Platinum complex catalyst and preparation method thereof

Abstract

The invention discloses a platinum complex catalyst and a preparation method thereof, and the preparation method of the platinum complex catalyst comprises the following steps: loading a platinum complex and silicon resin to form a silicon resin loaded platinum complex; mixing the silicon resin loaded platinum complex with a first emulsifier to form silicon resin loaded platinum complex microspheres; mixing the silicon resin loaded platinum complex microspheres with a wall material and a second emulsifier to form a microcapsule suspension; and carrying out post-treatment on the microcapsule suspension to form the microcapsule platinum complex catalyst. The microcapsule platinum complex catalyst needs to be activated to release effective components under specific conditions; therefore, when the microcapsule platinum complex catalyst is used for synthesizing organic silicon, the microcapsule platinum complex catalyst can be stored together with a cross-linking agent, and the operation time is long.

Description

Technical Field

[0001] The present application relates to the field of catalyst technology, and in particular to a platinum complex catalyst and a preparation method thereof. Background Art

[0002] Silicone and modified silicone resin products are widely used in defense and military industry, electrical industry, leather industry, light industrial products, rubber and plastics, food hygiene and other industries due to their excellent thermal oxidation stability, electrical insulation performance, weather resistance, waterproofness, salt spray resistance, mildew resistance, biocompatibility and other properties, playing an irreplaceable role.

[0003] Platinum complex catalysts play a vital role in the synthesis of organosilicon. Summary of the invention

[0004] The platinum complex catalyst and preparation method thereof provided in the present application are in a microcapsule state. The platinum complex catalyst needs to be activated under specific conditions to release the effective ingredients; therefore, when the platinum complex catalyst is used to synthesize silicone, the platinum complex catalyst can be stored together with the cross-linking agent and has a longer operating time.

[0005] In order to solve the above technical problems, the first technical solution provided in the present application is: to provide a method for preparing a platinum complex catalyst, comprising: loading a platinum complex with a silicone resin to form a silicone resin-loaded platinum complex; mixing the silicone resin-loaded platinum complex with a first emulsifier to form silicone resin-loaded platinum complex microspheres; mixing the silicone resin-loaded platinum complex microspheres with a wall material and a second emulsifier to form a microcapsule suspension; and post-treating the microcapsule suspension to form a microcapsule platinum complex catalyst.

[0006] In one embodiment, the step of mixing the silicone-supported platinum complex with the first emulsifier to form silicone-supported platinum complex microspheres includes: mixing the silicone-supported platinum complex with the first emulsifier, stirring and emulsifying at 60° C.-100° C. for 20 min-30 min to form silicone-supported platinum complex microspheres.

[0007] In one embodiment, the amount of the first emulsifier added is 1%-20% of the mass of the silicone-supported platinum complex.

[0008] In one embodiment, the first emulsifier includes at least one of carboxymethyl cellulose, polyvinyl alcohol, polyacrylates, and hydroxyethyl cellulose.

[0009] In one embodiment, the step of mixing silicone-supported platinum complex microspheres with a wall material and a second emulsifier to form a microcapsule suspension includes: mixing silicone-supported platinum complex microspheres with a wall material and a second emulsifier, stirring and emulsifying at 45°C-55°C for 30min-40min, and then heating to 50°C-100°C and stirring and reacting for 2h-3h to form a microcapsule suspension.

[0010] In one embodiment, the amount of the wall material added is 30%-80% of the mass of the silicone resin-loaded platinum complex microspheres; and / or the amount of the second emulsifier added is 1%-20% of the mass of the silicone resin-loaded platinum complex microspheres.

[0011] In one embodiment, the wall material includes zinc stearate; and / or the second emulsifier includes at least one of carboxymethyl cellulose, polyvinyl alcohol, polyacrylates, and hydroxyethyl cellulose.

[0012] In one embodiment, the silicone resin comprises silicone resin having a softening point of 50°C to 120°C.

[0013] In one embodiment, a platinum complex is loaded on a silicone resin, and the concentration of the platinum complex is 1 ppm to 380,000 ppm.

[0014] In one embodiment, the platinum complex includes at least one of a vinyl platinum complex, an alkyl platinum complex, and an acyl platinum complex.

[0015] In one embodiment, the platinum complex includes a vinyl platinum complex, and the preparation method of the platinum complex includes: providing sodium bicarbonate, chloroplatinic acid, an alcohol solution, and a vinyl double head; dissolving 5g-10g of chloroplatinic acid with 50g-100g of alcohol solution to form an alcohol solution of chloroplatinic acid; adding 20g-50g of sodium bicarbonate to the alcohol solution of chloroplatinic acid to form a first mixed solution; stirring the first mixed solution and 50g-80g of vinyl double head at 50°C-80°C for 1h-3h to form a vinyl platinum complex.

