![]() COMPOSITION AND PROCEDURE FOR THE OBTAINING AND APPLICATION OF A BIOACTIVE COMPOUND CONTAINING FLUOR
专利摘要:
Composition and process for obtaining a bioactive material in which the composition comprises a first element composition comprises a first component comprising at least one of the following compounds: phosphate β-tetracalcium, phosphate α-tric calcic, tetracalcium phosphate, oxyapatite, hydroxyapatite, calcium deficient hydroxyapatite, a second component comprising at least one of the following compounds: monocalcium phosphate monohydrate or any other calcium phosphate acid such as calcium dihydrogen phosphate (Synonym: calcium phosphate monobasic, monocalcium orthophosphate, monocalcium phosphate, calcium phosphate, acid calcium phosphate) or meta-phosphoric acid and/or ortho-phosphoric acid, two fluoride-releasing molecules and a PH-regulator, which are mixed together and reacted with an aqueous solution and/or saline to proceed after dehydration and grinding, obtaining a material that, put in contact or with an aqueous solution such as saliva, it is transformed into apatite containing fluorine and fluorapatite. (Machine-translation by Google Translate, not legally binding) 公开号:ES2716942A1 申请号:ES201830630 申请日:2018-06-22 公开日:2019-06-18 发明作者:Feitosa Victor Pinheiro;Salvatore Sauro 申请人:CARDENAL HERRERA CEU, University of; IPC主号:
专利说明:
[0001] [0002] COMPOSITION AND PROCEDURE FOR THE OBTAINING AND APPLICATION OF A BIOACTIVE COMPOUND CONTAINING FLUORIDE AND THE PRODUCT OBTAINED. [0003] [0004] The invention, as its name suggests, refers to a composition for obtaining a bioactive particle that in contact with an aqueous and / or saline solution is capable of transforming into apatite containing fluorine and fluorapatite, as well as the process for its obtaining and its applications. [0005] [0006] The sector of the technique to which it belongs is that of the compositions for use in oral health and odontology. [0007] [0008] BACKGROUND OF THE INVENTION [0009] [0010] It is common the use of bioactive materials in the clinical and home settings, either as bone restorative elements, or as elements for uses related to dentistry since these bioactive compounds have a great resistance, which makes them suitable for implants, composites, adhesives, crowns, endodontic cements and also for prevention elements and dental cosmetics such as toothpastes, rinses and remineralizing treatments of enamel and dentin. [0011] On the other hand fluorides are also commonly used in the field of oral hygiene treatments or for, when exchanged with hydroxide groups of tooth enamel, make the tooth more resistant to attacks from, for example, tooth decay and tooth erosion. [0012] [0013] Various patents are known which relate to compositions for a bioactive material comprising fluoride. Among those closest to the invention that is intended is the patent US4775646, which comprises SiO2, CaO, Na2O, P2O5 (Bioactive glasses). [0014] [0015] Another patent also close to US2013 / 0171220 relates to a composition for a bioactive material comprising one or more bioactive glasses containing SiO 2 , P 2 O 5 and a fluoride. [0016] [0017] Unlike the cited patents, the invention that is intended is much less complex in its composition because it is not a bioactive glass but a modified calcium / phosphate. In addition, this invention is of lower economic cost and the procedure for obtaining it is very simple. [0018] DESCRIPTION OF THE INVENTION [0019] [0020] The invention relates to a composition for obtaining a bioactive material, preferably in powder, containing fluoride. [0021] [0022] For this a reaction is provoked that, if not manipulated, would result in the formation of brushite. [0023] [0024] Specifically, it is a combination of a first component and a second component that, when reacted, would generate brushite, but when the pH is controlled in the reaction, brushite is not formed. [0025] [0026] Therefore, to avoid the formation of brushite, the pH is controlled by adding a pH regulator to the compound in such a way that a different formation is obtained. [0027] [0028] For this, the composition comprises: [0029] [0030] A first component comprising at least one of the following compounds: phosphate (B-tricalcium, a-tricalcium phosphate, tetracalcium phosphate, oxyapatite, hydroxyapatite, calcium deficient hydroxyapatite [0031] 2. A second component comprising at least one of the following compounds: monocalcium phosphate monohydrate or any other calcium phosphate acid such as calcium dihydrogen phosphate (Synonym: monobasic calcium phosphate, monocalcium orthophosphate, monocalcium phosphate, calcium biphosphate , calcium phosphate acid) or meta-phosphoric acid and / or orthophosphoric acid [0032] 3. Two fluoride releasing molecules. [0033] 4. A PH regulator [0034] [0035] As for the fluorine-releasing molecules, calcium fluoride and sodium fluoride have been successfully tested, although it is not excluded that there may be other fluorine-releasing molecules that can be used in the composition. [0036] [0037] For its part, the pH regulator with which tests have been made with optimal results is calcium hydroxide, although it is not ruled out that there may be other pH regulators equally effective. [0038] [0039] The process by which this bioactive material is prepared and obtained is divided into the following stages: [0040] [0041] 1.- Mixing stage: [0042] [0043] In this mixing step, a homogenous mixture of; [0044] [0045] - 30-60% of the first component. [0046] - 30-60% of the second component. [0047] - 5-40% A pH regulator such as calcium hydroxide can be [0048] - 1-30% Fluorine-releasing molecules such as sodium fluoride or calcium fluoride. [0049] [0050] The best results are obtained if the percentage of the first component and the second component are similar. We will understand by similar when the percentage difference between one and another does not exceed 40%. [0051] [0052] 2. - Hydration stage: [0053] [0054] In this second stage of hydration, the mixture obtained in the first stage, a hydrating element is added. This hydrating element can be distilled water or another type of aqueous and saline solution such as PBS (phosphate bufferedsaline) which contains sodium chloride, sodium phosphate, potassium chloride and potassium phosphate. The use of other solutions is not ruled out. [0055] [0056] In particular, a possible proportion to carry out this second stage would be: [0057] [0058] - 50% the mixture obtained in the first stage. [0059] - 50% hydrating element, such as distilled water. [0060] [0061] The tests carried out were carried out with a hydration in which the mixture obtained from the first phase was mixed in equal parts with the moisturizing fluid, although it is not ruled out that other similar percentages could give similar results. [0062] [0063] We will understand by similar when the percentage difference between one and another does not exceed 40%. [0064] [0065] There may be reactions different from those described in terms of various variables, although the reactions that have been experienced have been indicated. [0066] [0067] This second stage is of short duration, between 1 and 10 minutes which are the times in which the reaction takes place, although nothing prevents that this phase can be prolonged for a longer time. [0068] [0069] 3. - Dehydrated stage. [0070] [0071] In this third stage, moisture is removed from the mixture. One option to remove this moisture is to allow the mixture to dry at a temperature of 40 ° to 55 ° C for 24 hours in a vacuum dryer containing silica to remove all excess water. [0072] [0073] This drying option is not the only one, although from the tests performed a good result is obtained. [0074] [0075] 4. - Grinding stage [0076] In this fourth stage, the already dehydrated product is milled until it reaches a particle size of less than 300 ^ m; then you can continue with the grinding stage until you reach a particle <10 ^ m. [0077] [0078] The process for obtaining the raw material with which to obtain the bioactive powder is composed of these stages 1 to 4. [0079] [0080] In order to obtain the reaction for the formation of apatite enriched with fluorine and / or fluorapatite, it is necessary to react this powder or cement by carrying out the step explained below. [0081] [0082] 5.