CN107411975A - A kind of preparation method of carious tooth filling patching material - Google Patents
A kind of preparation method of carious tooth filling patching material Download PDFInfo
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- CN107411975A CN107411975A CN201710190842.1A CN201710190842A CN107411975A CN 107411975 A CN107411975 A CN 107411975A CN 201710190842 A CN201710190842 A CN 201710190842A CN 107411975 A CN107411975 A CN 107411975A
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- carious tooth
- patching material
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- powder
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
- A61K6/831—Preparations for artificial teeth, for filling teeth or for capping teeth comprising non-metallic elements or compounds thereof, e.g. carbon
- A61K6/838—Phosphorus compounds, e.g. apatite
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
- A61K6/831—Preparations for artificial teeth, for filling teeth or for capping teeth comprising non-metallic elements or compounds thereof, e.g. carbon
- A61K6/836—Glass
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
- A61K6/884—Preparations for artificial teeth, for filling teeth or for capping teeth comprising natural or synthetic resins
- A61K6/887—Compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- A61K6/889—Polycarboxylate cements; Glass ionomer cements
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- Health & Medical Sciences (AREA)
- Oral & Maxillofacial Surgery (AREA)
- Plastic & Reconstructive Surgery (AREA)
- Epidemiology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Dental Preparations (AREA)
Abstract
The present invention relates to a kind of preparation method of carious tooth filling patching material, belong to gear division reparation technical field.The present invention is using fresh ox bone as raw material, native hydroxyl apatite powder is made, it is and compound with CPP, silicate glass powder is handled through hydrofluoric acid surface coarsening again, it is and compound with it with nano titanium oxide, aluminum fluoride, the good modified glass powder of biocidal property is made, finally by the ball milling such as modified glass powder and polyacrylic acid, itaconic acid, calcirm-fluoride into cement, and carious tooth filling patching material is made with composite natral hydroxyapatite powder ball milling.The present invention improves anti-microbial property using titanium dioxide and fluorine ion; and improve the adhesive property of cement; the carious tooth filling patching material for preparing the present invention is adhered tightly to dentin surface; deposit hydroxyapatite layer; realize the remineralization of dentine; one layer of firm fine and close protective layer is formed, effectively repairs carious tooth.
Description
Technical field
The present invention relates to a kind of preparation method of carious tooth filling patching material, belong to gear division reparation technical field.
Background technology
During China human mortality is still in slow increase, along with expanding economy and the raising of people's schooling
And the attention to child-bearing, the visible carious tooth control aspect in children have been obtained for certain success.Dental caries, which are used as, to be permitted
The latency of more serious mouth diseases, more early to find its presence, more early control will obtain bigger effect with treatment, therefore
The various common oral pathogenic bacteria for causing dental caries are studied then necessary.While oral cavity pathogen is controlled, for
Dental caries early stage caused by it, it is also desirable to by promoting the method for remineralization to make impaired glaze paint be repaired as early as possible, preferably to subtract
Harm caused by low dental caries.
Dental caries are under the influence of many factors based on bacterium, and a kind of chronic broken of demineralization formation occurs for dental hard tissue
Bad disease.Oversaturated Ca in saliva and dental plaque fluid under normal circumstances2+And PO43-The dissolving of enamel, enamel can be prevented
In hydroxyapatite crystal Mg be present2+、CO3 2-Deng heteroion, when bacterial plaque acid production reduces oral pH, H+It is first
First attack Mg2+、CO3 2-The weaker lattice sites at place, cause Ca2+﹑ OH-﹑ PO4 3-﹑ F-Removed simultaneously from lattice Deng priority
Diffuse in the liquid phase environment between crystal, destroy perfection of lattice, dental enamel dissolution demineralization is caused, when enamel whole corrosion
Afterwards, dentine will be exposed, the problems such as causing hemodia, carious tooth.Therefore the repairing research of demineralization enamel is for carious tooth
Prevent and treat significant.Although present carious tooth repair materials are in itself for repairing cavity or tooth defect more
Effectively, but the purpose for preventing carious tooth from occurring again is unable to reach, therefore, one layer of firmly densification is re-formed in dentin surface
Hydroxyapatite protective layer, it appears it is particularly important.
