Developing coating as well as preparation method and application thereof

Abstract

The invention discloses a developing coating as well as a preparation method and application thereof, and relates to the technical field of medical development, the developing coating comprises the following components in percentage by mass: 45-55% of acrylic resin, 15-25% of n-butyl alcohol, 8-15% of n-hexane, 3-5% of color paste, 2-4% of fumed silica, 8-12% of barium sulfate, 3-8% of nano tungsten oxide, 1-2% of a flatting agent and 1-2% of a wetting agent; wherein the nanometer tungsten oxide and the barium sulfate are compounded to form BaSO4 (at) X / WO3 particles. The developing coating is prepared and obtained, the effects that the developing coating is perfectly attached to the skin of a patient, the developing pattern is clear, use is convenient and fast, errors and surgical wounds are reduced are achieved, the surgical efficiency is improved, and meanwhile operation damage in an operation is effectively reduced; and meanwhile, the problem of developing blind areas or inconsistent contrast caused by excessive concentration of barium sulfate and nano tungsten oxide locally is solved.

Description

Technical Field

[0001] The present application relates to the field of medical imaging technology, and particularly relates to a developing coating, a preparation method thereof, and an application thereof. Background Art

[0002] The developing coating is a material with special functions and has important applications in the orthopedic field. At present, the main components of orthopedic developing coatings include a polymer matrix, a developer, and other additives. The polymer matrix is usually a material with good biocompatibility, such as polymethyl methacrylate (PMMA), etc., which provides adhesiveness and mechanical properties for the coating. The developer is the key component, and commonly used ones include barium sulfate, tantalum oxide, etc. These substances can absorb or scatter rays during imaging examinations, thus forming an obvious contrast on the image.

[0003] Chinese Patent with Publication No. CN115645605B discloses a developing bone cement, a preparation method thereof, and uses thereof. The developing bone cement is composed of a powder containing a developer and a liquid. The developer includes insoluble tungsten compounds. The tungsten compounds are barium tungstate (BaWO4), strontium tungstate (SrWO4), calcium tungstate (CaWO4), cobalt tungstate (CoWO4), cadmium tungstate (CdWO4), ferrous tungstate (FeWO4), and tungsten-containing ceramics including tungsten carbide (WC), tungsten oxide (WO3), tungsten boride (WB2), etc.; and the insoluble tungsten compound is one or more of tungsten carbide, tungsten oxide, and tungsten boride.

[0004] However, although the mass ratio of the tungsten-containing developer in the developing bone cement, its preparation method, and uses is reduced to 10% and a good developing effect is achieved, it still has the problem of toxicity caused by contact with the human body. Moreover, during the addition process of the developer, its dispersibility and stability among the components are also insufficient, which also affects the imaging effect and diagnostic accuracy and needs to be improved. Summary of the Invention

[0005] In view of this, the first object of the present application is to provide a developing coating to achieve the purpose of improving the developing effect and having strong adhesion. The specific scheme is as follows: A developing coating, comprising 45 - 55% by mass of acrylic resin, 15 - 25% of n-butanol, 8 - 15% of n-hexane, 3 - 5% of color paste, 2 - 4% of fumed silica, 8 - 12% of barium sulfate, 3 - 8% of nano tungsten oxide, 1 - 2% of leveling agent, and 1 - 2% of wetting agent; Wherein, the nano tungsten oxide and the barium sulfate are compounded to form BaSO 4 @X / WO 3Particles, and the nano tungsten oxide is ICG-modified nano rod-shaped tungsten oxide, and the ICG-modified nano rod-shaped tungsten oxide is obtained by ICG loading.

[0006] Preferably, the leveling agent is a fluorine-modified acrylic leveling agent, a natural oil leveling agent or a silicone leveling agent.

[0007] Preferably, the wetting agent is a polyether wetting agent, a sugar derivative wetting agent or a siloxane wetting agent.

[0008] Preferably, the BaSO 4 @X / WO 3 The preparation of the particles includes step ① obtaining a dispersion solvent in a water or ethanol solution containing 1-3 wt% PVP; step ② putting the ICG-modified nano rod-shaped tungsten oxide into the dispersion solvent for dispersion to obtain a tungsten oxide suspension containing 1-5 wt%, and putting barium sulfate into the dispersion solvent for dispersion to obtain a barium sulfate suspension containing 10-30 wt%; step ③ dropping the tungsten oxide suspension into the stirred barium sulfate suspension, and continuing to stir for 1-2 h after the dropping is completed to obtain a stirred composite liquid; step ④ standing and aging the stirred composite liquid for 12-24 h, and then obtaining the finished BaSO 4 @X / WO 3 particles.