- Rehydration stage and bioactive transformation [0083] [0084] To obtain with this raw material to obtain formation of fluorapatite and / or apatite enriched with fluorine, a further step is necessary which involves contacting these powders with an aqueous and saline solution such as PBS (phosphate bufferedsaline) or saliva (artificial). or biological). [0085] [0086] In this hydration stage, for example, the following reactions take place: [0087] [0088] Ca3 (P04) 2 Ca (H2P04) 2.H20 CaF2 NaF NaOH => 1 / 2Cal0 (PO4) 6F2 2HF Na2H (P04) 2H2O [0089] [0090] Ca3 (P04) 2 Ca (H2P04) 2.H20 CaF2 NaF NaOH => 1/2 Ca10 (PO4) 6 (OH) F 3HF Na2H (PO4) H2O [0091] [0092] The reaction occurs in an approximate time of between 5 and 20 days, normally 15 days. [0093] [0094] The applications are numerous and thus, only in the field of dentistry can we find applications for implants, composites, adhesives, endodontic cements and also for prevention elements and dental cosmetics such as toothpastes, rinses and remineralizing treatments. [0095] [0096] DESCRICPION OF A WAY TO CARRY OUT THE INVENTION [0097] [0098] There is described here a way of carrying out the invention that is not limiting without merely exposing. [0099] [0100] The invention relates to a bioactive material and to the process for obtaining it. [0101] The bioactive material reacts with an aqueous and saline solution obtaining fluorapatite or apatite enriched with fluorine, which makes this material especially suitable for use in implants, composites, adhesives, crowns, endodontic cements and also for prevention elements and dental cosmetics such as, toothpastes, rinses or remineralizing treatments among others. [0102] [0103] This bioactive compound comprises a first component, in this case beta-tricalcium phosphate, a second component, in this case monohydrogen calcium phosphate anhydrous, fluorine-releasing molecules, in this case sodium fluoride and calcium fluoride, a pH regulator , specifically calcium hydroxide. [0104] [0105] To obtain this biomaterial, the previous composition is reacted keeping the pH controlled so that brushite is not obtained but the biomaterial of interest. For this the procedure comprises the following stages. [0106] [0107] 1.- Mixing stage: [0108] [0109] In this mixing step, a homogenous mixture of; [0110] [0111] - 40% Beta-tricalcium phosphate [0112] - 40% monocalcium phosphate monohydrate [0113] - 10% Calcium hydroxide [0114] - 5% Sodium fluoride. [0115] - 5% Calcium fluoride. [0116] [0117] 2. - Hydration stage: [0118] [0119] In this second stage of hydration, the mixture obtained in the first stage is added, a hydrating element, in this case distilled water, in the following proportions: [0120] [0121] - 50% of the mixture obtained in the first stage. [0122] - 50% distilled water. [0123] [0124] This second stage is of short duration, between 1 and 10 minutes, which are the times in which the reaction takes place. [0125] [0126] 3. - Dehydrated stage. [0127] [0128] In this third stage, moisture is removed from the mixture. For this, the mixture is allowed to dry at a temperature of 45 ° C for 24 hours and then a vacuum dryer containing silica is used to remove all the excess water. [0129] 4.- Grinding stage [0130] [0131] In this fourth stage, the already dehydrated product is milled until it reaches a particle size of less than 30 ^ m. [0132] [0133] With these four stages the product or raw material is obtained which will then react giving rise to the formation of fluorapatite or apatite enriched with fluorine. [0134] To obtain the bioactive material, it is necessary to react this cement by carrying out the step explained below. [0135] [0136] 5.- Rehydration stage and bioactive transformation [0137] [0138] In order to obtain fluorapatite and / or apatite enriched with fluorine with the product obtained with stages 1 to 4, it is necessary to put it in contact with that product with an aqueous and saline solution such as PBS (phosphate bufferedsaline) or saliva ( artificial or biological). [0139] [0140] In this stage of hydration the following reactions take place: [0141] [0142] Ca3 (P04) 2 Ca (H2P04) 2.H20 CaF2 NaF NaOH => 1/2 CAL0 (PO4) 6F2 2HF Na2H (P04) 2H2O [0143] [0144] Ca3 (P04) 2 Ca (H2P04) 2.H20 CaF2 NaF NaOH => 1/2 Ca10 (PO4) 6 (OH) F 3HF Na2H (PO4) H2O [0145] [0146] The reaction occurs in an approximate time of 15 days.
