CN112842582B - Surface treatment method for denture implant - Google Patents
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61C—DENTISTRY; APPARATUS OR METHODS FOR ORAL OR DENTAL HYGIENE
- A61C8/00—Means to be fixed to the jaw-bone for consolidating natural teeth or for fixing dental prostheses thereon; Dental implants; Implanting tools
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Abstract
The application relates to the field of denture implants, and particularly discloses a surface treatment method of a denture implant. The surface treatment method of the denture implant comprises the steps of forming holes on the surface of the denture implant and soaking treatment liquid, wherein the treatment liquid is prepared by dissolving modified chitosan in dilute hydrochloric acid, the modified chitosan is beta-cyclodextrin modified chitosan, and the mass ratio of the modified chitosan to the dilute hydrochloric acid is 1: (10-20). The preparation method has the effect of increasing the hydrophilicity of the surface of the denture implant, so that the wound repair time is shortened.
Description
Technical Field
The present application relates to the field of denture implants, and more particularly, to a surface treatment method for denture implants.
Background
With the continuous improvement of living standard and the continuous progress of medical technology, denture implantation has become an important component of oral treatment. In recent years, with the development of dental implantology, it has become common practice in dentistry that implants with a rough surface structure with threads are more easily combined with bone, wherein secondary pit structures produced by large-particle blasting-acid etching are most representative. But the implant surface after the secondary pit treatment produced by large particle blasting-acid etching has poor hydrophilic properties.
The research shows that the surface hydrophobic implant has insufficient bioactivity. After the denture implant with poor hydrophilicity is implanted into a human body, the denture implant gradually becomes a hydrophilic surface under the continuous action of blood and body fluid, but the process generally needs several hours to more than ten hours, and the golden period of healing after surgical wounds is just the time, so the denture implant with poor hydrophilicity is not beneficial to the quick contact and attachment of the blood and the body fluid, and the healing of wound tissues is slower.
Disclosure of Invention
In order to solve the problem that wound tissues are slow to heal, the application provides a surface treatment method of a denture implant.
The surface treatment method for the denture implant adopts the following technical scheme:
the surface treatment method of the denture implant comprises the step of forming a hole on the surface of the denture implant and the step of soaking treatment liquid, wherein the treatment liquid is prepared by dissolving modified chitosan in dilute hydrochloric acid, the modified chitosan is chitosan modified by beta-cyclodextrin, and the mass ratio of the modified chitosan to the dilute hydrochloric acid is 1: (10-20).
By adopting the technical scheme, after being soaked by the treatment solution, the-OH is formed on the surface of the denture implant, so that the surface of the denture implant has hydrophilicity, the denture implant with hydrophilic groups can be quickly infiltrated by blood and body fluid of a person, and the denture implant can be quickly combined with the human body, thereby shortening the wound repair time.
Preferably, the preparation step of the modified chitosan comprises:
s1, dissolving beta-cyclodextrin in an organic solvent to prepare a mixed solution;
s2, adding epichlorohydrin into the mixed solution, then adding a sodium hydroxide solution, stirring, adding chitosan, stirring, filtering, and cleaning to neutrality to obtain modified chitosan;
the mass ratio of the beta-cyclodextrin to the epichlorohydrin to the sodium hydroxide to the chitosan is (2-4): (0.15-0.3): (0.9-1.3): (0.4-0.7), wherein the organic solvent is a mixed solution of dimethyl sulfoxide and isopropanol.
By adopting the technical scheme, the number of hydrophilic groups on the surface of the denture implant is large, the hydrophilicity of the denture implant is improved, the chitosan modified by the beta-cyclodextrin has an affinity behavior with human plasma protein, and the time for healing the wound tissue is further shortened.
Preferably, the mass ratio of the dimethyl sulfoxide to the isopropanol is 1: 1.
by adopting the technical scheme, the purity of the modified chitosan is higher, so that the surface hydrophilicity of the denture implant is improved, the combination of the denture implant and human tissues is promoted, and the possibility of shortening the healing time of wound tissues is improved.
Preferably, the mass ratio of the beta-cyclodextrin to the epichlorohydrin to the sodium hydroxide to the chitosan is 3: (0.2-0.23): 1: (0.4-0.7).
