Mineralized glycerol gels, methods of making and use

Abstract

The present application relates to a kind of mineralized glycerol gel, preparation method and application, preparation method includes: the cation source is dissolved in glycerol solution, to obtain first solution;The anion source is dissolved in glycerol solution, to obtain second solution;Second solution is added to first solution and mixed, forms mineralized glycerol gel.Its advantage is that the glycerol solution containing cation source is directly mixed with the glycerol solution containing anion source to prepare mineralized glycerol gel, the preparation method is simple, without additional additives, reduce the kind of raw material and raw material consumption, greatly reduce production cost;Prepared mineralized glycerol gel contains glycerol and mineral, it is in gel form below 50 DEG C, it is convenient to store, transport and use, reduce use cost;Mineralized glycerol gel can be remineralized to tooth surface, repair dental enamel, and avoid caries to develop again.

Description

Technical Field

[0001] This invention relates to the field of dental restoration technology, and in particular to a mineralized glycerin gel, its preparation method, and its application. Background Technology

[0002] Dental caries is a common disease that endangers human health, and it can generally be divided into superficial caries, moderate caries, and deep caries. Among them, superficial caries, which occurs on the enamel layer of the tooth surface, is the most common. If superficial caries is not treated in time, it can easily lead to deeper cavities, further damaging the dentin and pulp.

[0003] Currently, the common method for treating superficial caries is to fill them with dental resin. However, this method often results in gaps forming between the resin and the tooth, leading to recurrence of the caries. Furthermore, the composition of dental resin differs significantly from that of teeth, and their mechanical properties are mismatched, resulting in less than ideal restorative effects and functional reconstruction.

[0004] The main component of teeth is hydroxyapatite, a calcium phosphate compound. Enamel caries primarily results from the loss of this calcium phosphate. Remineralization of the tooth surface to form a new calcium phosphate layer with a microstructure similar to or identical to enamel is an ideal enamel repair strategy. In recent years, some dental restorative products have appeared on the market, offering some degree of repair to the mineral deposits on the tooth surface. However, a product that perfectly achieves the aforementioned strategy has yet to emerge.

[0005] Currently, no effective solutions have been proposed for the problems of inability to remineralize tooth surfaces and low mineralization efficiency in related technologies. Summary of the Invention

[0006] The purpose of this application is to address the shortcomings of the prior art by providing a mineralized glycerol gel, its preparation method, and its application, so as to at least solve the problems of the inability to remineralize the tooth surface and the low mineralization efficiency in the related technologies.

[0007] To achieve the above objectives, the technical solution adopted in this application is as follows:

[0008] In a first aspect, the present invention provides a method for preparing a mineralized glycerol gel, comprising:

[0009] The cation source is dissolved in a glycerol solution to obtain a first solution;

[0010] The anion source is dissolved in a glycerol solution to obtain a second solution;

[0011] The second solution is added to the first solution and mixed to form a mineralized glycerol gel;

[0012] The mineralized glycerol gel is gel-like at temperatures below 50°C.

[0013] Wherein, the cation source is a water-soluble mineral salt, and the anion source is a water-soluble inorganic acid and / or a water-soluble inorganic acid salt;

[0014] In the mixed solution, the concentration of the cation source is 0.01–10 mol / L, the concentration of the anion source is 0.01–10 mol / L, and the molar ratio of the cation source to the anion source is 0.1–5:1.

[0015] In some of these embodiments, the mineralized glycerol gel is gel-like at temperatures below 45°C.

[0016] In some of these embodiments, the mineralized glycerol gel is gel-like at temperatures below 40°C.

[0017] In some of these embodiments, the mineralized glycerol gel is gel-like at temperatures below 38°C.

[0018] In some of these embodiments, the mineralized glycerol gel is gel-like at 4–38°C.

[0019] In some of these embodiments, the viscosity of the mineralized glycerol gel is greater than or equal to 2500 mPa·s.

[0020] In some embodiments, the cation source is one or a combination of calcium ions and magnesium ions.

[0021] In some of these embodiments, the cation source is one or a combination of water-soluble calcium salts and water-soluble magnesium salts.

[0022] In some of these embodiments, the cation source is one or a combination of calcium chloride, calcium nitrate, calcium acetate, magnesium chloride, magnesium nitrate, and magnesium acetate.

[0023] In some of these embodiments, the anion source is one or a combination of phosphate ions, sulfate ions, and carbonate ions.

[0024] In some embodiments, the anion source is one or a combination of several of water-soluble phosphates, water-soluble sulfates, and water-soluble carbonates.

[0025] In some of these embodiments, the anion source is a water-soluble sodium salt containing phosphate, a water-soluble potassium salt containing phosphate, a water-soluble ammonium salt containing phosphate, a water-soluble sodium salt containing sulfate, a water-soluble potassium salt containing sulfate, a water-soluble ammonium salt containing sulfate, a water-soluble sodium salt containing carbonate, a water-soluble potassium salt containing carbonate, or a water-soluble ammonium salt containing carbonate.

