CN116850066A - Anti-collapsibility injectable hydraulic paste material, and preparation method and application thereof - Google Patents
Anti-collapsibility injectable hydraulic paste material, and preparation method and application thereof Download PDFInfo
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- CN116850066A CN116850066A CN202310676095.8A CN202310676095A CN116850066A CN 116850066 A CN116850066 A CN 116850066A CN 202310676095 A CN202310676095 A CN 202310676095A CN 116850066 A CN116850066 A CN 116850066A
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- powder
- collapsibility
- injectable
- paste material
- hydraulic paste
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- 239000000463 material Substances 0.000 title claims abstract description 88
- 238000002360 preparation method Methods 0.000 title abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 120
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 claims abstract description 48
- 239000001506 calcium phosphate Substances 0.000 claims abstract description 46
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 claims abstract description 41
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 claims abstract description 41
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 claims abstract description 41
- 235000019691 monocalcium phosphate Nutrition 0.000 claims abstract description 41
- YYRMJZQKEFZXMX-UHFFFAOYSA-L calcium bis(dihydrogenphosphate) Chemical compound [Ca+2].OP(O)([O-])=O.OP(O)([O-])=O YYRMJZQKEFZXMX-UHFFFAOYSA-L 0.000 claims abstract description 40
- 229910000150 monocalcium phosphate Inorganic materials 0.000 claims abstract description 40
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 claims abstract description 38
- BCAARMUWIRURQS-UHFFFAOYSA-N dicalcium;oxocalcium;silicate Chemical compound [Ca+2].[Ca+2].[Ca]=O.[O-][Si]([O-])([O-])[O-] BCAARMUWIRURQS-UHFFFAOYSA-N 0.000 claims abstract description 34
- 229910021534 tricalcium silicate Inorganic materials 0.000 claims abstract description 34
- 235000019976 tricalcium silicate Nutrition 0.000 claims abstract description 34
- 239000007788 liquid Substances 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 19
- 210000004262 dental pulp cavity Anatomy 0.000 claims abstract description 6
- 238000007493 shaping process Methods 0.000 claims abstract description 4
- 239000002245 particle Substances 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 7
- 239000011344 liquid material Substances 0.000 claims description 4
- 229910052588 hydroxylapatite Inorganic materials 0.000 abstract 1
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 23
- 239000000243 solution Substances 0.000 description 17
- 239000000203 mixture Substances 0.000 description 14
- 238000002347 injection Methods 0.000 description 13
- 239000007924 injection Substances 0.000 description 13
- 229910052918 calcium silicate Inorganic materials 0.000 description 12
- 239000002131 composite material Substances 0.000 description 12
- 239000008367 deionised water Substances 0.000 description 12
- 229910021641 deionized water Inorganic materials 0.000 description 12
- 235000012241 calcium silicate Nutrition 0.000 description 11
- 238000003756 stirring Methods 0.000 description 11
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 10
- 239000000378 calcium silicate Substances 0.000 description 10
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 10
- 239000002639 bone cement Substances 0.000 description 9
- 239000007790 solid phase Substances 0.000 description 9
- 238000005303 weighing Methods 0.000 description 9
- 229910052586 apatite Inorganic materials 0.000 description 7
- 229910000389 calcium phosphate Inorganic materials 0.000 description 7
- 239000011812 mixed powder Substances 0.000 description 7
- VSIIXMUUUJUKCM-UHFFFAOYSA-D pentacalcium;fluoride;triphosphate Chemical compound [F-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O VSIIXMUUUJUKCM-UHFFFAOYSA-D 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 6
- 229960001714 calcium phosphate Drugs 0.000 description 6
- 235000011010 calcium phosphates Nutrition 0.000 description 6
- 238000006703 hydration reaction Methods 0.000 description 6
- 239000002002 slurry Substances 0.000 description 6
- 238000011049 filling Methods 0.000 description 5
- 239000011521 glass Substances 0.000 description 5
- 239000007791 liquid phase Substances 0.000 description 5
- 230000000975 bioactive effect Effects 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- 239000005548 dental material Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 230000036571 hydration Effects 0.000 description 4
- 238000007789 sealing Methods 0.000 description 4
- 239000012890 simulated body fluid Substances 0.000 description 4
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 3
- 239000003462 bioceramic Substances 0.000 description 3
- 230000033558 biomineral tissue development Effects 0.000 description 3
- 239000001110 calcium chloride Substances 0.000 description 3
- 229910001628 calcium chloride Inorganic materials 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 229960003943 hypromellose Drugs 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 230000008439 repair process Effects 0.000 description 3
- 238000007711 solidification Methods 0.000 description 3
- 230000008023 solidification Effects 0.000 description 3
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 210000000988 bone and bone Anatomy 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 238000006073 displacement reaction Methods 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000003628 erosive effect Effects 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- GVALZJMUIHGIMD-UHFFFAOYSA-H magnesium phosphate Chemical compound [Mg+2].[Mg+2].[Mg+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O GVALZJMUIHGIMD-UHFFFAOYSA-H 0.000 description 2
- 239000004137 magnesium phosphate Substances 0.000 description 2
- 229910000157 magnesium phosphate Inorganic materials 0.000 description 2
- 229960002261 magnesium phosphate Drugs 0.000 description 2
- 235000010994 magnesium phosphates Nutrition 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- -1 monocalcium phosphate compound Chemical class 0.000 description 2
