CN114939067B - Ceramic corrosive for dentistry and preparation method thereof - Google Patents
Ceramic corrosive for dentistry and preparation method thereof Download PDFInfo
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- CN114939067B CN114939067B CN202210173435.0A CN202210173435A CN114939067B CN 114939067 B CN114939067 B CN 114939067B CN 202210173435 A CN202210173435 A CN 202210173435A CN 114939067 B CN114939067 B CN 114939067B
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Abstract
The invention provides a ceramic corrosive for dentistry and a preparation method thereof. The invention uses strong alkali to assist peroxide, can realize good corrosion effect on dental ceramics, does not contain hydrofluoric acid which is harmful to human body, and the ceramic corrosive agent is an anhydrous system, thus improving the stability of the whole system.
Description
Technical Field
The invention relates to the field of dental restoration, in particular to a ceramic corrosive for dentistry and a preparation method thereof.
Background
The teeth can cause pathological phenomena such as decayed teeth, abrasion, periodontal disease and the like along with time or improper use, and at the moment, the teeth need to be treated or repaired in time. Among them, dental ceramics are glass ceramic materials and products for dental treatment and restoration, and are used in many cases because of their advantages of good hardness, biocompatibility, chemical stability, etc.
The use of dental ceramics brings market to ceramic etchants. At present, in the field of dental restoration, an acid etching agent for ceramics is a commonly used medical instrument. The functional components of the adhesive are hydrofluoric acid, and the other components are water, a gelling agent and pigment. Hydrofluoric acid is a weak acid, has extremely strong corrosiveness, and can strongly corrode metals, glass and objects containing silicon. Such as inhalation of vapors or contact with the skin, can cause burns that are difficult to heal. Hydrofluoric acid is strongly irritating and corrosive to the skin. Hydrogen ions in hydrofluoric acid have dehydration and corrosion effects on human tissues, and fluorine is one of the most active nonmetallic elements. After the skin is contacted with hydrofluoric acid, fluoride ions are continuously dissociated and permeate into deep tissues to dissolve cell membranes, so that the epidermis, dermis, subcutaneous tissue and even muscular layers are liquefied and necrotized. Fluoride ions can also interfere with enolase activity and inhibit the oxygen uptake capacity of skin cells. It is estimated that ingestion of 1.5g hydrofluoric acid by humans may cause immediate death. Inhalation of high concentration hydrofluoric acid mist causes bronchitis and hemorrhagic pulmonary edema. Hydrofluoric acid can also be absorbed transdermally to cause severe poisoning. Therefore, if the ceramic corrosive agent mainly containing hydrofluoric acid is used and operated improperly, the ceramic corrosive agent is liable to cause serious damage to human body.
In addition to hydrofluoric acid, high concentrations of strong bases can also attack ceramic surfaces, for example, sodium hydroxide reacts with ceramic as follows: siO (SiO) 2 +2NaOH＝Na 2 SiO 3 +H 2 O. Strong bases are much less hazardous than hydrofluoric acid, however, the existing strong base etchants generally have a corrosive effect.
Accordingly, the present invention is directed to providing a ceramic etchant that does not use hydrofluoric acid as a raw material while securing the etching effect.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention provides the ceramic corrosive for dentistry and the preparation method thereof, and the ceramic corrosive does not contain hydrofluoric acid with great harm to human health, and has good corrosion effect and stable quality.
The invention provides a dental ceramic corrosive agent which comprises an effective component and a carrier, wherein the effective component consists of a main agent and an auxiliary agent, the main agent is strong alkali, and the auxiliary agent is peroxide.
The present strong alkali corrosive agent does not contain hydrofluoric acid which has great harm to human bodies, but has unsatisfactory corrosion effect, and the invention discovers that better corrosion effect can be obtained by selecting peroxide as the oxidant and matching strong alkali for corroding ceramics.
The strong alkali can be one or more of lithium hydroxide, sodium hydroxide, potassium hydroxide and other strong alkali.
The peroxide can be one or more of hydrogen peroxide, sodium peroxide, carbamide peroxide and the like.
Further, the carrier is an anhydrous system. In order to impart better stability to ceramic etchants, the present invention foregoes the use of an aqueous system, using an anhydrous system as the carrier for the etchant.