[0016] In one embodiment, the step of post-treating the microcapsule suspension to form a microcapsule platinum complex catalyst includes: diluting and filtering the microcapsule suspension to obtain a preform; and drying the preform at 25° C.-35° C. under nitrogen and / or inert gas protection to obtain a microcapsule platinum complex catalyst.

[0017] In order to solve the above technical problems, the second technical solution provided in the present application is: to provide a platinum complex catalyst prepared by any of the above-mentioned methods for preparing a platinum complex catalyst, comprising a silicone resin-loaded platinum complex and a wall material film stacked sequentially from the inside to the outside.

[0018] In one embodiment, the particle size of the platinum complex catalyst is 1 nm to 100 μm.

[0019] Beneficial effects of the present application: Different from the prior art, the present application discloses a platinum complex catalyst and a preparation method thereof, the preparation method of the platinum complex catalyst comprising loading the platinum complex with silicone resin to form a silicone-loaded platinum complex; mixing the silicone-loaded platinum complex with a first emulsifier to form silicone-loaded platinum complex microspheres; mixing the silicone-loaded platinum complex microspheres with a wall material and a second emulsifier to form a microcapsule suspension; post-treating the microcapsule suspension to form a microcapsule platinum complex catalyst. The microcapsule platinum complex catalyst needs to be activated under specific conditions to release the active ingredient; therefore, when the microcapsule platinum complex catalyst is used to synthesize organosilicon, the microcapsule platinum complex catalyst can be stored together with a cross-linking agent and has a longer operating time. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] In order to more clearly illustrate the technical solutions in the embodiments of the present application, the drawings required for use in the description of the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present application. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.

[0021] Figure 1 Schematic diagram of the process for preparing the platinum complex catalyst provided in the examples of the present application;

[0022] Figure 2 yes Figure 1 The schematic flow chart of step S01 shown;

[0023] Figure 3 yes Figure 1 The flowchart of step S04 is shown in FIG. DETAILED DESCRIPTION

[0024] The following will be combined with the drawings in the embodiments of the present application to clearly and completely describe the technical solutions in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, not all of the embodiments. Based on the embodiments in the present application, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of this application.

[0025] In the following description, for the purpose of explanation rather than limitation, specific details such as specific system structures, interfaces, and technologies are provided to facilitate a thorough understanding of the present application.

[0026] The terms "first", "second", and "third" in this application are only used for descriptive purposes, and cannot be understood as indicating or implying relative importance or implicitly indicating the number of indicated technical features. Thus, the features defined as "first", "second", and "third" can explicitly or implicitly include at least one of the features. In the description of this application, the meaning of "multiple" is at least two, such as two, three, etc., unless otherwise clearly and specifically defined. All directional indications in the embodiments of this application (such as up, down, left, right, front, back...) are only used to explain the relative position relationship, movement, etc. between the components under a certain specific posture (as shown in the accompanying drawings). If the specific posture changes, the directional indication also changes accordingly. The terms "including" and "having" in the embodiments of this application and any of their variations are intended to cover non-exclusive inclusions. For example, a process, method, system, product, or device that includes a series of steps or units is not limited to the listed steps or units, but optionally also includes steps or units that are not listed, or optionally also includes other steps or components inherent to these processes, methods, products, or devices.

[0027] Reference to "embodiments" herein means that a particular feature, structure, or characteristic described in conjunction with the embodiments may be included in at least one embodiment of the present application. The appearance of the phrase in various locations in the specification does not necessarily refer to the same embodiment, nor is it an independent or alternative embodiment that is mutually exclusive with other embodiments. It is explicitly and implicitly understood by those skilled in the art that the embodiments described herein may be combined with other embodiments.

[0028] The present application is described in detail below with reference to the accompanying drawings and embodiments.

[0029] Silicone and modified silicone resin products are widely used in defense and military industry, electrical industry, leather industry, light industrial products, rubber and plastics, food hygiene and other industries due to their excellent thermal oxidation stability, electrical insulation performance, weather resistance, waterproofness, salt spray resistance, mildew resistance, biocompatibility and other properties, playing an irreplaceable role.

