CN115341203B - Surface polysaccharide modification method and equipment for titanium implant - Google Patents
Surface polysaccharide modification method and equipment for titanium implant Download PDFInfo
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- CN115341203B CN115341203B CN202211008967.5A CN202211008967A CN115341203B CN 115341203 B CN115341203 B CN 115341203B CN 202211008967 A CN202211008967 A CN 202211008967A CN 115341203 B CN115341203 B CN 115341203B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/60—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using alkaline aqueous solutions with pH greater than 8
- C23C22/64—Treatment of refractory metals or alloys based thereon
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61C—DENTISTRY; APPARATUS OR METHODS FOR ORAL OR DENTAL HYGIENE
- A61C5/00—Filling or capping teeth
Abstract
The invention discloses a method and equipment for modifying surface polysaccharide of a titanium implant; the surface polysaccharide modification method of the titanium implant comprises a porous introduction step, wherein a nano porous structure is introduced into the surface of titanium through hydrothermal alkali treatment; a Ti-PDA preparation step, namely introducing a Polydopamine (PDA) anchor layer on the surface of the titanium metal product by using a dopamine aqueous solution; a Ti-EUP-Sr preparing step of immersing Ti-PDA in an EUP-Sr saturated solution for 8-48 hours to obtain a product to which a corresponding amount of EUP-Sr is attached; EUP-Sr is bonded to the surface of Ti-PDA in the form of hydrogen bond and glycosidic bond after soaking, thereby producing a Ti-EUP-Sr product. The surface polysaccharide modification equipment of the titanium implant comprises an annular bracket, a sliding rail arranged on the annular bracket, a clamping device connected with the sliding rail in a sliding way, and a porous introducing device, a Ti-PDA manufacturing device and a Ti-EUP-Sr manufacturing device which are arranged on the outer side of the annular bracket. According to the invention, the Polydopamine (PDA) anchor layer is introduced on the surface of the titanium metal product by using the dopamine aqueous solution, and the surface modification is beneficial to improving the cell compatibility of the titanium implant.
Description
Technical Field
The invention relates to an implant surface improvement method, in particular to a surface polysaccharide modification method and device of a titanium implant.
Background
Dentition defect and dentition defect caused by the influence of various congenital or acquired diseases in oral diseases greatly reduce the life quality of patients; severely affecting the physiological developmental process of the patient; inevitably, a certain influence is caused to the social life of the patient. The current dental implant is used as a main treatment means of the diseases, is gradually accepted by the masses through the development technology and the continuous intensive research and development of clinic for more than 40 years, is accepted by a great number of doctors of dental implant surgeons, and has high reliability in the corresponding technical maturity.
However, during the implantation process, the postoperative implant is often detached, and the reasons for the failure of the implant are that the local inflammatory reaction and the biological inertia and biological activity of the implant can cause insufficient osseointegration, so that a large number of students find the implant through researches. Titanium implants are implanted as an implant in the human body and the immune system of the body responds accordingly over time. Titanium implants do not have a local inflammation-inhibiting effect on their own.
Thus, the ability to inhibit the occurrence of peri-implant inflammation and to alter local osseointegration is two key factors in achieving success of dental implant implantation. There is a need to develop a novel implant surface modification coating that enhances local osseointegration and reduces local inflammatory response to reduce failure rate of the implant and enhance the satisfaction of the patient's use experience.
Disclosure of Invention
The present invention has been made keeping in mind the above problems occurring in the prior art, and an object of the present invention is to provide a method and apparatus for modifying surface polysaccharides of titanium implants.