By adopting the technical scheme, other conditions are kept unchanged, and the mass ratio of the beta-cyclodextrin to the epichlorohydrin to the sodium hydroxide to the chitosan is 3: (0.2-0.23): 1: (0.4-0.7), the prepared modified chitosan has better treatment effect on the denture implant, and further promotes the combination of the denture implant and the wound tissue.
Preferably, a surface treatment method of a denture implant includes the steps of:
forming a hole on the surface of the denture implant: carrying out ultrasonic cleaning on the denture implant, carrying out sand blasting treatment, cleaning, soaking the cleaned denture implant in an acid solution for 3-5min, and then carrying out neutralization treatment to obtain the denture implant with a hole formed on the surface, wherein the acid solution is a mixed solution of hydrofluoric acid and nitric acid;
soaking in a treatment solution: soaking the denture implant after pore-forming treatment in the treatment solution for 30-50min, dripping sodium hydroxide solution until the pH of the solution is 8-9, continuing soaking for 20-40min, washing with distilled water, and drying.
By adopting the technical scheme, the hole forming on the surface of the denture implant is rough, and the hydrophilicity of the surface of the denture implant is improved by treating the treatment liquid, so that the denture implant is quickly combined with human tissues.
Preferably, the sand blasting pressure is 0.2-0.4MPa, the granularity of the blasting material is 30-50 meshes, and the sand blasting time is 80-90 s.
By adopting the technical scheme, the sand blasting treatment of the denture implant is realized.
Preferably, the mass ratio of the hydrofluoric acid to the nitric acid is (1-3): 2.
by adopting the technical scheme, the prepared denture implant has more surface holes, so that more surface hydrophilic groups are provided, and the possibility of quickly combining the denture implant with a human body is further improved.
Preferably, the concentration of the hydrofluoric acid is (1.78-2.35) mol/L, and the concentration of the nitric acid is (2.45-3.14) mol/L.
By adopting the technical scheme, the manufactured denture implant has larger surface roughness, so that the surface hydrophilicity of the denture implant is higher.
In summary, the present application has the following beneficial effects:
1. because the treatment solution is prepared by dissolving the modified chitosan in dilute hydrochloric acid, the surface of the denture implant is hydrophilic due to-OH groups formed on the surface of the denture implant, the denture implant with hydrophilic groups can be quickly infiltrated by blood and body fluid of a person, and the denture implant can be quickly combined with the human body, so that the wound repair time is shortened.
2. Beta-cyclodextrin modified chitosan is preferably adopted in the application, so that the denture implant has affinity with human plasma protein, and the time for healing wound tissues is further shortened.
Detailed Description
The following preparations and examples further illustrate the present application in detail.
The raw material sources used in the preparation examples and the examples are shown in the following table 1:
TABLE 1 preparation examples, sources of examples
Preparation example of treating liquid
Preparation example 1
A treatment solution is prepared by dissolving 10g modified chitosan in 200g dilute hydrochloric acid with mass concentration of 0.15.
The modified chitosan is prepared by the following steps:
s1, dissolving 1g of beta-cyclodextrin in 40g of organic solvent to prepare a mixed solution;
s2, dropwise adding 0.32g of epoxy chloropropane into the mixed solution, dropwise adding 1.5g of sodium hydroxide solution with the mass concentration of 0.5g/mL, stirring, adding 0.3g of chitosan, stirring for 1h, filtering, and washing to be neutral to obtain the modified chitosan; the organic solvent was prepared by mixing 30g of dimethyl sulfoxide and 10g of isopropanol.
Preparation examples 2 to 3
Preparation examples 2 to 3 are based on preparation example 1 and differ from preparation example 1 only in that: the mass ratio of the modified chitosan to the diluted hydrochloric acid is different, and the specific mass ratio is shown in table 2.
TABLE 2 preparation examples 1 to 3 Mass ratios of modified Chitosan to dilute hydrochloric acid
| Preparation example | Preparation example 1 | Preparation example 2 | Preparation example 3 |
| Modified chitosan: dilute hydrochloric acid (mass ratio) | 1：20 | 1：10 | 1：15 |
Preparation examples 4 to 6
Preparation examples 4 to 6 are based on preparation example 1, differing from preparation example 1 only in that: the raw materials for preparing the modified chitosan have different proportions, and are shown in table 3.