权利要求:
Claims (29) [1] 1. - COMPOSITION FOR THE OBTAINING OF A BIOACTIVE COMPOUND characterized in that it comprises: - A first component. - A second component. - A pH regulator - Fluorine releasing molecules. Where; The first component comprises at least one of the following compounds; P-tricalcium phosphate, a-tricalcium phosphate, tetracalcium phosphate, oxyapatite, hydroxyapatite or hydroxyapatite deficient in calcium. The second comprises at least one of the following compounds: monocalcium phosphate monohydrate, calcium dihydrogen phosphate (Synonym: calcium phosphate monobasic, monocalcium orthophosphate, monocalcium phosphate, calcium biphosphate, calcium phosphate acid) or also metaphosphoric acid, acid orthophosphoric or any other acid calcium phosphate. [2] 2. - COMPOSITION FOR THE OBTAINING OF A BIOACTIVE COMPOUND according to claim 1 characterized in that the components intervene in the following percentages: - 30-60% of the first component. - 30-60% of the second component. - 5-40% pH regulator. - 1-30% Fluorine-releasing molecules. [3] 3. - COMPOSITION FOR THE OBTAINING OF A BIOACTIVE COMPOUND according to claim 1, characterized in that the first component is beta-tricalcium phosphate. [4] 4. COMPOSITION FOR OBTAINING A BIOACTIVE COMPOUND according to claim 1, characterized in that the second component is monocalcium phosphate monohydrate. [5] 5. - COMPOSITION FOR THE OBTAINING OF A BIOACTIVE COMPOUND according to claim 1, characterized in that the pH regulator is calcium hydroxide. [6] 6. - COMPOSITION FOR THE OBTAINING OF A BIOACTIVE COMPOUND according to claim 1, characterized in that the fluorine-releasing molecule is sodium fluoride. [7] 7. - COMPOSITION FOR THE OBTAINING OF A BIOACTIVE COMPOUND according to claim 1, characterized in that the fluorine-releasing molecule is calcium fluoride. [8] 8. - PROCEDURE FOR THE OBTAINING AND APPLICATION OF A BIOACTIVE COMPOUND characterized in that it comprises a first step of mixing stage in which proceeds to obtain a homogeneous mixture of a first component, a second component, a pH regulator and fluoride-releasing molecules, all in the following proportions: - 30-60% first component. - 30-60% second make up. - 5-40% pH regulator. - 1-30% Fluorine-releasing molecules. [9] 9. - PROCEDURE FOR THE OBTAINING AND APPLICATION OF A BIOACTIVE COMPOUND according to claim 8, characterized in that: 1. The first component comprises at least one of the following neutral / basic calcium phosphate compounds is Beta-tricalcium phosphate. 2. The second component comprises at least one of the following compounds; monocalcium phosphate monohydrate, calcium dihydrogen phosphate (Synonym: monobasic calcium phosphate, monocalcium orthophosphate, monocalcium phosphate, calcium biphosphate, calcium phosphate acid) or also metaphosphoric acid, orthophosphoric acid or any other calcium phosphate acid. 3. The pH regulator is calcium hydroxide 4. The fluorine-releasing molecule is sodium fluoride. [10] 10. - PROCEDURE FOR THE OBTAINING AND APPLICATION OF A BIOACTIVE COMPOUND according to claim 9 characterized in that the fluorine-releasing molecule is calcium fluoride. [11] 11. - PROCEDURE FOR THE OBTAINING AND APPLICATION OF A BIOACTIVE COMPOUND according to claim 8 characterized in that the first component and the second component are contributed to the mixture in similar percentages. [12] 12. - PROCEDURE FOR THE OBTAINING AND APPLICATION OF A BIOACTIVE COMPOUND according to claim 8 characterized in that it also comprises a second stage of hydration in which is added to the mixture obtained in the first stage, a moisturizing