CN108113893A - Suspending stabilized premixing magnesium phosphate base dental filling material and its preparation method and application - Google Patents

Suspending stabilized premixing magnesium phosphate base dental filling material and its preparation method and application Download PDF

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Publication number
CN108113893A
CN108113893A CN201711458900.0A CN201711458900A CN108113893A CN 108113893 A CN108113893 A CN 108113893A CN 201711458900 A CN201711458900 A CN 201711458900A CN 108113893 A CN108113893 A CN 108113893A
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China
Prior art keywords
filling material
dental filling
magnesium phosphate
phosphate base
component
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CN201711458900.0A
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CN108113893B (en
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吴秉民
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BEIJING SAIRUTE ORAL CAVITY MEDICAL INSTRUMENT Co.,Ltd.
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吴秉民
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Priority to CN201711458900.0A priority Critical patent/CN108113893B/en
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Priority to PCT/CN2018/000215 priority patent/WO2019127612A1/en
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K6/00Preparations for dentistry
    • A61K6/80Preparations for artificial teeth, for filling teeth or for capping teeth
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K6/00Preparations for dentistry
    • A61K6/80Preparations for artificial teeth, for filling teeth or for capping teeth
    • A61K6/831Preparations for artificial teeth, for filling teeth or for capping teeth comprising non-metallic elements or compounds thereof, e.g. carbon
    • A61K6/836Glass
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K6/00Preparations for dentistry
    • A61K6/80Preparations for artificial teeth, for filling teeth or for capping teeth
    • A61K6/831Preparations for artificial teeth, for filling teeth or for capping teeth comprising non-metallic elements or compounds thereof, e.g. carbon
    • A61K6/838Phosphorus compounds, e.g. apatite

Abstract

The invention discloses a kind of suspending stabilized premixing magnesium phosphate base dental filling materials and its preparation method and application.The filler of the present invention penetrates material preparation as main phase, at least one and miscible Examples of non-aqueous solvents of water and at least one resistance using magnesia and at least one phosphate and goes out the dental filling material with excellent syringeability energy, wherein the packing material may also include at least one bio-vitric.The material keeps fluid under air-proof condition, is filled into after touching physiological fluid in tooth, aquation setting and hardening.The present invention is prepared into suspending stabilized premixing magnesium phosphate base dental filling material, can be used as filler for fields such as pulp capping, root canal therapy, dental prosthetic arts using the excellent biocompatibility of phosphoric acid mg-based material, bioactivity.

