within the scope of the present invention.
Claims (8)
1. a kind of preparation method for the bioceramic material for adulterating dicalcium silicate nano powder, which is characterized in that include the following steps:
(1) by 1-5 parts of thiodipropionic acid dilauryl cinnamic acid ester, 4-10 parts of sodium tetraborate, 2-6 parts of methyl triacetoxysilane, wood
1-4 parts of 4-9 parts of quality sodium sulfonate, 4-9 parts of dicalcium silicate nano powder, 1-3 parts of zinc stearate, orange osmanthus acid barium mixed injection Muffle furnaces
Middle carry out compressive reaction, reaction temperature be 105 DEG C, pressure is set as 8MPa, sustained response 5h, then add in 1-3 parts of lubricant,
1-2 parts of antifoaming agent, persistently stirs 50min, and reduction of blood pressure in high-speed to normal pressure is kept the temperature spare;
(2) by 20-25 parts of aluminium oxide ceramics powder, 15-20 parts of clay, 5-10 parts of carbon black, 2-5 parts of polyethylene wax, spodumene 5-10
Part mixing, ball milling 20-24 hours is then continuous drying at a temperature of 70-80 DEG C in electric vacunm drying case, after being completely dried
It is sieved in inert gas flow, sealing is spare;
(3) will the reactant of step (1) and the sieving of step (2) injection vacuum sintering furnace in carry out three-step approach sintering, first
Step sintering keeps the temperature 30min, second step is sintered with the heating of 5 DEG C/min with the heating rate of 10 DEG C/min to 100-110 DEG C of heat preservation
Speed is warming up to 130-135 DEG C, keeps the temperature 30min, and third step sintering keeps the temperature 12-18h controlled at 150-160 DEG C;
(4) the reaction paste injection double screw extruder in step (3) is squeezed, obtains masterbatch;
(5) masterbatch in step (4) is got product through vacuum dehydration, plastotype, high pressure steam sterilization, 65 DEG C of dryings, packaging.
2. the preparation method of the bioceramic material of doping dicalcium silicate nano powder according to claim 1, feature exist
In the lubricant in the step (1) is one or more of ethylene glycol, polyethylene glycol, silicone oil, glycerine.
3. the preparation method of the bioceramic material of doping dicalcium silicate nano powder according to claim 1, feature exist
In the antifoaming agent in the step (1) is octadecyl alcolol stearate and triethanolamine stearate mass ratio 1:1 mixed liquor.
4. the preparation method of the bioceramic material of doping dicalcium silicate nano powder according to claim 1, feature exist
In the inert gas in the step (2) is argon gas.
5. the preparation method of the bioceramic material of doping dicalcium silicate nano powder according to claim 1, feature exist
In the mesh size of crossing in the step (2) is 7000 mesh.
6. the preparation method of the bioceramic material of doping dicalcium silicate nano powder according to claim 1, feature exist
In double-screw extruder screw temperature is 180-200 DEG C in the step (4), and rotating speed is 500-700 revs/min.
7. the preparation method of the bioceramic material of doping dicalcium silicate nano powder according to claim 1, feature exist
In the vacuum meter parameter in the step (5) is is increased to 450mmHg, dewatering time 90sec in 1min.