- 229910000402 monopotassium phosphate Inorganic materials 0.000 description 2
- 235000019796 monopotassium phosphate Nutrition 0.000 description 2
- 208000028169 periodontal disease Diseases 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 229920001223 polyethylene glycol Polymers 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 239000000661 sodium alginate Substances 0.000 description 2
- 235000010413 sodium alginate Nutrition 0.000 description 2
- 229940005550 sodium alginate Drugs 0.000 description 2
- 229910000497 Amalgam Inorganic materials 0.000 description 1
- 229920001661 Chitosan Polymers 0.000 description 1
- 108010010803 Gelatin Proteins 0.000 description 1
- 239000000899 Gutta-Percha Substances 0.000 description 1
- 229920002752 Konjac Polymers 0.000 description 1
- 208000025157 Oral disease Diseases 0.000 description 1
- 240000000342 Palaquium gutta Species 0.000 description 1
- 208000024216 Periapical disease Diseases 0.000 description 1
- 239000011398 Portland cement Substances 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 206010066901 Treatment failure Diseases 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 238000004026 adhesive bonding Methods 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- AGWMJKGGLUJAPB-UHFFFAOYSA-N aluminum;dicalcium;iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Al+3].[Ca+2].[Ca+2].[Fe+3] AGWMJKGGLUJAPB-UHFFFAOYSA-N 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910000416 bismuth oxide Inorganic materials 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 229940062672 calcium dihydrogen phosphate Drugs 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- FUFJGUQYACFECW-UHFFFAOYSA-L calcium hydrogenphosphate Chemical compound [Ca+2].OP([O-])([O-])=O FUFJGUQYACFECW-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- JHLNERQLKQQLRZ-UHFFFAOYSA-N calcium silicate Chemical compound [Ca+2].[Ca+2].[O-][Si]([O-])([O-])[O-] JHLNERQLKQQLRZ-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229940045110 chitosan Drugs 0.000 description 1
- 229960004106 citric acid Drugs 0.000 description 1
- 235000015165 citric acid Nutrition 0.000 description 1
- 239000010634 clove oil Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 208000002925 dental caries Diseases 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- HOOWDPSAHIOHCC-UHFFFAOYSA-N dialuminum tricalcium oxygen(2-) Chemical compound [O--].[O--].[O--].[O--].[O--].[O--].[Al+3].[Al+3].[Ca++].[Ca++].[Ca++] HOOWDPSAHIOHCC-UHFFFAOYSA-N 0.000 description 1
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 description 1
- RBLGLDWTCZMLRW-UHFFFAOYSA-K dicalcium phosphate dihydrate Substances O.O.[Ca+2].[Ca+2].[O-]P([O-])([O-])=O RBLGLDWTCZMLRW-UHFFFAOYSA-K 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 229920000159 gelatin Polymers 0.000 description 1
- 239000008273 gelatin Substances 0.000 description 1
- 235000019322 gelatine Nutrition 0.000 description 1
- 235000011852 gelatine desserts Nutrition 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 229920000588 gutta-percha Polymers 0.000 description 1
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 208000030194 mouth disease Diseases 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 235000011837 pasties Nutrition 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 239000001508 potassium citrate Substances 0.000 description 1
- 229960002635 potassium citrate Drugs 0.000 description 1
- QEEAPRPFLLJWCF-UHFFFAOYSA-K potassium citrate (anhydrous) Chemical compound [K+].[K+].[K+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O QEEAPRPFLLJWCF-UHFFFAOYSA-K 0.000 description 1
- 235000011082 potassium citrates Nutrition 0.000 description 1
- GNSKLFRGEWLPPA-UHFFFAOYSA-M potassium dihydrogen phosphate Chemical compound [K+].OP(O)([O-])=O GNSKLFRGEWLPPA-UHFFFAOYSA-M 0.000 description 1
- LWIHDJKSTIGBAC-UHFFFAOYSA-K potassium phosphate Substances [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000012113 quantitative test Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910000018 strontium carbonate Inorganic materials 0.000 description 1
- 229910014031 strontium zirconium oxide Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- GBNXLQPMFAUCOI-UHFFFAOYSA-H tetracalcium;oxygen(2-);diphosphate Chemical group [O-2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O GBNXLQPMFAUCOI-UHFFFAOYSA-H 0.000 description 1
- 210000001519 tissue Anatomy 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/50—Preparations specially adapted for dental root treatment
- A61K6/54—Filling; Sealing
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/15—Compositions characterised by their physical properties
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/50—Preparations specially adapted for dental root treatment
- A61K6/56—Apical treatment
-
- 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
-
- 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
Landscapes
- Health & Medical Sciences (AREA)
- Oral & Maxillofacial Surgery (AREA)
- Epidemiology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Plastic & Reconstructive Surgery (AREA)
- Materials For Medical Uses (AREA)
- Dental Preparations (AREA)
Abstract
The invention discloses an anti-collapsibility injectable hydraulic paste material, a preparation method and application thereof, and belongs to the field of biomedical materials. The hydraulic paste material comprises a powder component and a liquid component, wherein the powder component comprises tricalcium silicate powder, beta-tricalcium phosphate powder and anhydrous monocalcium phosphate; the liquid agent comprises 1-3% hydroxypropyl methyl cellulose water solution, and the mass ratio of the powder of the hydraulic paste material to the liquid agent is 1.5-2.5:1. The anti-collapsibility injectable hydraulic paste material prepared by the invention not only has excellent anti-collapsibility and injectability, but also can be automatically and rapidly solidified, is convenient to operate and easy to fill, can prevent the paste from being eroded in an aqueous environment, can induce the generation of bone-like hydroxyapatite, and can be used in the dental restoration fields such as medullary covering, root tip shaping, root canal treatment and the like.