[0026] In some of these embodiments, the anion source is one or a combination of several of the following: phosphoric acid, sodium phosphate, sodium monohydrogen phosphate, sodium dihydrogen phosphate, potassium phosphate, potassium monohydrogen phosphate, potassium dihydrogen phosphate, ammonium phosphate, ammonium monohydrogen phosphate, ammonium dihydrogen phosphate, sodium sulfate, sodium bisulfate, potassium sulfate, potassium bisulfate, ammonium sulfate, ammonium bisulfate, sodium carbonate, sodium bicarbonate, potassium carbonate, potassium bicarbonate, ammonium carbonate, and ammonium bicarbonate.

[0027] In some of these embodiments, the glycerol solution is a pure glycerol solution or a glycerol solution containing water;

[0028] In the aqueous glycerol solution, the water content is less than 50% by mass.

[0029] In some embodiments, the method of adding the second solution to the first solution for mixing includes:

[0030] Stirring method; and / or, ultrasonic method; and / or, vortex oscillation method.

[0031] In some embodiments, the stirring method includes:

[0032] The stirring time is greater than 1 second, and the stirring speed is 40 to 10,000 rpm.

[0033] In some embodiments, the second solution is added to the first solution at a dropping rate of 0.1 to 10,000 ml / min.

[0034] In some of these embodiments, the temperature at which the second solution is added to the first solution and mixed is 0–60°C.

[0035] In some embodiments, the temperature at which the second solution is added to the first solution and mixed is 0–50°C.

[0036] In a second aspect, the present invention provides a mineralized glycerol gel, prepared by the preparation method of the first aspect, comprising minerals and glycerol;

[0037] The mineralized glycerol gel is gel-like at temperatures below 50°C.

[0038] The viscosity of the mineralized glycerol gel is greater than or equal to 2500 mPa·s.

[0039] In some of these embodiments, the mineral is 0.1% to 5% by mass.

[0040] In some embodiments, water is also included, wherein the water mass percentage is less than or equal to 20%.

[0041] In some of these embodiments, the mineral is one or a combination of calcium phosphate, calcium carbonate, calcium sulfate, magnesium phosphate, magnesium carbonate, and magnesium sulfate.

[0042] Thirdly, the present invention provides an application of mineralized glycerin as described in the second aspect in the repair of teeth.

[0043] Compared to related technologies, the mineralized glycerol gel, preparation method, and application provided in this application embodiment can be prepared by directly mixing a glycerol solution containing a cationic source and a glycerol solution containing an anionic source. The preparation method is simple, requires no additional additives, reduces the types and amounts of raw materials, and significantly reduces production costs. The prepared mineralized glycerol gel contains glycerol and minerals, and is gel-like below 50°C, making it easy to store, transport, and use, thus reducing usage costs. The mineralized glycerol gel can remineralize the tooth surface, repair tooth enamel, and prevent the recurrence of tooth decay. Attached Figure Description

[0044] The accompanying drawings, which are included to provide a further understanding of this application and form part of this application, illustrate exemplary embodiments and are used to explain this application, but do not constitute an undue limitation of this application. In the drawings:

[0045] Figure 1A This is a schematic diagram of the calcium phosphate-containing mineralized glycerol gel of the present invention;

[0046] Figure 1B This is a schematic diagram of pure glycerol solvent;

[0047] Figure 2A This is a schematic diagram of the calcium phosphate-containing mineralized glycerol gel of the present invention;

[0048] Figure 2B This is a schematic diagram of the calcium carbonate-containing mineralized glycerol gel of the present invention;

[0049] Figure 2C This is a schematic diagram of the magnesium carbonate-containing mineralized glycerol gel of the present invention;

[0050] Figure 2D This is a schematic diagram of the calcium sulfate-containing mineralized glycerol gel of the present invention;

[0051] Figure 2E This is a schematic diagram of the magnesium sulfate-containing mineralized glycerol gel of the present invention;

[0052] Figure 3 This is a transmission electron microscope image of the mineralized glycerol gel of the present invention;

[0053] Figure 4A This is a scanning electron microscope image of the corroded tooth surface;

[0054] Figure 4B This is a scanning electron microscope image of a corroded tooth surface coated with the mineralized glycerol gel of the present invention for 1 hour;

[0055] Figure 4C This is a scanning electron microscope image of a corroded tooth surface coated with the mineralized glycerol gel of the present invention for 24 hours;

[0056] Figure 4D This is a scanning electron microscope image of the corroded tooth surface after being coated with ordinary calcium phosphate for 24 hours.