[0009] The second object of the present application is to provide a preparation method of a developing coating, including the following steps: Step 1, prepare materials: prepare acrylic resin, n-butanol, n-hexane, color paste, fumed silica, barium sulfate, nano tungsten oxide, leveling agent and wetting agent according to the corresponding mass percentages for standby; Step 2, modification treatment: subject barium sulfate to surface activation treatment to obtain activated barium sulfate, obtain ICG-modified nano rod-shaped tungsten oxide by ICG loading of nano tungsten oxide, and then compound the activated barium sulfate with the ICG-modified nano rod-shaped tungsten oxide to form BaSO 4 @X / WO 3 particles for standby; Step 3, mix for standby: mix acrylic resin, n-butanol, n-hexane, color paste, fumed silica, leveling agent and wetting agent evenly, and then add BaSO 4 @X / WO 3 particles and continue to stir and mix evenly to obtain the finished developing coating for standby.

[0010] Preferably, the barium sulfate is surface-activated barium sulfate, and the surface activation treatment is silane coupling agent modification treatment, carboxylation treatment, surfactant modification treatment or mixing with barium chloride in a mass ratio of 1:0.02-0.1 and then subjecting to precipitation treatment.

[0011] Preferably: the silane coupling agent is γ-aminopropyltriethoxysilane, and the modification treatment of the silane coupling agent includes putting γ-aminopropyltriethoxysilane and barium sulfate into ethanol, methanol or DMF, and stirring at 40-80 °C for 2-4 h to obtain surface-activated barium sulfate; the carboxylation treatment includes putting succinic anhydride and barium sulfate into DMSO, and stirring at 60-80 °C for 6-12 h to obtain activated barium sulfate; the precipitation method treatment includes mixing barium sulfate and barium chloride at a mass ratio of 1:0.02-0.1 in deionized water, and then stirring and reacting at 50-70 °C to obtain surface-activated barium sulfate, and the concentrations of barium sulfate and barium chloride are 0.1-0.5 mol / L; the surface activation treatment also includes centrifugation, washing and precipitation, and dry barium sulfate is obtained.

[0012] Preferably: the preparation of the ICG-modified nanorod tungsten oxide includes step ① putting nanorod tungsten oxide into DMSO for dispersion to obtain a tungsten oxide suspension containing 1-2 wt%, and putting ICG into ethanol to obtain a 1-10 wt% ICG solution; step ② mixing the tungsten oxide suspension and the ICG solution and stirring to obtain a preliminary mixed material; step ③ subjecting the preliminary mixed material to ultrasonic treatment, controlling the ultrasonic treatment time to be 1-2 h and the power to be 100-300 W to obtain ICG-modified nanorod tungsten oxide.

[0013] The third object of the present application is to provide an application of a developing coating, including using the developing coating as described above and applying it to the production of a medical orthopedic imaging surgical positioning film.

[0014] Preferably: the medical orthopedic imaging surgical positioning film includes a medical adhesive, a permeable mesh and a polymer imaging film layer; the polymer imaging film layer is formed by coating and photo / thermal curing of the developing coating.

[0015] As can be seen from the above solutions, the present application provides a developing coating, its preparation method and application. The preparation method of the developing coating has the effect of preparing a developing coating with effectively improved imaging effect and strong adhesion, and the application of the developing coating has the effects of perfect fitting with the patient's skin, clear imaging pattern, convenient use, reducing errors and surgical wounds, so as to significantly improve the surgical efficiency while effectively avoiding unnecessary harm to the patient during the operation. The developing coating has the effect of synergistically improving the medical imaging effect of barium sulfate and nano tungsten oxide, while effectively avoiding the problem that barium sulfate blocks the absorption and scattering of near-infrared light by nano tungsten oxide or nano tungsten oxide blocks barium sulfate, and further resulting in the formation of imaging blind areas or inconsistent contrast due to the excessive concentration of barium sulfate and nano tungsten oxide locally. At the same time, using BaSO formed by compounding barium sulfate and nano tungsten oxide 4 @X / WO3 The particles have barium sulfate carried on the nanorod structure of tungsten oxide nanowires, which further promotes the development performance of the developer coating. Description of the Drawings

[0016] In order to more clearly illustrate the technical solutions in the embodiments of the present application or the prior art, the following will briefly introduce the drawings required for the description of the embodiments or the prior art. Obviously, the drawings in the following description are only the embodiments of the present application. For those of ordinary skill in the art, without creative efforts, other drawings can be obtained based on the provided drawings.

[0017] Figure 1 It is a schematic structural diagram of the medical orthopedic imaging surgical positioning film disclosed in the present application.