TABLE 3 preparation examples 4-6 compounding ratio of modified Chitosan
Preparation example 7
Preparation 7 is based on preparation 1 and differs from preparation 1 only in that: the mass ratio of dimethyl sulfoxide to isopropanol is 1: 1.
preparation examples 8 to 10
Preparation examples 8 to 10 are based on preparation example 1, differing from preparation example 1 only in that: the raw materials for preparing the modified chitosan have different proportions, and are shown in table 4.
TABLE 4 preparation examples 8-10 compounding ratios of modified chitosans
Examples
Example 1
A surface treatment method of a denture implant comprises the following steps:
forming a hole on the surface of the denture implant: ultrasonically cleaning the denture implant in distilled water for 15min, wherein the power of ultrasonic cleaning is 0.3W/cm2Then setting the output pressure of an air compressor to be 0.2MPa, selecting a spray material with the granularity of 40 meshes to perform sand blasting treatment on the cleaned denture implant, wherein the sand blasting time is 80s, the sand blasting pressure is 0.3MPa, and the distance between a nozzle and a product is 6 cm; after the sand blasting is finished, removing spray materials on the denture implant by using 0.3MPa compressed air, then cleaning the denture implant by using distilled water, soaking the cleaned denture implant in a mixed solution of 5g of hydrofluoric acid with the concentration of 1.5mol/L and 10g of nitric acid with the concentration of 2.35mol/L for 3min, and then cleaning the acid-etched denture implant by using distilled water until the water attached to the surface of the denture is neutral;
soaking in a treatment solution: and soaking the denture implant subjected to hole forming treatment in a treatment solution for 30min, then dripping a sodium hydroxide solution with the concentration of 0.53g/mL until the pH value of the solution is 8, continuing to soak for 40min, washing with distilled water, and drying to obtain a finished denture implant product, wherein the treatment solution is derived from preparation example 1.
Examples 2 to 4
Examples 2 to 4 are based on example 1 and differ from example 1 only in that: the denture implant surface treatment conditions were varied and are shown in table 5.
TABLE 5 surface treatment conditions of examples 1 to 4
Examples 5 to 7
Examples 5 to 7 are based on example 1 and differ from example 1 only in that: the mass ratio of hydrofluoric acid to nitric acid was varied and is shown in Table 6.
TABLE 6 Mass ratio of hydrofluoric acid to nitric acid
| Examples | Example 5 | Example 6 | Example 7 |
| Hydrofluoric acid: nitric acid (mass ratio) | 1：2 | 1：1 | 3：1 |
Examples 8 to 10
Examples 8 to 10 are based on example 7 and differ from example 1 only in that: the concentrations of hydrofluoric acid and nitric acid used were varied and are shown in Table 7.
TABLE 7 hydrofluoric and nitric acid concentrations
| Examples | Example 8 | Example 9 | Example 10 |
| Hydrofluoric acid (mol/L) | 1.78 | 2.35 | 2.03 |
| Nitric acid (mol/L) | 3.14 | 2.87 | 2.45 |
Examples 11 to 17
Examples 11 to 17 are based on example 1 and differ from example 1 only in that: the source of the treatment solution was varied and is shown in Table 8.
TABLE 8 sources of treatment solutions for examples 11-17
Comparative example
Comparative example 1
Comparative example 1 is based on example 1 and differs from example 1 only in that: and replacing the treatment liquid with dilute hydrochloric acid with the same amount as the treatment liquid to treat the denture implant, wherein the mass fraction of the dilute hydrochloric acid is 10%.
Comparative example 2
Comparative example 2 is based on example 1 and differs from example 1 only in that: the false tooth implant is treated by using the same amount of distilled water instead of the treatment solution.
