CN103142418A - Calcium phosphate composite material for filling root canal and preparation method thereof - Google Patents

Calcium phosphate composite material for filling root canal and preparation method thereof Download PDF

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CN103142418A
CN103142418A CN2013100646141A CN201310064614A CN103142418A CN 103142418 A CN103142418 A CN 103142418A CN 2013100646141 A CN2013100646141 A CN 2013100646141A CN 201310064614 A CN201310064614 A CN 201310064614A CN 103142418 A CN103142418 A CN 103142418A
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composite material
root canal
calcium phosphate
phosphate
phase component
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CN103142418B (en
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戴红莲
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XIAMEN BAIMEITE BIOLOGICAL MATERIALS SCIENCE AND TECHNOLOGY CO.,LTD.
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WUHAN BAIMEITE BIOLOGICAL MATERIAL TECHNOLOGY Co Ltd
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Abstract

The invention provides a calcium phosphate composite material for filling a root canal. The composite material consists of a solid-phase component and a liquid-phase component, wherein the solid-phase component is a mixture of calcium phosphate, magnesium oxide, soluble hydrophosphate and iodoform; and the liquid-phase component is an aqueous solution of sugar, hydrophosphate and citric acid. The invention also provides a method for preparing the composite material. In the composite material, the injection property and collapse resistance of the composite material can be improved by the gelation of the sugar in the liquid-phase component and the chelation of inorganic ions in the solid-phase component, the magnesium phosphate generated by a hydration reaction has relatively strong adhesive force, the bonding strength between the root filling material and the root canal wall can be promoted, and leakage is avoided; and the iodoform can be used for enhancing the X-ray opacity and diminish inflammation to improve the curative effect of root canal therapy.

Description

Root canal is filled with calcium phosphate magnesium base composite material and preparation method thereof
[technical field]
The present invention relates to bio-medical packing material field, relate in particular to a kind of root canal and fill with calcium phosphate magnesium base composite material and the method for preparing this composite.
[background technology]
Root canal is the most basic, the effective method for the treatment of at present dental pulp disease and periapical disease, and the treatment success or failure depend primarily on root canal filling material.
At present root canal filling material used mainly can be divided into solid, paste and liquid three class root canal filling materials according to form clinically.
The solid kind root canal filling material (as sharp in gutta percha point, Ti-Ni alloy point, silver point, plastics etc.) no adhesion, can not bond with root pipe inner structure, can not enter crooked root tube and collateral canal, can't form tight sealing, gutta percha point must coordinate oxpara to use.
Volume contraction can occur in paste root canal filling material (as pastes such as zinc oxide clove oil, calcium hydroxide, iodoform, resinae, glass ionomer classes) in solidification process, and be dissolved in water or tissue fluid, and there is micro gap to cause little seepage between root canal wall, can not seals apical foramen of tooth fully.Play certain improvement effect though paste uses together with gutta percha point, be difficult to tackle the problem at its root, and the clinical manipulation time is long.
Liquid root canal filling material (as FR phenolic resins) easily infiltrates dentinal tubule and causes tooth discoloration, affect attractive in appearance, during polymerization to organizing irritant and cytotoxicity.
Although oneself becomes the most frequently used clinically canal filling method to gutta percha point in conjunction with the paste root canal filling material, but biocompatibility is poor, if accidentally exceed outside the tip of a root, forming long-term foreign body stimulates, wherein some material has stimulation and corrosivity to tissue, even causes the hypoplasia of succession permanent teeth etc.
Calcium phosphate bone cement (Calcium Phosphate Cement, CPC) is to be sent out with the liquid phase generation aquation of mediation use by the mixture of one or more synthos powder to answer, and can obtain the cured product close with body bone tissue by self-curing under physiological condition.Calcium phosphate bone cement because of good biocompatibility, sufficiently high linear comprcssive strength, can become a kind of biological activity packing material that has according to the defect random-shaping.