[0018] Description of the reference numerals: 1, polymer imaging film layer; 2, permeable mesh; 3, medical adhesive. Detailed Embodiments

[0019] The following will clearly and completely describe the technical solutions in the embodiments of the present application with reference to the drawings in the embodiments of the present application. Obviously, the described embodiments are only a part of the embodiments of the present application, rather than all of the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those of ordinary skill in the art without creative efforts belong to the scope of protection of the present application.

[0020] It should be mentioned that directly optimizing and reducing the particle size of tungsten oxide nanowires to achieve the imaging performance and the dispersion performance of tungsten oxide nanowires in the developer coating is obviously a conventional implementation method. However, when the particle size of tungsten oxide nanowires is small enough, it will significantly affect the preparation cost of the developer coating, and when the particle size continues to decrease, it is difficult to substantially improve the imaging performance. Therefore, in the embodiments of the present application, the particle size distribution of barium sulfate is controlled to be 0.5 - 1 μm, and the particle size distribution of tungsten oxide nanowires is 50 - 100 nm.

[0021] At the same time, in the present application, the leveling agent can be a fluorine-modified acrylic leveling agent, a natural oil leveling agent, or a silicone leveling agent. The wetting agent can be a polyether wetting agent, a sugar derivative wetting agent, or a siloxane wetting agent. Details are not elaborated here. Of course, the leveling agent in the embodiments of the present application is BYK-333 purchased from BYK, and the wetting agent is TEGO270 purchased from Degussa.

[0022] The following will specifically describe the developer coating of the present application, its preparation method, and its application.

[0023] A developing coating, comprising 45 - 55% by mass of acrylic resin, 15 - 25% of n-butanol, 8 - 15% of n-hexane, 3 - 5% of color paste, 2 - 4% of fumed silica, 8 - 12% of barium sulfate, 3 - 8% of nano tungsten oxide, 1 - 2% of leveling agent, and 1 - 2% of wetting agent. Among them, nano tungsten oxide and barium sulfate are compounded to form BaSO 4 @X / WO 3 particles. At the same time, the nano tungsten oxide is ICG-modified nano rod-shaped tungsten oxide, and the ICG-modified nano rod-shaped tungsten oxide is obtained by ICG loading.

[0024] It should be noted that the preparation of BaSO 4 @X / WO 3 particles includes the following steps: Step ①, obtaining a dispersion solvent in a water or ethanol solution containing 1 - 3 wt% of PVP; Step ②, putting the ICG-modified nano rod-shaped tungsten oxide into the dispersion solvent for dispersion to obtain a tungsten oxide suspension containing 1 - 5 wt%, and putting barium sulfate into the dispersion solvent for dispersion to obtain a barium sulfate suspension containing 10 - 30 wt%; Step ③, dropping the tungsten oxide suspension into the stirred barium sulfate suspension, and continuing to stir for 1 - 2 h after dropping to obtain a stirred composite liquid; Step ④, standing and aging the stirred composite liquid for 12 - 24 h, and then successively centrifuging, washing with deionized water, and drying to obtain the finished BaSO 4 @X / WO 3 particles.

[0025] A preparation method of a developing coating, comprising the following steps: Step 1, preparing materials: preparing acrylic resin, n-butanol, n-hexane, color paste, fumed silica, barium sulfate, nano tungsten oxide, leveling agent, and wetting agent according to the corresponding mass percentages for standby; Step 2, modification treatment: subjecting barium sulfate to surface active treatment to obtain active barium sulfate, obtaining ICG-modified nano rod-shaped tungsten oxide by ICG loading of nano tungsten oxide, and then compounding the active barium sulfate with the ICG-modified nano rod-shaped tungsten oxide to form BaSO 4 @X / WO 3 particles for standby; Step 3, mixing for standby: mixing acrylic resin, n-butanol, n-hexane, color paste, fumed silica, leveling agent, and wetting agent evenly, adding BaSO 4 @X / WO 3 particles and continuing to stir and mix evenly to obtain the finished developing coating for standby.

[0026] Among them, the barium sulfate is surface-activated barium sulfate. The surface activation treatment is silane coupling agent modification treatment, carboxylation treatment, surfactant modification treatment, or mixing with barium chloride at a mass ratio of 1:0.02 - 0.1 and then treating by precipitation method.

