CN108113893B - Suspension-stable premixed magnesium phosphate-based dental filling material and preparation method and application thereof - Google Patents
Suspension-stable premixed magnesium phosphate-based dental filling material and preparation method and application thereof Download PDFInfo
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- CN108113893B CN108113893B CN201711458900.0A CN201711458900A CN108113893B CN 108113893 B CN108113893 B CN 108113893B CN 201711458900 A CN201711458900 A CN 201711458900A CN 108113893 B CN108113893 B CN 108113893B
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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
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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
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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
- A61K6/836—Glass
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Abstract
The invention discloses a suspension-stable premixed magnesium phosphate-based dental filling material and a preparation method and application thereof. The filling material of the invention takes magnesium oxide and at least one phosphate as main phases, at least one water-miscible non-aqueous phase solvent and at least one jet-retarding material to prepare the dental filling material with excellent injectability, wherein the filling material can also comprise at least one bioglass. The material can keep fluid under sealed condition, and can be hydrated, solidified and hardened after being filled into teeth and contacting with physiological body fluid. The invention utilizes the excellent biocompatibility and bioactivity of the magnesium phosphate-based material to prepare the premixed magnesium phosphate-based dental filling material with stable suspension, and the premixed magnesium phosphate-based dental filling material can be used as a filling material in the fields of capping marrow surgery, root canal therapy, dental restoration and the like.
Description
Technical Field
The invention relates to a dental filling material and a preparation method and application thereof, in particular to a premixed magnesium phosphate-based dental filling material with stable suspension and a preparation method and application thereof. The invention belongs to the technical field of medical materials.
Background
Dental filling materials have found wide application in dental clinics. It can be classified into a dental cement filling material, a dental prosthetic filling material and a dental filling material for protection according to functions. The development of dental filling materials has undergone a long process, and many materials such as clove oil zinc oxide, zinc phosphate, silver amalgam, glass cement composite resin, etc. are used as dental filling materials. An ideal dental filling material must have good biocompatibility, antibacterial properties and clinical handling properties. In addition, biological activity is used as a measure of the bonding performance of the material to the tooth, and therefore, biological cement or biological glass materials are also receiving increasing attention from dentists and researchers.
The calcium silicate material most used in the dental filling material is a trioxide Material (MTA). Mahmoud torabenejad first disclosed in 1998 a method of repairing a tooth cavity with MTA material (U.S. patent No. 5,769,638). The main components of the MTA material are tricalcium silicate and dicalcium silicate, and the MTA material is similar to Portland cement, can be used in a root canal filling material, but is troublesome to prepare and causes waste. Chinese patent "premixed biological hydraulic cement paste composition and its application" (patent No. CN200880011743.1) discloses a premixed cement paste for medical or dental use, which is prepared by premixing tricalcium silicate, dicalcium silicate and an organic solvent, and is convenient for a doctor to use, but the setting time is too long, some of them require 72 hours to set, and the too long setting time not only results in prolonged waiting time of a patient, but also makes the surgical procedure more complicated. The portland cement does not contain phosphorus element, can not form hydroxyapatite, and has biocompatibility inferior to phosphate with dentin.
Chinese patent 'injectable efficient suspension stable calcium phosphate cement and preparation method and application thereof' (patent No. CN200910197934.8) discloses an injectable calcium phosphate cement material system, which improves the suspension stability of a calcium phosphate cement premix system by adding fumed silica and modified products thereof. The defects are that the calcium phosphate cement has insufficient strength and is easy to break.
Therefore, the further development of the dental filling material with short coagulation time, high biological activity, sufficient compressive strength and good clinical operation performance has very important significance.
Magnesium Phosphate Cement (MPC) is mainly prepared by sintered magnesium oxide, dihydric phosphate and a retarder according to a certain proportion, and has the characteristics of quick setting and high early strength. MPC is similar to Calcium Phosphate Cement (CPC) and can be self-solidified under the physiological environment of human body, and the hydration product is phosphate. Many years of research show that MPC has good biocompatibility and is an ideal bone defect repair material, but MPC has two problems of too fast hydration reaction speed and great hydration heat release, so that MPC has not been paid enough attention and research for a long time. Such problems have not been well solved, as MPC has reached a maximum hydration temperature of approximately 70 ℃ under adiabatic conditions. Patent CN102807335A proposes a method for synthesizing magnesium phosphate bone cement by self-coating controlled hydration reaction, namely, a method for pre-reacting magnesium oxide surface with a small amount of potassium dihydrogen phosphate is adopted, the setting time of magnesium phosphate bone cement is prolonged from 0.7-4 minutes before coating to 6-17 minutes after coating, and the peak value of exothermic temperature is reduced from 55.1-70.5 ℃ to 32.6-38.3 ℃, thus having certain beneficial effect. The invention pre-mixes solid phase components such as magnesium oxide and the like with the organic solvent, similarly solves the 2 problems caused by the over-high reaction speed, the condensation time reaches 3 to 15 hours, and the peak value of the exothermic temperature is basically consistent with the ambient temperature without increasing.