In a specific embodiment of the present invention, the carrier comprises one or more of glycerol, polyethylene glycol.
Further preferably, the carrier comprises a mixture of glycerol and polyethylene glycol in a mass ratio of 45:55 to 55:45.
Further, the carrier also comprises a gel forming agent, wherein the gel forming agent can be one or more of xanthan gum, polyvinylpyrrolidone, cellulose gum and carbomer. The addition amount of the sizing agent is 0.01-10 wt%, preferably 1-5 wt%, of the weight of the anhydrous system solvent.
Further, the peroxide is added in an amount of 0.01wt.% to 10wt.%, preferably 1wt.% to 5wt.% of the carrier.
Further, the mass ratio of the strong base to the rest of the components in the ceramic etchant is 0.5:1-1:0.5, preferably 0.7:1-1:0.7.
The invention also provides a preparation method of the dental ceramic corrosive, which comprises the following steps: mixing the carrier with the peroxide, mixing the obtained mixed system with the strong base, and standing.
In a specific embodiment of the invention, the preparation method comprises the following steps:
(1) Mixing glycerol and polyethylene glycol to form a stable and uniform phase;
(2) Adding 0.01-10 wt.% of gelling agent into the liquid obtained in the step (1), stirring for 30-120min, and standing at 10-50 ℃ for 12-72h;
(3) Adding 0.01-10wt.% of peroxide into the liquid obtained in the step (2), standing for 8-72 hours, and stirring for 1-24 hours at 1-200 rmp;
(4) Adding strong alkali into the liquid obtained in the step (3), wherein the mass ratio of the strong alkali to the liquid obtained in the step (3) is 0.5:1-1:0.5, and stirring for 1-24 hours at 1-200 rmp;
(5) And (3) standing the liquid obtained in the step (4) at the temperature of 0-30 ℃ for 1-24 hours to obtain the ceramic corrosive.
Further preferably, the preparation method comprises the steps of:
(1) Taking glycerol and polyethylene glycol with the mass ratio of 45:55-55:45, and stirring to form a stable and uniform phase;
(2) Adding 1-5 wt.% of gelling agent into the liquid obtained in the step (1), stirring for 60-150min, and standing at 25-35 ℃ for 24-48h;
(3) Adding 1-5 wt.% of peroxide into the liquid obtained in the step (2), standing for 12-24 hours, and stirring at 10-50rpm for 1-10 hours;
(4) Adding strong alkali into the liquid obtained in the step (3), wherein the mass ratio of the strong alkali to the liquid obtained in the step (3) is 0.7:1-1:0.7, and stirring at 10-50rpm for 1-10 hours;
(5) And (3) standing the liquid obtained in the step (4) at the temperature of 5-20 ℃ for 8-12 hours to obtain the ceramic corrosive.
The invention provides a ceramic corrosive for dentistry and a preparation method thereof, which utilizes strong alkali to assist with peroxide, can realize good corrosion effect on dentistry ceramic, does not contain hydrofluoric acid which is harmful to human body, and is an anhydrous system, thus improving the stability of the whole system.
Drawings
FIG. 1 is a graph of the surface topography of a ceramic wafer prior to application;
FIGS. 2-10 are graphs showing the surface topography of the ceramic wafers after the application of the etchants of examples 1-9, respectively.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Unless defined otherwise, technical or scientific terms used herein should be given the ordinary meaning as understood by one of ordinary skill in the art to which this invention belongs. The specific techniques or conditions are not identified in the examples and are described in the literature in this field or are carried out in accordance with the product specifications.
Example 1
The embodiment provides a dental ceramic corrosive agent, which is prepared by the following steps:
(1) 100g of solvent is taken, wherein the mass ratio of glycerin to polyethylene glycol is 45:55, and uniform phase is formed through stirring.
(2) 1g of polyvinylpyrrolidone was added to the liquid obtained in the step (1), followed by stirring for 60 minutes, and then, the mixture was allowed to stand in a incubator at 25℃for 24 hours.
(3) To the liquid obtained in the step (2), 1g of carbamide peroxide was added, and after standing for 12 hours, the mixture was stirred at 10rpm for 1 hour.
(4) 70g of sodium hydroxide was added to the liquid obtained in the step (3), and stirred at a speed of 10rpm for 1 hour.
