CN115068679A - Anti-tissue adhesion titanium surface modification method for oral implantation, product and application thereof - Google Patents
Anti-tissue adhesion titanium surface modification method for oral implantation, product and application thereof Download PDFInfo
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Abstract
The invention discloses an anti-tissue adhesion titanium surface modification method for oral implantation, a product and application thereof. The surface-modified titanium screw for implantation of the invention can be used as a promising clinical technique, and the screw can be more easily disassembled in the bone implantation removal operation.
Description
Technical Field
The invention belongs to the technical field of titanium metal surface modification for oral implantation, and particularly relates to an anti-tissue adhesion titanium surface modification method for oral implantation, and a product and application thereof.
Background
The dental implant is the first choice of treatment method commonly used in clinic. Usually, the patient is required to wait at least 3 months for the implant procedure after tooth extraction. During this time, the absorption of the alveolar ridge results in a reduction in the width and height of the alveolar ridge. Some variations in the healing process of the alveolar ridge may occur, which may make the installation of the prosthesis-guided implant difficult. A large number of researches show that the tent type tooth implantation technology (TST) is a feasible strategy for increasing the width and height of an alveolar ridge based on a Guided Bone Regeneration (GBR) principle, an implant, a screw or a fixed autologous cortical bone block is implanted into the bone wall of the alveolar ridge bone defect to support and restore the bone defect area, the height and width contour of the alveolar ridge bone defect area is maintained, after bone implantation materials are filled, the height and width of the bone implantation area are maintained, conditions required by bone defect reconstruction are met, and the final bone formation effect is improved. Therefore, space maintenance is a critical factor in successful healing of TST procedures. With the widespread use of TST, a new problem arises. Insertion of titanium screws into cancellous bone can achieve good bone fusion, resulting in difficulty in removal. Therefore, the aim of successfully taking out the supported tent screw after the operation by weakening the bone combination between the titanium screw and the alveolar bone is urgently needed.
However, the high degree of osteogenic integration results in a titanium screw removal process that is too difficult to affect the bone healing microenvironment. Previous studies have focused on the modification of the titanium surface to enhance osseointegration, but neglected the opposite removal process. Therefore, how to solve the problem of the titanium screw removal difficulty caused by the osseointegration between the titanium screw and the alveolar bone is a technical problem to be solved.
Disclosure of Invention
The invention aims to provide a simple, convenient and effective titanium surface modification method for implantation, which is characterized in that a titanium screw is fixed to support and restore the outline of bone defect, and after bone grafting materials are implanted and a surface covering barrier film is covered, the aim of bone regeneration is fulfilled, and the adhesion of protein, cells and tissues can be reduced, so that the width and height of a tooth socket are prevented from being reduced, and the titanium screw can be conveniently and smoothly removed. In this section, as well as in the abstract and the title of the invention of this application, simplifications or omissions may be made to avoid obscuring the purpose of the section, the abstract and the title, and such simplifications or omissions are not intended to limit the scope of the invention.
As one aspect of the invention, the invention provides a method for modifying the surface of titanium for oral implantation for resisting tissue adhesion, which comprises the following steps:
step 1: cleaning titanium metal, putting the titanium metal into a sodium hydroxide solution, heating, drying, soaking the titanium metal in toluene containing 3-Aminopropyltriethoxysilane (APTES), reacting, and baking in an oven;
step 2: in CH 2 Cl 2 Adding Trimethylamine (TEA) and 2-bromoisobutyryl bromide (BIBB), immersing the titanium metal obtained in the step 1, and reacting;
and step 3: dissolving polyethylene glycol dimethacrylate, copper chloride and ligand tri- (N, N-dimethylaminoethyl) amine in methanol/H 2 Continuously introducing N into the mixed solution of O 2 Adding vitamin C to obtain a reaction solution;
and 4, step 4: putting the titanium metal obtained in the step 2 into a container, adding the reaction solution obtained in the step 3, immersing the titanium metal obtained in the step 2 in the reaction solution, adding carboxymethyl methacrylate, sealing the container, reacting, cleaning and drying.