Description

Suspending stabilized premixing magnesium phosphate base dental filling material and preparation method thereof and Using
Technical field
It is more particularly to a kind of suspending stabilized pre- the present invention relates to a kind of dental filling material and its preparation method and application Mixed phosphate magnesium-based dental filling material and its preparation method and application.The invention belongs to medical material tech fields.
Background technology
Dental filling material has a wide range of applications on dental clinic.According to function, it can be divided into dental bonding and fill Filling chock material, dental prosthetic filler and the dental filling material to shield.The development experience of dental filling material Very long process, many materials such as zinc oxide eugenol, trbasic zinc phosphate, the sub- spit of fland compound resin of silver amalgam, glass water valve etc. are all It is used as dental filling material.Preferable dental filling material must have good biocompatibility, antibiotic property and clinical behaviour Make performance.In addition, bioactivity is as the foundation for weighing material and tooth body binding ability, therefore, biological cement or life Object glass material is also paid attention to be subject to more and more dentists and researcher.
It is at present three oxygen mineralizer material (Mineral using most calcium silicates class materials in dental filling material Trioxide Aggregate,MTA).Mahmoud Torabinejad were disclosed with MTA materials in 1998 first to dental cavity The method (United States Patent (USP), 5,769,638) repaired.The MTA materials main component is tricalcium silicate and dicalcium silicate and ripple Special orchid cement is similar, available in canal filling material, but allocates cumbersome, also results in waste.Chinese patent be " premixing Biological hydraulic cement paste composition and its application " (patent No. CN200880011743.1) discloses one kind and can be used for Tricalcium silicate, dicalcium silicate and organic solvent are pre-mixed by the premixed cement paste of medicine or dental use, the patent, side Doctor use, but setting time is long, could be solidified when some need 72 is small, and long setting time not only causes patient Stand-by period extends, and makes surgical procedure more complicated.Portland cement not phosphorus element-containing, it is impossible to hydroxyapatite is formed, It is not so good as phosphate with the biocompatibility of dentine.
Chinese patent " efficiently suspending stabilized calcium phosphate bone cement of injectable and preparation method and application " (patent No. CN200910197934.8 a kind of injectable calcium phosphate bone cement material system) is disclosed, the patent is by adding gas phase dioxy SiClx and its modified product improve the suspension stability of calcium phosphate bone cement premix system.It is disadvantageous in that calcium phosphate bone water Mud intensity deficiency, is easily broken.
Therefore, further research and development setting time is short, bioactivity is high, compression strength is enough, clinical manipulation performance is good Dental filling material has very important significance.
Magnesium phosphate cement (Magnesia-PhosphateCement, MPC) mainly by sintered magnesia, dihydric phosphate and Retarder is formulated by a certain percentage, has fast solidifying, high early strong characteristic.MPC is similar with calcium phosphate bone cement (CPC), energy Voluntarily cure under human physiological environment, hydrated product is phosphoric acid salt.Research for many years shows that MPC has good biofacies Capacitive is a kind of preferable bone impairment renovation material, but hydration reaction speed is too fast and hydration heat amount is very big since MPC has Two large problems cause it to be all not affected by the enough attention and research of people for a long time.Such as MPC under adiabatic conditions, highest water Change temperature and reach nearly 70 DEG C, these problems are not well solved always.Patent CN102807335A proposes a kind of utilization It is from the method for cladding control hydration reaction synthesis magnesium phosphate cement, i.e., anti-with a small amount of potassium dihydrogen phosphate in advance by mgo surface The setting time of magnesium phosphate cement from the 0.7--4 minutes before cladding are extended to the 6--17 minutes after cladding by the method answered, Exothermic temperature peak value is down to 32.6--38.3 degree by 55.1 to 70.5 degree, is provided with certain advantageous effect.The present invention is by magnesia Solid-phase components is waited to be pre-mixed with organic solvent, similarly solve the problems, such as that reaction speed is too fast this 2 caused, setting time reaches To 3-15 it is small when, exothermic temperature peak value is substantially consistent with environment temperature, has no rise.
The filler of the present invention is using magnesia and at least one phosphate as main phase, at least one miscible with water non- Aqueous phase solvent, at least one resistance penetrate material preparation and go out the dental filling material with excellent syringeability energy, wherein described fills out It fills material and may also include at least one bio-vitric.The material keeps fluid under air-proof condition, is filled into tooth and touches After physiological fluid, aquation setting and hardening.The present invention is using the excellent biocompatibility of phosphoric acid mg-based material, bioactivity, by it Suspending stabilized premixing magnesium phosphate base dental filling material is prepared into, filler can be used as pulp capping, root canal The fields such as art, dental prosthetic art.
The content of the invention
It is an object of the invention to provide a kind of setting time is short, bioactivity is high, the good premix of clinical manipulation performance Close magnesium phosphate base dental filling material.
In order to achieve the above object, present invention employs following technological means:
A kind of suspending stabilized premixing magnesium phosphate base dental filling material of the present invention, including following components:(a) aoxidize Magnesium;(b) at least one phosphate compounds;(c) a kind of bio-vitric;(d) material is penetrated at least one resistance;And (e) at least one The kind Examples of non-aqueous solvents miscible with water;