The aim of the invention is achieved by the following technical scheme:
the surface polysaccharide modification method of the titanium implant comprises the following steps:
a step of introducing a porous structure into the surface of titanium through hydrothermal alkali treatment, immersing the cleaned titanium metal product into 9-11mol/L alkali metal hydroxide solution, and keeping the titanium metal product at 135-145 ℃ for 1-4 hours;
a Ti-PDA preparation step, namely introducing a Polydopamine (PDA) anchor layer on the surface of the titanium metal product by using a dopamine aqueous solution: dissolving dopamine in Tris (Tris reagent) buffer at a concentration of 2mg/mL, ph=8.5; immediately immersing the treated titanium metal product in a dopamine solution for 2-24 hours to obtain corresponding PDA anchors, then flushing to remove residues, and finally preparing the Ti-PDA;
a Ti-EUP-Sr preparing step of immersing Ti-PDA in an EUP-Sr saturated solution for 8-48 hours to obtain a product to which a corresponding amount of EUP-Sr is attached; EUP-Sr is bonded to the surface of Ti-PDA in the form of hydrogen bond and glycosidic bond after soaking, thereby producing a Ti-EUP-Sr product.
Preferably, before the porous introducing step, a polishing step of polishing the titanium metal article stepwise with 240, 600, 800, 1000 and 2000 mesh waterproof sandpaper, followed by polishing with a diamond powder paste, and then ultrasonic cleaning with absolute ethanol, absolute acetone and ultrapure water in this orderWashing; after the porous introducing step, a washing step of cooling the titanium metal product to room temperature, rinsing with pure water twice, and maintaining in NaHCO 3 Placing the solution on a shaking table for 10-14 hours to fully neutralize alkali possibly remained in the surface pores; finally, the titanium metal product is boiled in water for 50 to 70 minutes and then is washed by water; to remove salt slag.
Preferably, in the Ti-PDA manufacturing step, the treated titanium metal product is immersed in the dopamine solution for 15-24 hours; naHCO in the porous introducing step 3 The concentration of the solution is 4-6%.
Preferably, in the step of preparing Ti-EUP-Sr, EUP-Sr (eucommia ulmoides polysaccharide strontium) is dissolved in 10mM Tris-HCl buffer solution to obtain EUP-Sr saturated solution; then soaking Ti-PDA in the solution for 12-24 hours; the EUP-Sr saturated solution in the step of preparing Ti-EUP-Sr is obtained by dissolving EUP-Sr (eucommia polysaccharide strontium) in 10mM Tris-HCl buffer solution; and/or the alkali metal hydroxide solution in the step of introducing the plurality of pores is a NaOH solution or a potassium hydroxide solution.
The orthopedic implant is made of a titanium implant body by the surface polysaccharide modification method.
The invention relates to surface polysaccharide modification equipment of a titanium implant, which comprises an annular bracket, a sliding rail arranged on the annular bracket, a clamping device connected with the sliding rail in a sliding way, and a porous introducing device, a Ti-PDA manufacturing device and a Ti-EUP-Sr manufacturing device which are arranged on the outer side of the annular bracket;
the porous introducing device comprises an alkali metal hydroxide solution immersing station, a rinsing station, a shaking table station, a water boiling station and a flushing station;
the Ti-PDA manufacturing device comprises a dopamine solution station and a flushing station;
the Ti-EUP-Sr manufacturing device comprises an EUP-Sr saturated solution soaking station;
the clamping device comprises a clamping seat which is in sliding connection with the sliding rail, a lifting rod which is arranged below the clamping seat, a clamping mechanism which is arranged below the lifting rod, and a hollowed-out jig which is detachably connected with the clamping mechanism; an inner cavity for accommodating titanium metal products is arranged below the hollowed-out jig.
Preferably, the dopamine solution station is provided with a Tris buffer solution working groove, more than two fixing notches are arranged above the Tris buffer solution working groove, and the fixing notches are used for fixing the hollow jig.
Preferably, the table station is provided with at least two discharging notches, and the fixing notches are used for fixing the hollowed-out jig.
Preferably, the hollow-out jig is provided with a hollow-out part for forming the inner cavity, a cover plate part and a connecting part, wherein the cover plate part and the connecting part are arranged above the hollow-out part, the cover plate part is used for being placed at the notch of each station, and the connecting part is detachably connected with the clamping mechanism.