[0030] Since the early 1950s, my country's organic silicon industry has made great progress in material performance, mechanism and application. With the increasing demand for high temperature resistant materials, organic silicon polymers, as a type of material with outstanding characteristics, can be modified and matched with organic resins and inorganic materials to achieve structural and functional integration, and have broad application prospects in high-tech industries and cutting-edge fields.

[0031] After the crosslinker and catalyst in the addition silicone system are mixed, the hydrosilylation reaction will be quickly initiated, resulting in a shorter operation time. Addition silicone is usually designed as a two-component system, including component A and component B. Component A includes a crosslinker and component B includes a catalyst. Components A and B need to be stored separately to prevent premature curing reactions during storage. Storing components A and B separately means that the two components need to be accurately measured and mixed before each use, which increases the complexity and time cost of the operation.

[0032] In view of this, an embodiment of the present application provides a platinum complex catalyst and a preparation method thereof. The platinum complex catalyst is in a microcapsule state, and the platinum complex catalyst needs to be activated under specific conditions to release the effective ingredients; therefore, when the platinum complex catalyst is used to synthesize silicone, the platinum complex catalyst can be stored together with the cross-linking agent and has a longer operating time.

[0033] See also Figure 1 , Figure 1 It is a schematic flow chart of the preparation method of the platinum complex catalyst provided in the examples of the present application.

[0034] The preparation method of the platinum complex catalyst provided in the embodiment of the present application specifically includes:

[0035] Step S01: loading the platinum complex with silicone resin to form a silicone resin-loaded platinum complex.

[0036] Platinum complexes can promote addition reactions in organosilicon chemistry. The process of loading platinum complexes on silicone resin is achieved through physical adsorption. When silicone resin is used as a carrier to load platinum complexes, the physical adsorption between the two helps maintain the structural stability and activity of the catalyst, especially maintaining a good dispersion state during the catalytic process, which is conducive to the catalytic reaction.

[0037] In one embodiment, the platinum complex includes at least one of a vinyl platinum complex, an alkyl platinum complex, and an acyl platinum complex.

[0038] In one embodiment, see Figure 2 , Figure 2 yes Figure 1 In the schematic flow diagram of step S01 shown in the figure, the platinum complex includes a vinyl platinum complex, and the preparation method of the platinum complex includes:

[0039] Step S011: providing sodium bicarbonate, chloroplatinic acid, alcohol solution, and vinyl double head.

[0040] Step S012: dissolving 5g-10g of chloroplatinic acid with 50g-100g of an alcohol solution to form an alcohol solution of chloroplatinic acid.

[0041] Step S013: adding 20 g to 50 g of sodium bicarbonate to the alcohol solution of chloroplatinic acid to form a first mixed solution.

[0042] Step S014: stirring the first mixed solution and 50 g-80 g of a vinyl double-capped end cap at 50° C.-80° C. for 1 h-3 h to form a vinyl platinum complex.

[0043] Optionally, the alcohol solution includes at least one of isopropanol and ethanol.

[0044] It should be noted that the vinyl double end cap is also called tetramethyl divinyl disiloxane. Chloroplatinic acid is dissolved in alcohol (such as isopropanol or ethanol) to form a transparent solution; the addition of sodium bicarbonate can neutralize the acidity of the alcohol solution of chloroplatinic acid, adjust the pH value, help stabilize the platinum ions, and promote the formation of the complex; at a certain temperature, the double bonds on the vinyl double end cap can form coordination bonds with the platinum ions to form a vinyl platinum complex. After the formation of the vinyl platinum complex, it can be further processed, such as cooling, filtering, washing and drying, etc., to obtain a pure product. Exemplarily, after the formation of the vinyl platinum complex, it is filtered after being stored in the dark for 20 hours, and then the filtered product is loaded with silicone resin.

[0045] In one embodiment, the silicone resin includes a silicone resin having a softening point of 50°C-120°C. The above arrangement is conducive to maintaining the stability of the silicon-supported platinum complex, maintaining the stability of the silicon-supported platinum complex during the subsequent step S02 operation, reducing the probability of the platinum complex migrating or detaching from the silicone resin, and maintaining the overall activity of the silicon-supported platinum complex. In addition, it is also conducive to the final microcapsule platinum complex catalyst to maintain good structural stability during the entire reaction process of forming silicone by addition reaction. The silicone resin can be selected from silicone resins having a softening point temperature of 50°C, 60°C, 70°C, 80°C, 90°C, 100°C, 110°C, 120°C, etc., and can also be selected from a range consisting of any two of the above values, for example, 50°C-60°C, 50°C-80°C, etc.