In the premixing magnesium phosphate base dental filling material, solid constituent (a), (b), (c) and (d) accounts for premixing The 40%-92% of magnesium phosphate base dental filling material gross mass, liquid component (e) account for suspending stabilized pre-mixed material gross mass 8%-60%;
Wherein, in solid constituent, component (a) and (b) account for premixing magnesium phosphate base dental filling material gross mass The mass ratio of 10%-89%, component (a) and (b) is:(0.05-3):1;
Component (c) accounts for the 0%-50% of premixing magnesium phosphate base dental filling material gross mass;
Component (d) accounts for the 10%-40% of premixing magnesium phosphate base dental filling material gross mass.
Wherein, it is preferred that component (b) is selected from:Potassium dihydrogen phosphate, sodium dihydrogen phosphate, ammonium dihydrogen phosphate, calcium dihydrogen phosphate, At least one of magnesium phosphate, hydroxyapatite.
Wherein, it is preferred that component (c) is selected from:In bio-vitric 45S, bio-vitric 58S and bio-vitric 63S extremely Few one kind.
Wherein, it is preferred that component (d) is selected from:At least one of zirconium oxide, bismuth oxide, tantalum oxide.
Wherein, it is preferred that component (e) is selected from:Glycerine, propylene glycol, ethylene glycol, polyethylene glycol, silicone oil, caryophyllus oil, animal At least one of oil, vegetable oil.
Further, the invention also provides the premixing magnesium phosphate base dental filling material is preparing odontotherapy Packing material in application.
Compared to the prior art, the advantage of the invention is that:
(1) compared to calcium-phosphate cement, premixing magnesium phosphate base dental filling material setting time of the invention is long, is convenient for Doctor's operation, reaction heating unobvious;
(2) compared to premixing calcium silicates dental filling material, premixing magnesium phosphate base dental filling material of the invention It has the following advantages:
(A) solidification is fast;
(B) phosphate ratio silicate good biocompatibility forms hydroxyapatite;
(C) compression strength is adjustable, by adjusting the ratio of magnesium phosphate and bio-vitric, meets different requirements;Such as it is adjusted to 30-40MA is used for root canal filling material, lower than calcium silicates paste intensity, may be advantageously employed in re-treatment;Such as adjust hard, Ke Yiyong In repairing,
Description of the drawings
Fig. 1 is the photo for the sample that embodiment 2 obtains.
The microphotograph of material after the hydraulic that Fig. 2 obtains for embodiment 2.
Specific embodiment
The invention will now be further described with reference to specific embodiments, the advantages and features of the present invention will be with description and It is apparent.But embodiment is only exemplary, does not form any restrictions to the scope of the present invention.Those skilled in the art should It should be appreciated that the details and form of technical solution of the present invention can be repaiied without departing from the spirit and scope of the invention Change or replace, but these modifications and replacement are each fallen in protection scope of the present invention.
The preparation 1 of the suspending stabilized premixing magnesium phosphate base dental filling material of embodiment 1
(1) each raw material is weighed according to following weight percent:(a) dead burned magnesia 21%;(b) potassium dihydrogen phosphate 23%; (c) zirconium oxide 37% and (d) polyethylene glycol 19%;
(2) component of step (1) is sequentially placed into glass container, carries out mechanical mixture with stainless steel stirring rod, fully Reconciliation 5min;
(3) mixing paste is transferred in the injector for medical purpose equipped with injection hose syringe needle after, you can obtain suspending steady Fixed premixing magnesium phosphate base dental filling material.
The material keeps fluid under air-proof condition, squeezes out sample preparation and is placed on 37 DEG C, in more than 95% humidity climatic chamber (or being filled into teeth contact to physiological fluid), aquation setting and hardening, aquation setting and hardening, setting time:5 it is small when.
The preparation 2 of the suspending stabilized premixing magnesium phosphate base dental filling material of embodiment 2
(1) each raw material is weighed according to following weight percent:(a) light calcined magnesia 9%;(b) sodium dihydrogen phosphate 12%; (c) bio-vitric 63S 10%;(d) anhydrous dihydro calcium phosphate 15%;And (e) tantalum oxide 33% (f) polyethylene glycol 21%;
(2) component of step (1) is sequentially placed into glass container, carries out mechanical mixture with stainless steel stirring rod, fully Reconciliation 5min;
(3) mixing paste is transferred in the injector for medical purpose equipped with injection hose syringe needle after, you can obtain suspending steady Fixed premixing magnesium phosphate base dental filling material.
Fig. 1 is the photo for the sample that the present embodiment 2 obtains.The material keeps fluid under air-proof condition, squeezes out sample preparation and puts In 37 DEG C, more than 95% humidity climatic chamber (or being filled into teeth contact to physiological fluid), aquation setting and hardening, solidification Time:13 it is small when.Fig. 2 is the microphotograph that the present embodiment 2 obtains the material after hydraulic.
The preparation 3 of the suspending stabilized premixing magnesium phosphate base dental filling material of embodiment 3
(1) each raw material is weighed according to following weight percent:(a) dead burned magnesia 7%;(b) ammonium di-hydrogen phosphate 7%;(c) Calcium dihydrogen phosphate 20%;(d) bismuth oxide 35% and (e) glycerine 31%.
(2) component of step (1) is sequentially placed into glass container, carries out mechanical mixture with stainless steel stirring rod, fully Reconciliation 5min;
(3) mixing paste is transferred in the injector for medical purpose equipped with injection hose syringe needle after, you can obtain suspending steady Fixed premixing magnesium phosphate base dental filling material.
The material keeps fluid under air-proof condition, squeezes out sample preparation and is placed on 37 DEG C, in more than 95% humidity climatic chamber (or being filled into teeth contact to physiological fluid), aquation setting and hardening, setting time:15 it is small when.

