CN108264373A - The preparation method of medical reinforced porous biological ceramic material - Google Patents
The preparation method of medical reinforced porous biological ceramic material Download PDFInfo
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Abstract
The invention discloses the preparation methods of medical reinforced porous biological ceramic material, the technique is by lauryl amine base sodium sulfonate, ammonium chloride, iron oxide, hydroxypropyl methyl cellulose, polysiloxanes, thiodipropionic acid dilauryl cinnamic acid ester etc. carries out compressive reaction, add the organic components of lubricant and antifoaming agent making material, then ball-milling technology is utilized by hydroxyapatite, baryta fledspar, lepidolite, the mixture of raw material such as diatomite 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. medical reinforced porous biological ceramic material is prepared.The medical reinforced porous biological ceramic material being prepared, safe and non-toxic, density is gently, porous breathable is good, compression strength is high, has preferable application prospect.
Description
Technical field
The present invention relates to this technical fields of material, are related specifically to the preparation of medical reinforced porous biological ceramic material
Method.
Background technology
As inorganic porous product for clinical purposes, for example, by calcining or being sintered the more of bioceramic acquisition
Hole ceramics are known.However, when being used in the application of the shelf such as rebuild for live body bone tissue, prosthetic material or the like
When, due to such porous ceramics show it is hard but it is crisp the shortcomings that, so always have after surgery due to slight collision and
Cause the danger of damage.In addition, in field of surgery, processing and change the shape of porous ceramics come match live body bone tissue by
The shape of the part of damage is also difficult.Further, since 10 years or more extended time cycle are required in some cases,
Until it is substituted completely by live body bone, so keeping the danger for causing adverse effect by its damage during the period.So
In order to avoid the risk of above-mentioned adverse effect to greatest extent, this invention address that research medical reinforced porous biological ceramic material
Material is combined by optimizing various material combinations and proportioning, is optimized to simplify to prepare and be tempted so that the bioceramic material being prepared
Reduce brittleness on the basis of hard, and it is safe and non-toxic, density is light, porous breathable is good, compression strength is high, have preferable
Application prospect.
Invention content
In order to solve the above technical problems, the invention discloses the preparation method of medical reinforced porous biological ceramic material,
The technique is by lauryl amine base sodium sulfonate, ammonium chloride, iron oxide, hydroxypropyl methyl cellulose, polysiloxanes, thiodipropionic acid dilauryl
Cinnamic acid ester etc. carries out compressive reaction, adds the organic components of lubricant and antifoaming agent making material, then will using ball-milling technology
The mixture of raw material such as hydroxyapatite, baryta fledspar, lepidolite, diatomite are ground, dry, activating, crossing screening and choosing, prepare
Above-mentioned organic components and ceramic masterbatch are further carried out progressive sintering step by step, finally utilize twin-screw extrusion skill by ceramic masterbatch
Art is granulated, vacuum dehydration, plastotype, high pressure steam sterilization and etc. medical reinforced porous biological ceramic material is prepared
Material.The medical reinforced porous biological ceramic material being prepared, safe and non-toxic, density is light, porous breathable is good, pressure resistance
Degree is high, has preferable application prospect.