(5) And (3) standing the liquid obtained in the step (4) at the temperature of 5 ℃ for 8 hours to obtain the ceramic corrosive.
Example 2
The embodiment provides a dental ceramic corrosive agent, which is prepared by the following steps:
(1) 100g of solvent is taken, wherein the mass ratio of glycerin to polyethylene glycol is 50:50, and uniform phase is formed through stirring.
(2) 1g of polyvinylpyrrolidone was added to the liquid obtained in the step (1), followed by stirring for 60 minutes, and then, the mixture was allowed to stand in a incubator at 25℃for 24 hours.
(3) To the liquid obtained in the step (2), 1g of carbamide peroxide was added, and after standing for 12 hours, the mixture was stirred at 10rpm for 1 hour.
(4) 70g of sodium hydroxide was added to the liquid obtained in the step (3), and stirred at a speed of 10rpm for 1 hour.
(5) And (3) standing the liquid obtained in the step (4) at the temperature of 5 ℃ for 8 hours to obtain the ceramic corrosive.
Example 3
The embodiment provides a dental ceramic corrosive agent, which is prepared by the following steps:
(1) 100g of solvent is taken, wherein the mass ratio of glycerin to polyethylene glycol is 55:45, and uniform phase is formed through stirring.
(2) 1g of polyvinylpyrrolidone was added to the liquid obtained in the step (1), followed by stirring for 60 minutes, and then, the mixture was allowed to stand in a incubator at 25℃for 24 hours.
(3) To the liquid obtained in the step (2), 1g of carbamide peroxide was added, and after standing for 12 hours, the mixture was stirred at 10rpm for 1 hour.
(4) 70g of sodium hydroxide was added to the liquid obtained in the step (3), and stirred at a speed of 10rpm for 1 hour.
(5) And (3) standing the liquid obtained in the step (4) at the temperature of 5 ℃ for 8 hours to obtain the ceramic corrosive.
Example 4
The embodiment provides a dental ceramic corrosive agent, which is prepared by the following steps:
(1) 100g of solvent is taken, wherein the mass ratio of glycerin to polyethylene glycol is 45:55, and uniform phase is formed through stirring.
(2) 1g of carbomer was added to the liquid obtained in the step (1), and after stirring for 60 minutes, the mixture was allowed to stand in a incubator at 25℃for 24 hours.
(3) To the liquid obtained in the step (2), 1g of carbamide peroxide was added, and after standing for 12 hours, the mixture was stirred at 10rpm for 1 hour.
(4) 70g of sodium hydroxide was added to the liquid obtained in the step (3), and stirred at a speed of 10rpm for 1 hour.
(5) And (3) standing the liquid obtained in the step (4) at the temperature of 5 ℃ for 8 hours to obtain the ceramic corrosive.
Example 5
The embodiment provides a dental ceramic corrosive agent, which is prepared by the following steps:
(1) 100g of solvent is taken, wherein the mass ratio of glycerin to polyethylene glycol is 45:55, and uniform phase is formed through stirring.
(2) 1g of polyvinylpyrrolidone was added to the liquid obtained in the step (1), followed by stirring for 60 minutes, and then, the mixture was allowed to stand in a incubator at 25℃for 24 hours.
(3) To the liquid obtained in the step (2), 1g of hydrogen peroxide was added, and after standing for 12 hours, the mixture was stirred at 10rpm for 1 hour.
(4) 70g of sodium hydroxide was added to the liquid obtained in the step (3), and stirred at a speed of 10rpm for 1 hour.
(5) And (3) standing the liquid obtained in the step (4) at the temperature of 5 ℃ for 8 hours to obtain the ceramic corrosive.
Example 6
The embodiment provides a dental ceramic corrosive agent, which is prepared by the following steps:
(1) 100g of solvent is taken, wherein the mass ratio of glycerin to polyethylene glycol is 45:55, and uniform phase is formed through stirring.
(2) 1g of polyvinylpyrrolidone was added to the liquid obtained in the step (1), followed by stirring for 60 minutes, and then, the mixture was allowed to stand in a incubator at 25℃for 24 hours.
(3) To the liquid obtained in the step (2), 1g of carbamide peroxide was added, and after standing for 12 hours, the mixture was stirred at 10rpm for 1 hour.