Description
Technical Field
The invention relates to the field of biomedical materials, in particular to an anti-collapsibility injectable hydraulic paste material, a preparation method and application thereof.
Background
In 2022, the global oral health report issued by the world health organization indicates that about 45% of the population worldwide suffers from different types of oral diseases, caries, periodontal disease, pulp periapical disease, etc. are the most common oral problems, which place an urgent need for high-performance dental filling materials. The dental materials used clinically are various in variety and different in style, and mainly comprise silver amalgam, gutta-percha point, zinc oxide clove oil water valve, glass ion water valve, bioactive ceramic materials and the like. Calcium silicate based bioactive materials are very promising dental materials. Mahmoud Torabinejad has successfully developed aggregates of minerals trioxide (Mineral Trioxide Aggregate, MTA) as a calcium silicate-based bioactive ceramic material for use in the dental field in 1993, and was approved by the United states food and drug administration (Food and Drug Administraton, FDA) in 1998 for use in pulp-related disease treatment for good clinical efficacy.
The MTA has intrinsic solidification performance, good biocompatibility, sealing performance, X-ray radiation resistance and certain antibacterial performance, and is widely applied to the treatment of periodontal diseases such as root canal filling, root tip shaping, medullary covering, active medullary cutting, pulp chamber bottom perforation repair and the like. The main components of MTA are tricalcium silicate, dicalcium silicate, tricalcium aluminate, tetracalcium aluminoferrite, bismuth oxide and the like. The self-setting properties of the cementitious phase of portland cement in MTA are a precondition for its applicability in the field of endodontics. In clinical use, the solid powder and the liquid agent are mixed according to a certain proportion to form pasty slurry, and a hydration reaction is carried out, so that a solidified substance with mechanical strength is gradually formed by flowing plastic paste. However, insufficient curing properties (curing time up to 3-4 hours), poor collapsibility, poor handling properties are major problems with conventional MTA dental materials. The newly prepared calcium silicate-based self-curing material can freely collapse when encountering aqueous liquid phase, which not only easily causes paste to not tightly fill the tooth body and form micro-leakage to cause treatment failure, but also is unfavorable for the performance development of filling materials.
Inorganic salts such as calcium chloride, calcium carbonate, and sodium carbonate have been reported to promote the curing reaction of calcium silicate-based materials, shortening the curing time. The organic matters such as konjaku gum, sodium alginate and gelatin can effectively improve the collapsibility and injection performance of bone cement such as silicate, etc., and the method mainly improves the bonding force among particles by forming an organic film on the surface of paste through the organic matters, enhances the erosion effect of water solution and improves the injection performance of slurry, but the organic film layer can inevitably obstruct the curing reaction of silicate, so that the curing time of silicate can be prolonged.
Chinese patent CN105999418A discloses an injectable bioactive bone cement material and a preparation method thereof, the bone cement material comprises a calcium silicate-based inorganic material, a high molecular polymer such as glycerol and additives such as hypromellose and calcium chloride, the material only contains a single calcium silicate-based self-curing system, and forms a premixed paste through glycerol and the like, so that the bone cement has a slow curing reaction, in addition, the hypromellose is added into the bone cement material as an additive, the system does not contain an aqueous phase, the hypromellose exists only in the form of powder particles, and an aqueous solution is not formed, so that the binding effect and film forming characteristics cannot be exerted, and the anti-collapsibility of the bone cement material is poor.