[0046] Optionally, the silicone resin includes silicone resin with a softening point of 50°C-60°C, so that the prepared microcapsule platinum complex catalyst can be activated at a relatively low temperature to release effective catalytic components, thereby reducing activation requirements.

[0047] In one embodiment, the platinum complex is loaded with silicone resin, and the platinum complex is 1ppm-380,000ppm. Through the above arrangement, the loading density of the platinum complex on the silicone resin is suitable, and the distribution of the platinum complex on the silicone resin is relatively uniform, so that the silicon-loaded platinum complex is kept to have a high activity, and then the microcapsule platinum complex catalyst finally formed is kept to have a high activity. The platinum complex can be 1ppm, 10ppm, 50ppm, 100ppm, 1000ppm, 10,000ppm, 100,000ppm, 200,000ppm, 380,000ppm, etc., or it can be a range composed of any two of the above values, for example, 1ppm-100ppm, 50ppm-1000ppm, etc.

[0048] In one embodiment, after the vinyl platinum complex is loaded with the silicone resin, it can be further processed, for example, the solvent is removed, and then step S02 is performed.

[0049] In a specific embodiment, 20g of sodium bicarbonate is weighed and poured into a flask; 5g of 10% chloroplatinic acid-isopropanol solution is added and stirred; 50g of vinyl double-capped is poured into the flask, and stirred for reaction at a temperature of 75°C for 1.5h to form a vinyl platinum complex. The vinyl platinum complex formed above is stored in the dark for 20h and then filtered to obtain a relatively pure vinyl platinum complex. The relatively pure vinyl platinum complex is loaded with a silicone resin with a softening point of 60°C, and the solvent in the flask is removed under reduced pressure to obtain a silicone resin-loaded platinum complex.

[0050] Step S02: mixing the silicone resin-supported platinum complex with the first emulsifier to form silicone resin-supported platinum complex microspheres.

[0051] Specifically, the step of mixing the silicone-supported platinum complex with the first emulsifier to form silicone-supported platinum complex microspheres includes: mixing the silicone-supported platinum complex with the first emulsifier, stirring and emulsifying at 60° C.-100° C. for 20 min-30 min to form silicone-supported platinum complex microspheres.

[0052] The silicone-supported platinum complex is mixed with the first emulsifier. Under the action of the first emulsifier, the silicone-supported platinum complex is promoted to form fine droplets, and at the same time, the silicone-supported platinum complex droplets are coated to prevent the droplets from merging, thereby forming a stable emulsion system. By controlling the emulsification conditions, the emulsification conditions are 60°C-100°C, stirring, and the emulsification time is 20min-30min, so that the silicone-supported platinum complex is fully emulsified. For example, carboxymethyl cellulose is used at 80°C to fully emulsify the silicone-supported platinum complex.

[0053] The temperature may be 60°C, 70°C, 80°C, 90°C, 100°C, etc., or a range consisting of any two of the above values, for example, 70°C-90°C, 60°C-80°C, etc. The emulsification time may be 20min, 21min, 22min, 23min, 24min, 25min, 26min, 27min, 28min, 29min, 30min, etc., or a range consisting of any two of the above values, for example, 20min-25min, 22min-28min, etc.

[0054] In one embodiment, the amount of the first emulsifier added is 1%-20% of the mass of the silicone-supported platinum complex, so as to keep the silicone-supported platinum complex fully emulsified. The amount of the first emulsifier added can be 1%, 5%, 10%, 15%, 20%, etc. of the mass of the silicone-supported platinum complex, or can be a range consisting of any two of the above values, such as 1%-10%, 5%-20%, etc.

[0055] In one embodiment, the first emulsifier includes at least one of carboxymethyl cellulose (CMC), polyvinyl alcohol, polyacrylates, and hydroxyethyl cellulose, which has a good emulsifying effect on the silicone-supported platinum complex and maintains the stability of the emulsion system. In a specific embodiment, the first emulsifier includes carboxymethyl cellulose.

[0056] In one embodiment, the emulsification is carried out for 20-30 minutes using a mixing device under a water bath condition of 60°C-100°C. The use of a mixing device for dispersion accelerates the dispersion and the emulsification process, which is beneficial to shortening the emulsification time for the silicone-supported platinum complex to be fully emulsified; in addition, it is beneficial to reduce agglomeration and maintain the stability of the emulsion system. Optionally, the mixing device is a high-speed dispersant.