As a preferable scheme of the titanium surface modification method for the oral implant for resisting the tissue adhesion, the method comprises the following steps: in the step 1, the concentration of the sodium hydroxide solution is 10-15M.
As a preferable scheme of the titanium surface modification method for the oral implant for resisting the tissue adhesion, the method comprises the following steps: in the step 1, the heating temperature is 80-100 ℃, and the time is 1-5 h.
As a preferable scheme of the titanium surface modification method for the oral implant for resisting the tissue adhesion, the method comprises the following steps: in the step 1, the baking time is 4-10 hours, and the temperature is 120-130 ℃.
As a preferable scheme of the titanium surface modification method for the oral implant for resisting the tissue adhesion, the method comprises the following steps: in step 1, the concentration of APTES was 1 vol%.
As a preferable scheme of the titanium surface modification method for the oral implant for resisting the tissue adhesion, the method comprises the following steps: in the step 2, the concentration of TEA is 1 vol%, the concentration of BIBB is 1 vol%, and the reaction is carried out by firstly reacting for 2 hours in an ice-water bath environment, then removing the ice-water bath, and continuing to react for 12 hours at room temperature.
As a preferable scheme of the titanium surface modification method for the oral implant for resisting the tissue adhesion, the method comprises the following steps: in step 3, 8.57g of polyethylene glycol dimethacrylate, 17mg of copper chloride and 26.6. mu.L of the ligand tris- (N, N-dimethylaminoethyl) amine were dissolved in 24mL of methanol and H 2 O, wherein methanol: h 2 The volume ratio of O is 1:1, and N is continuously introduced into the mixed solution 2 And 176.2mg of vitamin C was added to obtain a reaction solution; the polymerization degree of the polyethylene glycol dimethacrylate is 300.
As a preferable scheme of the titanium surface modification tissue adhesion method for oral implantation for resisting the adhesion of bone marrow stem cells, the method comprises the following steps: in the step 4, the amount of the added carboxymethyl methacrylate is 200-400 mu L. The invention has the beneficial effects that: the titanium screw prepared by titanium surface modification has the effects of resisting tissue and cell adhesion, and effectively reduces bone formation and bone fusion of the temporary titanium screw before implant implantation. The surface-modified titanium screw for implantation of the invention can be used as a promising clinical technique, and the screw can be more easily disassembled in the bone implantation removal operation.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without inventive exercise. Wherein:
FIG. 1 is a flow diagram of the reaction steps of example 1.
FIG. 2 is a cell viability assay.
FIG. 3 is a graph of bone volume fraction around implants at weeks 4, 8 and 12 observed with micro-CT.
FIG. 4 is a graph showing the trabecular separation around the implant at weeks 4, 8 and 12 using micro-CT.
Figure 5 is a graph of trabecular bone thickness around the implant at 4, 8 and 12 weeks observed with micro-CT.
Fig. 6 shows the removal torque values at 4, 8 and 12 weeks for different implants.
Fig. 7 is a histological section of rat tibia at 4 weeks and 8 weeks after implantation.
Fig. 8 shows the regeneration of bone around the implant at weeks 4 and 8.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with examples are described in detail below.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described and will be readily apparent to those of ordinary skill in the art without departing from the spirit of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.
Furthermore, the references herein to "one embodiment" or "an embodiment" refer to a particular feature, structure, or characteristic that may be included in at least one implementation of the present invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
Example 1:
the first step is as follows: titanium screw or titanium sheet (1 × 1 cm) for oral implantation 2 ) Heating at 90 ℃ for 1h in 10M NaOH solution after ultrasonic cleaning, soaking in APTES/toluene solution (solute APTES concentration is 1 vol%) after drying, reacting at 37 ℃ for 1h, cleaning, and baking in an oven at 120 ℃ for 6 h.
The second step is that: in CH 2 Cl 2 Adding TEA and BIBB to prepare TEA/CH with the final concentration of solute of 1 vol% 2 Cl 2 And BIBB/CH 2 Cl 2 Immersing the titanium screw or titanium sheet sample obtained in the first step in the solution, placing the solution in an ice water bath environment for reaction for 2 hours, then removing the ice water bath, and continuing the reaction for 12 hours at room temperature.