Chinese patent CN111110571a discloses a high-efficiency sealing treatment composition for tooth root canal system, and preparation method and application thereof, wherein silicate in the composition is tricalcium silicate, beta-dicalcium silicate, and contains dicalcium phosphate dihydrate, the composition has accelerated curing reaction, but the problems of poor collapsibility resistance and insufficient operability of calcium silicate-based paste are not solved, and excessive acidic phosphate is unfavorable for the development of hydration performance of silicate. Chinese patent CN112843341A discloses an injectable calcium silicate based self-curing bioceramic, a preparation method and application thereof, and the technology of the patent is that tricalcium silicate, calcium chloride, strontium carbonate, zirconium oxide and amorphous calcium phosphate are mixed with polyethylene glycol to form a premixed paste, the self-curing bioceramic material is a premixed paste, and has good injectability and operability, but the curing of the material is based on the substitution of polyethylene glycol with water molecules in an aqueous environment, so that the silicate is subjected to hydration reaction, the curing time of a system is longer, and the amorphous calcium phosphate in the material does not have curing characteristics and cannot improve the curing reaction rate of the system.
In addition, chinese patent CN103007340a discloses a self-curing composite bone repair material for repairing hard tissue of human body and application, the material is composed of solid phase powder and liquid phase, wherein the solid phase contains tricalcium silicate, electrofused magnesia, calcium phosphate bone cement, monopotassium phosphate, etc.; the liquid phase is one or more of deionized water, soluble phosphate, sodium alginate, citric acid, potassium citrate and chitosan. The composite bone repair material has shortened curing time, but the composite material system contains various curing reaction materials such as calcium phosphate, magnesium phosphate and the like, so that the material has poor operation performance, is difficult to inject, and the silicate in the composite material is only a small amount of minor phase, and does not solve the defect of poor anti-collapsibility of silicate bone cement.
In summary, various methods have been proposed at home and abroad to solve the problems of insufficient curing performance and poor anti-collapsibility of calcium silicate-based dental materials, but different strategies have certain defects, and the construction of an injectable anti-collapsibility type biological ceramic self-curing material is a problem to be solved in the field.
Disclosure of Invention
The invention aims to solve the problems of poor collapsibility and poor operability of the existing silicate-based material, overcome the defect that a single organic collapsibility-resistant material damages the solidification performance of the silicate material, and provide an anti-collapsibility injectable hydraulic paste material through beta-tricalcium phosphate powder, anhydrous monocalcium phosphate and hydroxypropyl methyl cellulose aqueous solution for the first time, and a preparation method and application thereof.
Although other self-curing systems such as calcium phosphate or magnesium phosphate are involved in the prior art to enhance the curing performance of the calcium silicate-based paste, the calcium phosphate system is tetra-calcium phosphate or alpha-tricalcium phosphate, and potassium dihydrogen phosphate and the like are additionally added (such as the technology mentioned in the background art), at present, no beta-tricalcium phosphate powder/anhydrous monocalcium phosphate complex is introduced into the tricalcium silicate curing system, and the hydroxypropyl methylcellulose solution is used as a liquid phase in an auxiliary way, so that the injectable collapsibility-resistant hydraulic paste material is constructed. The system strengthens the solidification performance and the anti-collapsibility of the tricalcium silicate material by inorganic-organic composite.
The technical problems to be solved by the invention are realized by adopting the following technical scheme:
an anti-collapsibility injectable hydraulic paste material, which is composed of powder and liquid; the powder comprises the following components in percentage by mass: 5-20% of tricalcium silicate powder, beta-tricalcium phosphate powder/anhydrous monocalcium phosphate powder; the liquid agent is hydroxypropyl methyl cellulose solution; wherein, the mol ratio of the beta-tricalcium phosphate powder to the anhydrous monocalcium phosphate powder is 0.6-1.4: 1.
preferably, the mass ratio of the powder to the liquid is 1.5-2.5: 1.
preferably, the concentration of the hydroxypropyl methylcellulose solution is 1 to 3wt%.
Preferably, the particle size of the tricalcium silicate powder is 0.1-10 mu m.
Preferably, the particle size of the beta-tricalcium phosphate powder is 0.1-10 mu m.
Preferably, the particle size of the anhydrous calcium dihydrogen phosphate powder is 0.1-50 μm.
The invention also provides a preparation method of the anti-collapsibility injectable hydraulic paste material, which comprises the following steps:
mixing tricalcium silicate powder, beta-tricalcium phosphate powder and anhydrous monocalcium phosphate powder in proportion to obtain powder material; adding hydroxypropyl methyl cellulose into water for dissolution to obtain a liquid material; uniformly blending the powder material and the liquid material according to the mass ratio of 1.5-2.5:1 to obtain the anti-collapsibility injectable hydraulic paste material.
The invention also provides application of the anti-collapsibility injectable hydraulic paste material in the dental restoration fields of medullary coverage, root tip shaping, root canal treatment and the like.