[0027] It should be noted that the silane coupling agent is γ-aminopropyltriethoxysilane, and the silane coupling agent modification treatment includes putting γ-aminopropyltriethoxysilane and barium sulfate into ethanol, methanol or DMF, and stirring at 40 - 80 °C for 2 - 4 h to obtain surface-activated barium sulfate. The carboxylation treatment includes putting succinic anhydride and barium sulfate into DMSO, and stirring at 60 - 80 °C for 6 - 12 h to obtain activated barium sulfate. The precipitation method treatment includes putting barium sulfate and barium chloride at a mass ratio of 1:0.02 - 0.1 into deionized water for mixing, and then stirring and reacting at 50 - 70 °C to obtain surface-activated barium sulfate, and the concentrations of the barium sulfate and barium chloride are 0.1 - 0.5 mol / L; the surface activation treatment also includes centrifugation, washing and precipitation, and obtaining dried barium sulfate. Of course, in the embodiments of the present application, the silane coupling agent modification treatment is mainly adopted, and details are not described here.

[0028] In the embodiments of the present application, the preparation of ICG-modified nanorod tungsten oxide includes step ① putting nanorod tungsten oxide into DMSO for dispersion to obtain a tungsten oxide suspension containing 1 - 2 wt%, and putting ICG into ethanol to obtain a 1 - 10 wt% ICG solution; step ② mixing the tungsten oxide suspension and the ICG solution and stirring to obtain a preliminary mixed material; step ③ subjecting the preliminary mixed material to ultrasonic treatment, controlling the ultrasonic treatment time to be 1 - 2 h and the power to be 100 - 300 W to obtain ICG-modified nanorod tungsten oxide.

[0029] An application of a developing coating, including using the developing coating as described above and applying it to the production of a medical orthopedic developing surgical positioning film. As Figure 1 shown, the medical orthopedic developing surgical positioning film includes a medical adhesive, a permeable mesh and a polymer developing film layer, and the polymer developing film layer is formed by coating the developing coating and curing by light / heat.

[0030] Example 1 A developing coating, including 45% acrylic resin, 15% n-butanol, 15% n-hexane, 5% color paste, 2% fumed silica, 10% barium sulfate, 5% nanometer tungsten oxide, 2% leveling agent and 1% wetting agent by mass percentage. Among them, the nanometer tungsten oxide and barium sulfate are compounded to form BaSO 4 @X / WO 3 particles. At the same time, the nanometer tungsten oxide is ICG-modified nanorod tungsten oxide, and the ICG-modified nanorod tungsten oxide is obtained by ICG loading.

[0031] It should be noted that BaSO 4 @X / WO 3 The preparation of the particles includes the following steps: Step ①: Obtain a dispersion solvent in a water or ethanol solution containing 1 wt% PVP; Step ②: Put the ICG-modified nanorod tungsten oxide into the dispersion solvent for dispersion to obtain a tungsten oxide suspension containing 1 wt%, and put barium sulfate into the dispersion solvent for dispersion to obtain a barium sulfate suspension containing 10 wt%; Step ③: Drop the tungsten oxide suspension into the stirred barium sulfate suspension, and continue stirring for 1 h after the dropping is completed to obtain a stirred composite liquid; Step ④: Let the stirred composite liquid stand for aging treatment for 12 h, and then obtain the finished BaSO 4 @X / WO 3 particles after centrifugation, washing with deionized water and drying in sequence.

[0032] A method for preparing a developing coating includes the following steps: Step 1, Prepare materials: Prepare acrylic resin, n-butanol, n-hexane, color paste, fumed silica, barium sulfate, nano tungsten oxide, leveling agent and wetting agent according to the corresponding mass percentages for standby; Step 2, Modification treatment: Subject barium sulfate to surface activation treatment to obtain activated barium sulfate, carry ICG on nano tungsten oxide to obtain ICG-modified nanorod tungsten oxide, and then compound the activated barium sulfate with the ICG-modified nanorod tungsten oxide to form BaSO 4 @X / WO 3 particles for standby; Step 3, Mix for standby: Mix acrylic resin, n-butanol, n-hexane, color paste, fumed silica, leveling agent and wetting agent evenly, and then add BaSO 4 @X / WO 3 particles and continue to stir and mix evenly to obtain the finished developing coating for standby.

[0033] Among them, the barium sulfate is surface-activated barium sulfate. The surface activation treatment is silane coupling agent modification treatment, carboxylation treatment, surfactant modification treatment or mixing with barium chloride in a mass ratio of 1:0.02 - 0.1 and then subjecting to precipitation treatment.

[0034] It should be noted that the silane coupling agent is γ-aminopropyltriethoxysilane, and the silane coupling agent modification treatment includes putting γ-aminopropyltriethoxysilane and barium sulfate into ethanol, methanol or DMF, and stirring at 40 °C for 2 h to obtain surface-activated barium sulfate.