[0057] Figure 5A It is a scanning electron microscope image of the tooth surface exposing the dentinal tubules;

[0058] Figure 5B This is a scanning electron microscope image of the tooth surface with exposed dentinal tubules after being coated with the mineralized glycerol gel of the present invention for 24 hours. Detailed Implementation

[0059] To make the objectives, technical solutions, and advantages of this application clearer, the application is described and illustrated below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative and not intended to limit the scope of this application. All other embodiments obtained by those skilled in the art based on the embodiments provided in this application without inventive effort are within the scope of protection of this application.

[0060] Obviously, the accompanying drawings described below are merely some examples or embodiments of this application. Those skilled in the art can apply this application to other similar scenarios based on these drawings without any inventive effort. Furthermore, it is understood that although the efforts made in this development process may be complex and lengthy, for those skilled in the art related to the content disclosed in this application, any changes to design, manufacturing, or production based on the technical content disclosed in this application are merely conventional technical means and should not be construed as insufficient disclosure of the content of this application.

[0061] In this application, the reference to "embodiment" means that a specific feature, structure, or characteristic described in connection with an embodiment may be included in at least one embodiment of this application. The appearance of this phrase in various places in the specification does not necessarily refer to the same embodiment, nor is it a separate or alternative embodiment that is mutually exclusive with other embodiments. It will be explicitly and implicitly understood by those skilled in the art that the embodiments described in this application may be combined with other embodiments without conflict.

[0062] Unless otherwise defined, the technical or scientific terms used in this application shall have the ordinary meaning understood by one of ordinary skill in the art to which this application pertains. The terms “a,” “an,” “an,” “the,” and similar words used in this application do not indicate quantity limitation and may indicate singular or plural. The terms “comprising,” “including,” “having,” and any variations thereof used in this application are intended to cover non-exclusive inclusion; for example, a process, method, system, product, or device that includes a series of steps or modules (units) is not limited to the listed steps or units, but may also include steps or units not listed, or may include other steps or units inherent to these processes, methods, products, or devices. The terms “connected,” “linked,” “coupled,” and similar words used in this application are not limited to physical or mechanical connections, but may include electrical connections, whether direct or indirect. “Multiple” used in this application refers to two or more. “And / or” describes the relationship between related objects, indicating that three relationships may exist; for example, “A and / or B” can represent: A alone, A and B simultaneously, and B alone. The character " / " generally indicates that the preceding and following objects are in an "or" relationship. The terms "first," "second," and "third" used in this application are merely to distinguish similar objects and do not represent a specific ordering of the objects.

[0063] Example 1

[0064] This embodiment is an illustrative example of the present invention, relating to mineralized glycerol gel, its preparation method, and its application.

[0065] A method for preparing a mineralized glycerol gel, comprising:

[0066] Step S102: Dissolve the cation source in a glycerol solution to obtain a first solution;

[0067] Step S104: Dissolve the anion source in a glycerol solution to obtain a second solution;

[0068] Step S106: Add the second solution to the first solution and mix to form a mineralized glycerol gel.

[0069] Among them, mineralized glycerol gel is gel-like at temperatures below 50°C;

[0070] The cation source is a water-soluble mineral salt, and the anion source is a water-soluble inorganic acid and / or a water-soluble inorganic acid salt.

[0071] In the mixed solution, the concentration of the cation source is 0.01–10 mol / L, the concentration of the anion source is 0.01–10 mol / L, and the molar ratio of the cation source to the anion source is 0.1–5:1.

[0072] Preferably, the mineralized glycerol gel is gel-like at temperatures below 45°C; preferably, the mineralized glycerol gel is gel-like at temperatures below 40°C; the mineralized glycerol gel is gel-like at temperatures below 38°C; the mineralized glycerol gel is gel-like at temperatures between 4°C and 38°C.

[0073] In some of these embodiments, the viscosity of the mineralized glycerol gel is greater than or equal to 2500 mPa·s.

[0074] In some of these embodiments, the cation source is one or a combination of calcium ions and magnesium ions.

[0075] In some of these embodiments, the cation source is one or a combination of water-soluble calcium salts and water-soluble magnesium salts.

[0076] In some of these embodiments, the cation source is one or a combination of calcium chloride, calcium nitrate, calcium acetate, magnesium chloride, magnesium nitrate, and magnesium acetate.

[0077] In some of these embodiments, the anion source is one or a combination of phosphate ions, sulfate ions, and carbonate ions.

[0078] In some of these embodiments, the anion source is one or a combination of several of water-soluble phosphates, water-soluble sulfates, and water-soluble carbonates.

[0079] In some of these embodiments, the anion source is a water-soluble sodium salt containing phosphate, a water-soluble potassium salt containing phosphate, a water-soluble ammonium salt containing phosphate, a water-soluble sodium salt containing sulfate, a water-soluble potassium salt containing sulfate, a water-soluble ammonium salt containing sulfate, a water-soluble sodium salt containing carbonate, a water-soluble potassium salt containing carbonate, or a water-soluble ammonium salt containing carbonate.