Preferably, the connecting part is provided with a circumferential groove, and the clamping mechanism is provided with at least two lock tongues corresponding to the circumferential groove and an electromagnet for driving the lock tongues to move in a telescopic manner.
Compared with the prior art, the invention has the beneficial effects that: according to the invention, the Polydopamine (PDA) anchor layer is introduced on the surface of the titanium metal product by using the dopamine aqueous solution, and the surface modification is beneficial to improving the cell compatibility of the titanium implant. Gene expression analysis shows that Ti-EUP-Sr has positive effects on inflammation inhibition, bone formation and angiogenesis. The method for modifying the titanium surface by using the polysaccharide compound can modify EUP-Sr to the Ti surface, and further optimize the current implant. The Ti-eup-sr implant manufactured in this way has good application prospect in dental application, and is a simple and useful method for introducing Ti surface. According to the equipment, the titanium metal product is placed in the hollowed-out jig below the clamping seat through the clamping seat which is in sliding connection with the guide rail, so that the titanium metal product can move among different stations, automatic operation is realized, and the cost and errors of personnel operation are reduced. The clamping mechanism can realize automatic clamping of the hollow jig, and is high in efficiency. The filter is arranged below the container, so that the solution used at each station can be filtered in time, each process effect is guaranteed, the solution can be used for a long time, the replacement times are reduced, and the cost is reduced.
Drawings
FIG. 1 is a schematic view showing the steps of an embodiment of a method for modifying surface polysaccharides of a titanium implant according to the present invention;
FIG. 2 is a scanning electron microscope image of Ti (A), ti-PDA (B), ti-EUP-Sr-12H (C) and Ti-EUP-Sr-24H (D) subjected to hydrothermal alkaline treatment, and EDS result image (E) of strontium content;
FIG. 3 is a FTIR spectrum of EUP-Sr, ti-PDA, ti-EUP-Sr-12H and Ti-EUP-Sr-24H;
FIG. 4 is an enlarged view of water contact angles of Ti (A), ti-PDA (B), 12h modified Ti-EUP-Sr (C) and 24h modified Ti-EUP-Sr (D);
FIG. 5 shows a graph of the results of cell proliferation assays using the MTS method [ RAW264.7 (A), HABOBs (B) and HUVECs (C) with mean.+ -. Standard deviation ].
FIG. 6 is a schematic plan view of an embodiment of a surface polysaccharide modifying apparatus for titanium implants of the present invention;
FIG. 7 is a cross-sectional block diagram of a station such as a dip, soak, etc. in the embodiment of FIG. 6;
FIG. 8 is a cross-sectional block diagram of a station such as a rinse or rinse station in the embodiment of FIG. 6;
FIG. 9 is a cross-sectional view and a partial enlarged view of the center of the clamping seat and the hollow jig in the embodiment of FIG. 6;
fig. 10 is a circuit block diagram of the embodiment of fig. 6.
Reference numerals
10. Annular support 11 slide rail
19. Fixed orifices 20 clamping device
21. Lifting rod of clamping seat 22
29. Porous introducing device for electromagnetic lock pin 30
31. Alkali metal hydroxide solution immersion station
32. Rinsing station
33. Station 34 of cradle
35. Flushing station 40 Ti-PDA making device
41. Dopamine solution station 42 flushing station
50 Ti-EUP-Sr manufacturing device
51 EUP-Sr saturated solution soaking station
60. Clamping mechanism 61 lock tongue
62. Electromagnet 64 spring
70. Hollowed-out part of hollowed-out jig 71
72. Cover plate portion 73 coupling portion
80. Soaking type container 81 container body
82. Valve 83 filter
84. Infusion pump 86 bottom bracket
88. Fixed notch 89 flushing type container
90. Master control circuit 91 presss from both sides material control panel
92. Sliding rail motor of discharging level sensor 93
94. 99 station control circuit of electric push rod
700. Annular groove of inner cavity 731
801. Liquid inlet 802 liquid inlet
831. Liquid leakage switch S titanium metal product
Detailed Description
The technical solutions of the present invention will be clearly and completely described below by the following examples, which are only some of the embodiments of the present invention, but not all of them. 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.