The beneficial effects of the invention are as follows:
1. the preparation method is characterized in that the beta-tricalcium phosphate powder/anhydrous monocalcium phosphate complex and the hydroxypropyl methylcellulose solution are used for solving the technical problems of poor anti-collapsibility and insufficient solidifying performance of the tricalcium silicate biological ceramic paste material for the first time, the hardening rate of the composite paste is enhanced by introducing a beta-tricalcium phosphate powder/anhydrous monocalcium phosphate self-solidifying system, and simultaneously, the monetite generated by the reaction of the beta-tricalcium phosphate powder and the anhydrous monocalcium phosphate can react with calcium hydroxide of a tricalcium silicate hydration product to form apatite, so that the solidifying reaction of the paste is further improved, the solidifying time is shortened, the gluing and bonding characteristics among paste particles are enhanced, and the anti-collapsibility of the paste is improved. In addition, hydroxypropyl methylcellulose enhances the granule strength of the paste and improves the resistance to water erosion, so that the hydraulic paste has excellent injectability and collapsibility.
2. The beta-tricalcium phosphate powder/anhydrous monocalcium phosphate complex is mixed with hydroxypropyl methyl cellulose for introduction, so that the defect that the traditional organic anti-collapsibility agent weakens hydration capacity of tricalcium silicate-based paste can be overcome, the anti-collapsibility of the paste can be effectively improved, the flowing characteristic of beta-tricalcium phosphate/anhydrous monocalcium phosphate particles is enhanced through interaction of hydroxypropyl methyl cellulose and the beta-tricalcium phosphate powder/anhydrous monocalcium phosphate complex, the operation and injection performance of the system are enhanced, and the technical problem that the anti-collapsibility and hardening process of the bioceramic bone cement material cannot be synergistically enhanced is solved. On the other hand, the beta-tricalcium phosphate powder/anhydrous monocalcium phosphate compound can compensate the hydration hysteresis effect of hydroxypropyl methyl cellulose, and the self-curing reaction rate of the system is improved.
3. The hydraulic paste has good operability, is easy to fill, can seal small and complex root canal systems, and improves the sealing filling quality.
4. The hydraulic paste has good biocompatibility and apatite forming capability, can induce bone-like apatite deposition, improves the bonding strength of filling materials and dental bodies, and reduces the risk of micro leakage.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the invention and together with the description, serve to explain the principles of the invention, wherein:
FIG. 1 is a photograph showing the characterization of the anti-collapsibility of the hydraulic paste materials prepared in comparative examples 1 to 4;
FIG. 2 is a photograph showing characterization of anti-collapsibility of an injectable hydraulic paste material prepared in examples 1 to 3 and a hydraulic paste material prepared in comparative example 3;
FIG. 3 is an anti-collapsibility quantitative result of an injectable hydraulic paste material of examples 1 to 3 and a hydraulic paste material of comparative example 3;
FIG. 4 shows the injectability of an anti-collapsing injectable hydraulic paste material prepared in examples 1 to 3 and a hydraulic paste material prepared in comparative example 3;
FIG. 5 shows the injection force and displacement results of an anti-collapsing injectable hydraulic paste material prepared in example 3 of the present invention;
FIG. 6 is a graph showing the setting time results of an anti-collapsibility injectable hydraulic paste material prepared in examples 1 to 3 and a hydraulic paste material prepared in comparative example 3;
fig. 7 is an SEM image of an anti-collapsibility injectable hydraulic paste material prepared in example 2 according to the present invention after soaking simulated body fluid.
FIG. 8 is a photograph showing the anti-collapsibility of an injectable hydraulic paste material prepared in example 6 of the present invention;
FIG. 9 is a photograph showing the anti-collapsibility of an injectable hydraulic paste material prepared in example 7 of the present invention.
Detailed Description
The following disclosure provides many different embodiments, or examples, for implementing different features of the invention. In order to simplify the present disclosure, components and arrangements of specific examples are described below. They are, of course, merely examples and are not intended to limit the invention. Furthermore, the present invention may repeat reference numerals and/or letters in the various examples, which are for the purpose of brevity and clarity, and which do not themselves indicate the relationship between the various embodiments and/or arrangements discussed.
Example 1
Weighing solid phase powder according to the following mass percent: 95% tricalcium silicate powder, the rest 5% beta-tricalcium phosphate powder and anhydrous monocalcium phosphate mixed powder, and the mol ratio of the beta-tricalcium phosphate powder to the anhydrous monocalcium phosphate is 1:1, uniformly mixing three kinds of powder to form powder;
0.2g of hydroxypropyl methylcellulose is dissolved in 9.8g of deionized water to prepare a hydroxypropyl methylcellulose solution with the concentration of 2 percent as a liquid agent;
and then the powder and the liquid are mixed according to the mass ratio of 2:1, stirring the mixture fully and uniformly to prepare the hydraulic paste material.