[0080] In some of these embodiments, the anion source is one or a combination of several of the following: phosphoric acid, sodium phosphate, sodium monohydrogen phosphate, sodium dihydrogen phosphate, potassium phosphate, potassium monohydrogen phosphate, potassium dihydrogen phosphate, ammonium phosphate, ammonium monohydrogen phosphate, ammonium dihydrogen phosphate, sodium sulfate, sodium bisulfate, potassium sulfate, potassium bisulfate, ammonium sulfate, ammonium bisulfate, sodium carbonate, sodium bicarbonate, potassium carbonate, potassium bicarbonate, ammonium carbonate, and ammonium bicarbonate.

[0081] In some of these embodiments, the glycerol solution is a pure glycerol solution or a glycerol solution containing water;

[0082] In the aqueous glycerol solution, the water content is less than 50% by mass.

[0083] In some embodiments, the method of adding the second solution to the first solution for mixing includes:

[0084] Stirring method; and / or, ultrasonic method; and / or, vortex oscillation method.

[0085] In some embodiments, the stirring method includes:

[0086] The stirring time is greater than 1 second, and the stirring speed is 40 to 10,000 rpm.

[0087] In some of these embodiments, the second solution is added to the first solution at a dropping rate of 0.1 to 10,000 ml / min.

[0088] In some embodiments, the temperature at which the second solution is added to the first solution and mixed is 0–60°C. Preferably, the temperature at which the second solution is added to the first solution and mixed is 0–50°C.

[0089] Preferably, the concentration of the cation source in the mixed solution is 0.1–8 mol / L; preferably, the concentration of the cation source in the mixed solution is 0.2–6 mol / L; preferably, the concentration of the cation source in the mixed solution is 0.5–4 mol / L; preferably, the concentration of the cation source in the mixed solution is 0.5–2 mol / L.

[0090] Preferably, the concentration of the anion source in the mixed solution is 0.1–8 mol / L; preferably, the concentration of the anion source in the mixed solution is 0.2–6 mol / L; preferably, the concentration of the anion source in the mixed solution is 0.5–4 mol / L; preferably, the concentration of the anion source in the mixed solution is 0.5–2 mol / L.

[0091] Preferably, the molar ratio of the cation source to the anion source is 0.2 to 4:1; more preferably, the molar ratio of the cation source to the anion source is 0.2 to 3:1; even more preferably, the molar ratio of the cation source to the anion source is 0.3 to 2:1; most preferably, the molar ratio of the cation source to the anion source is 0.5 to 2:1.

[0092] In some embodiments, the method of adding the second solution to the first solution for mixing includes:

[0093] Stirring method; and / or, ultrasonic method; and / or, vortex oscillation method; and / or, settling method.

[0094] In some embodiments, the stirring method includes:

[0095] The stirring time is greater than 1 second, and the stirring speed is 40 to 10,000 rpm.

[0096] In some of these embodiments, the second solution is added to the first solution at a dropping rate of 0.1 to 10,000 ml / min.

[0097] Furthermore, the preparation method also includes:

[0098] Step S108: Before the mixed solution forms a gel, remove impurities from the mixed solution to obtain a mineralized glycerol gel.

[0099] In step S108, the impurities removed are non-mineral water-soluble inorganic salts resulting from the reaction of a cation source and an anion source.

[0100] In addition, impurities may also include unreacted cation and anion sources.

[0101] In some embodiments, the method for removing impurities from the mixed solution includes:

[0102] High-speed centrifugation; and / or chromatography; and / or dialysis.

[0103] In the high-speed centrifugation method, the centrifugation speed is 5000 to 20000 rpm.

[0104] Chromatographic methods include, but are not limited to, gel chromatography, thin-layer chromatography, ion exchange chromatography, adsorption chromatography, and partition chromatography.

[0105] In this embodiment, in step S106, the mixed solution can be used directly (i.e., without removing impurities) or after removing impurities. This is because the unreacted cation source, anion source, and the soluble inorganic salts generated in the reaction are all non-toxic, water-soluble substances. In actual use, these substances can all be dissolved in the aqueous solution and flow with the aqueous solution, without causing deposition or adsorption.

[0106] The prepared mineralized glycerol gel comprises minerals and glycerol, wherein the minerals account for 0.1% to 5% of the mass.

[0107] The mineralized glycerol gel may contain impurities or be free of impurities.

[0108] Preferably, the mineralized glycerol gel is a mineralized glycerol gel free of impurities.

[0109] like Figures 1A-1B as well as Figures 2A-2E As shown, compared with glycerol solvent, the mineralized glycerol gel prepared by the present invention is gel-like below 50°C and has a viscosity of more than 2500 mPa·s. When the container storing the mineralized glycerol gel is turned upside down, the mineralized glycerol gel will not be displaced.