Develop self-curable calcium phosphate paste (TTCP/DCPA) on bibliographical information CPC basis and be used for the filling of root pipe, this material is as tip of a root barrier, the permission mesenchymal tissue is grown into, promote sclerous tissues's deposition, the sealing apical foramen of tooth, can not cause when material exceeds the tip of a root that root fills reaction, the material that exceeds can also play the effect of inducting osseous tissue regeneration.But this material cured time of clinical discovery is long, anti-collapsibility is poor, runs into blood rare faling apart easily occurs, and injection property is undesirable, and forms fine and close HAP after solidifying, and vivo degradation is not slowly even degraded, and new bone is difficult to grow into.In addition, very difficult during this material injection material, root canal morphology is irregular, and particularly flat when pipe can't guarantee that material arrives the tip of a root, easily causes charge less, and this has limited its clinical practice to a certain extent.For the damaged property of the apex of root of tooth surrounding bone cavity that is caused by many dental disorders, for example fistula type apex of root of tooth week cavity, the TTCP/DCPA packing material is faced with in apex of root of tooth week fill area the poor or difficult problem of skeletonization not for a long time of osteogenic.
[summary of the invention]
In view of this, the technical issues that need to address of the present invention are to provide a kind of calcium phosphate magnesium base composite material of root canal filling with good biocompatibility and anti-collapsibility.
A kind of root canal filling calcium phosphate magnesium base composite material, described composite is comprised of solid phase components and liquid phase component.Described solid phase components is by the mixture of synthos, magnesium oxide, soluble phosphoric acid hydrogen salt and iodoform, and described liquid phase component is by sugar, hydrophosphate and Fructus Citri Limoniae aqueous acid.
Preferably, in described solid phase components, the mass percent of synthos is 70 ~ 90%, and magnesian mass percent is 1 ~ 20%, and the mass percent of hydrophosphate is 0~20%, and the mass percent of iodoform is 5 ~ 15%.
Preferably, in described liquid phase component, the concentration of citric acid is 0.1 ~ 1.0 mol/L, and the mass percent concentration of hydrophosphate is 1 ~ 20%, and the mass percent concentration of sugar is 1 ~ 20%.
Preferably, described solid phase components in synthos be following one or more mixture: (α, β)-tricalcium phosphate, tetracalcium phosphate, OCP, calcium phosphate dibasic anhydrous, dicalcium phosphate dehydrate, dalcium biphosphate, calcium pyrophosphate, hydroxyapatite, fluor-apatite, saamite, contain carbonic acid apatite.
Preferably, the soluble phosphoric acid hydrogen salt in described solid phase components is following one or more mixture: sodium dihydrogen phosphate, sodium hydrogen phosphate, potassium dihydrogen phosphate, dipotassium hydrogen phosphate.
Preferably, the sugar in described liquid phase component is following one or more mixture: polysaccharide, sugar derivatives, glucose, sucrose, dextrin, cellulose, chitosan, fructose, lactose, amino sugar, aminoglucose polysaccharide, glycolipid.
Preferably, the magnesium oxide in described solid phase components adopts by the magnesium oxide after 1300 ~ 1600 ℃ of heat treatments.
Preferably, the hydrophosphate in described liquid phase component is following one or more mixture: sodium dihydrogen phosphate, sodium hydrogen phosphate, potassium dihydrogen phosphate, dipotassium hydrogen phosphate.
In view of this, the present invention also provides a kind of method that above-mentioned root canal filling is used the calcium phosphate magnesium base composite material for preparing.
A kind of root canal filling comprises the following steps: the various raw materials in described solid phase components are made particle diameter less than the powder of 20 μ m with the preparation method of calcium phosphate magnesium base composite material; With described solid phase components and described liquid phase component with liquid phase component: the ratio mix homogeneously of solid phase components=(0.1 ~ 1) ml:1mg is in harmonious proportion and forms slurry.
root canal filling provided by the present invention calcium phosphate magnesium base composite material, the gelatification of the sugar in liquid phase component and can improve syringeability and the anti-collapsibility of calcium phosphate magnesium base composite material with the chelation of inorganic ions in solid phase components, the magnesium phosphate that in the root pipe, the generation hydration reaction produces has stronger bonding force, can promote the adhesion strength of root canal filling material and root canal wall, avoid producing seepage, iodoform not only can make the x-ray opacity strengthen but also can antiinflammatory improve the curative effect of root canal, root canal filling of the present invention can disposable injection molding process with the calcium phosphate magnesium base composite material and is infiltrated in root canal dentinal tubules, combine closely with root canal wall, simplify root and fill operation, improve curative effect, Shorten the Treatment Process.