element leaving the mixture during a certain time. [13] 13. - PROCEDURE FOR THE OBTAINING AND APPLICATION OF A BIOACTIVE COMPOUND according to claim 12, characterized in that the moisturizing element is an aqueous saline solution. [14] 14. - PROCEDURE FOR THE OBTAINING AND APPLICATION OF A BIOACTIVE COMPOUND according to claim 12 characterized in that the moisturizing element contains sodium chloride, sodium phosphate, potassium chloride and potassium phosphate. [15] 15. - PROCEDURE FOR THE OBTAINING AND APPLICATION OF A BIOACTIVE COMPOUND according to claim 12, characterized in that the product obtained in the first stage and the hydrating element are added to the mixture by similar parts. [16] 16. - PROCEDURE FOR THE OBTAINMENT AND APPLICATION OF A BIOACTIVE COMPOUND according to claim 12, characterized in that its duration is from 1 to 10 minutes. [17] 17. - PROCEDURE FOR THE OBTAINING AND APPLICATION OF A BIOACTIVE COMPOUND according to claim 12, characterized in that it also comprises a dehydration step. [18] 18. PROCEDURE FOR THE OBTAINING AND APPLICATION OF A BIOACTIVE COMPOUND according to claim 17, characterized in that the dehydration step comprises a sub-step of allowing the mixture to dry at a temperature of 40 to 55 ° C for 24 hours. [19] 19. PROCEDURE FOR THE OBTAINING AND APPLICATION OF A BIOACTIVE COMPOUND according to claim 17, characterized in that the dehydration step comprises a sub-step of subjecting the mixture to a vacuum dryer containing silica for the elimination of all excess water. [20] 20. - PROCEDURE FOR THE OBTAINING AND APPLICATION OF A BIOACTIVE COMPOUND according to claim 17, characterized in that it also comprises a step of grinding the already dehydrated product that is milled until reaching a suitable particle size. [21] 21. PROCEDURE FOR THE OBTAINING AND APPLICATION OF A BIOACTIVE COMPOUND according to claim 20 characterized in that in the milling stage a particle size of less than 300pm is obtained. [22] 22. PROCEDURE FOR THE OBTAINING AND APPLICATION OF A BIOACTIVE COMPOUND according to claim 20 characterized in that in the milling stage a particle size of less than 30pm is obtained. [23] 23. - PROCEDURE FOR THE OBTAINING AND APPLICATION OF A BIOACTIVE COMPOUND according to claim 20, characterized in that it also comprises a fifth stage in which the result of steps 1 to 4 is brought into contact with an aqueous and saline solution. one [24] 24. - PROCEDURE FOR THE OBTAINING AND APPLICATION OF A BIOACTIVE COMPOUND according to claim characterized in that the aqueous and saline solution is saliva. [25] 25. - PROCEDURE FOR THE OBTAINING AND APPLICATION OF A BIOACTIVE COMPOUND according to claim 23 characterized in that the aqueous solution and salt is PBS. [26] 26. - METHOD OF OBTAINING AND APPLICATION OF A BIOACTIVE COMPOSITE according to claim 23 wherein the reaction Ca3 (P04) 2 Ca (H2P04) 2.H20 CaF2 NaF NaOH => 1/2 CAL0 (PO4) 6F2 2HF occurs Na2H (P04) 2H2O. [27] 27.- PROCEDURE FOR THE OBTAINING AND APPLICATION OF A BIOACTIVE COMPOUND according to claim 23, characterized in that the reaction occurs Ca3 (P04) 2 Ca (H2P04) 2.H20 CaF2 NaF NaOH => 1/2 Ca10 (PO4) 6 (OH ) F 3HF Na2H (PO4) H2O. [28] 28.- PROCEDURE FOR THE OBTAINING AND APPLICATION OF A BIOACTIVE COMPOUND according to claim 23 characterized in that this fifth stage has a duration of between 10 and 20 days. [29] 29. BIOACTIVE COMPOUND characterized by being obtained with the composition and process described in the preceding claims as well as implants, composites, adhesives, crowns, endodontic cements, toothpastes, rinses and remineralizing treatments containing it.