[0110] As can be seen from the preparation method, mineralized glycerol gel comprises minerals and glycerol. For example... Figure 3As shown, the minerals therein are extremely small particles (average particle size less than 10 nm).

[0111] In some embodiments, the mineralized glycerol gel further includes water, wherein the water mass percentage is less than or equal to 20%.

[0112] Preferably, the water mass percentage is less than or equal to 15%; preferably, the water mass percentage is less than or equal to 10%; preferably, the water mass percentage is less than or equal to 5%; preferably, the water mass percentage is 0.2% to 2%.

[0113] The aforementioned mineralized glycerol gel can be used to repair hard tissues in teeth.

[0114] Specifically, mineralized glycerin gel can be used as a single ingredient or in combination with other ingredients.

[0115] like Figures 4A-4D As shown, the mineralized glycerol gel prepared according to this invention is coated onto the surface of a tooth whose enamel is damaged by corrosion. Figure 4A In comparison, in a short period of time ( Figure 4B Good restorative results can be achieved by penetrating into the gaps and grooves created on the surface of corroded teeth, forming a hydroxyapatite nanorod mineralization layer; over a long period of time ( Figure 4C The coated tooth surface is smoother, resulting in a better restorative effect. In contrast, ordinary calcium phosphate treatment of corroded tooth enamel still leaves obvious gaps and grooves, and cannot effectively repair corroded tooth enamel. Figure 4D ).

[0116] like Figures 5A-5B As shown, the mineralized glycerol gel prepared according to this invention is coated onto the surface of a tooth whose dentinal tubules have been exposed due to corrosion. Figure 5A In comparison, in a short period of time ( Figure 5B This process can produce a dense mineralized layer that covers the dentinal tubules, thus achieving a good restorative effect.

[0117] The advantages of this invention are that mineralized glycerol gel can be prepared by directly mixing a glycerol solution containing a cationic source and a glycerol solution containing an anionic source. The preparation method is simple, requires no additional additives, reduces the types and amounts of raw materials, and significantly reduces production costs. The prepared mineralized glycerol gel is gel-like below 50°C, which facilitates storage, transportation, and use, reducing usage costs. The mineralized glycerol gel fills the gaps in the tooth interface, preventing the recurrence of tooth decay. The mineralized glycerol gel contains minerals, which can remineralize the tooth surface.

[0118] Example 2

[0119] This embodiment is a specific implementation of the present invention.

[0120] Prepare 50 mL of a 0.04 mol / L sodium dodecahydrate glycerol solution as the first solution;

[0121] Prepare 10 mL of a 0.3 mol / L calcium chloride dihydrate glycerol solution as the second solution;

[0122] The second solution is mixed evenly with the first solution and allowed to stand at 37°C for 24 hours to obtain mineralized glycerol gel.

[0123] Below 50°C, mineralized glycerol gel is a white gel with no obvious fluidity.

[0124] In the mineralized glycerol gel, the mass percentages of minerals, water, and glycerol are 0.4%, 0.7%, and 98.9%, respectively.

[0125] The viscosity of the mineralized glycerol gel is 14000 mPa·s.

[0126] Example 3

[0127] This embodiment is a specific implementation of the present invention.

[0128] Prepare 50 mL of a 0.08 mol / L sodium dodecahydrate glycerol solution as the first solution;

[0129] Prepare 10 mL of a 0.6 mol / L calcium chloride dihydrate glycerol solution as the second solution;

[0130] The second solution is mixed evenly with the first solution and allowed to stand at 37°C for 24 hours to obtain mineralized glycerol gel.

[0131] Below 50°C, mineralized glycerol gel is a white gel with no obvious fluidity.

[0132] In the mineralized glycerol gel, the mass percentages of minerals, water, and glycerol are 0.8%, 1.4%, and 97.8%, respectively.

[0133] The viscosity of the mineralized glycerol gel is 44000 mPa·s.

[0134] Example 4

[0135] This embodiment is a specific implementation of the present invention.

[0136] Prepare 50 mL of a 0.08 mol / L sodium dodecahydrate glycerol solution as the first solution;

[0137] Prepare 10 mL of a 0.6 mol / L magnesium chloride hexahydrate glycerol solution as the second solution;

[0138] The second solution is mixed evenly with the first solution and allowed to stand at 37°C for 24 hours to obtain mineralized glycerol gel.

[0139] Below 50°C, mineralized glycerol gel is a white gel with no obvious fluidity.

[0140] In the mineralized glycerol gel, the mass percentages of minerals, water, and glycerol are 0.6%, 2.0%, and 97.4%, respectively.

[0141] The viscosity of the mineralized glycerol gel is 13000 mPa·s.

[0142] Example 5

[0143] This embodiment is a specific implementation of the present invention.

