Hydrofluoric acid etchant and method of making same

Abstract

The application relates to the technical field of acid etching agents, and discloses a hydrofluoric acid acid etching agent and a preparation method thereof, wherein the hydrofluoric acid acid etching agent comprises the following components in parts by weight: 70-75 parts of hydrofluoric acid, 40-45 parts of carrageenan, 25-30 parts of a humectant, 35-40 parts of chromium trioxide and 125-130 parts of water. Through the technical scheme, the problems of easy oxidation, complex raw materials, complicated preparation process and low stability of the acid etching agent in the prior art are solved.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of acid etching agent, in particular, relates to a hydrofluoric acid acid etching agent and a preparation method thereof. BACKGROUND

[0002] The bonding technology of tooth is very widely used in clinic, and the treatment of the bonding surface is a very important step in the bonding process. The acid etching agent can form micro voids on the surface of the tooth, increase the bonding area of the tooth surface and the adhesive, and enhance the bonding effect.

[0003] The patent application file with the application number 202111507525.0 provides an acid etching agent and a preparation method and application thereof, including product preparation raw materials and manufacturing method. The raw materials of the product include acid, organic thickening agent, silicon dioxide, curing agent, dye, and water. The manufacturing method is to uniformly stir and mix the raw materials and then perform secondary stirring, and the stirring speed is specified. This invention does not limit the specific components of the dye, and the components of the curing agent used are prone to oxidation, and hexane has certain irritancy.

[0004] The patent application file with the application number 202010430317.4 provides a phosphoric acid acid etching agent and a preparation method thereof, including product formula and preparation method. The product formula includes phosphoric acid, water, fumed silica, glycerol, dodecanol ether sodium sulfate, polyethylene glycol, and methylene blue. The manufacturing method is to mix and stir the raw materials, specify the stirring speed, and then canning. The components of this invention are relatively complex, the operation steps are too many, which will cause waste of materials in the process, and the preparation process is complex.

[0005] The patent application file with the application number 202110187877.6 provides an oral acid etching agent and a preparation method and application thereof, including product formula, application and characteristics. The product formula includes theaflavin, glycolic acid, antioxidant, thickening agent, buffer, surfactant, anti-flocculating agent, and deionized water. This invention has many raw materials and complex components, and the preparation process is prone to uneven stirring problems.

[0006] In summary, the acid etching agent has the problems of easy oxidation, complex raw materials, complicated preparation process, and high difficulty. SUMMARY

[0007] The present application provides a hydrofluoric acid acid etching agent and a preparation method thereof, which solves the problems of easy oxidation, complex raw materials, complicated preparation process, and low stability of the acid etching agent in the related art.

[0008] The technical solution of the present application is as follows:

[0009] A hydrofluoric acid etching agent, comprising the following components by weight: hydrofluoric acid 70-75 parts, carrageenan 40-45 parts, humectant 25-30 parts, chromium sesquioxide 35-40 parts, and water 125-130 parts.

[0010] The raw material components of the hydrofluoric acid etching agent are simple, only five kinds, and the raw material cost is very low, the market is universal, and it is convenient to purchase.

[0011] The release of fluoride ions in hydrofluoric acid can better protect the teeth, mainly because fluoride can effectively prevent dental caries, fluoride ions can combine with the minerals inside the teeth to form fluorinated minerals, which can enhance the ability of the teeth to prevent dental caries and make the teeth enamel stronger. At the same time, fluoride can effectively remineralize demineralized enamel, which also has a certain effect on the early treatment of dental caries.

[0012] Carrageenan has strong gel-forming properties, making the product gel better, and can form a hydrophilic colloid with high elasticity, high transparency and excellent stability. In addition, carrageenan itself has good stability and is not easy to lose its own properties during production.

[0013] As a further technical solution, the humectant includes one or more of glycerol, sorbitol, and polyethylene glycol.

[0014] As a further technical solution, the humectant is glycerol.

[0015] The application also includes a preparation method of a hydrofluoric acid etching agent, comprising the following steps:

[0016] S1, mixing carrageenan and part of the water uniformly to obtain a carrageenan solution;

[0017] S2, mixing hydrofluoric acid, a humectant, chromium sesquioxide, and the remaining water uniformly to obtain a mixture;

[0018] S3, adding the carrageenan solution to the mixture to obtain a hydrofluoric acid etching agent.