[0035] In the embodiment of the present application, the preparation of ICG-modified nanorod tungsten oxide includes the following steps: Step ①, put nanorod tungsten oxide into DMSO for dispersion to obtain a tungsten oxide suspension containing 1 wt%, and put ICG into ethanol to obtain a 1 wt% ICG solution; Step ②, mix the tungsten oxide suspension and the ICG solution and stir them to obtain a preliminarily mixed material; Step ③, perform ultrasonic treatment on the preliminarily mixed material, control the ultrasonic treatment time to be 1 h and the power to be 300 W to obtain ICG-modified nanorod tungsten oxide.

[0036] The application of a developing coating includes using the developing coating as described above and applying it to the production of a medical orthopedic imaging surgery positioning film. As Figure 1 shown, the medical orthopedic imaging surgery positioning film includes a medical adhesive, a permeable mesh, and a polymer imaging film layer, and the polymer imaging film layer is formed by coating and photo / thermal curing of the developing coating.

[0037] Example Two A developing coating includes 55% acrylic resin, 17% n-butanol, 8% n-hexane, 3% color paste, 2.8% fumed silica, 8% barium sulfate, 3% nanometer tungsten oxide, 2% leveling agent, and 1.2% wetting agent by mass percentage. Among them, nanometer tungsten oxide and barium sulfate are compounded to form BaSO 4 @X / WO 3 particles. At the same time, the nanometer tungsten oxide is ICG-modified nanorod tungsten oxide, and the ICG-modified nanorod tungsten oxide is obtained by ICG loading.

[0038] It should be noted that the preparation of BaSO 4 @X / WO 3 particles includes the following steps: Step ①, obtain a dispersion solvent in a water or ethanol solution containing 1-3 wt% PVP; Step ②, put the ICG-modified nanorod tungsten oxide into the dispersion solvent for dispersion to obtain a tungsten oxide suspension containing 3 wt%, and put barium sulfate into the dispersion solvent for dispersion to obtain a barium sulfate suspension containing 20 wt%; Step ③, drop the tungsten oxide suspension into the stirred barium sulfate suspension, and continue stirring for 1.5 h after dropping to obtain a stirred composite liquid; Step ④, let the stirred composite liquid stand for aging for 18 h, and then obtain the finished BaSO 4 @X / WO 3 particles after centrifugation, deionized water washing, and drying in sequence.

[0039] A preparation method of a developing coating includes the following steps: Step 1, prepare materials: prepare acrylic resin, n-butanol, n-hexane, color paste, fumed silica, barium sulfate, nanometer tungsten oxide, leveling agent, and wetting agent according to the corresponding mass percentages for standby; Step 2, modification treatment: Treat barium sulfate with a surfactant to obtain activated barium sulfate. Load nano tungsten oxide with ICG to obtain ICG-modified nano rod-shaped tungsten oxide. Then, compound the activated barium sulfate with the ICG-modified nano rod-shaped tungsten oxide to form BaSO 4 @X / WO 3 particles for standby; Step 3, mixing for standby: Mix acrylic resin, n-butanol, n-hexane, color paste, fumed silica, leveling agent, and wetting agent evenly, and then add BaSO 4 @X / WO 3 particles and continue to stir and mix evenly to obtain the finished developing coating for standby.

[0040] Among them, the barium sulfate is surface-activated barium sulfate. The surface activation treatment is silane coupling agent modification treatment, carboxylation treatment, surfactant modification treatment, or mixing with barium chloride in a mass ratio of 1:0.02 - 0.1 and then treating by precipitation method.

[0041] It should be noted that the silane coupling agent is γ-aminopropyltriethoxysilane, and the silane coupling agent modification treatment includes putting γ-aminopropyltriethoxysilane and barium sulfate into ethanol, methanol, or DMF, and stirring at 80°C for 2 h to obtain the surface-activated barium sulfate.

[0042] In the embodiment of the present application, the preparation of the ICG-modified nano rod-shaped tungsten oxide includes Step ① putting the nano rod-shaped tungsten oxide into DMSO for dispersion to obtain a tungsten oxide suspension containing 1 - 2 wt%, and putting ICG into ethanol to obtain a 5 wt% ICG solution; Step ② mixing the tungsten oxide suspension and the ICG solution and stirring to obtain a preliminary mixed material; Step ③ performing ultrasonic treatment on the preliminary mixed material, controlling the ultrasonic treatment time to be 1.5 h and the power to be 200 W to obtain the ICG-modified nano rod-shaped tungsten oxide.

[0043] An application of a developing coating, including using the developing coating as described above and applying it to the production of a medical orthopedic imaging surgical positioning film. As Figure 1 shown, the medical orthopedic imaging surgical positioning film includes a medical adhesive, a permeable mesh, and a polymer imaging film layer, and the polymer imaging film layer is formed by coating the developing coating and then curing by light / heat.