[0144] Prepare 50 mL of a 0.04 mol / L sodium dodecahydrate glycerol solution as the first solution;

[0145] Prepare 10 mL of a 0.3 mol / L magnesium chloride hexahydrate glycerol solution as the second solution;

[0146] The second solution is mixed evenly with the first solution and allowed to stand at 37°C for 24 hours to obtain mineralized glycerol gel.

[0147] Below 50°C, mineralized glycerol gel is a white gel with no obvious fluidity.

[0148] In the mineralized glycerol gel, the mass percentages of minerals, water, and glycerol are 0.3%, 1.0%, and 98.7%, respectively.

[0149] The viscosity of the mineralized glycerol gel is 6600 mPa·s.

[0150] Example 6

[0151] This embodiment is a specific implementation of the present invention.

[0152] Prepare 50 mL of a 0.08 mol / L sodium sulfate decahydrate glycerol solution as the first solution;

[0153] Prepare 10 mL of a 0.4 mol / L calcium chloride dihydrate glycerol solution as the second solution;

[0154] The second solution is mixed evenly with the first solution and allowed to stand at 37°C for 24 hours to obtain mineralized glycerol gel.

[0155] Below 50°C, mineralized glycerol gel is a white gel with no obvious fluidity.

[0156] In the mineralized glycerol gel, the mass percentages of minerals, water, and glycerol are 0.5%, 0.2%, and 97.3%, respectively.

[0157] The viscosity of the mineralized glycerol gel is 25000 mPa·s.

[0158] Example 7

[0159] This embodiment is a specific implementation of the present invention.

[0160] Prepare 50 mL of a 0.08 mol / L sodium sulfate decahydrate glycerol solution as the first solution;

[0161] Prepare 10 mL of a 0.6 mol / L calcium chloride dihydrate glycerol solution as the second solution;

[0162] The second solution is mixed evenly with the first solution and allowed to stand at 37°C for 24 hours to obtain mineralized glycerol gel.

[0163] Below 50°C, mineralized glycerol gel is a white gel with no obvious fluidity.

[0164] In the mineralized glycerol gel, the mass percentages of minerals, water, and glycerol are 0.7%, 1.1%, and 98.2%, respectively.

[0165] The viscosity of the mineralized glycerol gel is 24000 mPa·s.

[0166] Example 8

[0167] This embodiment is a specific implementation of the present invention.

[0168] Prepare 50 mL of a 0.08 mol / L sodium carbonate glycerol solution as the first solution;

[0169] Prepare 10 mL of a 0.6 mol / L magnesium chloride glycerol solution as the second solution;

[0170] The second solution is mixed evenly with the first solution and allowed to stand at 37°C for 24 hours to obtain mineralized glycerol gel.

[0171] Below 50°C, mineralized glycerol gel is a white gel with no obvious fluidity.

[0172] In the mineralized glycerol gel, the mass percentages of minerals, water, and glycerol are 0.4%, 0.6%, and 99%, respectively.

[0173] The viscosity of the mineralized glycerol gel is 32000 mPa·s.

[0174] Example 9

[0175] This embodiment is a specific implementation of the present invention.

[0176] Prepare 50 mL of a 0.08 mol / L sodium sulfate glycerol solution as the first solution;

[0177] Prepare 10 mL of a 0.6 mol / L magnesium chloride glycerol solution as the second solution;

[0178] The second solution is mixed evenly with the first solution and allowed to stand at 37°C for 24 hours to obtain mineralized glycerol gel.

[0179] Below 50°C, mineralized glycerol gel is a white gel with no obvious fluidity.

[0180] In the mineralized glycerol gel, the mass percentages of minerals, water, and glycerol are 0.6%, 1.4%, and 98%, respectively.

[0181] The viscosity of the mineralized glycerol gel is 22000 mPa·s.

[0182] Example 10

[0183] This embodiment is a specific implementation of the present invention.

[0184] Prepare 50 mL of a 0.1 mol / L potassium phosphate glycerol solution as the first solution;

[0185] Prepare 10 mL of a 0.6 mol / L calcium acetate glycerol solution as the second solution;

[0186] The second solution is mixed evenly with the first solution and allowed to stand at 37°C for 24 hours to obtain mineralized glycerol gel.

[0187] Below 50°C, mineralized glycerol gel is a white gel with no obvious fluidity.

[0188] In the mineralized glycerol gel, the mass percentages of minerals, water, and glycerol are 0.9%, 0.5%, and 98.4%, respectively.

[0189] The viscosity of the mineralized glycerol gel is 14500 mPa·s.

[0190] Example 11

[0191] This embodiment is a specific implementation of the present invention.

[0192] Prepare 50 mL of a 0.08 mol / L potassium sulfate glycerol solution as the first solution;

[0193] Prepare 10 mL of a 0.6 mol / L calcium nitrate tetrahydrate glycerol solution as the second solution;

[0194] The second solution is mixed evenly with the first solution and allowed to stand at 37°C for 24 hours to obtain mineralized glycerol gel.