The content of the invention
The technical problems to be solved by the invention:For present carious tooth repair materials in itself for repairing cavity or tooth
Tooth defect is more effective, but is unable to reach the problem of preventing carious tooth from occurring again, and the invention provides a kind of filling of carious tooth to repair
Mend the preparation method of material, native hydroxyl apatite powder is made using fresh ox bone as raw material in the present invention, and with casein phosphoric acid
Peptide is compound, then silicate glass powder is handled through hydrofluoric acid surface coarsening, and compound with it with nano titanium oxide, aluminum fluoride,
The good modified glass powder of biocidal property is made, finally by the ball milling such as modified glass powder and polyacrylic acid, itaconic acid, calcirm-fluoride into cementation
Agent, and carious tooth filling patching material is made with composite natral hydroxyapatite powder ball milling.The present invention utilizes titanium dioxide and fluorine
Ion improves anti-microbial property, and improves the adhesive property of cement, carious tooth filling patching material prepared by the present invention is closely glued
Dentin surface is attached to, deposits hydroxyapatite layer, realizes the remineralization of dentine, forms one layer of firm fine and close protection
Layer, effectively repairs carious tooth.
In order to solve the above technical problems, the technical solution adopted by the present invention is:
(1) the fresh ox bones of 1~2kg are weighed, are placed in drying box, are dried at 105~110 DEG C to constant weight, then by drying
Ox bone afterwards, which is fitted into pulverizer, to be crushed, and is crossed 60 mesh sieves, the ox bone particle after sieving is placed in Muffle furnace, at 600~700 DEG C
1~2h of lower calcining, after being cooled to room temperature, then calcined product and 100~200g CPPs be transferred in ball mill, with
300~400r/min, 30~40min of ball milling, 200 mesh sieves are crossed, obtain composite natral hydroxyapatite powder, it is standby;
(2) 100~200g silicate glass powder is weighed, 20~30min in 1.5~3.0L deionized waters is placed in, adds
80~100mL mass fractions are 40% hydrofluoric acid, stir 6~10h with 300~400r/min, then continue in centrifuge, with
5000~6000r/min centrifuges 10~12min, collects precipitation, precipitation is washed with deionized 3~5 times, then precipitation is put
In drying box, dried at 110~120 DEG C to constant weight, obtain surface roughening glass dust;
(3) above-mentioned surface roughening glass dust is immersed in 500~600mL toluene, and with 300W ultrasonic disperses 30~
40min, add 50~80mL silane resin acceptor kh-550s, 3~5g nano titanium oxides, 1~2g aluminum fluorides, at 80~90 DEG C
Under water bath with thermostatic control, with 500~600r/min, 6~8h of insulated and stirred, then filtering, is washed with absolute ethyl alcohol and deionized water successively
Filter residue 3~5 times, then filter residue is placed in vacuum drying chamber, dried at 105~110 DEG C to constant weight, obtain modified glass powder;
(4) the above-mentioned modified glass flakes of 40~50g, 12~15mL polyacrylic acid PAAS, 2~3g itaconic acid, 1~2g are weighed
Calcirm-fluoride, 1~3g zirconium oxides, is fitted into ball mill, with 300~400r/min, 30~40min of ball milling, obtains modified glass ion and glues
Gu agent, adding the composite natral hydroxyapatite powder of 5~6g steps (1) preparation, continue 20~30min of ball milling, obtain carious tooth
Fill patching material.
The present invention application process be:By solid-to-liquid ratio 9:Carious tooth produced by the present invention is filled patching material and deionization by 1
Water mixes, and stirs 20~30min with 60~80r/min, pastel is made, then by one layer of Y- of carious tooth enamel surface even spread
Chloropropyl triethoxysilane, then 12~15s is dried up with compressed air, carious tooth hole or breakage then are filled with pastel,
It is 2~3g/cm to control dosage2, the pastel that surrounding is overflowed is removed after filling, you can.
The method have the benefit that:
(1) the carious tooth filling patching material that prepared by the present invention can effectively suppress the cariogenic bacteria around carious tooth hole for a long time
Growth and breeding, the metabolic activity of bacterium is influenceed, reduce its acid producing ability, reduce the incidence of enamel decalcification;(2) present invention system
Standby carious tooth filling patching material Efficient software patching both carious surfaces adamantine layer and can fill up said minuscule hole, realize the ore deposit again of dentine
Change.