[0057] In one embodiment, the speed of stirring is 6000rpm-27000rpm. By setting the speed as above, high-speed dispersion can significantly accelerate the emulsification speed and shorten the emulsification time compared with static mixing or other low-speed stirring methods. Wherein, the speed of stirring can be 6000rpm, 7000rpm, 8000rpm, 9000rpm, 10000rpm, 11000rpm, 11500rpm, 12000rpm, 12500rpm, 13000rpm, 15000rpm, 20000rpm, 25000rpm, 27000rpm, etc., or it can be a range composed of any two of the above values, for example, 10000rpm-13000rpm, 11000rpm-15000rpm, etc.

[0058] Exemplarily, the rotation speed of the high-speed dispersant is 12000 rpm.

[0059] Step S03: mixing the silicone resin-loaded platinum complex microspheres with the wall material and the second emulsifier to form a microcapsule suspension.

[0060] Specifically, the step of mixing silicone-supported platinum complex microspheres with a wall material and a second emulsifier to form a microcapsule suspension includes: mixing silicone-supported platinum complex microspheres with a wall material and a second emulsifier, stirring and emulsifying at 45°C-55°C for 30min-40min, and then heating to 50°C-100°C and stirring and reacting for 2h-3h to form a microcapsule suspension.

[0061] The silicone-loaded platinum complex microspheres are mixed with the wall material and the second emulsifier to maintain the uniform distribution of the wall material. The wall material gathers around the silicone-loaded platinum complex microspheres. The wall material is deposited and cross-linked on the surface of the silicone-loaded platinum complex microspheres, gradually forming a continuous shell that wraps the silicone-loaded platinum complex microspheres to form a microcapsule structure. After emulsification at 45°C-55°C for 30min-40min, the temperature is raised to 50°C-100°C and the reaction is continued with stirring for 2h-3h to ensure sufficient emulsification and film formation of the wall material, establish a stable microcapsule structure, and maintain stable formation of the microcapsules. By controlling the stirring reaction at 50°C-100°C, a high embedding rate of the microcapsules is maintained; illustratively, after adding the wall material zinc stearate, the embedding rate of the microcapsules is high at 80°C.

[0062] The emulsification temperature may be 45°C, 46°C, 47°C, 48°C, 49°C, 50°C, 51°C, 52°C, 53°C, 54°C, 55°C, etc., or a range consisting of any two of the above values, for example, 48°C-52°C, 49°C-55°C, etc. The emulsification time may be 30min, 31min, 32min, 33min, 34min, 35min, 36min, 37min, 38min, 39min, 40min, etc., or a range consisting of any two of the above values, for example, 30min-35min, 32min-38min, etc.

[0063] The reaction temperature can be 50°C, 60°C, 70°C, 75°C, 76°C, 77°C, 78°C, 79°C, 80°C, 81°C, 82°C, 83°C, 84°C, 85°C, 90°C, 100°C, etc., or a range consisting of any two of the above values, for example, 75°C-80°C, 79°C-84°C, etc. The reaction time can be 2h, 2.2h, 2.4h, 2.5h, 2.6h, 3h, etc., or a range consisting of any two of the above values, for example, 2h-2.5h, etc.

[0064] Optionally, the step of mixing the silicone-supported platinum complex microspheres with the wall material and the second emulsifier to form a microcapsule suspension includes: mixing the silicone-supported platinum complex microspheres with the wall material and the second emulsifier, stirring and emulsifying at 45°C-55°C for 30min-40min, and then heating to 75°C-85°C and stirring and reacting for 2h-3h to form a microcapsule suspension. By designing the reaction temperature after emulsification to be 75°C-85°C, a high encapsulation rate of the microcapsules can be maintained.

[0065] In one embodiment, the amount of the wall material added is 30%-80% of the mass of the silicone-supported platinum complex microspheres; and / or the amount of the second emulsifier added is 1%-20% of the mass of the silicone-supported platinum complex microspheres. Through the above arrangement, the wall material has good coating properties on the silicone-supported platinum complex microspheres, the stability of the formed microcapsule structure is maintained, and at the same time, it can be broken under certain triggering conditions to release the effective catalytic components of the silicone-supported platinum complex microspheres.

[0066] The amount of the wall material added can be 30%, 40%, 50%, 60%, 70%, 80%, etc. of the mass of the silicone resin-loaded platinum complex microspheres, or a range consisting of any two of the above values, such as 30%-50%, 40%-70%, etc. The amount of the second emulsifier added can be 1%, 5%, 10%, 15%, 20%, etc. of the mass of the silicone resin-loaded platinum complex microspheres, or a range consisting of any two of the above values, such as 1%-15%, 10%-20%, etc.