[0195] Below 50°C, mineralized glycerol gel is a white gel with no obvious fluidity.

[0196] In the mineralized glycerol gel, the mass percentages of minerals, water, and glycerol are 0.6%, 0.8%, and 98.6%, respectively.

[0197] Example 12

[0198] This embodiment is a specific implementation of the present invention.

[0199] Prepare 50 mL of a 0.1 mol / L potassium carbonate glycerol solution as the first solution;

[0200] Prepare 10 mL of a 0.4 mol / L magnesium nitrate hexahydrate glycerol solution as the second solution;

[0201] The second solution is mixed evenly with the first solution and allowed to stand at 37°C for 24 hours to obtain mineralized glycerol gel.

[0202] Below 50°C, mineralized glycerol gel is a white gel with no obvious fluidity.

[0203] In the mineralized glycerol gel, the mass percentages of minerals, water, and glycerol are 0.5%, 0.8%, and 98.3%, respectively.

[0204] Example 13

[0205] This embodiment is a specific implementation of the present invention.

[0206] Prepare 50 mL of a 0.1 mol / L ammonium phosphate glycerol solution as the first solution;

[0207] Prepare 10 mL of a 0.5 mol / L magnesium acetate tetrahydrate glycerol solution as the second solution;

[0208] The second solution is mixed evenly with the first solution and allowed to stand at 37°C for 24 hours to obtain mineralized glycerol gel.

[0209] Below 50°C, mineralized glycerol gel is a white gel with no obvious fluidity.

[0210] In the mineralized glycerol gel, the mass percentages of minerals, water, and glycerol are 0.5%, 1.0%, and 98.5%, respectively.

[0211] Example 14

[0212] This embodiment is a specific implementation of the present invention.

[0213] Prepare 50 mL of a 0.12 mol / L ammonium sulfate glycerol solution as the first solution;

[0214] Prepare 10 mL of a 0.7 mol / L calcium acetate monohydrate glycerol solution as the second solution;

[0215] The second solution is mixed evenly with the first solution and allowed to stand at 37°C for 24 hours to obtain mineralized glycerol gel.

[0216] Below 50°C, mineralized glycerol gel is a white gel with no obvious fluidity.

[0217] In the mineralized glycerol gel, the mass percentages of minerals, water, and glycerol are 1.0%, 0.6%, and 98.4%, respectively.

[0218] Example 15

[0219] This embodiment is a specific implementation of the present invention.

[0220] Prepare 50 mL of a 0.12 mol / L ammonium carbonate glycerol solution as the first solution;

[0221] Prepare 10 mL of a 0.9 mol / L magnesium acetate glycerol solution as the second solution;

[0222] The second solution is mixed evenly with the first solution and allowed to stand at 37°C for 24 hours to obtain mineralized glycerol gel.

[0223] Below 50°C, mineralized glycerol gel is a white gel with no obvious fluidity.

[0224] In the mineralized glycerol gel, the mass percentages of minerals, water, and glycerol are 1.6%, 0.5%, and 97.9%, respectively.

[0225] Example 16

[0226] This embodiment is a specific implementation of the present invention.

[0227] Prepare 50 mL of a 0.1 mol / L sodium hydrogen phosphate dodecahydrate glycerol solution as the first solution;

[0228] Prepare 10 mL of a 0.6 mol / L magnesium chloride hexahydrate glycerol solution as the second solution;

[0229] The second solution is mixed evenly with the first solution and allowed to stand at 37°C for 24 hours to obtain mineralized glycerol gel.

[0230] Below 50°C, mineralized glycerol gel is a white gel with no obvious fluidity.

[0231] In the mineralized glycerol gel, the mass percentages of minerals, water, and glycerol are 0.8%, 0.6%, and 97.4%, respectively.

[0232] Example 17

[0233] This embodiment is a specific implementation of the present invention.

[0234] Prepare 50 mL of a 0.15 mol / L potassium hydrogen sulfate solution in glycerol as the first solution;

[0235] Prepare 10 mL of a 0.5 mol / L calcium acetate glycerol solution as the second solution;

[0236] The second solution is mixed evenly with the first solution and allowed to stand at 37°C for 24 hours to obtain mineralized glycerol gel.

[0237] Below 50°C, mineralized glycerol gel is a white gel with no obvious fluidity.

[0238] In the mineralized glycerol gel, the mass percentages of minerals, water, and glycerol are 0.7%, 0.8%, and 98.5%, respectively.

[0239] Example 18

[0240] This embodiment is a specific implementation of the present invention.

[0241] Prepare 50 mL of a 0.12 mol / L ammonium bicarbonate glycerol solution as the first solution;

[0242] Prepare 10 mL of a 0.6 mol / L calcium chloride glycerol solution as the second solution;

[0243] The second solution is mixed evenly with the first solution and allowed to stand at 37°C for 24 hours to obtain mineralized glycerol gel.