The filling material of the invention takes magnesium oxide and at least one phosphate as main phases, at least one water-miscible non-aqueous phase solvent and at least one jet-retarding material to prepare the dental filling material with excellent injectability, wherein the filling material can also comprise at least one bioglass. The material can keep fluid under sealed condition, and can be hydrated, solidified and hardened after being filled into teeth and contacting with physiological body fluid. The invention utilizes the excellent biocompatibility and bioactivity of the magnesium phosphate-based material to prepare the premixed magnesium phosphate-based dental filling material with stable suspension, and the premixed magnesium phosphate-based dental filling material can be used as a filling material in the fields of capping marrow surgery, root canal therapy, dental restoration and the like.
Disclosure of Invention
The invention aims to provide a premixed magnesium phosphate-based dental filling material which has short coagulation time, high bioactivity and good clinical operability.
In order to achieve the purpose, the invention adopts the following technical means:
the invention relates to a suspension-stable premixed magnesium phosphate-based dental filling material, which comprises the following components: (a) magnesium oxide; (b) at least one phosphate compound; (c) a bioglass; (d) at least one radiation-blocking material; and (e) at least one water-miscible, non-aqueous solvent;
in the premixed magnesium phosphate base dental filling material, the solid components (a), (b), (c) and (d) account for 40 to 92 percent of the total mass of the premixed magnesium phosphate base dental filling material, and the liquid component (e) accounts for 8 to 60 percent of the total mass of the premixed material with stable suspension;
wherein, in the solid components, the components (a) and (b) account for 10-89% of the total mass of the premixed magnesium phosphate-based dental filling material, and the mass ratio of the components (a) and (b) is as follows: (0.05-3): 1;
the component (c) accounts for 0 to 50 percent of the total mass of the premixed magnesium phosphate-based dental filling material;
the component (d) accounts for 10 to 40 percent of the total mass of the premixed magnesium phosphate based dental filling material.
Among them, preferably, component (b) is selected from: at least one of potassium dihydrogen phosphate, sodium dihydrogen phosphate, ammonium dihydrogen phosphate, calcium dihydrogen phosphate, magnesium phosphate, and hydroxyapatite.
Among them, preferably, component (c) is selected from: at least one of bioglass 45S, bioglass 58S, and bioglass 63S.
Among them, preferably, component (d) is selected from: at least one of zirconium oxide, bismuth oxide and tantalum oxide.
Among them, preferably, component (e) is selected from: glycerin, propylene glycol, ethylene glycol, polyethylene glycol, silicone oil, clove oil, animal oil, and vegetable oil.
Furthermore, the invention also provides the application of the premixed magnesium phosphate-based dental filling material in the preparation of filling materials for dental treatment.
Compared with the prior art, the invention has the advantages that:
(1) compared with calcium phosphate cement, the premixed magnesium phosphate-based dental filling material has long solidification time, is convenient for a doctor to operate, and has unobvious reaction temperature rise;
(2) compared with the premixed calcium silicate dental filling material, the premixed magnesium phosphate based dental filling material has the following advantages:
(A) the solidification is fast;
(B) the phosphate has better biocompatibility than silicate, and forms hydroxyapatite;
(C) the compressive strength is adjustable, and different requirements are met by adjusting the proportion of the magnesium phosphate and the bioglass; if the strength of the calcium silicate paste is adjusted to 30-40MA for root canal filling materials, the calcium silicate paste has lower strength and can be well used for retreatment; such as, for example, hard-tuning, may be used for repair,
drawings
FIG. 1 is a photograph of a sample obtained in example 2.
FIG. 2 is a photomicrograph of the material obtained in example 2 after water hardening.
Detailed Description
The invention will be further described with reference to specific embodiments, and the advantages and features of the invention will become apparent as the description proceeds. The examples are illustrative only and do not limit the scope of the present invention in any way. It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention, and that such changes and modifications may be made without departing from the spirit and scope of the invention.
Example 1 preparation of suspension-stabilized premixed magnesium phosphate-based dental filling Material 1
(1) Weighing the following raw materials in percentage by weight: (a) heavy-burned magnesia of 21 percent; (b) 23% of monopotassium phosphate; (c) 37% of zirconium oxide and (d) 19% of polyethylene glycol;
(2) sequentially putting the components in the step (1) into a glass container, mechanically mixing by using a stainless steel stirring rod, and fully blending for 5 min;
(3) and then transferring the mixed paste into a medical injector with an injection hose needle to obtain the premixed magnesium phosphate-based dental filling material with stable suspension.
