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CN-121975329-A - Liquid silica gel material and preparation method and application thereof

CN121975329ACN 121975329 ACN121975329 ACN 121975329ACN-121975329-A

Abstract

The invention relates to the technical field of organic silicon materials and perfume slow release, and discloses a liquid silica gel material, a preparation method and application thereof, wherein the liquid silica gel comprises vinyl polysiloxane, a modified mesoporous silica carrier, The components such as cyclodextrin inclusion compound, polyethylene glycol pore-forming agent and the like are used for constructing a multi-layer slow-release system in a compact silicon rubber matrix through triple synergistic strategies of mesoporous carrier adsorption load, cyclodextrin inclusion protection and sacrificial template pore-forming, so that 30-90 days of sustained release of the agilawood active component is realized.

Inventors

  • XIAO JIANLIN

Assignees

  • 广东鸿强新材料科技有限公司

Dates

Publication Date
20260505
Application Date
20260210

Claims (10)

  1. 1. A liquid silica gel is characterized by comprising the following raw materials, by weight, 100-140 parts of vinyl polysiloxane, 0.15-0.35 part of platinum complex, 25-40 parts of modified mesoporous silica carrier, 1-4 parts of white carbon black modifier, 7-12 parts of polydimethylsiloxane, 5-8 parts of hexamethyldisilazane, 16-25 parts of MQ silicone resin and 3-15 parts of modified mesoporous silica carrier -Cyclodextrin inclusion compound, 2-8 parts of polyethylene glycol porogen; the modified mesoporous silica carrier is mesoporous loaded with agilawood extract after being surface modified by a silane coupling agent Particles; The said The cyclodextrin inclusion compound is a volatile component of agilawood -Inclusion compounds prepared by inclusion reaction of cyclodextrin; The polyethylene glycol pore-forming agent is polyethylene glycol with the molecular weight of 2000-6000.
  2. 2. The liquid silica gel according to claim 1, wherein the preparation method of the modified mesoporous silica carrier comprises the following steps: Will mesoporous Soaking the granule in lignum Aquilariae Resinatum extract solution, vacuum soaking at 25-50deg.C for 2-6 hr, filtering, and drying to obtain mesoporous powder Granule, and loading the mesoporous of lignum Aquilariae Resinatum extract Dispersing the particles in absolute ethyl alcohol, adding a silane coupling agent, carrying out reflux reaction for 2-4 hours at 60-80 ℃, filtering, washing and drying to obtain a modified mesoporous silica carrier; The mesoporous pores The particles are selected from one or two of MCM-41 mesoporous silica and SBA-15 mesoporous silica, and have pore diameter of 2-10nm and specific surface area of 600-1200 /g; The agilawood extract solution is ethanol solution of agilawood extract, and the concentration is 50-200mg/mL; The silane coupling agent is selected from vinyl trimethoxy silane, vinyl tri (2-methoxyethoxy) silane, One or more of the methacryloxypropyl trimethoxy silanes in the amount of mesopores 3-10% Of the weight of the granule.
  3. 3. The liquid silica gel according to claim 1, wherein the silica gel comprises The preparation method of the cyclodextrin inclusion compound comprises the following steps: Will be Dissolving cyclodextrin in 50-70deg.C hot water to form saturated solution, preparing lignum Aquilariae Resinatum volatile oil into solution with absolute ethanol as solvent, and slowly dripping into the solution Stirring and clathrating the solution in cyclodextrin saturated solution at 40-60deg.C for 2-4 hr, cooling to room temperature, refrigerating at 4-10deg.C, standing for 12-24 hr, filtering, collecting precipitate, and drying -Cyclodextrin inclusion compound; The agilawood volatile oil The molar ratio of cyclodextrin is 1 (6-10) The inclusion rate of the cyclodextrin inclusion compound is 60-85%.
  4. 4. The liquid silica gel according to claim 1, wherein the active component of the eaglewood extract comprises agalloch eaglewood spirool, -One or more of agarofuran, agalloch eaglewood tetrol, 2- (2-phenethyl) chromones.