Example 2
Weighing solid phase powder according to the following mass percent: 90% of tricalcium silicate powder, the balance of 10% of beta-tricalcium phosphate powder and anhydrous monocalcium phosphate mixed powder, and the molar ratio of beta-tricalcium phosphate powder to anhydrous monocalcium phosphate is 1:1, uniformly mixing three kinds of powder to form powder;
0.2g of hydroxypropyl methylcellulose is dissolved in 9.8g of deionized water to prepare a hydroxypropyl methylcellulose solution with the concentration of 2 percent as a liquid agent;
and then the powder and the liquid are mixed according to the mass ratio of 2:1, stirring the mixture fully and uniformly to prepare the hydraulic paste material.
Example 3
Weighing solid phase powder according to the following mass percent: 80% of tricalcium silicate powder, the balance of 20% of beta-tricalcium phosphate powder and anhydrous monocalcium phosphate mixed powder, and the molar ratio of the beta-tricalcium phosphate powder to the anhydrous monocalcium phosphate is 1:1, uniformly mixing three kinds of powder to form powder;
0.2g of hydroxypropyl methylcellulose is dissolved in 9.8g of deionized water to prepare a hydroxypropyl methylcellulose solution with the concentration of 2 percent as a liquid agent;
and then the powder and the liquid are mixed according to the mass ratio of 2:1, stirring the mixture fully and uniformly to prepare the hydraulic paste material.
Example 4
Weighing solid phase powder according to the following mass percent: 90% of tricalcium silicate powder, the balance of 10% of beta-tricalcium phosphate powder and anhydrous monocalcium phosphate mixed powder, and the molar ratio of beta-tricalcium phosphate powder to anhydrous monocalcium phosphate is 1:1, uniformly mixing three kinds of powder to form powder;
0.1g of hydroxypropyl methylcellulose is dissolved in 9.9g of deionized water to prepare a hydroxypropyl methylcellulose solution with the concentration of 1 percent as a liquid agent;
and then the powder and the liquid are mixed according to the mass ratio of 2.5:1, stirring the mixture fully and uniformly to prepare the hydraulic paste material.
Example 5
Weighing solid phase powder according to the following mass percent: 95% tricalcium silicate powder, the rest 5% beta-tricalcium phosphate powder and anhydrous monocalcium phosphate mixed powder, and the mol ratio of the beta-tricalcium phosphate powder to the anhydrous monocalcium phosphate is 1:1, uniformly mixing three kinds of powder to form powder;
0.3g of hydroxypropyl methylcellulose is dissolved in 9.7g of deionized water to prepare a hydroxypropyl methylcellulose solution with the concentration of 3 percent as a liquid agent;
and then the powder and the liquid are mixed according to the mass ratio of 1.5:1, stirring the mixture fully and uniformly to prepare the hydraulic paste material.
Example 6
Weighing solid phase powder according to the following mass percent: 95% tricalcium silicate powder, the rest 5% beta-tricalcium phosphate powder and anhydrous monocalcium phosphate mixed powder, and the molar ratio of the beta-tricalcium phosphate powder to the anhydrous monocalcium phosphate is 0.6:1, uniformly mixing three kinds of powder to form powder;
0.2g of hydroxypropyl methylcellulose is dissolved in 9.8g of deionized water to prepare a hydroxypropyl methylcellulose solution with the concentration of 2 percent as a liquid agent;
and then the powder and the liquid are mixed according to the mass ratio of 2:1, stirring the mixture fully and uniformly to prepare the hydraulic paste material.
Example 7
Weighing solid phase powder according to the following mass percent: 90% of tricalcium silicate powder, the balance of 10% of beta-tricalcium phosphate powder and anhydrous monocalcium phosphate mixed powder, and the molar ratio of beta-tricalcium phosphate powder to anhydrous monocalcium phosphate is 1.4:1, uniformly mixing three kinds of powder to form powder;
0.2g of hydroxypropyl methylcellulose is dissolved in 9.8g of deionized water to prepare a hydroxypropyl methylcellulose solution with the concentration of 2 percent as a liquid agent;
and then the powder and the liquid are mixed according to the mass ratio of 1.5:1, stirring the mixture fully and uniformly to prepare the hydraulic paste material.
Comparative example 1
Single tricalcium silicate powder is taken as powder;
deionized water solution is used;
and then the powder and the liquid are mixed according to the mass ratio of 2:1, stirring the mixture fully and uniformly to prepare the hydraulic paste material.
Comparative example 2
Weighing 100% tricalcium silicate powder by mass percent as powder forming agent;
0.1g of hydroxypropyl methylcellulose is dissolved in 9.9g of deionized water to prepare a hydroxypropyl methylcellulose solution with the concentration of 1 percent as a liquid agent;
and then the powder and the liquid are mixed according to the mass ratio of 2:1, stirring the mixture fully and uniformly to prepare the hydraulic paste material.