The material keeps fluid under the sealing condition, is extruded and sampled to be placed in a constant temperature and humidity box (or filled to the teeth to contact with physiological body fluid) with the humidity of more than 95 percent at the temperature of 37 ℃, is hydrated, solidified and hardened, and has the following setting time: for 5 hours.
EXAMPLE 2 preparation of suspension-Stable premixed magnesium phosphate-based dental filling Material 2
(1) Weighing the following raw materials in percentage by weight: (a) 9% of light-burned magnesium oxide; (b) 12% of sodium dihydrogen phosphate; (c) 63S 10% of bioglass; (d) 15% of anhydrous calcium dihydrogen phosphate; and (e) tantalum oxide 33% (f) polyethylene glycol 21%;
(2) sequentially putting the components in the step (1) into a glass container, mechanically mixing by using a stainless steel stirring rod, and fully blending for 5 min;
(3) and then transferring the mixed paste into a medical injector with an injection hose needle to obtain the premixed magnesium phosphate-based dental filling material with stable suspension.
FIG. 1 is a photograph of a sample obtained in example 2. The material keeps fluid under the sealing condition, is extruded and sampled to be placed in a constant temperature and humidity box with the temperature of 37 ℃ and the humidity of more than 95% (or is filled to the condition that teeth are contacted with physiological body fluid), is hydrated, solidified and hardened, and has the following solidification time: for 13 hours. FIG. 2 is a photomicrograph of the material obtained after water has been cured in example 2.
EXAMPLE 3 preparation of suspension-Stable premixed magnesium phosphate-based dental filling Material 3
(1) Weighing the following raw materials in percentage by weight: (a) 7% of dead burned magnesium oxide; (b) 7% of ammonium dihydrogen phosphate; (c) 20% of calcium dihydrogen phosphate; (d) 35% of bismuth trioxide and 31% of (e) glycerol.
(2) Sequentially putting the components in the step (1) into a glass container, mechanically mixing by using a stainless steel stirring rod, and fully blending for 5 min;
(3) and then transferring the mixed paste into a medical injector with an injection hose needle to obtain the premixed magnesium phosphate-based dental filling material with stable suspension.
The material keeps fluid under the sealing condition, is extruded and sampled to be placed in a constant temperature and humidity box with the temperature of 37 ℃ and the humidity of more than 95% (or is filled to the condition that teeth are contacted with physiological body fluid), is hydrated, solidified and hardened, and has the following solidification time: for 15 hours.
Claims (6)
1. A suspension-stable premixed magnesium phosphate-based dental filling material, characterized in that it comprises the following components: (a) magnesium oxide; (b) at least one phosphate compound; (c) a bioglass; (d) at least one radiation-blocking material; and (e) at least one water-miscible, non-aqueous solvent; the suspension-stable premixed magnesium phosphate-based dental filling material does not contain calcium silicate compounds;
in the premixed magnesium phosphate base dental filling material, the solid components (a), (b), (c) and (d) account for 40 to 92 percent of the total mass of the premixed magnesium phosphate base dental filling material, and the liquid component (e) accounts for 19 to 31 percent of the total mass of the premixed material with stable suspension;
wherein, in the solid components, the components (a) and (b) account for 34 to 44 percent of the total mass of the premixed magnesium phosphate-based dental filling material, and the mass ratio of the components (a) to (b) is as follows: (0.05-3): 1;
the component (c) accounts for 0 to 10 percent of the total mass of the premixed magnesium phosphate-based dental filling material;
the component (d) accounts for 33 to 37 percent of the total mass of the premixed magnesium phosphate-based dental filling material;
the sum of the mass percentages of the components is 100 percent;
wherein component (e) is selected from: at least one of glycerol, propylene glycol, ethylene glycol, polyethylene glycol, silicone oil, animal oil, and vegetable oil.
2. The suspension-stable premixed magnesium phosphate-based dental filling material according to claim 1, wherein component (b) is selected from the group consisting of: at least one of potassium dihydrogen phosphate, sodium dihydrogen phosphate, calcium dihydrogen phosphate, ammonium dihydrogen phosphate, and hydroxyapatite.
3. The suspension-stable premixed magnesium phosphate-based dental filling material according to claim 1, wherein component (c) is selected from the group consisting of: at least one of bioglass 45S, bioglass 58S, and bioglass 63S.
4. The suspension-stable premixed magnesium phosphate-based dental filling material according to claim 1, wherein component (d) is selected from the group consisting of: at least one of zirconium oxide, bismuth oxide and tantalum oxide.