The purpose of the present invention can be achieved through the following technical solutions:
The preparation method of medical reinforced porous biological ceramic material, includes the following steps:
(1) by 3-8 parts of lauryl amine base sodium sulfonate, 1-6 parts of ammonium chloride, 3-6 parts of iron oxide, hydroxypropyl methyl cellulose 4-6
Compressive reaction, reaction temperature are carried out in 1-3 parts of part, 3-4 parts of polysiloxanes, thiodipropionic acid dilauryl cinnamic acid ester mixed injection Muffle furnaces
It is 105 DEG C to spend, and pressure is set as 8MPa, sustained response 5h, then adds in 1-3 parts of lubricant, 1-2 parts of antifoaming agent, lasting to stir
50min, reduction of blood pressure in high-speed to normal pressure, heat preservation are spare;
(2) by 1-4 parts of 4-9 parts of hydroxyapatite, 3-7 parts of baryta fledspar, 6-9 parts of lepidolite, diatomite mixing, ball milling 20-
It is 24 hours, then continuous drying at a temperature of 70-80 DEG C in electric vacunm drying case, after being completely dried in inert gas flow
Sieving, sealing are 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 medical reinforced porous biological ceramic material of the invention is by lauryl amine base sodium sulfonate, chlorination
Ammonium, iron oxide, hydroxypropyl methyl cellulose, polysiloxanes, thiodipropionic acid dilauryl cinnamic acid ester etc. carry out compressive reaction, addition profit
The organic components of lubrication prescription and antifoaming agent making material, then using ball-milling technology by hydroxyapatite, baryta fledspar, lepidolite, silicon
The mixture of raw material such as diatomaceous earth are ground, dry, activating, crossing screening and choosing, prepare ceramic masterbatch, further have unit by above-mentioned
Part and ceramic masterbatch carry out progressive sintering step by step, be finally granulated using twin-screw extrusion technology, vacuum dehydration, plastotype, height
Pressure steam sterilizing and etc. medical reinforced porous biological ceramic material is prepared.The medical reinforced porous life being prepared
Object ceramic material, safe and non-toxic, density is gently, porous breathable is good, compression strength is high, has preferable application prospect.
(2) medical reinforced porous biological ceramic material feedstock of the invention is easy to get, is simple for process, suitable for large-scale industry
Change and use, it is highly practical.
Specific embodiment
The technical solution of invention is described in detail with reference to specific embodiment.
Embodiment 1
(1) by 3 parts of lauryl amine base sodium sulfonate, 1 part of ammonium chloride, 3 parts of iron oxide, 4 parts of hydroxypropyl methyl cellulose, poly- silica
Compressive reaction is carried out in 1 part of 3 parts of alkane, thiodipropionic acid dilauryl cinnamic acid ester mixed injection Muffle furnace, reaction temperature is 105 DEG C, pressure
8MPa, sustained response 5h are set as by force, 1 part of ethylene glycol, 1 part of antifoaming agent is then added in, persistently stirs 50min, reduction of blood pressure in high-speed is extremely
Normal pressure, heat preservation is spare, and wherein antifoaming agent is octadecyl alcolol stearate and triethanolamine stearate mass ratio 1:1 mixed liquor;
(2) 4 parts of hydroxyapatite, 3 parts of baryta fledspar, 6 parts of lepidolite, 1 part of diatomite are mixed, ball milling 20 hours, then
It is continuous drying at a temperature of 70-80 DEG C in electric vacunm drying case, it is sieved in an argon stream after being completely dried, crossing mesh size is
7000 mesh, sealing are 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 medical reinforced porous biological ceramic material obtained are as shown in table 1.
Embodiment 2
(1) by 5 parts of lauryl amine base sodium sulfonate, 3 parts of ammonium chloride, 4 parts of iron oxide, 4 parts of hydroxypropyl methyl cellulose, poly- silica
Compressive reaction is carried out in 1 part of 3 parts of alkane, thiodipropionic acid dilauryl cinnamic acid ester mixed injection Muffle furnace, reaction temperature is 105 DEG C, pressure
8MPa, sustained response 5h are set as by force, 2 parts of polyethylene glycol, 1 part of antifoaming agent is then added in, persistently stirs 50min, 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) 5 parts of hydroxyapatite, 4 parts of baryta fledspar, 7 parts of lepidolite, 2 parts of diatomite are mixed, ball milling 21 hours, then
It is continuous drying at a temperature of 70-80 DEG C in electric vacunm drying case, it is sieved in an argon stream after being completely dried, crossing mesh size is
7000 mesh, sealing are 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
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 medical reinforced porous biological ceramic material obtained are as shown in table 1.