Claims (6)

  1. A kind of 1. suspending stabilized premixing magnesium phosphate base dental filling material, which is characterized in that the dental filling material Including following components:(a) magnesia;(b) at least one phosphate compounds;(c) a kind of bio-vitric;(d) at least one resistance Penetrate material;And (e) is at least one with the miscible Examples of non-aqueous solvents of water;
    In the premixing magnesium phosphate base dental filling material, solid constituent (a), (b), (c) and (d) accounts for premixing phosphoric acid The 40%-92% of magnesium-based dental filling material gross mass, liquid component (e) account for suspending stabilized pre-mixed material gross mass 8%-60%;
    Wherein, in solid constituent, component (a) and (b) account for the 10%- for being pre-mixed magnesium phosphate base dental filling material gross mass 89%, the mass ratio of component (a) and (b) is:(0.05-3):1;
    Component (c) accounts for the 0%-50% of premixing magnesium phosphate base dental filling material gross mass;
    Component (d) accounts for the 10%-40% of premixing magnesium phosphate base dental filling material gross mass.
  2. 2. suspending stabilized premixing magnesium phosphate base dental filling material as described in claim 1, which is characterized in that component (b) it is selected from:At least one of potassium dihydrogen phosphate, sodium dihydrogen phosphate, calcium dihydrogen phosphate, ammonium dihydrogen phosphate, hydroxyapatite.
  3. 3. suspending stabilized premixing magnesium phosphate base dental filling material as described in claim 1, which is characterized in that component (c) it is selected from:At least one of bio-vitric 45S, bio-vitric 58S and bio-vitric 63S.
  4. 4. suspending stabilized premixing magnesium phosphate base dental filling material as described in claim 1, which is characterized in that component (d) it is selected from:At least one of zirconium oxide, bismuth oxide, tantalum oxide.
  5. 5. suspending stabilized premixing magnesium phosphate base dental filling material as described in claim 1, which is characterized in that component (e) it is selected from:At least one of glycerine, propylene glycol, ethylene glycol, polyethylene glycol, silicone oil, caryophyllus oil, animal oil, vegetable oil.
  6. 6. claim 1-5 any one of them is pre-mixed magnesium phosphate base dental filling material and is preparing the filling material of odontotherapy Application in material.
CN201711458900.0A 2017-12-28 2017-12-28 Suspension-stable premixed magnesium phosphate-based dental filling material and preparation method and application thereof Active CN108113893B (en)

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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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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2019127612A1 (en) * 2017-12-28 2019-07-04 吴秉民 Stably suspended premixed magnesium- phosphate-based dental filling material, preparation method therefor and use thereof
CN111888521A (en) * 2020-06-11 2020-11-06 上海蕴邦生物科技有限公司 Bone repair material and preparation method thereof

Citations (6)

* Cited by examiner, † Cited by third party
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
US20130156864A1 (en) * 2010-03-12 2013-06-20 Universitat Politecnica De Catalunya Inorganic Cement for Biomedical uses, Preparation Method Thereof and Use of Same
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 (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Patent Citations (6)

* Cited by examiner, † Cited by third party
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
US20130156864A1 (en) * 2010-03-12 2013-06-20 Universitat Politecnica De Catalunya Inorganic Cement for Biomedical uses, Preparation Method Thereof and Use of Same
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

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2019127612A1 (en) * 2017-12-28 2019-07-04 吴秉民 Stably suspended premixed magnesium- phosphate-based dental filling material, preparation method therefor and use thereof
CN111888521A (en) * 2020-06-11 2020-11-06 上海蕴邦生物科技有限公司 Bone repair material and preparation method thereof

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CN108113893B (en) 2020-02-14

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Effective date of registration: 20200612

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Patentee before: Wu Bingmin