Embodiment
The fresh ox bones of 1~2kg are weighed, are placed in drying box, are dried at 105~110 DEG C to constant weight, then will be dried
Ox bone, which is fitted into pulverizer, to be crushed, and crosses 60 mesh sieves, the ox bone particle after sieving is placed in Muffle furnace, forged at 600~700 DEG C
1~2h is burnt, after being cooled to room temperature, then calcined product and 100~200g CPPs is transferred in ball mill, with 300~
400r/min 30~40min of ball milling, 200 mesh sieves are crossed, obtain composite natral hydroxyapatite powder;Weigh 100~200g silicate
Glass dust, 20~30min in 1.5~3.0L deionized waters is placed in, it is 40% hydrofluoric acid to add 80~100mL mass fractions,
With 300~400r/min stir 6~10h, then continue in centrifuge, with 5000~6000r/min centrifuge 10~
12min, precipitation is collected, precipitation is washed with deionized 3~5 times, then precipitation is placed in drying box, done at 110~120 DEG C
It is dry to constant weight, obtain surface roughening glass dust;Above-mentioned surface roughening glass dust is immersed in 500~600mL toluene, and with
300W 30~40min of ultrasonic disperse, add 50~80mL silane resin acceptor kh-550s, 3~5g nano titanium oxides, 1~2g
Aluminum fluoride, under 80~90 DEG C of waters bath with thermostatic control, with 500~600r/min, 6~8h of insulated and stirred, then filtering, successively with anhydrous
Ethanol and deionized water wash filter residue 3~5 times, then filter residue is placed in vacuum drying chamber, are dried at 105~110 DEG C to perseverance
Weight, obtains modified glass powder;Weigh the above-mentioned modified glass flakes of 40~50g, 12~15mL polyacrylic acid PAAS, 2~3g itaconic acid,
1~2g calcirm-fluoride, 1~3g zirconium oxides, is fitted into ball mill, with 300~400r/min, 30~40min of ball milling, obtains modified glass
Ionomer cement, the above-mentioned composite natral hydroxyapatite powders of 5~6g are added, continue 20~30min of ball milling, obtain carious tooth filling
Patching material.
Example 1
The fresh ox bones of 1kg are weighed, are placed in drying box, it is dry at 105 DEG C to load to constant weight, then by dried ox bone
Crushed in pulverizer, cross 60 mesh sieves, the ox bone particle after sieving is placed in Muffle furnace, 1h is calcined at 600 DEG C, is cooled to room
Wen Hou, then calcined product and 100g CPPs are transferred in ball mill, with 300r/min ball milling 30min, cross 200 mesh
Sieve, obtains composite natral hydroxyapatite powder;100g silicate glass powder is weighed, is placed in 20min in 1.5L deionized waters, then add
It is 40% hydrofluoric acid to enter 80mL mass fractions, stirs 6h with 300r/min, then continues in centrifuge, centrifuged with 5000r/min
10min is separated, collects precipitation, precipitation is washed with deionized 3 times, then precipitation is placed in drying box, is dried extremely at 110 DEG C
Constant weight, obtain surface roughening glass dust;Above-mentioned surface roughening glass dust is immersed in 500mL toluene, and with 300W ultrasounds
Scattered 30min, adds 50mL silane resin acceptor kh-550s, 3g nano titanium oxides, 1g aluminum fluorides, in 80 DEG C of waters bath with thermostatic control
Under, with 500r/min insulated and stirred 6h, then filtering, washs filter residue 3 times with absolute ethyl alcohol and deionized water successively, then by filter residue
It is placed in vacuum drying chamber, is dried at 105 DEG C to constant weight, obtain modified glass powder;The above-mentioned modified glass flakes of 40g are weighed,
12mL polyacrylic acid PAAS, 2g itaconic acid, 1g calcirm-fluoride, 1g zirconium oxides, is fitted into ball mill, with 300r/min ball milling 30min,
Modified glass ionomer cement is obtained, adds the above-mentioned composite natral hydroxyapatite powders of 5g, continues ball milling 20min, obtains carious tooth
Fill patching material.
The present invention application process be:By solid-to-liquid ratio 9:Carious tooth produced by the present invention is filled patching material and deionization by 1
Water mixes, and stirs 20min with 60r/min, pastel is made, then by one layer of Y- chloropropyl three of carious tooth enamel surface even spread
Ethoxysilane, then 12s is dried up with compressed air, carious tooth hole or breakage then are filled with pastel, it is 2g/ to control dosage
cm2, the pastel that surrounding is overflowed is removed after filling, you can.