5. The suspension-stable, premixed magnesium phosphate-based dental filling material according to claim 1, wherein the vegetable oil comprises clove oil.
6. Use of a premixed magnesium phosphate based dental filling material according to any of claims 1 to 5 for the preparation of a filling material for dental treatment.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711458900.0A CN108113893B (en) | 2017-12-28 | 2017-12-28 | Suspension-stable premixed magnesium phosphate-based dental filling material and preparation method and application thereof |
| PCT/CN2018/000215 WO2019127612A1 (en) | 2017-12-28 | 2018-06-06 | Stably suspended premixed magnesium- phosphate-based dental filling material, preparation method therefor and use thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711458900.0A CN108113893B (en) | 2017-12-28 | 2017-12-28 | Suspension-stable premixed magnesium phosphate-based dental filling material and preparation method and application thereof |
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| Publication Number | Publication Date |
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| CN108113893A CN108113893A (en) | 2018-06-05 |
| CN108113893B true CN108113893B (en) | 2020-02-14 |
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| CN201711458900.0A Active CN108113893B (en) | 2017-12-28 | 2017-12-28 | Suspension-stable premixed magnesium phosphate-based dental filling material and preparation method and application thereof |
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| WO (1) | WO2019127612A1 (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108113893B (en) * | 2017-12-28 | 2020-02-14 | 吴秉民 | Suspension-stable premixed magnesium phosphate-based dental filling material and preparation method and application thereof |
| CN111888521B (en) * | 2020-06-11 | 2021-12-17 | 上海禾麦医学科技有限公司 | Bone repair material and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1103283A (en) * | 1993-06-24 | 1995-06-07 | 丹茨普利股份有限公司 | Dental prosthesis |
| CN1691929A (en) * | 2002-10-24 | 2005-11-02 | 彭特恩临床科技有限公司 | Dental filling material |
| CN102807335A (en) * | 2012-07-13 | 2012-12-05 | 西安理工大学 | Method for synthesizing magnesium phosphate biological bone cement through self-covering controlled hydration reaction |
| CN107080697A (en) * | 2017-03-31 | 2017-08-22 | 烟台正海生物科技股份有限公司 | A kind of suspending stabilized premixing calcium silicates base canal filling material and preparation method and application |
| CN107411976A (en) * | 2017-03-31 | 2017-12-01 | 烟台正海生物科技股份有限公司 | Compound self-curing root canal filling material of the calcium silicates of a kind of premixing/magnesium phosphate two-phase and preparation method and application |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| ES2365091B1 (en) * | 2010-03-12 | 2013-01-24 | Universitat Politècnica De Catalunya | AN INORGANIC CEMENT FOR BIOMEDICAL APPLICATIONS, PROCEDURE FOR THE PREPARATION AND USE OF SUCH CEMENT. |
| CN108113893B (en) * | 2017-12-28 | 2020-02-14 | 吴秉民 | Suspension-stable premixed magnesium phosphate-based dental filling material and preparation method and application thereof |
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- 2017-12-28 CN CN201711458900.0A patent/CN108113893B/en active Active
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- 2018-06-06 WO PCT/CN2018/000215 patent/WO2019127612A1/en active Application Filing
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1103283A (en) * | 1993-06-24 | 1995-06-07 | 丹茨普利股份有限公司 | Dental prosthesis |
| CN1691929A (en) * | 2002-10-24 | 2005-11-02 | 彭特恩临床科技有限公司 | Dental filling material |
| CN102807335A (en) * | 2012-07-13 | 2012-12-05 | 西安理工大学 | Method for synthesizing magnesium phosphate biological bone cement through self-covering controlled hydration reaction |
| CN107080697A (en) * | 2017-03-31 | 2017-08-22 | 烟台正海生物科技股份有限公司 | A kind of suspending stabilized premixing calcium silicates base canal filling material and preparation method and application |
| CN107411976A (en) * | 2017-03-31 | 2017-12-01 | 烟台正海生物科技股份有限公司 | Compound self-curing root canal filling material of the calcium silicates of a kind of premixing/magnesium phosphate two-phase and preparation method and application |
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| Publication number | Publication date |
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| CN108113893A (en) | 2018-06-05 |
| WO2019127612A1 (en) | 2019-07-04 |
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Effective date of registration: 20200612 Address after: 101300 301, building 10, yard 12, Juyuan Middle Road, Mapo Town, Shunyi District, Beijing Patentee after: BEIJING SAIRUTE ORAL CAVITY MEDICAL INSTRUMENT Co.,Ltd. Address before: 300102 Tianjin Nankai District wide open four road style spring garden 25 Building 1 door 301. Patentee before: Wu Bingmin |