The third step: will be provided with8.57g PEGMA (DP 300), 17mg copper chloride, and 26.6. mu.L tris- (N, N-dimethylaminoethyl) amine (Me6TREN) were dissolved in 24mL methanol/H 2 O, wherein methanol: h 2 The volume ratio of O is 1:1, and N is continuously introduced into the mixed solution 2 And 176.2mg of vitamin C was added to obtain a reaction solution.
The fourth step: and (3) flatly paving the titanium screw or titanium sheet sample obtained in the second step in a container, quickly transferring the reaction solution prepared in the third step into the container to submerge the titanium screw or titanium sheet sample, adding 400 mu L of carboxymethyl methacrylate (CAS 6852-90-0), sealing the container, reacting for 4h in an environment at 37 ℃, and finally cleaning and drying to obtain the functionalized surface of the titanium screw or titanium sheet.
The flow chart of the reaction steps is shown in figure 1.
In the invention, in the step 1, the baking temperature and time can affect the subsequent polymerization reaction, the baking time is less than 4h, which can easily cause the breakage of chemical bonds in the subsequent steps, and the performance of the product can be affected by too long baking time; the concentration of the APTES influences the ammoniation degree of the titanium surface, and further influences the final performance of a product, the concentration of the APTES is optimal to be 1 vol%, the subsequent anti-adhesion effect is reduced due to the fact that the concentration of the APTES is lower than 0.5%, and reaction failure is caused due to hydrolysis of the APTES when the concentration of the APTES is higher than 5%. And the addition of the carboxymethyl methacrylate in the fourth step plays a role in improving the anti-bone marrow mesenchymal stem cell adhesion of the titanium screw and facilitating the removal of the implant, if the carboxymethyl methacrylate is added in the third step, the effect is reduced, and the addition of the carboxymethyl methacrylate in the third step causes advanced polymerization, so that the grafting effect in the fourth step is influenced.
PEGMA has a polymerization degree of 300, and a polymerization degree of more than 700 causes a decrease in the effect of anti-bone marrow stem cell adhesion.
Example 2:
the untreated titanium plate and the titanium plate sample obtained in example 1 were placed on a DSA 100 contact angle measuring system (Kruss, germany), respectively, and the Static Contact Angle (SCA) was measured by dropping a drop of water (2 μ L) onto the prepared surface. The test results are shown in Table 1.
TABLE 1
| Before treatment | Example 1 sample | |
| Contact angle (°) | 65.7 | 25 |
Example 3:
bone marrow mesenchymal stem cells were seeded on 1X 1cm of the stem cells prepared in example 1, respectively 2 Functionalized titanium flakes and untreated titanium flakes were cultured in 0.5mL of medium at a density of 5X 10 3 Individual cell/cm 2 The culture was carried out for 1 day and 3 days, respectively. Culture was performed in the dark for 4 hours using a medium containing 10% Alamar-Blue reagent (Gibco, USA). An aliquot (100L) of the solution extracted from each sample was transferred to a new 96-well plate and read at the absorbance wavelength 540nm and the scattering wavelength of the scattered light in a microplate spectrophotometer (spectrum M2, molecular, usa). 3 samples (n-3) were prepared per group, each sample being replicated in 3 replicates. The results are shown in FIG. 2. FIG. 2 is a graph of cell viability assessed with Alamar Blue on days 1, 3 and 7, respectively. P < 0.05, p < 0.01.
Example 4:
a total of 60 large rats (12 weeks old) were used in this experiment. All procedures were performed under strictly sterile conditions. Before surgery, different implants (example 1 titanium screws and unmodified control titanium screws) were sterilized under uv light. The implant is then placed on the medical aspect of the distal tibia near the metaphysis of the trabecular bone. Implants of different coatings were randomly placed on both legs. The incision was closed with 4-0 sutures. After surgery, each rat was given an intramuscular injection of penicillin for 3 days to prevent possible infection. Plants containing the tibia were harvested at weeks 4, 8, and 12 and various groups were evaluated for osteointegrative ability.