[0067] In one embodiment, the wall material includes zinc stearate; and / or the second emulsifier includes at least one of carboxymethyl cellulose, polyvinyl alcohol, polyacrylates, and hydroxyethyl cellulose. Through the above configuration, sufficient emulsification and the formation of the capsule wall are ensured to establish a stable microcapsule structure. It should be noted that the wall material includes but is not limited to zinc stearate, and the material of the wall material is incompatible with silicone oil.

[0068] In one specific embodiment, the wall material comprises zinc stearate, and the second emulsifier comprises carboxymethyl cellulose.

[0069] Step S04: post-treating the microcapsule suspension to form a microcapsule platinum complex catalyst.

[0070] Specifically, see Figure 3 , Figure 3 yes Figure 1 The schematic flow diagram of step S04 shown in the figure, the step of post-treating the microcapsule suspension to form a microcapsule platinum complex catalyst includes:

[0071] Step S041: dilute and filter the microcapsule suspension to obtain a preform.

[0072] In one embodiment, the diluent comprises water, ie, the microcapsule suspension is diluted with water.

[0073] Step S042: drying the preform at 25° C.-35° C. under the protection of nitrogen and / or inert gas to obtain a microcapsule platinum complex catalyst.

[0074] Among them, the drying temperature can be 25°C, 26°C, 27°C, 28°C, 29°C, 30°C, 31°C, 32°C, 33°C, 34°C, 35°C, or a range consisting of any two of the above values, for example, 28°C-32°C, 29°C-35°C, etc.

[0075] The platinum complex catalyst prepared by the preparation method of the platinum complex catalyst provided by the embodiment of the present application is in a microcapsule state and needs to be activated to release the catalytic component under specific conditions (e.g., heating, illumination, contact with specific chemical substances, etc.), so that the reaction can be activated when needed. In the absence of a triggering state under specific conditions, before the shell of the microcapsule platinum complex (i.e., the film-forming wall material) is dissolved or ruptured, the catalytic component of the microcapsule platinum complex is isolated from the reactant, and the reaction will not start immediately. Therefore, when the microcapsule platinum complex catalyst is used to synthesize organosilicon, the microcapsule platinum complex catalyst can be stored together with a cross-linking agent and has a longer operating time. By controlling the regulation of triggering the rupture or dissolution of the shell, or controlling the type and amount of the wall material, the release rate of the catalytic component of the microcapsule platinum complex catalyst is controlled, and the reaction rate of synthesizing organosilicon using the microcapsule platinum complex catalyst is controlled.

[0076] The platinum complex catalyst provided in the embodiment of the present application is prepared in a solution, so that the particle size of the microcapsule platinum complex catalyst is relatively uniform. By controlling the operating conditions (temperature, duration, composition, addition amount, etc.) of each step, it is beneficial to maintain the uniformity of the particle size of the microcapsule platinum complex catalyst finally formed.

[0077] The present application also provides a platinum complex catalyst, which can be prepared by the preparation method of the platinum complex catalyst provided in the above embodiment. The platinum complex catalyst includes a silicone resin-supported platinum complex and a wall material film stacked sequentially from the inside to the outside. In other words, the wall material film wraps the silicone resin-supported platinum complex.

[0078] In one embodiment, the particle size of the platinum complex catalyst is nanometer-sized. Optionally, the particle size of the platinum complex catalyst is 1 nm-1000 nm.

[0079] In one embodiment, the particle size of the platinum complex catalyst is 1 nm-100 μm. The particle size of the platinum complex catalyst can be 1 nm, 10 nm, 50 nm, 100 nm, 1 μm, 10 μm, 50 μm, 100 μm, etc., or can be a range consisting of any two of the above values, for example, 1 nm-1 μm, 10 nm-100 nm, etc.

[0080] In order to make the technical problems, technical solutions and beneficial effects solved by the embodiments of the present application clearer, the following will be further described in detail in conjunction with the embodiments. Obviously, the described embodiments are only a part of the embodiments of the present application, rather than all of the embodiments. The following description of at least one exemplary embodiment is actually only illustrative and is by no means intended to limit the present application and its applications. Based on the embodiments in the present application, all other embodiments obtained by ordinary technicians in the field without creative work are within the scope of protection of the present application.

[0081] Embodiment 1:

[0082] 1. Weigh 20g of sodium bicarbonate and pour it into a flask; add 5g of 10% chloroplatinic acid-isopropanol solution and start stirring.

[0083] 2. Pour 50 vinyl double-capped vinyl into the flask. After the addition is complete, wait until the temperature reaches 75°C and continue stirring the reaction for 1.5 hours.