[0044] Example 3 A developing coating, including 46% acrylic resin, 18% n-butanol, 9% n-hexane, 4% color paste, 2% fumed silica, 10% barium sulfate, 8% nano tungsten oxide, 2% leveling agent, and 1% wetting agent by mass percentage. Among them, the nano tungsten oxide and barium sulfate are compounded to form BaSO 4 @X / WO 3Particles. Meanwhile, the nano tungsten oxide is ICG-modified nano rod-shaped tungsten oxide, and the ICG-modified nano rod-shaped tungsten oxide is obtained by ICG loading.

[0045] It should be noted that BaSO 4 @X / WO 3 The preparation of the particles includes the following steps: Step ① obtaining a dispersion solvent in a water or ethanol solution containing 3 wt% PVP; Step ② putting the ICG-modified nano rod-shaped tungsten oxide into the dispersion solvent for dispersion to obtain a tungsten oxide suspension containing 5 wt%, and putting barium sulfate into the dispersion solvent for dispersion to obtain a barium sulfate suspension containing 30 wt%; Step ③ dropping the tungsten oxide suspension into the stirred barium sulfate suspension, and continuing to stir for 2 h after the dropping is completed to obtain a stirred composite liquid; Step ④ standing and aging the stirred composite liquid for 24 h, and then obtaining the finished BaSO 4 @X / WO 3 particles.

[0046] A preparation method of a developing coating includes the following steps: Step 1, preparing materials: preparing acrylic resin, n-butanol, n-hexane, color paste, fumed silica, barium sulfate, nano tungsten oxide, leveling agent and wetting agent according to the corresponding mass percentages for standby; Step 2, modification treatment: subjecting barium sulfate to surface activation treatment to obtain activated barium sulfate, obtaining ICG-modified nano rod-shaped tungsten oxide by ICG loading of nano tungsten oxide, and then compounding the activated barium sulfate with the ICG-modified nano rod-shaped tungsten oxide to form BaSO 4 @X / WO 3 particles for standby; Step 3, mixing for standby: mixing acrylic resin, n-butanol, n-hexane, color paste, fumed silica, leveling agent and wetting agent evenly, and then adding BaSO 4 @X / WO 3 particles and continuing to stir and mix evenly to obtain the finished developing coating for standby.

[0047] Among them, the barium sulfate is surface-activated barium sulfate. The surface activation treatment is silane coupling agent modification treatment, carboxylation treatment, surfactant modification treatment or mixing with barium chloride in a mass ratio of 1:0.1 and then treating by the precipitation method.

[0048] It should be noted that the silane coupling agent is γ-aminopropyltriethoxysilane, and the silane coupling agent modification treatment includes putting γ-aminopropyltriethoxysilane and barium sulfate into DMF and stirring at 60 °C for 3 h to obtain surface-activated barium sulfate.

[0049] In the embodiments of the present application, the preparation of ICG-modified nanorod tungsten oxide includes the following steps: Step ①, put nanorod tungsten oxide into DMSO for dispersion to obtain a tungsten oxide suspension containing 2 wt%, and put ICG into ethanol to obtain a 10 wt% ICG solution; Step ②, mix the tungsten oxide suspension and the ICG solution and stir them to obtain a preliminary mixed material; Step ③, perform ultrasonic treatment on the preliminary mixed material, control the ultrasonic treatment time to be 2 h and the power to be 100 W to obtain ICG-modified nanorod tungsten oxide.

[0050] The application of a developing coating includes using the developing coating as described above and applying it to the production of a medical orthopedic developing surgical positioning film. As Figure 1 shown, the medical orthopedic developing surgical positioning film includes a medical adhesive, a permeable mesh, and a polymer developing film layer, and the polymer developing film layer is formed by coating the developing coating and curing it by light / heat.

[0051] Comparative Example 1 The difference between Comparative Example 1 and Example 2 is that the nano tungsten oxide in Comparative Example 1 is unloaded with ICG nanorod tungsten oxide.

[0052] Comparative Example 2 The difference between Comparative Example 2 and Example 2 is that the barium sulfate in Comparative Example 2 is not surface-activated.

[0053] Comparative Example 3 The difference between Comparative Example 3 and Example 2 is that the barium sulfate and nano tungsten oxide in Comparative Example 3 are directly mixed with the other components without being compounded to form BaSO 4 @X / WO 3 particles.

[0054] Comparative Example 4 The difference between Comparative Example 4 and Example 2 is that the nano tungsten oxide in Comparative Example 4 is unloaded with ICG nanorod tungsten oxide, and the barium sulfate is not surface-activated. And the barium sulfate and nano tungsten oxide are directly mixed with the other components without being compounded to form BaSO 4 @X / WO 3 particles.