It should be understood that the terms "comprises" and "comprising," when used in this specification and the appended claims, specify the presence of stated features, integers, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and/or groups thereof.
It is also to be understood that the terminology used in the description of the embodiments of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of embodiments of the invention. As used in the specification of the embodiments of the invention and the appended claims, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise.
As shown in the embodiment of fig. 1, the surface polysaccharide modification method of the titanium implant comprises the following steps:
a step of introducing a porous structure into the surface of titanium by hydrothermal alkali treatment, immersing the cleaned titanium metal product in 9-11mol/L NaOH solution, maintaining the temperature at 135-145 ℃ for 1-4 hours, cooling to room temperature, washing the treated titanium metal product twice with pure water, and maintaining the titanium metal product in NaHCO 3 Placing the solution on a shaking table for 10-14 hours to fully neutralize alkali possibly remained in the surface pores; finally, the titanium metal product is boiled in water for 50 to 70 minutes and then is washed by water; to remove salt slag;
a Ti-PDA preparation step, namely introducing a Polydopamine (PDA) anchor layer on the surface of the titanium metal product by using a dopamine aqueous solution: dissolving dopamine in Tris (Tris reagent) buffer at a concentration of 2mg/mL, ph=8.5; immediately immersing the treated titanium metal product in a dopamine solution for 2-24 hours to obtain corresponding PDA anchors, then flushing to remove residues, and finally preparing the Ti-PDA;
a Ti-EUP-Sr preparing step of immersing Ti-PDA in an EUP-Sr saturated solution for 8-48 hours to obtain a product to which a corresponding amount of EUP-Sr is attached; EUP-Sr is bonded to the surface of Ti-PDA in the form of hydrogen bond and glycosidic bond after soaking, thereby producing a Ti-EUP-Sr product.
More specifically, in the Ti-PDA manufacturing step, the treated titanium metal product is immersed in the dopamine solution for 15-24 hours; naHCO in the porous introducing step 3 Concentration of solutionThe degree is 4-6%.
More specifically, in the step of preparing Ti-EUP-Sr, EUP-Sr (eucommia ulmoides polysaccharide strontium) is dissolved in 10mM Tris-HCl buffer to obtain an EUP-Sr saturated solution; the Ti-PDA was then immersed in the solution for 12-24 hours.
More specifically, the EUP-Sr saturated solution in the step of preparing Ti-EUP-Sr is obtained by dissolving EUP-Sr (eucommia ulmoides polysaccharide strontium) in 10mM Tris-HCl buffer.
FIG. 2 shows the EDS results (E) of the strontium content of the scanning electron microscope images of Ti (A), ti-PDA (B), ti-EUP-Sr-12H (C) and Ti-EUP-Sr-24H (D) treated with hydrothermal alkalinity. In fig. 2 (E), the values shown are average±sd. p <0.01 or p <0.0001 represents a significant difference (no Sr signal was detected by Ti group). The EUP-Sr modified titanium is introduced on the surface of the titanium, so that the anti-inflammatory, angiogenic and osteogenic capabilities of the titanium are remarkably improved, and a better osteogenic fusion effect is achieved.
FIG. 3 is an FTIR spectrum of EUP-Sr, ti-PDA, ti-EUP-Sr-12H and Ti-EUP-Sr-24H. Successful attachment of EUP-Sr to titanium surfaces was verified by systematic material characterization. The cell compatibility, cellular inflammatory response, angiogenesis and osteogenic properties of the EUP-Sr modified titanium were evaluated by various in vitro biological studies. By this novel and widespread approach, titanium implants can be loaded with a variety of polysaccharide complexes, including anti-inflammatory and osteoinductive, according to specific clinical needs.