(4) 70g of potassium hydroxide was added to the liquid obtained in the step (3), and the mixture was stirred at a speed of 10rpm for 1 hour.
(5) And (3) standing the liquid obtained in the step (4) at the temperature of 5 ℃ for 8 hours to obtain the ceramic corrosive.
Example 7
The embodiment provides a dental ceramic corrosive agent, which is prepared by the following steps:
(1) 100g of solvent is taken, wherein the mass ratio of glycerin to polyethylene glycol is 45:55, and uniform phase is formed through stirring.
(2) 1g of polyvinylpyrrolidone was added to the liquid obtained in the step (1), followed by stirring for 60 minutes, and then, the mixture was allowed to stand in a incubator at 25℃for 24 hours.
(3) To the liquid obtained in the step (2), 5g of carbamide peroxide was added, and after standing for 12 hours, the mixture was stirred at 10rpm for 1 hour.
(4) 70g of sodium hydroxide was added to the liquid obtained in the step (3), and stirred at a speed of 10rpm for 1 hour.
(5) And (3) standing the liquid obtained in the step (4) at the temperature of 5 ℃ for 8 hours to obtain the ceramic corrosive.
Example 8
The embodiment provides a dental ceramic corrosive agent, which is prepared by the following steps:
(1) 100g of solvent is taken, wherein the mass ratio of glycerin to polyethylene glycol is 45:55, and uniform phase is formed through stirring.
(2) 1g of polyvinylpyrrolidone was added to the liquid obtained in the step (1), followed by stirring for 60 minutes, and then, the mixture was allowed to stand in a incubator at 25℃for 24 hours.
(3) To the liquid obtained in the step (2), 1g of carbamide peroxide was added, and after standing for 12 hours, the mixture was stirred at 10rpm for 1 hour.
(4) 130g of sodium hydroxide was added to the liquid obtained in the step (3), and stirred at a speed of 10rpm for 1 hour.
(5) And (3) standing the liquid obtained in the step (4) at the temperature of 5 ℃ for 8 hours to obtain the ceramic corrosive.
Example 9
The embodiment provides a dental ceramic corrosive agent, which is prepared by the following steps:
(1) 100g of solvent is taken, wherein the mass ratio of glycerin to polyethylene glycol is 45:55, and uniform phase is formed through stirring.
(2) 1g of polyvinylpyrrolidone was added to the liquid obtained in the step (1), followed by stirring for 60 minutes, and then, the mixture was allowed to stand in a incubator at 25℃for 24 hours.
(3) 70g of sodium hydroxide was added to the liquid obtained in the step (2), and stirred at a speed of 10rpm for 1 hour.
(4) And (3) standing the liquid obtained in the step (3) at the temperature of 5 ℃ for 8 hours to obtain a finished product.
Corrosion effectiveness verification
The experimental method is as follows:
taking a clean dental ceramic sheet, polishing the ceramic sheet by 1000-mesh sand paper, observing the surface of the ceramic sheet by using an electron microscope, respectively smearing corrosive agents of all embodiments, washing the ceramic sheet cleanly by flowing water after 30 seconds, and observing the surface of the ceramic sheet by using the electron microscope.
As a result, the surface morphology of the ceramic sheet before coating is shown in FIG. 1, and the surface morphology of the ceramic sheet after coating with the corrosive agent of examples 1 to 9 is shown in FIGS. 2 to 10.
From the electron micrograph, it was found that the etchants of examples 1-8 had an etching effect on the dental ceramic sheet, and the surface had a marked trace of etching, which became rough. Whereas the etchant of example 9 has no significant etching effect on the ceramic wafer.
The corrosives of examples 1 to 9 and the commercial aqueous ceramic acid etchants were measured according to the test method for shear strength in YY0518-2009, and the results are shown in table 1.
TABLE 1
As can be seen from the above table, examples 1-8 have a significant ability to enhance the bond shear strength of glass ceramics as does the commercial aqueous ceramic etchants, whereas the product of example 9 does not.
Stability test
The corrosive agents of examples 1 to 8 and the commercial aqueous ceramic acid corrosive agent were stored in an incubator at 60℃for 90 days, and after taking out, the adhesion ability was measured according to YY0518-2009, and the improvement value was calculated. The results of comparing the data before the placement are shown in Table 2.