A circle with the radius of 0.5mm away from the surface of the implant is taken as a target area. The measurement of bone volume fraction around the implant, trabecular separation, trabecular thickness was performed on a three-dimensional level using evaluation v6.5-3 software (Scanco Medical, switzerland).
Fig. 3 is the number of bone mass integrals around the implant at weeks 4, 8 and 12 observed with micro-CT, fig. 4 is the trabecular separation around the implant at weeks 4, 8 and 12 observed with micro-CT, and fig. 5 is the trabecular thickness around the implant at weeks 4, 8 and 12 observed with micro-CT. P < 0.05, p < 0.01(n ═ 6). Fig. 7 is a histological section of rat tibia at 4 weeks and 8 weeks after implantation.
Example 5:
to study the biomechanical properties of the bone-implant interface, removal torque tests were performed for the titanium screws of example 1 and for the unmodified control group. The extracted implant sample is trimmed into square bone implant blocks and then secured with a special jig. Subsequently, the specimen was removed from the bone as an axial compression load of 1kn at a rate of 1.0mm/min (trans-head speed) until the bone interface was broken by a commercial materials testing system (CTT 2500; MTS Corp., USA). The stress-strain curve was recorded and the maximum pull-out force during axial compression loading was calculated. 8 samples (n-8) were prepared per group.
Fig. 6 shows the removal torque values at 4, 8 and 12 weeks for different implants p < 0.05, p < 0.01 (n-8). Fig. 8 shows the regeneration of bone around the implant at weeks 4 and 8.
Example 6:
the first step is as follows: titanium screw or titanium sheet (1 × 1 cm) for oral implantation 2 ) Heating at 90 ℃ for 1.5h in 12M NaOH solution after ultrasonic cleaning, drying, soaking in APTES/toluene solution (solute APTES concentration is 1 vol%), reacting at 37 ℃ for 1h, cleaning, and baking in an oven at 130 ℃ for 7 h.
The second step is that: in CH 2 Cl 2 Adding TEA and BIBB, preparing TEA/CH with solute final concentration of 1 vol% 2 Cl 2 And BIBB/CH 2 Cl 2 Immersing the titanium screw or titanium sheet sample obtained in the first step in the solution, placing the solution in an ice water bath environment for reaction for 2 hours, then removing the ice water bath, and continuing the reaction for 12 hours at room temperature.
The third step: 8.57g PEGMA (degree of polymerization 300), 17mg copper chloride, and 26.6. mu.L Me6TREN were dissolved in 24mL methanol/H 2 O, wherein methanol: h 2 The volume ratio of O is 1:1, and N is continuously introduced into the mixed solution 2 And 176.2mg of vitamin C was added to obtain a reaction solution.
The fourth step: and (3) flatly paving the titanium screw or titanium sheet sample obtained in the second step in a container, quickly transferring the reaction solution prepared in the third step into the container to submerge the titanium screw or titanium sheet sample, adding 300 mu L of carboxymethyl methacrylate (CAS 6852-90-0), sealing the container, reacting for 4h in an environment at 37 ℃, and finally cleaning and drying to obtain the functionalized surface of the titanium screw or titanium sheet.
It should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
Claims (10)
1. An anti-tissue adhesion titanium surface modification method for oral implantation is characterized in that: the method comprises the following steps of (1),
step 1: cleaning titanium metal, then placing the titanium metal into a sodium hydroxide solution for heating, drying the titanium metal, then soaking the titanium metal into toluene containing 3-aminopropyl triethoxysilane, reacting the titanium metal and the toluene, and then placing the titanium metal into an oven for baking;
step 2: in CH 2 Cl 2 Adding trimethylamine and 2-bromo isobutyryl bromide, immersing the titanium metal obtained in the step 1, and reacting;
and step 3: mixing polyethylene glycol dimethacrylate and chlorineDissolving copper oxide and aglucon tris- (N, N-dimethylaminoethyl) amine in methanol/H 2 Continuously introducing N into the mixed solution of O 2 Adding vitamin C to obtain a reaction solution;
and 4, step 4: putting the titanium metal obtained in the step 2 into a container, adding the reaction solution obtained in the step 3, immersing the titanium metal obtained in the step 2 in the reaction solution, adding carboxymethyl methacrylate, sealing the container, reacting, cleaning and drying.