FIG. 4 is a graph of the contact angle of the non-contact on Ti (A), ti-PDA (B), 12h modified Ti-EUP-Sr (C) and 24h modified Ti-EUP-Sr (D). According to the above results, the Ti-EUP-Sr-24H group has a uniform porous surface, and the EUP has a higher EUP-Sr loading amount and also has a higher hydrophilicity. It is also possible to optimize the adjacent microenvironment by releasing the polysaccharide complex, thereby achieving a satisfactory concentration.
It can be seen that the surface of the modified samples containing PDA and EUP-SR was more hydrophilic than the surface of bare Ti. Furthermore, after EUP-Sr modification, the water contact angle was smaller than that of PDA treatment (FIGS. 4c and 4D). SEM and FTIR results in fig. 2 and 3 indicate that Ti-EUP-Sr is porous, with hydroxyl groups present on the surface, both contributing to the increase in wettability. Thus, the improvement of the surface hydrophilicity of Ti-EUP-Sr is attributed to both chemical and physical effects. An increase in hydrophilicity should result in better cell adhesion and viability. EUP-Sr was introduced into Ti surface having anti-inflammatory and osseointegrative properties, and its great improvement in modification and surface properties was confirmed by a combined technique of SEM/EDS, FTIR, ICP-OES and contact angle measurement.
FIG. 5 shows the detection of cell proliferation by MTS method. Cell proliferation experiments show that this surface modification is beneficial to improving the cell compatibility of titanium implants in FIG. 5. Gene expression analysis shows that Ti-EUP-Sr has positive effects on inflammation inhibition, bone formation and angiogenesis. Thus, it was confirmed that the method of modifying the titanium surface with the polysaccharide complex was effective, and that modification of the EUP-Sr to the Ti surface could further optimize the current implant in the above three aspects. The Ti-eup-sr implant made here should be a promising dental application material, the present invention being a simple and useful method of introducing Ti surfaces.
In other embodiments, prior to the porous introducing step, a polishing step of polishing the titanium metal article step by step with 240, 600, 800, 1000 and 2000 mesh waterproof sandpaper, followed by polishing with a diamond powder paste, and then ultrasonic cleaning with absolute ethanol, absolute acetone and ultra-pure water in that order is further included.
In other embodiments, the alkali metal hydroxide solution may also be a potassium hydroxide solution.
The invention also discloses an orthopaedics implant which is processed by adopting the surface polysaccharide modification method in the embodiment. The orthopaedics implant made of the titanium implant can be widely used for products such as implant teeth, skull, artificial bone joints, joint foot plates, broken bone fixing devices, intramedullary nails, artificial heart valves, skull, heart boxes, pacemakers, dental arch wires, vascular stents, artificial limbs, bone marrow needles and the like.
In order to implement the method for modifying the surface polysaccharide of the titanium implant, the inventor further develops corresponding integrated equipment. As shown in fig. 6 to 10, the surface polysaccharide modifying apparatus of the titanium implant of the present invention comprises an annular bracket 10, a slide rail 11 provided to the annular bracket, a clamping device 20 slidably coupled to the slide rail 11, and a porous introducing device 30, a Ti-PDA making device 40 and a Ti-EUP-Sr making device 50 provided to the outside of the annular bracket 10;
the porous introducing device 30 comprises an alkali metal hydroxide solution immersing station 31, a rinsing station 32, a shaking table station 33, a boiling station 34 and a flushing station 35;
the Ti-PDA fabrication apparatus 40 includes a dopamine solution station 41 and a rinse station 42;
the Ti-EUP-Sr manufacturing apparatus 50 includes an EUP-Sr saturated solution immersing station 51;
the clamping device 20 comprises a clamping seat 21 which is in sliding connection with the slide rail 11, a lifting rod 22 which is arranged below the clamping seat 21, a clamping mechanism 60 which is arranged below the lifting rod 22, and a hollowed-out jig 70 which is detachably connected with the clamping mechanism 60; an inner cavity 700 for accommodating the titanium product S is provided below the hollow jig 70.