TABLE 2
As is clear from the above table, the corrosives of examples 1 to 8 were aged at high temperature with no significant decrease in the ability to improve adhesion, whereas the commercially available aqueous ceramic acid etchants were significantly decreased in the ability to improve adhesion. From this, the ceramic etchant of the present invention has higher stability than the aqueous product.
In conclusion, the ceramic corrosive agent provided by the embodiment of the invention can realize a good corrosion effect on dental ceramics by using strong alkali and peroxide, does not contain hydrofluoric acid which is harmful to human bodies, does not contain water, and can improve the stability of the whole system.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (4)
1. The dental ceramic corrosive agent is characterized by comprising an effective component and a carrier, wherein the effective component consists of a main agent and an auxiliary agent, the main agent is strong base, the auxiliary agent is peroxide, the addition amount of the peroxide is 0.01-10 wt.% of the carrier, the mass ratio of the strong base to the rest components in the ceramic corrosive agent is 0.5:1-1:0.5, the carrier is an anhydrous system and comprises a mixture of glycerol and polyethylene glycol, the mass ratio of the glycerol to the polyethylene glycol is 45:55-55:45, and the carrier further comprises a gel forming agent which is one or more of xanthan gum, polyvinylpyrrolidone, cellulose gum and carbomer.
2. The dental ceramic etchant of claim 1, wherein the strong base is one or more of lithium hydroxide, sodium hydroxide, potassium hydroxide;
and/or the peroxide is one or more of hydrogen peroxide, sodium peroxide and carbamide peroxide.
3. A method of preparing a dental ceramic etchant according to claim 1 or 2, comprising: mixing the carrier with the peroxide, mixing the obtained mixed system with the strong base, and standing.
4. A method of preparing a dental ceramic etchant according to claim 3, comprising the steps of:
(1) Mixing glycerol and polyethylene glycol to form a stable and uniform phase;
(2) Adding 0.01-10 wt.% of gelling agent into the liquid obtained in the step (1), stirring for 30-120min, and standing at 10-50 ℃ for 12-72h;
(3) Adding 0.01-10wt.% of peroxide into the liquid obtained in the step (2), standing for 8-72 hours, and stirring for 1-24 hours at 1-200 rmp;
(4) Adding strong alkali into the liquid obtained in the step (3), wherein the mass ratio of the strong alkali to the liquid obtained in the step (3) is 0.5:1-1:0.5, and stirring for 1-24 hours at 1-200 rmp;
(5) And (3) standing the liquid obtained in the step (4) at the temperature of 0-30 ℃ for 1-24 hours to obtain the ceramic corrosive.
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Citations (4)
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| CN1368043A (en) * | 2001-01-27 | 2002-09-11 | 杰西技术公司 | Tooth blenching liquid harmless for dental enamel and its using method |
| CN1368042A (en) * | 2001-01-27 | 2002-09-11 | 杰西技术公司 | Tooth blenching liquid harmless for dental enamel and its using method |
| JP2014148518A (en) * | 2000-01-31 | 2014-08-21 | Ultradent Products Inc | Compositions and methods for whitening and desensitizing teeth |
| CN113995683A (en) * | 2021-09-14 | 2022-02-01 | 深圳爱尔创口腔技术有限公司 | Color-changeable phosphoric acid etching agent and preparation method thereof |
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2022
- 2022-02-24 CN CN202210173435.0A patent/CN114939067B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2014148518A (en) * | 2000-01-31 | 2014-08-21 | Ultradent Products Inc | Compositions and methods for whitening and desensitizing teeth |
| CN1368043A (en) * | 2001-01-27 | 2002-09-11 | 杰西技术公司 | Tooth blenching liquid harmless for dental enamel and its using method |
| CN1368042A (en) * | 2001-01-27 | 2002-09-11 | 杰西技术公司 | Tooth blenching liquid harmless for dental enamel and its using method |
| CN113995683A (en) * | 2021-09-14 | 2022-02-01 | 深圳爱尔创口腔技术有限公司 | Color-changeable phosphoric acid etching agent and preparation method thereof |
Non-Patent Citations (1)
| Title |
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| 牙科热压技术对新型玻璃陶瓷微观结构和化学稳定性的影响;王富 等;功能材料;第40卷(第07期);1192-1195 * |
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