Embodiment 3
(1) by 6 parts of lauryl amine base sodium sulfonate, 5 parts of ammonium chloride, 5 parts of iron oxide, 5 parts of hydroxypropyl methyl cellulose, poly- silica
Compressive reaction is carried out in 2 parts of 4 parts of alkane, thiodipropionic acid dilauryl cinnamic acid ester mixed injection Muffle furnaces, reaction temperature is 105 DEG C, pressure
8MPa, sustained response 5h are set as by force, 2 parts of silicone oil, 2 parts of antifoaming agent is then added in, persistently stirs 50min, reduction of blood pressure in high-speed is 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) 7 parts of hydroxyapatite, 6 parts of baryta fledspar, 8 parts of lepidolite, 3 parts of diatomite are mixed, ball milling 22 hours, then
It is continuous drying at a temperature of 70-80 DEG C in electric vacunm drying case, it is sieved in an argon stream after being completely dried, crossing mesh size is
7000 mesh, sealing are 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 medical reinforced porous biological ceramic material obtained are as shown in table 1.
Embodiment 4
(1) by 8 parts of lauryl amine base sodium sulfonate, 6 parts of ammonium chloride, 6 parts of iron oxide, 6 parts of hydroxypropyl methyl cellulose, poly- silica
Compressive reaction is carried out in 3 parts of 4 parts of alkane, thiodipropionic acid dilauryl cinnamic acid ester mixed injection Muffle furnaces, reaction temperature is 105 DEG C, pressure
8MPa, sustained response 5h are set as by force, 3 parts of glycerine, 2 parts of antifoaming agent is then added in, persistently stirs 50min, reduction of blood pressure in high-speed is extremely
Normal pressure, heat preservation is spare, and wherein antifoaming agent is octadecyl alcolol stearate and triethanolamine stearate mass ratio 1:1 mixed liquor;
(2) 9 parts of hydroxyapatite, 7 parts of baryta fledspar, 9 parts of lepidolite, 4 parts of diatomite are mixed, ball milling 24 hours, then
It is continuous drying at a temperature of 70-80 DEG C in electric vacunm drying case, it is sieved in an argon stream after being completely dried, crossing mesh size is
7000 mesh, sealing are 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 medical reinforced porous biological ceramic material obtained are as shown in table 1.
Comparative example 1
(1) by 3 parts of lauryl amine base sodium sulfonate, 1 part of ammonium chloride, 3 parts of iron oxide, 4 parts of hydroxypropyl methyl cellulose, poly- silica
It is reacted in 3 parts of mixed injection Muffle furnaces of alkane, reaction temperature is 105 DEG C, sustained response 5h, then adds in 1 part of ethylene glycol, disappears
1 part of infusion persistently stirs 50min, and heat preservation is spare, and wherein antifoaming agent is octadecyl alcolol stearate and triethanolamine stearate quality
Than 1:1 mixed liquor;
(2) 4 parts of hydroxyapatite, 3 parts of baryta fledspar, 6 parts of lepidolite, 1 part of diatomite are mixed, ball milling 20 hours, then
It is continuous drying at a temperature of 70-80 DEG C in electric vacunm drying case, it is sieved in an argon stream after being completely dried, crossing mesh size is
7000 mesh, sealing are 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 medical reinforced porous biological ceramic material obtained are as shown in table 1.
Comparative example 2
(1) by 8 parts of lauryl amine base sodium sulfonate, 6 parts of ammonium chloride, 6 parts of iron oxide, 6 parts of hydroxypropyl methyl cellulose, poly- silica
Compressive reaction is carried out in 3 parts of 4 parts of alkane, thiodipropionic acid dilauryl cinnamic acid ester mixed injection Muffle furnaces, reaction temperature is 105 DEG C, pressure
8MPa, sustained response 5h are set as by force, 3 parts of glycerine, 2 parts of antifoaming agent is then added in, persistently stirs 50min, reduction of blood pressure in high-speed is extremely
Normal pressure, heat preservation is spare, and wherein antifoaming agent is octadecyl alcolol stearate and triethanolamine stearate mass ratio 1:1 mixed liquor;
(2) 9 parts of hydroxyapatite, 7 parts of baryta fledspar, 9 parts of lepidolite, 4 parts of diatomite are mixed, ball milling 24 hours, then
The continuous drying rear sieving at a temperature of 70-80 DEG C in electric vacunm drying case, 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 medical reinforced porous biological ceramic material obtained are as shown in table 1.