Example 2
The fresh ox bones of 2kg are weighed, are placed in drying box, it is dry at 108 DEG C to load to constant weight, then by dried ox bone
Crushed in pulverizer, cross 60 mesh sieves, the ox bone particle after sieving is placed in Muffle furnace, 1h is calcined at 650 DEG C, is cooled to room
Wen Hou, then calcined product and 150g CPPs are transferred in ball mill, with 350r/min ball milling 35min, cross 200 mesh
Sieve, obtains composite natral hydroxyapatite powder;150g silicate glass powder is weighed, is placed in 25min in 1.9L deionized waters, then add
It is 40% hydrofluoric acid to enter 88mL mass fractions, stirs 8h with 350r/min, then continues in centrifuge, centrifuged with 5500r/min
11min is separated, collects precipitation, precipitation is washed with deionized 4 times, then precipitation is placed in drying box, is dried extremely at 115 DEG C
Constant weight, obtain surface roughening glass dust;Above-mentioned surface roughening glass dust is immersed in 550mL toluene, and with 300W ultrasounds
Scattered 35min, adds 60mL silane resin acceptor kh-550s, 4g nano titanium oxides, 1g aluminum fluorides, in 85 DEG C of waters bath with thermostatic control
Under, with 550r/min insulated and stirred 7h, then filtering, washs filter residue 4 times with absolute ethyl alcohol and deionized water successively, then by filter residue
It is placed in vacuum drying chamber, is dried at 108 DEG C to constant weight, obtain modified glass powder;The above-mentioned modified glass flakes of 45g are weighed,
13mL polyacrylic acid PAAS, 2g itaconic acid, 2g calcirm-fluoride, 2g zirconium oxides, is fitted into ball mill, with 350r/min ball milling 35min,
Modified glass ionomer cement is obtained, adds the above-mentioned composite natral hydroxyapatite powders of 5g, continues ball milling 25min, obtains carious tooth
Fill patching material.
The present invention application process be:By solid-to-liquid ratio 9:Carious tooth produced by the present invention is filled patching material and deionization by 1
Water mixes, and stirs 25min with 70r/min, pastel is made, then by one layer of Y- chloropropyl three of carious tooth enamel surface even spread
Ethoxysilane, then 13s is dried up with compressed air, carious tooth hole or breakage then are filled with pastel, it is 2g/ to control dosage
cm2, the pastel that surrounding is overflowed is removed after filling, you can.
Example 3
The fresh ox bones of 2kg are weighed, are placed in drying box, it is dry at 110 DEG C to load to constant weight, then by dried ox bone
Crushed in pulverizer, cross 60 mesh sieves, the ox bone particle after sieving is placed in Muffle furnace, 2h is calcined at 700 DEG C, is cooled to room
Wen Hou, then calcined product and 200g CPPs are transferred in ball mill, with 400r/min ball milling 40min, cross 200 mesh
Sieve, obtains composite natral hydroxyapatite powder;200g silicate glass powder is weighed, is placed in 30min in 3.0L deionized waters, then add
It is 40% hydrofluoric acid to enter 100mL mass fractions, with 400r/min stir 10h, then continue in centrifuge, with 6000r/min from
The heart separates 12min, collects precipitation, precipitation is washed with deionized 5 times, then precipitation is placed in drying box, is dried at 120 DEG C
To constant weight, surface roughening glass dust is obtained;Above-mentioned surface roughening glass dust is immersed in 600mL toluene, and surpassed with 300W
Sound disperses 40min, adds 80mL silane resin acceptor kh-550s, 5g nano titanium oxides, 2g aluminum fluorides, in 90 DEG C of waters bath with thermostatic control
Under, with 600r/min insulated and stirred 8h, then filtering, washs filter residue 5 times with absolute ethyl alcohol and deionized water successively, then by filter residue
It is placed in vacuum drying chamber, is dried at 110 DEG C to constant weight, obtain modified glass powder;The above-mentioned modified glass flakes of 50g are weighed,
15mL polyacrylic acid PAAS, 3g itaconic acid, 2g calcirm-fluoride, 3g zirconium oxides, is fitted into ball mill, with 400r/min ball milling 40min,
Modified glass ionomer cement is obtained, adds the above-mentioned composite natral hydroxyapatite powders of 6g, continues ball milling 30min, obtains carious tooth
Fill patching material.
The present invention application process be:By solid-to-liquid ratio 9:Carious tooth produced by the present invention is filled patching material and deionization by 1
Water mixes, and stirs 30min with 80r/min, pastel is made, then by one layer of Y- chloropropyl three of carious tooth enamel surface even spread
Ethoxysilane, then 15s is dried up with compressed air, carious tooth hole or breakage then are filled with pastel, it is 3g/ to control dosage
cm2, the pastel that surrounding is overflowed is removed after filling, you can.