[0084] 3. After storing in the dark for 20 hours, filter to obtain a vinyl platinum complex.

[0085] 4. The vinyl platinum complex is loaded onto silicone resin, wherein the vinyl platinum complex is 50 ppm, and the solvent in the flask is removed under reduced pressure to obtain a silicone resin-loaded platinum complex.

[0086] 5. Add 20 g of silicone resin-supported platinum complex and 4 g of carboxymethyl cellulose (CMC) into a beaker, and emulsify at 12,000 rpm for 20 min using a high-speed disperser in an 80° C. water bath; filter to obtain silicone resin-supported platinum complex microspheres.

[0087] 6. The above 15 g silicone resin-loaded platinum complex microspheres were transferred to a three-necked flask, and 12 g zinc stearate and 3 g carboxymethyl cellulose were added. After emulsification at 50 ° C for 30 min, the temperature was raised to 80 ° C, and the reaction was continued with stirring for 2 h to obtain a microcapsule suspension.

[0088] 7. The microcapsule suspension was diluted with water and allowed to stand for 24 hours, filtered, and dried under nitrogen at 30°C to obtain a microcapsule platinum complex catalyst, which was stored in a ziplock bag.

[0089] Embodiment 2:

[0090] 1. Weigh 20g of sodium bicarbonate and pour it into a flask; add 5g of 10% chloroplatinic acid-isopropanol solution and start stirring.

[0091] 2. Pour 50 vinyl double-capped vinyl into the flask. After the addition is complete, wait until the temperature reaches 75°C and continue stirring the reaction for 1.5 hours.

[0092] 3. After storing in the dark for 20 hours, filter to obtain a vinyl platinum complex.

[0093] 4. The vinyl platinum complex is loaded on silicone resin, wherein the vinyl platinum complex is 10000 ppm, and the solvent in the flask is removed under reduced pressure to obtain a silicone resin-loaded platinum complex.

[0094] 5. Add 20 g of silicone resin-loaded platinum complex and 2 g of carboxymethyl cellulose (CMC) into a beaker, and emulsify at 12,000 rpm for 20 min using a high-speed disperser in an 80° C. water bath; filter to obtain silicone resin-loaded platinum complex microspheres.

[0095] 6. The above 15 g silicone resin-loaded platinum complex microspheres were transferred to a three-necked flask, and 7.5 g zinc stearate and 1.5 g carboxymethyl cellulose were added. After emulsification at 50 ° C for 30 min, the temperature was raised to 80 ° C, and the reaction was continued with stirring for 2 h to obtain a microcapsule suspension.

[0096] 7. The microcapsule suspension was diluted with water and allowed to stand for 24 hours, filtered, and dried under nitrogen at 30°C to obtain a microcapsule platinum complex catalyst, which was stored in a ziplock bag.

[0097] Embodiment 3:

[0098] 1. Weigh 20g of sodium bicarbonate and pour it into a flask; add 5g of 10% chloroplatinic acid-isopropanol solution and start stirring.

[0099] 2. Pour 50 vinyl double-capped vinyl into the flask. After the addition is complete, wait until the temperature reaches 75°C and continue stirring the reaction for 1.5 hours.

[0100] 3. After storing in the dark for 20 hours, filter to obtain a vinyl platinum complex.

[0101] 4. The vinyl platinum complex is loaded with silicone resin, wherein the vinyl platinum complex is 380,000 ppm, and the solvent in the flask is removed under reduced pressure to obtain a silicone resin-loaded platinum complex.

[0102] 5. Add 20 g of silicone resin-loaded platinum complex and 0.2 g of carboxymethyl cellulose (CMC) into a beaker, and emulsify at 12,000 rpm for 20 min using a high-speed disperser in an 80° C. water bath; filter to obtain silicone resin-loaded platinum complex microspheres.

[0103] 6. The above 15 g silicone resin-loaded platinum complex microspheres were transferred to a three-necked flask, 4.5 g zinc stearate and 0.15 g carboxymethyl cellulose were added, and the mixture was emulsified at 50 ° C for 30 min, then the temperature was raised to 80 ° C, and the reaction was continued with stirring for 2 h to obtain a microcapsule suspension.

[0104] 7. The microcapsule suspension was diluted with water and allowed to stand for 24 hours, filtered, and dried under nitrogen at 30°C to obtain a microcapsule platinum complex catalyst, which was stored in a ziplock bag.