As shown in fig. 7, the soaking type container 80 with a plurality of fixing slots 88 can be used for soaking, immersing and other stations, such as a dopamine solution station, which is provided with a Tris buffer solution working groove, and more than two fixing slots are arranged above the Tris buffer solution working groove, wherein the fixing slots are used for fixing the hollow-out jig; the utility model also can be a table station, which is provided with at least two discharging notches, and the fixed notches are used for fixing the hollow-out jig. The soaking type container 80 comprises a container body 81, a liquid outlet 801 is arranged below one side of the container body, a liquid inlet 802 is arranged above the other side of the container body, and a valve 82, a filter 83 and an infusion pump 84 are sequentially connected between the liquid outlet and the liquid inlet through pipelines. The solution in which the titanium metal product S is immersed has impurities, and is transported to the filter 83 through a pipe, and the impurities are removed periodically. The solution may be allowed to change after a period of use. Saving the production cost. Further, a drain switch 831 is provided below the filter 83, and when the impurity is more, the drain switch 831 can be turned on to drain the impurity therein, and then the solution in the whole container is replaced. Generally, 5-10 times of impurities can be discharged, and the solution is completely replaced.
As shown in fig. 8, a rinse-type vessel 89 is provided with a fixed slot for use in stations such as rinsing, rinsing and the like. The same construction as the infusion type container 80 shown in fig. 7, except for the smaller size, having only one fixing notch; a spray nozzle 805 is further provided at the position of the liquid inlet 802, and sprays the liquid into the hollow jig 70 in a dispersed state to flush the titanium metal product therein. Further, the lifting rod 22 can be lifted up and down at a speed of one reciprocation of 1 to 5 seconds during washing and rinsing. This has a better flushing effect. Further, the step of lifting the lifting rod comprises an upward moving step of fixing the upper dead center and gradually moving the lower dead center upwards, and a downward moving step of fixing the lower dead center and gradually moving the upper dead center downwards; the changing reciprocating motion can change the position of the titanium metal product in the hollowed-out jig 70, so that a better flushing effect is realized. The cover plates 808 and 809 are provided above the soaking type container 80 and the rinsing type container 89, respectively.
Fig. 9 is a cross-sectional view of the center of the clamping seat and the hollow jig, the hollow jig 70 is provided with a hollow portion 71 for forming an inner cavity 700, a cover plate portion 72 and a coupling portion 73 disposed above the hollow portion 71, the cover plate portion 72 is disposed at a notch of each station, and the coupling portion 73 is detachably coupled with the clamping mechanism 60. The coupling portion 73 is provided with a circumferential groove 731, the clamping mechanism 60 is provided with at least two locking bolts 61 corresponding to the circumferential groove 731, an electromagnet 62 for driving the locking bolts 61 to perform telescopic movement, and a spring 64 for automatically ejecting the locking bolts 61.
As shown in the circuit block diagram of fig. 10, the surface polysaccharide modifying apparatus for titanium implant of the present invention further comprises a main control circuit 90 wired to each station control circuit 99, a clamping control board 91 wirelessly connected to the main control circuit 90, and a plurality of discharge level sensors 92 connected to the main control circuit 90. The nip control board 91 outputs control signals to the slide motor 93, the electric push rod 94 (i.e., the lifter bar 22), and the electromagnet 62 to drive them. The discharging level sensors 92 are arranged on the bearing surfaces or the side surfaces of the rollers 109 of the slide rail 11, and the number of the discharging level sensors corresponds to the fixed working number of the hollowed-out jig. Each station control circuit 99 includes an electrical circuit of the station itself and a communication module connected with the station control circuit, and the communication module realizes communication connection with the main control circuit 90.
More specifically, a discharge level sensor 92, which may be a touch switch or an electromagnetic switch, is provided at a position of the slide rail 11 corresponding to the fixing notch 88 of each station. In order to prevent the clamping seat from moving when the lifting rod works up and down, the side edge of the sliding rail 11 is provided with a fixing hole 19 corresponding to the discharging level sensor 92, and the clamping seat 21 is provided with an electromagnetic lock pin 29 for penetrating the fixing hole 19 so as to fix the clamping seat 21. With the structure, the number of electric devices is reduced as much as possible, and the positioning control of each discharging position can be realized. In particular, the number of discharge levels is greater than the number of stations, as some stations have multiple fixed slots and thus multiple discharge levels. The slide rail motor 93 is fixed on the clamping seat and drives four or at least one roller 931 to work through a transmission mechanism.