[description of drawings]
Fig. 1 is the X ray diffracting spectrum after calcium phosphate magnesium base composite material hydration reaction 24h of the present invention.
Fig. 2 is the X ray diffracting spectrum of calcium phosphate magnesium base composite material hydration reaction 24h after-hardening body of the present invention.
Fig. 3 is calcium phosphate magnesium base composite material of the present invention (left side) and the tissue slice comparison diagram of calcium hydroxide paste (right side) difference filling dog root canal after 20 weeks.
Fig. 4 is calcium phosphate magnesium base composite material of the present invention (left side) and calcium hydroxide paste (right side) the apical foramen of tooth section scanning electron microscope comparison diagram of filling dog root canal after 20 weeks respectively.
Fig. 5 is that calcium phosphate magnesium base composite material of the present invention (left side) is right with Vitapex() the tissue slice comparison diagram of difference filling rabbit periapical bone after damaged 6 months.
Fig. 6 is the x line sheet comparison diagram of four different angles after calcium phosphate magnesium base composite material filling dental root canal of the present invention.
Fig. 7 is the x line sheet comparison diagram of calcium phosphate magnesium base composite material filling periapical bone of the present invention damaged rear 4 months (left side) and 6 months (right side).
[specific embodiment]
In order to understand better the present invention, below with reference to accompanying drawing, embodiments of the invention are described in detail.
Can not form chemical bond with dentin wall for solving the root canal filling material that uses clinically at present, be difficult to guarantee good sealing, the biocompatibility of root of the tooth end poor, super fill form that long-term foreign body stimulates and apex of root of tooth week fill area in the poor or problem such as skeletonization not for a long time of osteogenic, the applicant carries out a large amount of experiment screenings, finally obtain producing solid phase components by synthos, magnesium oxide, soluble phosphoric acid hydrogen salt and iodoform, by sugar, hydrophosphate, the citric acid compatibility program that makes liquid phase component soluble in water.Synthos in solid phase components, hydrophosphate are under the effect of water, the hydration and sclerosis reaction occurs form the hydrated products such as hydroxyapatite, magnesium oxide and hydrophosphate generation hydration reaction form the adhesive property that magnesium phosphate improves material, and the iodoform in solid phase plays the effect of resistance X-ray and antiinflammatory.Sugar in liquid phase can make the hydrated product hydroxyapatite crystal be controlled by the organic frame of micromolecule base and realize self assembly, citric acid can with solid phase in Leaching Properties of Soluble Phosphorus acid calcium salt reaction form calcium citrate, the hardening time of controlled material, the size of constraint HAP crystal, thus improve the material ossification.
In described solid phase components, the mass percent of synthos is 70 ~ 90%, and magnesian mass percent is 1 ~ 20%, and the mass percent of soluble phosphoric acid hydrogen salt is 0~20%, and the mass percent of iodoform is 5 ~ 15%.In described liquid phase component, the concentration 0.1 ~ 1.0mol/L of citric acid, the mass percent concentration of hydrophosphate are 1 ~ 20%, and the mass percent concentration of sugar is 1 ~ 20%.
In solid phase components, synthos can select (α, β)-tricalcium phosphate, tetracalcium phosphate, OCP, calcium phosphate dibasic anhydrous, dicalcium phosphate dehydrate, dalcium biphosphate, calcium pyrophosphate, hydroxyapatite, fluor-apatite, saamite, contain one or more in carbonic acid apatite; Magnesium oxide is by 1300 ~ 1600 ℃ of heat treatments, and calcined magnesia can improve magnesian reactivity, hydration rate, setting time when regulating material aquation curing reaction; The soluble phosphoric acid hydrogen salt can be selected one or more in sodium dihydrogen phosphate, sodium hydrogen phosphate, potassium dihydrogen phosphate, dipotassium hydrogen phosphate.
In liquid phase component, sugar is one or more in polysaccharide, sugar derivatives, glucose, sucrose, dextrin, cellulose, chitosan, fructose, lactose, amino sugar, aminoglucose polysaccharide, glycolipid; Hydrophosphate is one or more in sodium dihydrogen phosphate, sodium hydrogen phosphate, potassium dihydrogen phosphate, dipotassium hydrogen phosphate, and it plays the pH value of regulator solution phase component and the effect of hydration and sclerosis response speed.