[0105] The above are only implementation methods of the present application, and are not intended to limit the patent scope of the present application. Any equivalent structure or equivalent process transformation made using the contents of the present application specification and drawings, or directly or indirectly applied in other related technical fields, are also included in the patent protection scope of the present application.

Claims

1. A method for preparing a platinum complex catalyst, characterized in that: include: loading the platinum complex with silicone resin to form a silicone resin-loaded platinum complex; Mixing the silicone resin-supported platinum complex with a first emulsifier to form silicone resin-supported platinum complex microspheres; Mixing the silicone resin-loaded platinum complex microspheres with a wall material and a second emulsifier to form a microcapsule suspension; The microcapsule suspension is post-treated to form a microcapsule platinum complex catalyst.

2. The method for preparing a platinum complex catalyst according to claim 1, characterized in that: The step of mixing the silicone resin-supported platinum complex with a first emulsifier to form silicone resin-supported platinum complex microspheres comprises: The silicone resin-supported platinum complex is mixed with the first emulsifier, and stirred and emulsified at 60° C.-100° C. for 20 min-30 min to form silicone resin-supported platinum complex microspheres.

3. The method for preparing a platinum complex catalyst according to claim 1, characterized in that: The added amount of the first emulsifier is 1%-20% of the mass of the silicone resin-supported platinum complex.

4. The method for preparing a platinum complex catalyst according to claim 1, characterized in that: The first emulsifier includes at least one of carboxymethyl cellulose, polyvinyl alcohol, polyacrylates, and hydroxyethyl cellulose.

5. The method for preparing a platinum complex catalyst according to claim 1, characterized in that: The step of mixing the silicone resin-loaded platinum complex microspheres with a wall material and a second emulsifier to form a microcapsule suspension comprises: The silicone resin-loaded platinum complex microspheres are mixed with the wall material and the second emulsifier, stirred and emulsified at 45° C.-55° C. for 30 min-40 min, and then heated to 50° C.-100° C. and stirred for reaction for 2 h-3 h to form a microcapsule suspension.

6. The method for preparing a platinum complex catalyst according to claim 1, characterized in that: The amount of the wall material added is 30%-80% of the mass of the silicone resin-loaded platinum complex microspheres; and / or the amount of the second emulsifier added is 1%-20% of the mass of the silicone resin-loaded platinum complex microspheres.

7. The method for preparing a platinum complex catalyst according to claim 1, characterized in that: The wall material includes zinc stearate; and / or the second emulsifier includes at least one of carboxymethyl cellulose, polyvinyl alcohol, polyacrylates, and hydroxyethyl cellulose.

8. The method for preparing a platinum complex catalyst according to claim 1, characterized in that: The silicone resin includes silicone resin having a softening point of 50°C-120°C.

9. The method for preparing a platinum complex catalyst according to claim 1, characterized in that: The platinum complex is loaded with silicone resin, wherein the platinum complex is 1 ppm to 380,000 ppm.

10. The method for preparing a platinum complex catalyst according to claim 1, characterized in that: The platinum complex includes at least one of a vinyl platinum complex, an alkyl platinum complex, and an acyl platinum complex.

11. The method for preparing a platinum complex catalyst according to claim 10, characterized in that: The platinum complex comprises a vinyl platinum complex, and the preparation method of the platinum complex comprises: Provide sodium bicarbonate, chloroplatinic acid, alcohol solution, vinyl double head; Dissolving 5 g to 10 g of the chloroplatinic acid with 50 g to 100 g of the alcohol solution to form an alcohol solution of chloroplatinic acid; Adding 20 g to 50 g of the sodium bicarbonate to the alcohol solution of chloroplatinic acid to form a first mixed solution; The first mixed liquid and 50 g to 80 g of the vinyl double end cap are stirred and reacted at 50° C. to 80° C. for 1 h to 3 h to form the vinyl platinum complex.

12. The method for preparing a platinum complex catalyst according to claim 1, characterized in that: The step of post-treating the microcapsule suspension to form a microcapsule platinum complex catalyst comprises: diluting and filtering the microcapsule suspension to obtain a preform; The preform is dried at 25° C.-35° C. under the protection of nitrogen and / or inert gas to obtain the microcapsule platinum complex catalyst.

13. A platinum complex catalyst prepared by the method for preparing a platinum complex catalyst according to any one of claims 1 to 12, characterized in that: It includes a silicone resin-loaded platinum complex and a wall material membrane which are stacked in sequence from the inside to the outside.

14. The platinum complex catalyst according to claim 13, characterized in that The particle size of the platinum complex catalyst is 1 nm-100 μm.

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