More specifically, each of the devices may be formed by adding corresponding components as needed, such as additional heating elements to be heated, a shaker function, a shaker base with a dipping-type container thereon. In order to facilitate the drainage, a bottom bracket 86 can be additionally arranged below the soaking type container and the flushing type container to form an operation space, thereby facilitating the operations of installing a pipeline, replacing a solution and the like. A jig temporary storage station 15 is also arranged between the devices and is used for placing unused hollow jigs. The device also comprises a starting station 13 for loading (i.e. pouring the titanium metal product to be modified into the hollow jig) and a terminating station 14 for taking out (i.e. taking down the hollow jig and pouring out the titanium metal product after modification).
More specifically, for achieving more accurate positioning, there may be two electromagnetic locking pins 29 provided on the clamping seat 21 for penetrating the fixing holes 19, and two fixing holes 19 for each discharging position; the matching surface 291 of the electromagnetic lock pin and the fixing hole is provided with taper, so that the transverse and longitudinal positioning is realized; therefore, a slide rail moving and positioning mechanism for accurate positioning is not needed, and the manufacturing cost and the assembly difficulty of the equipment are reduced.
In summary, the invention uses the dopamine aqueous solution to introduce the Polydopamine (PDA) anchor layer on the surface of the titanium metal product, and the surface modification is beneficial to improving the cell compatibility of the titanium implant. Gene expression analysis shows that Ti-EUP-Sr has positive effects on inflammation inhibition, bone formation and angiogenesis. The method for modifying the titanium surface by using the polysaccharide compound can modify EUP-Sr to the Ti surface, and further optimize the current implant. The Ti-eup-sr implant manufactured in this way has good application prospect in dental application, and is a simple and useful method for introducing Ti surface. According to the equipment, the titanium metal product is placed in the hollowed-out jig below the clamping seat through the clamping seat which is in sliding connection with the guide rail, so that the titanium metal product can move among different stations, automatic operation is realized, and the cost and errors of personnel operation are reduced. The clamping mechanism can realize automatic clamping of the hollow jig, and is high in efficiency. The filter is arranged below the container, so that the solution used at each station can be filtered in time, each process effect is guaranteed, the solution can be used for a long time, the replacement times are reduced, and the cost is reduced.
The foregoing examples are provided to further illustrate the technical contents of the present invention for the convenience of the reader, but are not intended to limit the embodiments of the present invention thereto, and any technical extension or re-creation according to the present invention is protected by the present invention. The protection scope of the invention is subject to the claims.
Claims (9)
1. The surface polysaccharide modification method of the titanium implant is characterized by comprising the following steps:
a step of introducing a porous structure into the surface of titanium through hydrothermal alkali treatment, immersing the cleaned titanium metal product into 9-11mol/L alkali metal hydroxide solution, and keeping the titanium metal product at 135-145 ℃ for 1-4 hours;
a Ti-PDA preparation step, namely introducing a Polydopamine (PDA) anchor layer on the surface of the titanium metal product by using a dopamine aqueous solution: dissolving dopamine in Tris (Tris reagent) buffer at a concentration of 2mg/mL, ph=8.5; immediately immersing the treated titanium metal product in a dopamine solution for 2-24 hours to obtain corresponding PDA anchors, then flushing to remove residues, and finally preparing the Ti-PDA;
a Ti-EUP-Sr preparing step of immersing Ti-PDA in an EUP-Sr saturated solution for 8-48 hours to obtain a product to which a corresponding amount of EUP-Sr is attached; the EUP-Sr is combined on the surface of the Ti-PDA in the form of hydrogen bond and glycosidic bond after soaking, so as to prepare the Ti-EUP-Sr product;
wherein, the above-mentioned each step adopts the integrated apparatus, the said integrated apparatus is surface polysaccharide modifying equipment of the titanium implant, the surface polysaccharide modifying equipment of the said titanium implant includes the annular support, locate the slide rail of the annular support, the clamp material device that couples to said slide rail slidably, and locate the porous introducing device, ti-PDA making device and Ti-EUP-Sr making device outside the said annular support;
the porous introducing device comprises an alkali metal hydroxide solution immersing station, a rinsing station, a shaking table station, a water boiling station and a flushing station;
the Ti-PDA manufacturing device comprises a dopamine solution station and a flushing station;
the Ti-EUP-Sr manufacturing device comprises an EUP-Sr saturated solution soaking station;
the clamping device comprises a clamping seat which is in sliding connection with the sliding rail, a lifting rod which is arranged below the clamping seat, a clamping mechanism which is arranged below the lifting rod, and a hollowed-out jig which is detachably connected with the clamping mechanism; an inner cavity for accommodating titanium metal products is arranged below the hollowed-out jig.