[0244] Below 50°C, mineralized glycerol gel is a white gel with no obvious fluidity.

[0245] In the mineralized glycerol gel, the mass percentages of minerals, water, and glycerol are 1%, 0.8%, and 98.2%, respectively.

[0246] Example 19

[0247] This embodiment is a specific implementation of the present invention.

[0248] Prepare 50 mL of a 0.12 mol / L potassium hydrogen sulfate solution in glycerol as the first solution;

[0249] Prepare 10 mL of a 0.8 mol / L magnesium chloride glycerol solution as the second solution;

[0250] The second solution is mixed evenly with the first solution and allowed to stand at 37°C for 24 hours to obtain mineralized glycerol gel.

[0251] Below 50°C, mineralized glycerol gel is a white gel with no obvious fluidity.

[0252] In the mineralized glycerol gel, the mass percentages of minerals, water, and glycerol are 1.2%, 0.6%, and 98.2%, respectively.

[0253] Example 20

[0254] This embodiment is a comparative experiment on the repair materials of the present invention and related technologies in the repair of dental hard tissues.

[0255] A 5×5×3mm enamel block was cut from the center of the labial and buccal surfaces of the crown using a diamond cutter. After resin embedding, the enamel interface was exposed and gradually polished with 800-2000# sandpaper. After cleaning with ethanol, it was air-dried. Then, it was etched with 37% phosphoric acid for 60 seconds, rinsed with deionized water, and air-dried for later use.

[0256] The mineralized glycerol gel prepared in Example 2 and the repair materials in the related technology were respectively coated on the acid-etched enamel interface. The enamel sample to be repaired was immersed in simulated saliva. The sample immersed in simulated saliva was placed in a constant temperature oven at 37°C for 24 hours and then taken out. It was rinsed under running water for 1 minute to remove impurities on the enamel interface repair layer and then air-dried.

[0257] like Figures 4A to 4D As shown, compared to the initial interface after enamel etching, the enamel surface coated with this invention forms a relatively dense hydroxyapatite nanorod mineralization layer in about 1 hour, and the repair layer is even smoother and denser after 24 hours. In contrast, ordinary calcium phosphate cannot effectively repair corroded enamel. Figure 4D ).

[0258] Example 21

[0259] This embodiment is a comparative experiment on the repair materials of the present invention and related technologies in the repair of dental hard tissues.

[0260] Dentin slices 1 mm above the pulp chamber of the tooth crown were cut using a diamond cutter, soaked in 10% EDTA solution for 5 minutes, then sonicated for 10 minutes, and washed with deionized water to obtain dentin samples with exposed tubules.

[0261] The mineralized glycerol gel prepared in Example 2 and the repair materials in the related technology were respectively coated on the acid-etched enamel interface. The enamel sample to be repaired was immersed in simulated saliva. The sample immersed in simulated saliva was placed in a constant temperature oven at 37°C for 24 hours and then taken out. It was rinsed under running water for 1 minute to remove impurities on the enamel interface repair layer and then air-dried.

[0262] like Figures 5A-5B As shown, the dentinal tubules are clearly exposed in the untreated sample. Figure 5A However, the sample surface treated with the prepared mineralized glycerol gel showed a short-term ( Figure 5B This process can produce a dense mineralized layer that covers the dentinal tubules, resulting in a good restorative outcome.

[0263] The technical features of the above embodiments can be combined in any way. For the sake of brevity, not all possible combinations of the technical features in the above embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0264] The embodiments described above are merely illustrative of several implementation methods of this application, and while the descriptions are relatively specific and detailed, they should not be construed as limiting the scope of the invention patent. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of this application, and these all fall within the protection scope of this application. Therefore, the protection scope of this patent application should be determined by the appended claims.

Claims

1. A method for preparing a mineralized glycerol gel, characterized in that, include: The cation source is dissolved in a glycerol solution to obtain a first solution; The anion source is dissolved in a glycerol solution to obtain a second solution; The second solution is added to the first solution and mixed to form a mineralized glycerol gel; The mineralized glycerol gel is gel-like at temperatures between 4 and 38°C. The cation source is one or a combination of calcium ions and magnesium ions, and the anion source is one or a combination of phosphate ions, sulfate ions, and carbonate ions. In the mixed solution, the concentration of the cation source is 0.01~10 mol / L, the concentration of the anion source is 0.01~10 mol / L, and the molar ratio of the cation source to the anion source is 0.1~5:

1. The glycerol solution is either a pure glycerol solution or a glycerol solution containing water. In the aqueous glycerol solution, the water content is less than 50% by mass. Wherein, the viscosity of the mineralized glycerol gel is greater than or equal to 13000 mPa·s; In the mineralized glycerol gel, the mass percentage of minerals is 0.1-5%.

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