[0055] It should be noted that for the above Examples 1 to 3 and Comparative Examples 1 to 3, the imaging performance tests are carried out, and the test methods are as follows: First, control the tube voltage of the X-ray to be 40 kV, 50 kV, and 60 kV respectively for testing.

[0056] Second, control the average thickness of the polymer developing film layer to be 30 - 35 μm, and the actual thickness in the embodiments of the present application is 31.6 ± 0.4 μm.

[0057] The development effects of the performance test results of the above-mentioned examples and comparative examples were evaluated, and were represented by I, II, III, IV, and V respectively.

[0058] Among them, I represents excellent development, II represents good development and no development blind area, III represents general development, IV represents general development and local development blind area, and V represents poor development and local development blind area. The test results are shown in Table 1 below.

[0059] Table 1 Performance test results of the medical orthopedic imaging surgery positioning film

[0060] As can be seen from Table 1 above, the BaSO 4 @X / WO 3 particles obtained by the preparation and compound preparation of barium sulfate and nano tungsten oxide in the examples of the present application have significantly improved the imaging performance of the obtained imaging coating in the application of the polymer imaging film layer, and effectively avoid the problems of imaging blind areas or inconsistent contrast caused by the excessive concentration of barium sulfate and nano tungsten oxide. At the same time, since ICG has the function of further promoting imaging, when it is carried on nano tungsten oxide, it will effectively enhance the imaging ability of nano tungsten oxide and promote the compounding ability with surface-treated barium sulfate. When the surface of barium sulfate is not treated with activity, it will be difficult to achieve a stable and uniformly dispersed surface between barium sulfate and ICG-modified nanorod-shaped tungsten oxide, thus affecting the distribution effect of BaSO 4 @X / WO 3 particles in the imaging coating, and further lead to the problem that the mutual shielding between barium sulfate and nano tungsten oxide affects the imaging effect.

[0061] In summary, the present application provides an imaging coating, its preparation method, and application. The preparation method of the imaging coating has the effect of preparing an imaging coating with effectively improved imaging effect and strong adhesion, and the application of the imaging coating has the effects of perfect fitting with the patient's skin, clear imaging pattern, convenient use, reduced error and surgical wound, thus significantly improving the surgical efficiency while effectively avoiding unnecessary harm to the patient during the surgery. The imaging coating has the effect of synergistically improving the medical imaging effect of barium sulfate and nano tungsten oxide, while effectively avoiding the problem that barium sulfate blocks the absorption and scattering of near-infrared light by nano tungsten oxide or nano tungsten oxide blocks barium sulfate, and further leading to the formation of imaging blind areas or inconsistent contrast due to the excessive concentration of barium sulfate and nano tungsten oxide locally. At the same time, the BaSO 4 @X / WO 3The particles have barium sulfate carried on the nanorod structure of tungsten oxide nanowires, and further promote the development performance of the development coating.

[0062] The "first", "second", "third", "fourth", etc. (if any) involved in this application are used to distinguish similar objects, and do not necessarily describe a specific order or sequence. It should be understood that the data used in this way can be interchanged under appropriate circumstances so that the embodiments described herein can be implemented in an order other than that shown or described herein. In addition, the terms "comprising" and "having" and any variations thereof are intended to cover non-exclusive inclusion. For example, a process, method, or device that includes a series of steps or units does not necessarily have to be limited to those steps or units clearly listed, but may include other steps or units that are not clearly listed or are inherent to these processes, methods, or devices.

[0063] It should be noted that the descriptions involving "first", "second", etc. in this application are only for descriptive purposes and should not be construed as indicating or implying their relative importance or implicitly indicating the quantity of the indicated technical features. Thus, the features defined with "first" and "second" may explicitly or implicitly include at least one such feature. Additionally, the technical solutions between various embodiments can be combined with each other, but it must be based on what can be achieved by those of ordinary skill in the art. When the combination of technical solutions results in contradictions or cannot be achieved, it should be considered that such a combination of technical solutions does not exist and is not within the scope of protection required by this application.

[0064] Specific examples are used herein to illustrate the principles and implementation manners of this application. The descriptions of the above embodiments are only for helping to understand the method and its core idea of this application; at the same time, for those of ordinary skill in the art, according to the idea of this application, there will be changes in the specific implementation manners and application scopes. In summary, the content of this specification should not be construed as a limitation to this application.

Claims

1. A developing coating, characterized in that: The composition comprises 45-55% acrylic resin, 15-25% n-butanol, 8-15% n-hexane, 3-5% color paste, 2-4% fumed silica, 8-12% barium sulfate, 3-8% nano tungsten oxide, 1-2% leveling agent and 1-2% wetting agent in percentage by mass; The nano-tungsten oxide and the barium sulfate are compounded to form BaSO4@X / WO3 particles, and the nano-tungsten oxide is ICG-modified nano-rod-shaped tungsten oxide, which is obtained by ICG loading.