类似技术:
公开号 | 公开日 | 专利标题 US5437857A|1995-08-01|Methods and compositions for mineralizing and fluoridating calcified tissues CA2172538C|1999-11-16|Self-setting calcium phosphate cements and methods for preparing and using them US4518430A|1985-05-21|Dental resptorative cement pastes CA2157890C|1999-02-23|Calcium phosphate hydroxyapatite precursor and methods for making and using the same USRE33221E|1990-05-22|Dental restorative cement pastes EP2626058B1|2019-05-01|Dentinal tubule sealant and method for producing the same Gjorgievska et al.2010|A preliminary study of enamel remineralization by dentifrices based on RECALDENTTM | and Novamin®| GB2102289A|1983-02-02|Dentifrice containing fluorine compounds and calcium and phosphate compounds US20100303737A1|2010-12-02|Tooth-Cleaning Formulation CZ297911B6|2007-04-25|Combined composition for whitening teeth or for treating skin complaints and mucous membrane disorders, as well as process for preparing such composition ES2365091B1|2013-01-24|AN INORGANIC CEMENT FOR BIOMEDICAL APPLICATIONS, PROCEDURE FOR THE PREPARATION AND USE OF SUCH CEMENT. ES2542990T3|2015-08-13|Dental material that forms hydroxylapatite with bioactive action ES2716942A1|2019-06-18|COMPOSITION AND PROCEDURE FOR THE OBTAINING AND APPLICATION OF A BIOACTIVE COMPOUND CONTAINING FLUORIDE AND THE PRODUCT OBTAINED. | Zhibarev et al.2013|Synthesis of hydroxyapatite for bioactive coatings Xie et al.1989|Calcium phosphate dental cements JP5543777B2|2014-07-09|Novel phosphorus-calcium-strontium compounds and their use in endodontic cement Maçon et al.2015|Bioactivity of toothpaste containing bioactive glass in remineralizing media: effect of fluoride release from the enzymatic cleavage of monofluorophosphate. JP2505545B2|1996-06-12|Method for curing curable composition Hemasathya et al.2015|Recent advances in root end filling materials: a review CA2028250A1|1991-04-24|Fluoride stability in dicalcium phosphate dihydrate composition Asmawati2017|Identification of inorganic compounds in eggshell as a dental remineralization material Saidin et al.2021|Fabrication of fluorapatite cement as an anti-caries agent based on calcium phosphate cement Davaie et al.2021|Bioactive Glass Modified Calcium Phosphate Cement with Improved Bioactive Properties: A Potential Material for Dental Pulp-Capping Approaches Haridy et al.2018|Micro Hardness Of Bleached Human Enamel Following Application Of Conventional Versus Nano Active Bioglass: An Invitro Study Amjad et al.1982|The remineralization of fluoride-treated bovine enamel surfaces
同族专利:
公开号 | 公开日 WO2019243592A1|2019-12-26| ES2716942B2|2021-03-29|
引用文献:
公开号 | 申请日 | 公开日 | 申请人 | 专利标题 US4855118A|1987-04-15|1989-08-08|Nichia Kagaku Kogyo K.K.|Method of producing fluorapatite| US20120128566A1|2010-06-22|2012-05-24|Peking University|Method for producing fluorapatite and its application| US4775646A|1984-04-27|1988-10-04|University Of Florida|Fluoride-containing Bioglass™ compositions| US5962028A|1988-04-20|1999-10-05|Norian Corporation|Carbonated hydroxyapatite compositions and uses| CN102448471B|2009-03-30|2017-04-12|可乐丽则武齿科株式会社|Dentine calcification agent and method for producing same| GB201010758D0|2010-06-25|2010-08-11|Queen Mary & Westfield College|Bioactive glass composition| JP6232671B2|2012-09-28|2017-11-22|クラレノリタケデンタル株式会社|Dental curable composition and method for producing the same|
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申请号 | 申请日 | 专利标题 ES201830630A|ES2716942B2|2018-06-22|2018-06-22|COMPOSITION AND PROCEDURE FOR OBTAINING AND APPLYING A BIOACTIVE COMPOUND CONTAINING FLUORIDE AND THE PRODUCT OBTAINED.|ES201830630A| ES2716942B2|2018-06-22|2018-06-22|COMPOSITION AND PROCEDURE FOR OBTAINING AND APPLYING A BIOACTIVE COMPOUND CONTAINING FLUORIDE AND THE PRODUCT OBTAINED.| PCT/EP2019/066506| WO2019243592A1|2018-06-22|2019-06-21|Preparation, composition and application of a bioactive fluoride-doped calcium phosphate able to induce controlled deposition of fluorapatite| 相关专利
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