Hydration reaction occurs in calcium phosphate magnesium base composite material of the present invention in the root pipe, the magnesium phosphate that produces has stronger bonding force, can promote the adhesion strength of root canal filling material and root canal wall, avoids producing seepage.Contain iodoform in solid phase components, the x-ray opacity is strengthened, can antiinflammatory improve the curative effect of root canal again.In addition, change formed lemon acid calcium in course of reaction, not only have conclusive effect on the size that limits phosphorite crystal and stable phosphorite crystal, can also promote new bone formation, can realize bony union.Therefore, calcium phosphate magnesium base composite material of the present invention is inserted root Guan Houchao and is filled and not only can not produce root and fill reaction, can induce the periapical osteanagenesis on the contrary, promotes the reparation of periapical lesion, seals apical foramen of tooth fully.
On preparation technology, raw material granularity and the proportioning optimized have been found, various raw materials in solid phase components are made particle diameter less than the powder of 20 μ m, with liquid phase component with liquid phase component: be in harmonious proportion after the ratio mix homogeneously of solid phase components=(0.1 ~ 1) ml:1mg and form slurry, can make the root canal filling that meets expectation calcium phosphate magnesium base composite material.X ray diffracting spectrum after calcium phosphate magnesium base composite material hydration reaction 24h of the present invention as shown in fig. 1, abscissa is the angle of diffraction 2 θ, ★ is KMgPO 46H 2The diffraction maximum of O; ● be Mg 3(PO 4) 2The X diffraction maximum; ▲ be Ca 3(PO 4) 2The X diffraction maximum; △ is KH 2PO 4The X diffraction maximum; ◇ is the characteristic peak of MgO.The X ray diffracting spectrum of calcium phosphate magnesium base composite material hydration reaction 24h after-hardening body of the present invention as shown in Figure 2.Because root canal filling of the present invention is excessive with raw material granularity and the proportioning test amount of calcium phosphate magnesium base composite material, give unnecessary details in this inconvenience.
The material safety experiment:
Calcium phosphate magnesium material of the present invention is carried out acute toxicity test, sub-acute toxicity test, muscular irritation test, hemolytic test and thrombotest to be detected.Testing result shows, calcium phosphate magnesium material of the present invention is without acute, toxic reaction, and is non-stimulated to muscle, and unlikely haemolysis, blood coagulation do not cause inflammation and rejection, have good biocompatibility.
The experiment of material effectiveness:
(1) the closed experiment of root pipe: the employing Canis familiaris L. is animal model, and the people is for causing butt to open and the periapical tissue wound.Take calcium phosphate magnesium base composite material of the present invention as experimental group, with the Ca (OH) that uses clinically 2Paste, HA paste are matched group.Each is organized material furnishing paste in proportion, carry out root-canal filling, then rebasing with zinc phosphate cement.After root fills, clap x-ray tooth sheet, check respectively the root-canal filling situation in 4,12,20 weeks.Root filled for 20 weeks, adopt the calcium phosphate magnesium base composite material group root pipe tip of a root of the present invention to be closed fully, the similar cellular cementum of calcified tissue (as shown in Fig. 3 is left), connective tissue disappears, periodontal membrane recovers normal thickness, arrange in order, connect calcification barrier and the new lamina dura that forms, inflammatory reaction disappears.Ca (OH) 2The group apical foramen of tooth is cellular cementum deposition, and periapical abscess forms, and the tip of a root does not seal (as shown in Fig. 3 is right).The scanning electron microscope result shows that calcium phosphate magnesium material group apical foramen of tooth is sealed (as shown in Fig. 4 is left), Ca (OH) fully by sclerous tissues 2Group is partially enclosed (as shown in Fig. 4 is right).Calcium phosphate magnesium of the present invention meets the bootable periapical osteanagenesis of material, seals apical foramen of tooth fully.