2. A developer coating according to claim 1, characterized in that: The leveling agent is a fluorine-modified acrylic leveling agent, a natural oil leveling agent or a silicone leveling agent.

3. A developer coating according to claim 2, characterized in that: The wetting agent is a polyether wetting agent, a sugar derivative wetting agent or a silicone wetting agent.

4. A developer coating according to claim 3, characterized in that: The preparation of the BaSO4@X / WO3 particles includes the steps of ① adding water or ethanol solution containing 1-3wt% PVP to obtain a dispersion solvent; ② adding ICG-modified nanorod-shaped tungsten oxide into the dispersion solvent to disperse and obtain a tungsten oxide suspension containing 1-5wt%, and adding barium sulfate into the dispersion solvent to disperse and obtain a barium sulfate suspension containing 10-30wt%; ③ adding the tungsten oxide suspension dropwise to the stirred barium sulfate suspension, and continuing to stir for 1-2h after the dropwise addition is completed to obtain a stirred composite liquid; and ④ placing the stirred composite liquid for aging for 12-24h, and then centrifuging, washing with deionized water and drying in sequence to obtain the finished BaSO4@X / WO3 particles.

5. A method for preparing a developer coating, for preparing the developer coating according to any one of claims 1 to 4, characterized in that: The steps include: Step 1, prepare materials: prepare acrylic resin, n-butanol, n-hexane, color paste, fumed silica, barium sulfate, nano tungsten oxide, leveling agent and wetting agent according to corresponding mass percentages for standby use; Step 2, modification treatment: subjecting barium sulfate to surface activity treatment to obtain active barium sulfate, subjecting nano-tungsten oxide to ICG loading to obtain ICG-modified nano-rod-shaped tungsten oxide, and then compounding the active barium sulfate and the ICG-modified nano-rod-shaped tungsten oxide to form BaSO4@X / WO3 particles for standby use; Step 3, mixing for standby use: after the acrylic resin, n-butanol, n-hexane, color paste, fumed silica, leveling agent and wetting agent are evenly mixed, BaSO4@X / WO3 particles are added and the mixture is stirred and mixed to obtain a finished developer coating for standby use.

6. The method for preparing a developer coating according to claim 5, characterized in that: The barium sulfate is barium sulfate treated with surface activity, and the surface activity treatment is silane coupling agent modification treatment, carboxylation treatment, surfactant modification treatment or mixing with barium chloride at a mass ratio of 1:0.02-0.1 and then treated by precipitation method.

7. The method for preparing a developer coating according to claim 6, characterized in that: The silane coupling agent is γ-aminopropyltriethoxysilane, and the silane coupling agent modification treatment includes adding γ-aminopropyltriethoxysilane and barium sulfate into ethanol, methanol or DMF, and stirring at 40-80°C for 2-4h to obtain surface-active barium sulfate; the carboxylation treatment includes adding succinic anhydride and barium sulfate into DMSO, and stirring at 60-80°C for 6-12h to obtain active barium sulfate; the precipitation treatment includes adding barium sulfate and barium chloride in a mass ratio of 1:0.02-0.1 into deionized water for mixing, and stirring at 50-70°C to obtain surface-active barium sulfate, and the concentration of the barium sulfate and the barium chloride is 0.1-0.5 mol / L; the surface activity treatment also includes centrifugation, washing and precipitation, and obtaining dry barium sulfate.

8. The method for preparing a developer coating according to claim 5, characterized in that: The preparation of the ICG-modified nanorod-shaped tungsten oxide comprises the steps of ① dispersing the nanorod-shaped tungsten oxide into DMSO to obtain a tungsten oxide suspension containing 1-2wt%, and dispersing ICG into ethanol to obtain a 1-10wt% ICG solution; ② mixing the tungsten oxide suspension with the ICG solution and stirring to obtain a primary mixed material; and ③ ultrasonically treating the primary mixed material, controlling the ultrasonic treatment time to be 1-2h and the power to be 100-300W, to obtain ICG-modified nanorod-shaped tungsten oxide.

9. An application of a developing coating, characterized in that: The invention comprises adopting the developing coating as claimed in any one of claims 1 to 4 and applying the developing coating to prepare a positioning film for medical orthopedic developing surgery.

10. The use of a developing coating according to claim 9, characterized in that: The medical orthopedic developing surgical positioning film comprises a medical adhesive backing, a permeable mesh film and a polymer developing film layer; the polymer developing film layer is formed by coating the developing coating and light / heat curing.

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