Comparative example 3
Single tricalcium silicate powder is taken as powder;
0.2g of hydroxypropyl methylcellulose is dissolved in 9.8g of deionized water to prepare a hydroxypropyl methylcellulose solution with the concentration of 2 percent as a liquid agent;
and then the powder and the liquid are mixed according to the mass ratio of 2:1, stirring the mixture fully and uniformly to prepare the hydraulic paste material.
Comparative example 4
Weighing 100% tricalcium silicate powder by mass percent as powder forming agent;
0.3g of hydroxypropyl methylcellulose is dissolved in 9.7g of deionized water to prepare a hydroxypropyl methylcellulose solution with the concentration of 3 percent as a liquid agent;
and then the powder and the liquid are mixed according to the mass ratio of 2:1, stirring the mixture fully and uniformly to prepare the hydraulic paste material.
In order to show the superiority of the material of the invention, the hydraulic paste materials prepared in examples 1 to 7 and comparative examples 1 to 4 are tested for collapsibility, curing time, injectability and apatite mineralization.
The method for characterizing the properties of the anti-collapsibility injectable hydraulic paste material is as follows:
the dynamic anti-collapsibility performance comprises qualitative test and quantitative test:
transferring the newly prepared paste material into a syringe, injecting the paste material into a water-containing glass dish, placing the glass dish into a vibrator (100 r/min or 150 r/min) for vibrating for different times, and observing the paste slurry collapse and free phenomenon; in addition, the prepared paste material was newly molded into a sphere, placed in a water-containing glass dish, vibrated in a vibrator at 150r/min for 15min, and the slurry was weighed before and after the test to calculate the anti-collapse rate.
Examples 1 to 7 and comparative examples 1 to 4 were subjected to a dynamic anti-collapse qualitative test, and the results of a part of the tests are shown in fig. 1, and when the paste in comparative example 1 was injected into water, the powder particles were free, and the whole injection process was difficult and the injection performance was poor, and when the paste was vibrated at 100r/min for 10min, the whole paste slurry was not collapsed and scattered over the glass dish. In contrast, the hydraulic pastes of comparative examples 2, 3 and 4, which showed enhanced anti-collapse properties, showed no significant free collapse of particles in their entirety after shaking under the same conditions, and maintained the original injection shape, and were easy to inject. In addition, examples 1 to 7 showed similar good anti-collapse ability, and were able to maintain the overall shape in the aqueous liquid phase without occurrence of paste collapse. From the above results, the hydroxypropyl methylcellulose can effectively improve the anti-collapsibility of the tricalcium silicate paste material, and the anti-collapsibility of the hydroxypropyl methylcellulose is proved.
To further verify the effect of the beta-tricalcium phosphate powder/anhydrous monocalcium phosphate complex on the anti-collapsibility of the tricalcium silicate paste, comparative example 3 and examples 1-3 were tested for anti-collapsibility at higher vibration speeds for longer periods of time, and as shown in fig. 2, all pastes were easy to inject, no particle free phenomenon occurred when water was just injected, and when vibration was carried out at 150r/min for 15min, no significant collapsibility occurred in the tricalcium silicate paste (comparative example 3) without the beta-tricalcium phosphate powder/anhydrous monocalcium phosphate complex, no particle free escaped, while the hydraulic pastes in examples 1-3 all remained in good shapes, no significant powder collapsibility occurred. As can be seen from fig. 8 and 9, the prepared hydraulic paste is easy to inject, has excellent anti-collapse property, and can maintain a good shape in water. Further, as shown in fig. 3, the quantitative results of the dynamic anti-collapse performance of comparative example 3 and examples 1 to 3 show that the paste anti-collapse performance of examples 1 to 3 is improved more than that of comparative example 3, and the maximum anti-collapse rate is more than 95%, and the results show that the beta-tricalcium phosphate powder/anhydrous monocalcium phosphate composite can further remarkably improve the anti-collapse ability of tricalcium silicate paste and can cooperate with hydroxypropyl methylcellulose to exert the anti-collapse property.
Injection performance:
the freshly prepared paste material was loaded into a 2.5mL syringe, and after 10min, the paste was injected and extruded using a universal tester with pressure applied, the ram movement speed was 15mm/min, and the maximum load was 100N. Injectability is expressed as a percentage of the paste weight after extrusion to the total weight of the raw paste.