(2) periapical bone defective region reparative experiment: adopt new zealand white rabbit to set up the damaged animal model of periapical bone, take calcium phosphate magnesium base composite material of the present invention as experimental group, the Vitapex material is the matched group bone defective region that filling is organized separately as the bone filler.Clap x-ray tooth sheet, histological observation in 2,4, observe respectively bone defect repair situation June.Postoperative 6 months, experimental group bony defect district is replaced by the normal bone tissues structure, reaches bony union (as shown in Fig. 5 is left).The subregion of matched group bone defective region is by Bone Void Filler, but still has more fibrous connective tissue composition, and the implantation region fibrous tissue is netted (as shown in Fig. 5 is right).Calcium phosphate magnesium base composite material of the present invention can be degraded gradually and be substituted by new bone, and the regeneration of degradation speed and bone is complementary.
The concrete using method of calcium phosphate magnesium base composite material of the present invention is as follows: when being used for root canal filling, with syringe, the solid-liquid two mixed slurries of component material being injected the root pipe and carries out filling, and then rebasing with zinc phosphate cement; When damaged for the periapical bone, with the solid-liquid two direct fillings of the mixed slurry of component material or damaged with syringe injection bone, tightly sew up the mucoperiosteum lobe.Below the preparation process of calcium phosphate magnesium base composite material of the present invention will be described with several specific embodiments.
Embodiment 1:
Take 5.0g type alpha tricalcium phosphate, 2.0g tetracalcium phosphate, 1.0g magnesium oxide, 1.5g potassium dihydrogen phosphate, 0.5g iodoform, particle diameter evenly is mixed into solid phase powder less than 20 μ m.Take 2.0g sodium dihydrogen phosphate, 0.5g sucrose, 0.5g glucose and fully be dissolved in the citric acid solution of 10 milliliters of 0.5mol/L, make the consolidation liquid of liquid phase.With liquid-solid ratio 0.3ml:1mg, consolidation liquid is poured in solid phase powder, be in harmonious proportion evenly in syringe, obtain packing material.
Embodiment 2:
Take 6.0g type alpha tricalcium phosphate, 1.5g magnesium oxide, 1.5g potassium dihydrogen phosphate, 1.0g iodoform, particle diameter evenly is mixed into solid phase powder less than 20 μ m.Take 1.0g sodium hydrogen phosphate, 1.0g sodium dihydrogen phosphate, 0.8g glucose and fully be dissolved in the citric acid solution of 10 milliliters of 0.6mol/L, make the consolidation liquid of liquid phase.With liquid-solid ratio 0.4ml:1mg, consolidation liquid is poured in solid phase powder, be in harmonious proportion evenly in vessel, obtain packing material.Embodiment 3:
Take 8.0g type alpha tricalcium phosphate, 1.0g magnesium oxide, 1.0g iodoform, particle diameter evenly is mixed into solid phase powder less than 20 μ m.Take the 2g potassium dihydrogen phosphate, the 1.0g dextrin fully is dissolved in the citric acid solution of 10 milliliters of 1.0mol/L, makes the consolidation liquid of liquid phase.With liquid-solid ratio 0.5ml:1mg, consolidation liquid is poured in solid phase powder, be in harmonious proportion evenly in vessel, obtain packing material.
Embodiment 4:
Take 6.5g type alpha tricalcium phosphate, 2.0g tetracalcium phosphate, 0.1g magnesium oxide, 1.4g iodoform, particle diameter evenly is mixed into solid phase powder less than 20 μ m.Take 1.0g sodium dihydrogen phosphate, 1.0g dipotassium hydrogen phosphate, 0.5g cellulose and fully be dissolved in the citric acid solution of 10 milliliters of 0.1mol/L, make consolidation liquid.With liquid-solid ratio 0.6(ml/mg) consolidation liquid is poured in solid phase powder, be in harmonious proportion evenly in syringe, obtain packing material.
Embodiment 5:
Take 6.0g tetracalcium phosphate, 2.0g calcium hydrogen phosphate, 1.0g magnesium oxide, 1.0 g iodoform, particle diameter evenly is mixed into solid phase powder less than 20 μ m.Take the 1.6g sodium hydrogen phosphate, the 0.5g chitosan fully is dissolved in the citric acid solution of 10 milliliters of 0.2mol/L, makes consolidation liquid.With liquid-solid ratio 0.8ml:1mg, consolidation liquid is poured in solid phase powder, be in harmonious proportion evenly in vessel, obtain packing material.