[0019] The preparation method of the hydrofluoric acid etching agent is simple and can be completed in three steps without technical difficulty. The product can be prepared by stirring with a stirrer, which can avoid unnecessary waste caused by too complex operation steps. Moreover, the equipment used is simple and convenient, and the product can be prepared by a planetary stirrer according to the stirring time and stirring speed. Finally, the color of the product can be checked to determine whether the mixture is uniform, which is easy to observe.

[0020] As a further technical solution, the amount of the part of water added in S1 is 20-25% of the total weight of water.

[0021] As a further technical solution, the rotation speed during the mixing in S2 is 10-25 rpm, and the mixing time is 30-40 min.

[0022] As a further technical solution, the mixing time in S3 is 10-20 min.

[0023] The working principle and beneficial effects of the present application are as follows:

[0024] 1. The pigment in the present application is chromium sesquioxide, which has multiple effects on the product. Chromium sesquioxide has a distinct color, which can better show whether the product has residues during use, so that residues can be removed in time to avoid damage to the teeth. Moreover, chromium sesquioxide plays a catalytic role in the raw material mixing reaction process, making the reaction more rapid and complete. On the other hand, chromium sesquioxide has a synergistic effect with carrageenan, which makes the hydrogen fluoride etchant prepared by the present application have good stability and oxidation resistance during the reaction process, avoiding oxidation during the process, so that the oxidation rate of the hydrogen fluoride etchant is reduced during storage.

[0025] 2. The carrageenan and glycerol in the present application have a synergistic effect, which can improve the elasticity and water retention of the hydrogen fluoride etchant. The product can maintain its gel strength and moisture under long-term storage. DETAILED DESCRIPTION

[0026] The technical solutions in the embodiments of the present application will be described clearly and completely below in combination with the embodiments of the present application. Obviously, the described embodiments are only a part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor are involved in the scope of protection of the present application.

[0027] Embodiment 1

[0028] A preparation method of a hydrogen fluoride etchant includes the following steps:

[0029] S1, uniformly mix 40 parts of carrageenan and 30 parts of water to obtain a carrageenan solution;

[0030] S2, add 70 parts of hydrogen fluoride, 25 parts of glycerol, 95 parts of chromium sesquioxide, and 95 parts of water into a planetary mixer, set the rotation speed of the mixer to 20 rpm, and stir for 40 min to obtain a mixture;

[0031] S3, add the carrageenan solution into the mixture and continue to stir for 20 min to obtain a hydrogen fluoride etchant.

[0032] Embodiment 2

[0033] A preparation method of a hydrofluoric acid etchant, comprising the following steps:

[0034] S1, 45 parts of carrageenan and 26 parts of water are uniformly mixed to obtain a carrageenan solution;

[0035] S2, 75 parts of hydrofluoric acid, 30 parts of glycerol, 40 parts of chromium trioxide and 104 parts of water are added to a planetary mixer, the rotating speed of the mixer is set to 10 rpm, and stirring is performed for 35 min to obtain a mixture;

[0036] S3, the carrageenan solution is added to the mixture and stirring is continued for 15 min to obtain the hydrofluoric acid etchant.

[0037] Example 3

[0038] A preparation method of a hydrofluoric acid etchant, comprising the following steps:

[0039] S1, 42 parts of carrageenan and 32 parts of water are uniformly mixed to obtain a carrageenan solution;

[0040] S2, 72 parts of hydrofluoric acid, 27 parts of glycerol, 37 parts of chromium trioxide and 96 parts of water are added to a planetary mixer, the rotating speed of the mixer is set to 25 rpm, and stirring is performed for 30 min to obtain a mixture;

[0041] S3, the carrageenan solution is added to the mixture and stirring is continued for 10 min to obtain the hydrofluoric acid etchant.

[0042] Example 4

[0043] Compared with example 3, the difference of example 4 is that the glycerol is 25 parts.

[0044] Example 5

[0045] Compared with example 3, the difference of example 5 is that the glycerol is 30 parts.

[0046] Example 6

[0047] Compared with example 3, the difference of example 6 is that the chromium trioxide is 35 parts.

[0048] Example 7

[0049] Compared with example 3, the difference of example 7 is that the chromium trioxide is 40 parts.

[0050] Comparative example 1

[0051] Compared with example 1, the glycerol in comparative example 1 is replaced by an equal amount of carrageenan, and the others are the same as example 1.

[0052] Comparative example 2

[0053] Comparative Example 2 is the same as Example 1 except that carrageenan is replaced by an equal amount of glycerol.

[0054] Comparative Example 3

[0055] Comparative Example 3 is the same as Example 1 except that CrO3 is replaced by an equal amount of carrageenan.