By the medical reinforced porous biological ceramic material obtained of embodiment 1-4 and comparative example 1-2 respectively into line density,
Bending strength, hardness, cytotoxicity (animal) this several performance tests.
Table 1
The present invention medical reinforced porous biological ceramic material preparation method by lauryl amine base sodium sulfonate, ammonium chloride,
Iron oxide, hydroxypropyl methyl cellulose, polysiloxanes, thiodipropionic acid dilauryl cinnamic acid ester etc. carry out compressive reaction, addition lubrication
Agent and the organic components of antifoaming agent making material, then using ball-milling technology by hydroxyapatite, baryta fledspar, lepidolite, diatom
The mixture of raw material such as soil are ground, dry, activating, crossing screening and choosing, ceramic masterbatch are prepared, further by above-mentioned organic components
With ceramic masterbatch carry out progressive sintering step by step, be finally granulated using twin-screw extrusion technology, vacuum dehydration, plastotype, high pressure
Steam sterilizing and etc. medical reinforced porous biological ceramic material is prepared.The medical reinforced porous biology being prepared
Ceramic material, safe and non-toxic, density is gently, porous breathable is good, compression strength is high, has preferable application prospect.The present invention
Medical reinforced porous biological ceramic material feedstock be easy to get, be simple for process, suitable for heavy industrialization use, it is 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. the preparation method of medical reinforced porous biological ceramic material, which is characterized in that include the following steps:
(1) by 3-8 parts of lauryl amine base sodium sulfonate, 1-6 parts of ammonium chloride, 3-6 parts of iron oxide, 4-6 parts of hydroxypropyl methyl cellulose, poly-
Compressive reaction is carried out in 1-3 parts of 3-4 parts of siloxanes, thiodipropionic acid dilauryl cinnamic acid ester mixed injection Muffle furnaces, reaction temperature is
105 DEG C, pressure is set as 8MPa, sustained response 5h, then adds in 1-3 parts of lubricant, 1-2 parts of antifoaming agent, lasting to stir
50min, reduction of blood pressure in high-speed to normal pressure, heat preservation are spare;
(2) 4-9 parts of hydroxyapatite, 3-7 parts of baryta fledspar, 6-9 parts of lepidolite, 1-4 parts of diatomite are mixed, ball milling 20-24 is small
When, it is then continuous drying at a temperature of 70-80 DEG C in electric vacunm drying case, after being completely dried in inert gas flow mistake
Sieve, sealing are 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 medical reinforced porous biological ceramic material according to claim 1, which is characterized in that described
Lubricant in step (1) is one or more of ethylene glycol, polyethylene glycol, silicone oil, glycerine.
3. the preparation method of medical reinforced porous biological ceramic material according to claim 1, which is characterized in that described
Antifoaming agent in step (1) is octadecyl alcolol stearate and triethanolamine stearate mass ratio 1:1 mixed liquor.
4. the preparation method of medical reinforced porous biological ceramic material according to claim 1, which is characterized in that described
Inert gas in step (2) is argon gas.
5. the preparation method of medical reinforced porous biological ceramic material according to claim 1, which is characterized in that described
Mesh size of crossing in step (2) is 7000 mesh.
6. the preparation method of medical reinforced porous biological ceramic material according to claim 1, which is characterized in that described
Double-screw extruder screw temperature is 180-200 DEG C in step (4), and rotating speed is 500-700 revs/min.
7. the preparation method of medical reinforced porous biological ceramic material according to claim 1, which is characterized in that described
Vacuum meter parameter in step (5) is is increased to 450mmHg, dewatering time 90sec in 1min.
8. the preparation method of medical reinforced porous biological ceramic material according to claim 1, which is characterized in that described
High pressure steam sterilization parameter in step (5) is pressure 103.4kPa, 121.3 DEG C of temperature, sterilization time 20min.
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CN106587937A (en) * | 2016-12-07 | 2017-04-26 | 苏州洛特兰新材料科技有限公司 | High-strength carbon fiber based composite ceramic material and preparation method thereof |
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JPS6364981A (en) * | 1986-09-03 | 1988-03-23 | 三菱化学株式会社 | Manufacture of porous ceramic sintered body |
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