Embodiment 6:
Take 5.5g tetracalcium phosphate, 2.0g calcium hydrogen phosphate, 1.5g magnesium oxide, 1.0 g iodoform, particle diameter evenly is mixed into solid phase powder less than 20 μ m.Take the 1.6g sodium dihydrogen phosphate, 0.6g sucrose fully is dissolved in the citric acid solution of 10 milliliters of 0.5mol/L, makes consolidation liquid.With liquid-solid ratio 0.6ml:1mg, consolidation liquid is poured in solid phase powder, be in harmonious proportion evenly in vessel, obtain packing material.
Clinical application effect:
Calcium phosphate magnesium base composite material mediation slurry of the present invention is injected in the root pipe, to suffer from patient's 188 examples between 8~65 years old of dental pulp and periapical disease age, totally 218 teeth have carried out root canal filling, before art, postoperative does 12 months regular follow-ups to 3 years of x-ray tooth sheet.Wherein, adult 181 people, child 7 people; Male 115 people (140), women 73 people (78).82 of labial teeths, 76 of bicuspids are ground one's teeth in sleep 60.Follow-up results shows, filler has no any change in volume in the root pipe, do not find root pipe cavitation, the tooth invariant color, the root-canal filling effect is produce effects, fills the tip of a root also without postoperative pain even surpass, but has played the effect of inducing periapical tissue regeneration, promote the reparation of periapical lesion, formed bone-cemental sealing biology at tip of a root end.
Calcium phosphate magnesium base composite material mediation slurry of the present invention is implemented filling treatment to the 66 damaged patients of routine periapical periodontitiss companion's bone, all patients are carried out the tracing study of one week of postoperative, half a year, 1 year.Wherein, male's 42 examples, women's 24 examples, age 23-64 year; Radicular cyst 8 examples, apical granuloma 58 examples.The all patient's wounds of postoperative one place mild hyperaemia edema, fistula heals substantially, and tooth is suffered from percussion slight discomfort, and part is suffered from odontoseisis I °-II °.Postoperative wound healing half a year is good, and fistula recovery from illness, percussion are suffered from tooth without sense of discomfort, non-loosening, and the bone defective region has new bone formation, the degraded of part filler.Postoperative 1 year, the filler degraded of bone defective region is replaced by freshman bone tissue, reaches bony union.
Calcium phosphate magnesium base composite material of the present invention can disposable injection molding process and is infiltrated into root canal dentinal tubules, combines closely with root canal wall, and super filling can be induced the periapical osteanagenesis, can reach bony union, seal apical foramen of tooth fully.Say in further detail, root canal filling of the present invention has the following advantages with the calcium phosphate magnesium base composite material:
At first, the gelatification of the sugar in liquid phase component and can improve syringeability and the anti-collapsibility of calcium phosphate magnesium base composite material with the chelation of inorganic ions in solid phase components, but one-time filling also infiltrates in root canal dentinal tubules, combine closely with root canal wall, simplify root and fill operation, root fills the operating time and significantly lowers, and improves curative effect, Shorten the Treatment Process.Even irregular pipe of form, crooked root tube, branched root Guan Yike filling can avoid the situation of charge less to occur.
Secondly, the calcium phosphate magnesium base composite material of the present invention magnesium phosphate that hydration reaction produces in the root pipe has stronger bonding force, can promote the adhesion strength of root canal filling material and root canal wall, avoids producing seepage; Contain iodoform in root canal filling material, but both the x-ray opacity strengthened, and can antiinflammatory improve curative effect again.
Again, the lemon acid calcium that calcium phosphate magnesium base composite material of the present invention forms in the hydration reaction process in the root pipe, when containing the apatite composition in the solid phase composition, lemon acid calcium has conclusive effect on the size that limits phosphorite crystal and stable phosphorite crystal, and can promote new bone formation, can realize bony union.Therefore, insert root Guan Houchao and fill and not only can not produce root and fill reaction, can induce the periapical osteanagenesis on the contrary, promote the reparation of periapical lesion, seal apical foramen of tooth fully.