Claims (1)
1. a kind of preparation method of carious tooth filling patching material, it is characterised in that specifically preparation process is:
(1) the fresh ox bones of 1~2kg are weighed, are placed in drying box, are dried at 105~110 DEG C to constant weight, then will be dried
Ox bone, which is fitted into pulverizer, to be crushed, and crosses 60 mesh sieves, the ox bone particle after sieving is placed in Muffle furnace, forged at 600~700 DEG C
1~2h is burnt, after being cooled to room temperature, then calcined product and 100~200g CPPs is transferred in ball mill, with 300~
400r/min 30~40min of ball milling, 200 mesh sieves are crossed, obtain composite natral hydroxyapatite powder, it is standby;
(2) 100~200g silicate glass powder is weighed, is placed in 20~30min in 1.5~3.0L deionized waters, add 80~
100mL mass fractions are 40% hydrofluoric acid, stir 6~10h with 300~400r/min, then continue in centrifuge, with 5000~
6000r/min centrifuges 10~12min, collects precipitation, precipitation is washed with deionized 3~5 times, then precipitation is placed in into drying
In case, dried at 110~120 DEG C to constant weight, obtain surface roughening glass dust;
(3) above-mentioned surface roughening glass dust is immersed in 500~600mL toluene, and with 300W ultrasonic disperses 30~
40min, add 50~80mL silane resin acceptor kh-550s, 3~5g nano titanium oxides, 1~2g aluminum fluorides, at 80~90 DEG C
Under water bath with thermostatic control, with 500~600r/min, 6~8h of insulated and stirred, then filtering, is washed with absolute ethyl alcohol and deionized water successively
Filter residue 3~5 times, then filter residue is placed in vacuum drying chamber, dried at 105~110 DEG C to constant weight, obtain modified glass powder;
(4) the above-mentioned modified glass flakes of 40~50g, 12~15mL polyacrylic acid PAAS, 2~3g itaconic acid, 1~2g fluorinations are weighed
Calcium, 1~3g zirconium oxides, is fitted into ball mill, with 300~400r/min, 30~40min of ball milling, obtains modified glass ionomer cements
Agent, the composite natral hydroxyapatite powder of 5~6g steps (1) preparation is added, continue 20~30min of ball milling, obtain carious tooth and fill
Fill out patching material.
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN108158828A (en) * | 2017-12-12 | 2018-06-15 | 常州蓝旗亚纺织品有限公司 | A kind of preparation method for repairing periodontium type apex radicis dentis packing material |
CN108618968A (en) * | 2018-06-05 | 2018-10-09 | 佛山皖阳生物科技有限公司 | A kind of preparation method of anti-demineralization type enamel repair materials |
CN112142454A (en) * | 2020-09-29 | 2020-12-29 | 成都贝施美生物科技有限公司 | Porcelain powder with self-repairing function |
CN112972270A (en) * | 2021-03-26 | 2021-06-18 | 浙江中医药大学 | Resin cement based on Chinese herbal medicine and nano-silver antibacterial agent |
CN116196222A (en) * | 2023-02-28 | 2023-06-02 | 上海沐良医疗器械有限公司 | Caries preventing additive, caries preventing material, dental diaphragm and invisible appliance |
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CN1714864A (en) * | 2005-06-15 | 2006-01-04 | 美晨集团股份有限公司 | Nano grade polypeptide anti-dental caries material and producing method and tooth-paste containing said material |
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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108158828A (en) * | 2017-12-12 | 2018-06-15 | 常州蓝旗亚纺织品有限公司 | A kind of preparation method for repairing periodontium type apex radicis dentis packing material |
CN108618968A (en) * | 2018-06-05 | 2018-10-09 | 佛山皖阳生物科技有限公司 | A kind of preparation method of anti-demineralization type enamel repair materials |
CN112142454A (en) * | 2020-09-29 | 2020-12-29 | 成都贝施美生物科技有限公司 | Porcelain powder with self-repairing function |
CN112142454B (en) * | 2020-09-29 | 2021-08-17 | 成都贝施美生物科技有限公司 | Porcelain powder with self-repairing function |
CN112972270A (en) * | 2021-03-26 | 2021-06-18 | 浙江中医药大学 | Resin cement based on Chinese herbal medicine and nano-silver antibacterial agent |
CN112972270B (en) * | 2021-03-26 | 2022-07-05 | 浙江中医药大学 | Resin cement based on Chinese herbal medicine and nano-silver antibacterial agent |
CN116196222A (en) * | 2023-02-28 | 2023-06-02 | 上海沐良医疗器械有限公司 | Caries preventing additive, caries preventing material, dental diaphragm and invisible appliance |
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Application publication date: 20171201 |