[0056] Comparative Example 4

[0057] Comparative Example 4 is the same as Example 1 except that carrageenan is replaced by an equal amount of CrO3.

[0058] Comparative Example 5

[0059] Comparative Example 5 is different from Example 3 in that glycerol is 32.5 parts and carrageenan is 32.5 parts.

[0060] Comparative Example 6

[0061] Comparative Example 6 is different from Example 3 in that carrageenan is 30 parts and CrO3 is 30 parts.

[0062] Test Example

[0063] The properties of the hydrofluoric acid etching agent prepared in the above examples and comparative examples were measured, and the test method was as follows:

[0064] Gel strength: The gel strength of the product was measured by a gel strength tester

[0065] Stability: After being placed at 25°C for 24 h, the color, state, and stratification of the product were observed, and the content of the product was measured by acid-base titration reaction;

[0066] Oxidation resistance: After being placed at 25°C for 24 h, the oxidation properties of the product before and after being placed were measured, and the oxidation resistance of the hydrofluoric acid etching agent was measured by a kit (Feiqing Biotechnology Co., Ltd.);

[0067] The measurement results are shown in Tables 1-2.

[0068] Table 1 Test results of the properties of the hydrofluoric acid etching agent prepared in Examples 1-3, 4-5 and Comparative Examples 1-2, 5

[0069]

[0070] Compared with Example 3, Examples 4-5 change the weight parts of glycerol, and Comparative Example 5 changes the mass parts of carrageenan and glycerol, and the gel strength and hydrogel strength of the hydrofluoric acid etching agent prepared in Examples 4-5 and Comparative Example 5 are lower than that of Example 3, which indicates that when the mass ratio of carrageenan and glycerol is 42:27, the gel strength and hydrogel strength of the hydrofluoric acid etching agent can be better improved.

[0071] Compared with Example 1, Comparative Example 1 does not add glycerol, and Comparative Example 2 does not add carrageenan, and the gel strength and hydrogel strength of the hydrofluoric acid etching agent prepared in Comparative Examples 1-2 are lower than that of Example 3, which indicates that the gel strength and hydrogel strength of the hydrofluoric acid etching agent prepared by simultaneously adding glycerol and carrageenan are better than that of adding only any one of glycerol and carrageenan.

[0072] Table 2 Performance test results of the hydrofluoric acid etching agent prepared in Examples 1-3, 6-7 and Comparative Examples 3-4, 6

[0073]

[0074] Compared with Example 3, Examples 6-7 change the weight parts of chromium trioxide, and Comparative Example 6 changes the weight parts of carrageenan and chromium trioxide, and the stability and oxidation resistance of Examples 6-7 and Comparative Example 6 are lower than that of Example 3, which indicates that when the mass ratio of carrageenan and glycerol is 42:27, the stability and oxidation resistance of the hydrofluoric acid etching agent can be better improved.

[0075] Compared with Example 1, Comparative Example 3 does not add chromium trioxide, and Comparative Example 4 does not add carrageenan, and the stability and oxidation resistance of the hydrofluoric acid etching agent prepared in Comparative Examples 3-4 are lower than that of Example 1, which indicates that the stability and oxidation resistance of the hydrofluoric acid etching agent can be improved by simultaneously adding carrageenan and chromium trioxide.

[0076] The above only describes preferred embodiments of the present application and is not intended to limit the present application, and any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application shall be included in the protection scope of the present application.

Claims

1. A hydrofluoric acid etchant, characterized by, The acid etching agent comprises the following components in parts by weight: 72 parts of hydrofluoric acid, 42 parts of carrageenan, 27 parts of glycerol, 37 parts of chromium trioxide, and 128 parts of water.

2. The method for preparing a hydrofluoric acid etching agent according to claim 1, characterized in that, The method comprises the following steps: S1, uniformly mixing carrageenan and part of water to obtain a carrageenan solution; S2, uniformly mixing hydrofluoric acid, glycerol, chromium trioxide, and the remaining water to obtain a mixture; S3, mixing the carrageenan solution into the mixture to obtain the acid etching agent.

3. The method for preparing a hydrofluoric acid etching agent according to claim 2, characterized in that, The amount of the part of water added in S1 is 20-25% of the total weight of water.

4. The method of claim 2, wherein the hydrofluoric acid etchant is prepared by adding 10 to 20 parts by weight of hydrofluoric acid to 80 to 90 parts by weight of water. The mixing speed in S2 is 10-25 rpm, and the mixing time is 30-40 min.

5. The method for preparing a hydrofluoric acid etching agent according to claim 2, characterized in that, The mixing time in S3 is 10-20 min.

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