2. The method for modifying a titanium surface for dental implantation to resist tissue adhesion of claim 1, wherein: in the step 1, the concentration of the sodium hydroxide solution is 10-15M.
3. The method for modifying a titanium surface for dental implantation to resist tissue adhesion according to claim 1 or 2, wherein: in the step 1, the heating temperature is 80-100 ℃, and the time is 1-5 h.
4. The method for modifying a titanium surface for dental implantation to resist tissue adhesion according to claim 1 or 2, wherein: in the step 1, the baking time is 4-10 hours, and the temperature is 120-130 ℃.
5. The method for modifying a titanium surface for dental implantation to resist tissue adhesion according to claim 1 or 2, wherein: in step 1, the concentration of 3-aminopropyltriethoxysilane was 1 vol%.
6. The method for modifying a titanium surface for dental implantation to resist tissue adhesion according to claim 1 or 2, wherein: in the step 2, the concentration of trimethylamine is 1 vol%, the concentration of 2-bromoisobutyryl bromide is 1 vol%, and the reaction is carried out by firstly reacting for 2 hours in an ice-water bath environment, then removing the ice-water bath, and continuing to react for 12 hours at room temperature.
7. The method for modifying the surface of titanium for dental implantation to resist tissue adhesion as set forth in claim 1 or 2, wherein the titanium is coated on the surface of the titaniumIn the following steps: in step 3, 8.57g of polyethylene glycol dimethacrylate, 17mg of copper chloride and 26.6. mu.L of the ligand tris- (N, N-dimethylaminoethyl) amine were dissolved in 24mL of methanol and H 2 O, wherein methanol: h 2 The volume ratio of O is 1:1, and N is continuously introduced into the mixed solution 2 And 176.2mg of vitamin C was added to obtain a reaction solution; the polymerization degree of the polyethylene glycol dimethacrylate is 300.
8. The method for modifying a titanium surface for dental implantation to resist tissue adhesion of claim 1, wherein: in the step 4, the amount of the added carboxymethyl methacrylate is 200-400 mu L.
9. The product of the process of claim 1.
10. Use of the product of claim 9 in an oral dental implant, wherein: the product has the effects of resisting tissues and cells, and effectively reducing bone formation and bone fusion after a planting operation.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104846354A (en) * | 2015-05-12 | 2015-08-19 | 中国船舶重工集团公司第七二五研究所 | Antifouling and antibacterial treatment method for titanium and titanium alloy surface |
| CN108348404A (en) * | 2015-11-06 | 2018-07-31 | 3M创新有限公司 | Utilize the polymerizable dental composition of the redox of photo-labile transition metal complex |
| US20200347191A1 (en) * | 2019-05-02 | 2020-11-05 | Sonendo, Inc. | Hydrogel materials for obturation |
| CN114272436A (en) * | 2021-12-28 | 2022-04-05 | 陈栋 | Surface chemical modification method for dental implant combined with alveolar bone and application |
-
2022
- 2022-06-30 CN CN202210759270.5A patent/CN115068679B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104846354A (en) * | 2015-05-12 | 2015-08-19 | 中国船舶重工集团公司第七二五研究所 | Antifouling and antibacterial treatment method for titanium and titanium alloy surface |
| CN108348404A (en) * | 2015-11-06 | 2018-07-31 | 3M创新有限公司 | Utilize the polymerizable dental composition of the redox of photo-labile transition metal complex |
| US20200347191A1 (en) * | 2019-05-02 | 2020-11-05 | Sonendo, Inc. | Hydrogel materials for obturation |
| CN114272436A (en) * | 2021-12-28 | 2022-04-05 | 陈栋 | Surface chemical modification method for dental implant combined with alveolar bone and application |
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