Comparative example 3
A surface treatment method of a denture implant comprises the following steps:
s1, firstly, soaking the denture implant to be treated in pure acetone for 10min, then taking out the implant, soaking the implant in absolute ethyl alcohol for 5-15 min to remove oil stains and finger prints, then taking out the implant, soaking the implant in deionized water for 15min, and drying for later use; carrying out sand blasting treatment on the cleaned implant, wherein the sand blasting pressure is 0.3MP, the sand blasting time is 60s, and the distance between a nozzle and a product is 5 cm;
s2, after the sand blasting is finished, blowing off large-particle sand materials remained on the surface of the implant by using compressed air with the air pressure of 0.3Mpa, cleaning, drying, and then performing acid etching, wherein the chemical solution for the acid etching contains 35% of sulfuric acid, 20% of hydrochloric acid and the balance of water by volume fraction, the acid etching time is 25min, and after the acid etching is finished, taking out the implant for neutralization treatment and drying.
Performance test
And (3) using deionized water on an easy drop Standard contact angle measuring system at room temperature, carrying out contact angle measurement on the denture implant subjected to surface treatment by adopting a liquid drop method, dropping 8 mu L of liquid on the surface of the titanium sheet, collecting a liquid drop image by adopting a digital imaging technology, and analyzing the shape of the liquid drop by utilizing DSA1 software, wherein the average value of the contact angles of the left side and the right side of the liquid drop is the measured value of the contact angle. Each denture implant was measured for 8 sites, and the average of the contact angles of the 8 sites was recorded as a measurement value.
The test results of examples 1 to 17 and comparative examples 1 to 3 are shown in Table 9.
TABLE 9 contact angles of examples 1 to 17 and comparative examples 1 to 3
| Examples | Contact angle (°) | Examples | Contact angle (°) |
| Example 1 | 14.89 | Example 11 | 12.15 |
| Example 2 | 16.31 | Example 12 | 11.32 |
| Example 3 | 15.64 | Example 13 | 10.61 |
| Example 4 | 16.12 | Example 14 | 9.37 |
| Example 5 | 15.18 | Example 15 | 6.13 |
| Example 6 | 14.87 | Example 16 | 5.03 |
| Example 7 | 14.26 | Example 17 | 4.98 |
| Example 8 | 13.25 | Comparative example 1 | 60.14 |
| Example 9 | 13.98 | Comparative example 2 | 66.25 |
| Example 10 | 14.01 | Comparative example 3 | 70.65 |
The test results of examples 1 to 17 and comparative examples 1 to 3 were analyzed to find that:
data for comparative examples 1-4: the denture implant of example 1 had the smallest contact angle, so example 1 is the best example of examples 1-4.
Examples 5-7 differ from example 1 only in the mass ratio of hydrofluoric acid to nitric acid, and the contact angles of examples 5-7 are all smaller than example 1, indicating that the mass ratio of hydrofluoric acid to nitric acid is (1-3): 2, the surface of the denture implant is provided with more holes, so that the surface of the denture implant is provided with more hydrophilic groups, thereby further improving the possibility of the denture implant being quickly combined with the human body.
Examples 8 to 10 are different from example 7 only in the concentration of hydrofluoric acid and nitric acid used, and the contact angles of examples 8 to 10 are all smaller than example 7, which shows that the surface roughness of the resulting denture implant is large and the surface hydrophilicity of the denture implant is high when the concentration of hydrofluoric acid is (1.78 to 2.35) mol/L and the concentration of nitric acid is (2.45 to 3.14) mol/L.
Compared with example 1, examples 11 to 13 are different only in the mixture ratio of raw materials for preparing modified chitosan, the contact angles of examples 11 to 13 are all smaller than that of example 1, and the mass ratio of beta-cyclodextrin, epichlorohydrin, sodium hydroxide and chitosan is (2-4): (0.15-0.3): (0.9-1.3): (0.4-0.7), the denture implant has more hydrophilic groups on the surface, and the hydrophilicity of the denture implant is improved.
Example 14 differs from example 1 only in that the mass ratio of dimethyl sulfoxide to isopropanol is 1: 1, the contact angle of example 14 is smaller than that of example 1, which shows that when the mass ratio of dimethyl sulfoxide to isopropanol is 1: 1, the surface hydrophilicity of the denture implant is improved, and the combination of the denture implant and human tissues is promoted, so that the possibility of shortening the healing time of wound tissues is improved.