The injectability test was conducted on examples 1 to 3 and comparative examples 1 and 3, and some of the test results are shown in fig. 4, in which the paste of comparative example 1 was difficult to inject and was prone to the occurrence of the press filtration phenomenon, particles were easily separated from the water phase during injection, the injectability in comparative example 3 was 91.68%, and the injectability in examples 1 to 3 was 94.81%, 94.62% and 88.55%, respectively, which had excellent injectability, and the injectability of the composite paste was slightly increased when the beta-tricalcium phosphate powder/anhydrous monocalcium phosphate complex content was 5% and 10%, and the injectability of the composite paste was slightly decreased when the beta-tricalcium phosphate powder/anhydrous monocalcium phosphate complex content was increased to 20%. The results show that the hydroxypropyl methylcellulose can effectively improve the injectability of the tricalcium silicate paste, and the hydraulic paste still has excellent injectability when the content of the beta-tricalcium phosphate powder/anhydrous monocalcium phosphate complex is in the range of 5-20%. Fig. 5 shows the change in injection force and displacement after 5 minutes of mixing the hydraulic paste of example 3, and shows that the paste injection force is lower than 30N, and the injection is easy and the injection performance is good.
Curing time:
the freshly prepared paste slurry was rapidly placed into a polytetrafluoroethylene mould (diameter 8mm, height 2 mm) and then placed in a 37 ℃ water bath and its cure time was measured by a vicat instrument.
The curing time test was conducted on examples 1-3 and comparative example 3, and as shown in fig. 6, it can be seen from the graph that the curing time of the hydraulic paste in examples 1-3 was significantly lower than that of the tricalcium silicate paste material in comparative example 3, and that 5% -20% of the beta-tricalcium phosphate powder/anhydrous monocalcium phosphate composite was introduced into the hydraulic paste in examples 1-3, compared with comparative example 3, which showed that the beta-tricalcium phosphate powder/anhydrous monocalcium phosphate composite significantly accelerated the curing reaction of the paste of the present invention, shortened the curing time thereof, and further confirmed the effectiveness of the beta-tricalcium phosphate powder/anhydrous monocalcium phosphate composite in promoting the hardening process of the tricalcium silicate paste.
Apatite mineralization performance experiment:
the freshly prepared paste material was filled into a mold and cured, then immersed in a Simulated Body Fluid (SBF), and the sample surface was characterized using a Scanning Electron Microscope (SEM).
Fig. 7 is an SEM photograph of the surface of the hydraulic paste according to example 2 of the present invention after soaking in SBF solution, and it can be seen that spherical bone-like apatite is formed on the surface of the hardened paste, and the result shows that the hydraulic paste according to the present invention has excellent apatite mineralization ability and can enhance the adhesive sealing property between paste and tooth.
Other embodiments of the invention will be apparent to those skilled in the art from consideration of the specification and practice of the invention herein. This invention is intended to cover any variations, uses, or adaptations of the invention following, in general, the principles of the invention and including such departures from the present disclosure as come within known or customary practice within the art to which the invention pertains. It is intended that the specification and examples be considered as exemplary only, with a true scope and spirit of the invention being indicated by the following claims.
It is to be understood that the invention is not limited to the precise arrangements and instrumentalities shown in the drawings, which have been described above, and that various modifications and changes may be effected without departing from the scope thereof. The scope of the invention is limited only by the appended claims.
Claims (8)
1. An anti-collapse injectable hydraulic paste material, characterized in that the hydraulic paste material consists of powder and liquid; the powder comprises the following components in percentage by mass: 5-20% of tricalcium silicate powder, beta-tricalcium phosphate powder/anhydrous monocalcium phosphate powder; the liquid agent is hydroxypropyl methyl cellulose solution; wherein the molar ratio of the beta-tricalcium phosphate powder to the anhydrous monocalcium phosphate powder is 0.6-1.4: 1.
2. the anti-collapsibility injectable hydraulic paste material according to claim 1, wherein the mass ratio of the powder and the liquid agent is 1.5 to 2.5:1.
3. an anti-collapsible injectable hydraulic paste material according to claim 1, wherein the concentration of the hydroxypropyl methylcellulose solution is 1-3 wt%.
4. An anti-collapsible injectable hydraulic paste material according to claim 1 wherein said tricalcium silicate powder has a particle size of 0.1-10 μm.
5. The anti-collapsibility injectable hydraulic paste material according to claim 1, wherein the particle size of the β -tricalcium phosphate powder is 0.1 to 10 μm.
6. The anti-collapsibility injectable hydraulic paste material according to claim 1, wherein the anhydrous monocalcium phosphate powder has a particle diameter of 0.1 to 50 μm.
7. A method of preparing an anti-collapsible injectable hydraulic paste material according to claim 1, comprising the steps of:
mixing the tricalcium silicate powder, the beta-tricalcium phosphate powder and the anhydrous monocalcium phosphate powder in proportion to obtain the powder material; adding hydroxypropyl methyl cellulose into water to dissolve, so as to obtain the liquid material; and uniformly blending the powder material and the liquid material according to the mass ratio of 1.5-2.5:1 to obtain the anti-collapsibility injectable hydraulic paste material.
8. Use of an anti-collapsibility injectable hydraulic paste material according to any one of claims 1 to 6 in the field of dental restorations such as pulp capping, root tip shaping, root canal treatment and the like.
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