Generally speaking, calcium phosphate magnesium base composite material of the present invention is made root canal and is filled, need not to do root resection, can keep the effective length of root of the tooth and increase its steadiness, be not only applicable to dental pulp disease, point week is sick, periodontal pocket communicates with sharp all pathological changes sharp Zhou Yinying, to root of the tooth not zoon present the flaring tip of a root, being bell-mouthed permanent teeth patient and periapical tissue at the treatment apical foramen of tooth especially, to destroy the patient more effective, its effect is better than existing other type root-canal filling product.
The above embodiment has only expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to the scope of the claims of the present invention.Should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.

Claims (9)

1. root canal filling calcium phosphate magnesium base composite material, described composite is comprised of solid phase components and liquid phase component, it is characterized in that: described solid phase components is by the mixture of synthos, magnesium oxide, soluble phosphoric acid hydrogen salt and iodoform, and described liquid phase component is by sugar, hydrophosphate and Fructus Citri Limoniae aqueous acid.
2. root canal filling according to claim 1 calcium phosphate magnesium base composite material, it is characterized in that: in described solid phase components, the mass percent of synthos is 70 ~ 90%, magnesian mass percent is 1 ~ 20%, the mass percent of soluble phosphoric acid hydrogen salt is 0~20%, and the mass percent of iodoform is 5 ~ 15%.
3. root canal filling according to claim 2 calcium phosphate magnesium base composite material, it is characterized in that: in described liquid phase component, the concentration of citric acid is 0.1 ~ 1.0mol/L, and the mass percent concentration of hydrophosphate is 1 ~ 20%, and the mass percent concentration of sugar is 1 ~ 20%.
4. root canal filling according to claim 1 calcium phosphate magnesium base composite material, it is characterized in that described solid phase components in synthos be following one or more mixture: (α, β)-tricalcium phosphate, tetracalcium phosphate, OCP, calcium phosphate dibasic anhydrous, dicalcium phosphate dehydrate, dalcium biphosphate, calcium pyrophosphate, hydroxyapatite, fluor-apatite, saamite, contain carbonic acid apatite.
5. root canal filling according to claim 1 calcium phosphate magnesium base composite material is characterized in that soluble phosphoric acid hydrogen salt in described solid phase components is following one or more mixture: sodium dihydrogen phosphate, sodium hydrogen phosphate, potassium dihydrogen phosphate, dipotassium hydrogen phosphate.
6. root canal filling according to claim 1 calcium phosphate magnesium base composite material is characterized in that sugar in described liquid phase component is following one or more mixture: sugar derivatives, glucose, sucrose, dextrin, cellulose, chitosan, fructose, lactose, amino sugar, aminoglucose polysaccharide, glycolipid.
7. root canal filling according to claim 1 calcium phosphate magnesium base composite material is characterized in that: the magnesium oxide in described solid phase components adopts by the magnesium oxide after 1300 ~ 1600 ℃ of heat treatments.
8. root canal filling according to claim 1 calcium phosphate magnesium base composite material is characterized in that hydrophosphate in described liquid phase component is following one or more mixture: sodium dihydrogen phosphate, sodium hydrogen phosphate, potassium dihydrogen phosphate, dipotassium hydrogen phosphate.
9. one kind prepares the described root canal filling of any one according to claim 1 to 8 with the method for calcium phosphate magnesium base composite material, it is characterized in that said method comprising the steps of:
Various raw materials in described solid phase components are made particle diameter less than the powder of 20 μ m;
With described solid phase components and described liquid phase component with liquid phase component: the weight ratio mix homogeneously of solid phase components=(0.1 ~ 1) ml:1mg is in harmonious proportion and forms slurry.
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CN108635624A (en) * 2018-04-25 2018-10-12 武汉理工大学 A kind of phosphoric acid magnesium-based bone cement of anti-collapsibility type injectable
CN110934750A (en) * 2019-12-27 2020-03-31 广州润虹医药科技股份有限公司 Root canal filler for treating pulpitis or periapicalitis and preparation method thereof
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CN113082296A (en) * 2021-04-26 2021-07-09 东南大学 Calcium phosphate bone cement with good injectability and preparation method thereof
CN115137653A (en) * 2018-03-30 2022-10-04 徐崇明 Filling paste for dental pulp conservation treatment and preparation method thereof

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CN105903063B (en) * 2016-05-16 2020-04-21 武汉理工大学 Magnesium-based medical bone binder material and preparation method thereof
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