8. the preparation method of the bioceramic material of doping dicalcium silicate nano powder according to claim 1, feature exist
In, high pressure steam sterilization parameter in the step (5) be pressure 103.4kPa, 121.3 DEG C of temperature, sterilization time 20min.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201810106677.1A CN108218291A (en) | 2018-02-02 | 2018-02-02 | A kind of preparation method for the bioceramic material for adulterating dicalcium silicate nano powder |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201810106677.1A CN108218291A (en) | 2018-02-02 | 2018-02-02 | A kind of preparation method for the bioceramic material for adulterating dicalcium silicate nano powder |
Publications (1)
Publication Number | Publication Date |
---|---|
CN108218291A true CN108218291A (en) | 2018-06-29 |
Family
ID=62670666
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201810106677.1A Withdrawn CN108218291A (en) | 2018-02-02 | 2018-02-02 | A kind of preparation method for the bioceramic material for adulterating dicalcium silicate nano powder |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN108218291A (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109467382A (en) * | 2018-10-24 | 2019-03-15 | 武汉理工大学 | One kind being based on γ-C2Conductive material of S and preparation method thereof |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106631011A (en) * | 2016-12-07 | 2017-05-10 | 苏州洛特兰新材料科技有限公司 | Thermosensitive conductive composite ceramic material and preparation method thereof |
CN106630964A (en) * | 2016-12-07 | 2017-05-10 | 苏州洛特兰新材料科技有限公司 | Ultraviolet-resistant weather-proof composite ceramic material and preparation method thereof |
CN106830897A (en) * | 2016-12-07 | 2017-06-13 | 苏州洛特兰新材料科技有限公司 | Titania modified composite ceramic material of one kind addition and preparation method thereof |
CN107185033A (en) * | 2017-06-27 | 2017-09-22 | 广东工业大学 | A kind of anti-infection bio ceramic artificial bone and its application |
-
2018
- 2018-02-02 CN CN201810106677.1A patent/CN108218291A/en not_active Withdrawn
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106631011A (en) * | 2016-12-07 | 2017-05-10 | 苏州洛特兰新材料科技有限公司 | Thermosensitive conductive composite ceramic material and preparation method thereof |
CN106630964A (en) * | 2016-12-07 | 2017-05-10 | 苏州洛特兰新材料科技有限公司 | Ultraviolet-resistant weather-proof composite ceramic material and preparation method thereof |
CN106830897A (en) * | 2016-12-07 | 2017-06-13 | 苏州洛特兰新材料科技有限公司 | Titania modified composite ceramic material of one kind addition and preparation method thereof |
CN107185033A (en) * | 2017-06-27 | 2017-09-22 | 广东工业大学 | A kind of anti-infection bio ceramic artificial bone and its application |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109467382A (en) * | 2018-10-24 | 2019-03-15 | 武汉理工大学 | One kind being based on γ-C2Conductive material of S and preparation method thereof |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN107418567B (en) | Biomass-based carbon quantum dot and preparation method thereof | |
CN107746212A (en) | Modified enhanced ground oligomer gel material of one kind and preparation method thereof | |
CN106729971B (en) | Water-soluble single-walled carbon nanotube modified calcium phosphate cement and preparation and application thereof | |
CN110128679B (en) | Preparation method of conductive double-layer hydrogel for electrical stimulation osteochondral integrated regeneration | |
CN105482500B (en) | The surface modifying method of silicone sealant antioxidant nano-calcium carbonate | |
CN101081932A (en) | Silk fibroin /calcium carbonate nano composite material and preparation method thereof | |
CN108187145A (en) | Gelatin-alginate composite mortar, gelatin-alginate compound rest and preparation method thereof | |
CN104845382A (en) | Silk protein/cellulose derivative blending hydrogel and preparation method thereof | |
CN109864042A (en) | Nano-graphene feeding silkworm rearing method for preparing high-thermal-conductivity silk and product thereof | |
CN109880305A (en) | A kind of method of hydrogel-elastomer composite 3D printing | |
CN109573997A (en) | A kind of preparation method of graphene oxide-loaded vulcanization carbon/carbon-copper composite material | |
CN114873943A (en) | Nano titanium dioxide/biochar composite material and preparation method and application thereof | |
CN108218291A (en) | A kind of preparation method for the bioceramic material for adulterating dicalcium silicate nano powder | |
CN110152068B (en) | Polyether-ether-ketone/nano-hydroxyapatite composite material and preparation method and application thereof | |
CN109293355A (en) | A kind of bioceramic and its preparation method and application | |
CN107569717B (en) | Bone repair material with tissue oxygenation function and application thereof | |
CN108653804B (en) | Preparation method of silicon-doped calcium phosphate bone repair material | |
CN110171979A (en) | A kind of preparation method of large scale personalized biological active ceramic implant | |
CN107324365B (en) | A kind of nanometer of barium hydroxide/graphene nanocomposite material and preparation method | |
CN103992499A (en) | 3D (three-dimensional) uniform porous scaffold material and preparing method thereof | |
CN106065148B (en) | Graphene-polyvinyl alcohol hybrid material and the method for preparing polyurethane resin based composites | |
CN106518020A (en) | 3D printing material based on ceramic and preparing method of 3D printing material | |
CN107384027A (en) | A kind of low-temp ceramics colored drawing/mark chalk and preparation method thereof | |
CN113274545A (en) | Manganese-doped calcium silicate porous ceramic support and preparation method and application thereof | |
CN104928908A (en) | Method for mineralizing silk fiber |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
WW01 | Invention patent application withdrawn after publication |
Application publication date: 20180629 |
|
WW01 | Invention patent application withdrawn after publication |