Compared with example 1, the difference between examples 15-17 is only that the raw material ratio for preparing the modified chitosan is different, the contact angles of examples 15-17 are all smaller than that of example 1, which shows that when the mass ratio of beta-cyclodextrin, epichlorohydrin, sodium hydroxide and chitosan is 3: (0.2-0.23): 1: (0.4-0.7), the prepared modified chitosan has better treatment effect on the denture implant, and further promotes the combination of the denture implant and the wound tissue.
Comparative examples 1-2 compared to example 1, comparative example 1 differs from example 1 only in that: the diluted hydrochloric acid with the mass fraction of 10 percent and the same amount as the treatment solution is used for replacing the treatment solution to treat the denture implant, and the comparative example 2 is different from the example 1 only in that: the same amount of distilled water is used for replacing the treatment liquid to treat the denture implant, and the contact angles of the comparative examples 1-2 are far larger than those of the example 1, so that-OH is formed on the surface of the denture implant after the denture implant is soaked in the treatment liquid, the surface of the denture implant is hydrophilic, the denture implant with hydrophilic groups can be quickly infiltrated by blood and body fluid of a person, and the denture implant can be quickly combined with the human body, so that the wound repair time is shortened.
Comparative example 3 is a method of surface-treating a denture implant in recent years, and compared to example 1, the value of the contact angle of comparative example 3 is much higher than that of example 1, and the value of the contact angle of comparative example 3 is higher than 65 °, the surface of which appears to be a hydrophobic surface, which demonstrates that the method of surface-treating a denture implant according to the present application significantly increases the hydrophilicity of the surface of the denture implant, thereby promoting the bonding of the denture implant to human tissue.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (6)
1. The surface treatment method of the denture implant comprises a step of forming a hole on the surface of the denture implant and is characterized by further comprising a step of soaking treatment liquid, wherein the treatment liquid is prepared by dissolving modified chitosan in dilute hydrochloric acid, the modified chitosan is chitosan modified by beta-cyclodextrin, and the mass ratio of the modified chitosan to the dilute hydrochloric acid is 1: (10-20);
the preparation method of the modified chitosan comprises the following steps:
s1, dissolving beta-cyclodextrin in an organic solvent to prepare a mixed solution;
s2, adding epichlorohydrin into the mixed solution, then adding a sodium hydroxide solution, stirring, adding chitosan, stirring, filtering, and cleaning to neutrality to obtain modified chitosan;
the mass ratio of the beta-cyclodextrin to the epichlorohydrin to the sodium hydroxide to the chitosan is (2-4): (0.15-0.3): (0.9-1.3): (0.4-0.7), wherein the organic solvent is a mixed solution of dimethyl sulfoxide and isopropanol;
the mass ratio of the dimethyl sulfoxide to the isopropanol is 1: 1.
2. the surface treatment method for a denture implant according to claim 1, wherein: the mass ratio of the beta-cyclodextrin to the epichlorohydrin to the sodium hydroxide to the chitosan is 3:0.22:1: 0.7.
3. The surface treatment method for a denture implant according to claim 1, comprising the steps of:
forming a hole on the surface of the denture implant: carrying out ultrasonic cleaning on the denture implant, carrying out sand blasting treatment, cleaning, soaking the cleaned denture implant in an acid solution for 3-5min, and then carrying out neutralization treatment to obtain the denture implant with a hole formed on the surface, wherein the acid solution is a mixed solution of hydrofluoric acid and nitric acid;
soaking in a treatment solution: soaking the denture implant after pore-forming treatment in the treatment solution for 30-50min, dripping sodium hydroxide solution until the pH of the solution is 8-9, continuing soaking for 20-40min, washing with distilled water, and drying.
4. The surface treatment method for a denture implant according to claim 3, wherein: the sand blasting pressure is 0.2-0.4MPa, the granularity of the material is 30-50 meshes, and the sand blasting time is 80-90 s.
5. The surface treatment method for a denture implant according to claim 3, wherein: the mass ratio of the hydrofluoric acid to the nitric acid is (1-3): 2.
6. the surface treatment method for a denture implant according to claim 5, wherein: the concentration of the hydrofluoric acid is (1.78-2.35) mol/L, and the concentration of the nitric acid is (2.45-3.14) mol/L.
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