2. The method for modifying surface polysaccharide of titanium implant according to claim 1, wherein:
before the porous introducing step, a polishing step is further included, wherein the polishing step is to polish the titanium metal product step by using 240, 600, 800, 1000 and 2000 mesh waterproof sand paper, then polish the titanium metal product by using diamond powder paste, and then sequentially use absolute ethyl alcohol, absolute acetone and ultrapure water for ultrasonic cleaning;
after the porous introducing step, a washing step of cooling the titanium metal product to room temperature, rinsing with pure water twice, and maintaining in NaHCO 3 Placing the solution on a shaking table for 10-14 hours to fully neutralize alkali possibly remained in the surface pores; finally, titanium is usedBoiling the product in water for 50-70 min, and washing with water; to remove salt slag.
3. The method for modifying surface polysaccharide of titanium implant according to claim 1 or 2, wherein in the step of preparing Ti-PDA, the treated titanium metal product is immersed in a dopamine solution for 15 to 24 hours; naHCO in the porous introducing step 3 The concentration of the solution is 4-6%.
4. The method for modifying surface polysaccharide of titanium implant according to claim 1 or 2, wherein in the step of preparing Ti-EUP-Sr, EUP-Sr (eucommia ulmoides polysaccharide strontium) is dissolved in 10mM Tris-HCl buffer to obtain EUP-Sr saturated solution; then soaking Ti-PDA in the solution for 12-24 hours; the EUP-Sr saturated solution in the step of preparing Ti-EUP-Sr is obtained by dissolving EUP-Sr (eucommia polysaccharide strontium) in 10mM Tris-HCl buffer solution;
and/or the number of the groups of groups,
the alkali metal hydroxide solution in the porous introducing step is NaOH solution or potassium hydroxide solution.
5. The surface polysaccharide modification method of the titanium implant according to claim 1, wherein the dopamine solution station is provided with a Tris buffer solution working groove, more than two fixing notches are arranged above the Tris buffer solution working groove, and the fixing notches are used for fixing the hollow jig.
6. The method for modifying surface polysaccharide of titanium implant according to claim 5, wherein the table station is provided with at least two discharging slots, and the fixing slots are used for fixing the hollow jig.
7. The surface polysaccharide modification method of a titanium implant according to claim 1, wherein the hollow jig is provided with a hollow part for forming the inner cavity, a cover plate part and a connecting part, wherein the cover plate part and the connecting part are arranged above the hollow part, the cover plate part is arranged at a notch of each station, and the connecting part is detachably connected with the clamping mechanism.
8. The method for modifying surface polysaccharide of titanium implant according to claim 7, wherein the coupling part is provided with a circumferential groove, and the clamping mechanism is provided with at least two lock tongues corresponding to the circumferential groove, and an electromagnet for driving the lock tongues to move in a telescopic manner.
9. An orthopedic implant employing a titanium implant characterized in that the titanium implant is processed by the surface polysaccharide modification method of claim 1.
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