  5. 5. The liquid silica gel according to claim 1, wherein the liquid silica gel comprises the following raw materials, by weight, 110-130 parts of vinyl polysiloxane, 0.2-0.3 part of platinum complex, 28-35 parts of modified mesoporous silica carrier, 1.5-3 parts of white carbon black modifier, 8-11 parts of polydimethylsiloxane, 6-7.5 parts of hexamethyldisilazane, 18-22 parts of MQ silicone resin, and 5-10 parts of MQ silicone resin -Cyclodextrin inclusion compound, 3-6 parts of polyethylene glycol porogen; the loading capacity of the agilawood extract in the modified mesoporous silica carrier is mesoporous 30-50% Of the weight of the granule.
  6. 6. The liquid silica gel according to claim 1, wherein the white carbon black modifier comprises tetramethyl disilazane, octamethyl-cyclotetrasilazane and vinyl trimethoxy silane, which are mixed in a weight ratio of 1 (0.5-0.8): 0.15-0.25.
  7. 7. A method for preparing a liquid silica gel according to any one of claims 1 to 6, comprising the steps of: Step one, preparing a modified mesoporous silica carrier, namely, preparing a mesoporous silica carrier Activating the granule at 120-180deg.C for 2-4 hr, cooling, soaking in ethanol solution of lignum Aquilariae Resinatum extract, soaking at 25-50deg.C under vacuum degree of-0.06-0.09 MPa for 2-6 hr, filtering, vacuum drying at 40-60deg.C for 8-12 hr to obtain mesoporous powder of loaded lignum Aquilariae Resinatum extract Granule, and loading the mesoporous of lignum Aquilariae Resinatum extract Dispersing the particles in absolute ethyl alcohol, adding a silane coupling agent, carrying out reflux reaction for 2-4 hours at 60-80 ℃, filtering, washing and drying to obtain a modified mesoporous silica carrier; step two, preparing Cyclodextrin inclusion compound, will Dissolving cyclodextrin in 50-70deg.C hot water to form saturated solution, slowly dripping anhydrous ethanol solution of lignum Aquilariae Resinatum volatile oil into the saturated solution, stirring at 40-60deg.C for inclusion for 2-4 hr, cooling to room temperature, refrigerating at 4-10deg.C, standing for 12-24 hr, filtering, collecting precipitate, and vacuum drying at 40-50deg.C to obtain the final product -Cyclodextrin inclusion compound; Step three, preparing base adhesive, namely adding vinyl polysiloxane, a modified mesoporous silica carrier and 45-55% by weight of hexamethyldisilazane into a vacuum kneader, mixing for 180-210min at 150-165 ℃ under vacuum condition, cooling to room temperature, and grinding by a three-roller mill to obtain the base adhesive; Step four, mixing and granulating, namely mixing the base gum with a platinum complex, Adding cyclodextrin clathrate, polyethylene glycol pore-forming agent, polydimethylsiloxane, MQ silicone resin, white carbon black modifier and the rest hexamethyldisilazane into a planetary mixer, stirring and mixing under vacuum for 30-60min to uniformity, removing bubbles, and filtering to obtain liquid silica gel loaded with lignum Aquilariae Resinatum extract.
  8. 8. The method of claim 7, wherein in the fourth step of granulating, the base gum and the platinum complex are mixed uniformly and then added sequentially And adding the polydimethylsiloxane, the MQ silicon resin, the white carbon black modifier and the rest hexamethyldisilazane after stirring the cyclodextrin inclusion compound and the polyethylene glycol pore-forming agent for 10-20min, and continuously stirring for 20-40min until the mixture is uniform, wherein the temperature is controlled at 20-35 ℃ in the whole mixing process.
  9. 9. The method of preparing the silica gel according to claim 7, wherein the step of forming pores by vulcanizing the liquid silica gel comprises immersing the vulcanized molded body in deionized water or an aqueous solution of 20-50% ethanol at 40-60 ℃ for 24-72 hours to dissolve out the polyethylene glycol pore-forming agent and form pores with diameters of 1-5 in the silicone rubber matrix M, drying to obtain a slow-release silicone rubber product with a gradient pore structure; The vulcanization molding conditions are that the temperature is 120-160 ℃, the pressure is 0.5-2MPa, and the time is 5-30min.
  10. 10. Use of a liquid silica gel according to any one of claims 1 to 6 for the preparation of pillows, mattresses, aromatherapy articles, automotive upholstery, home furnishing materials or wearable health devices.

Description

Liquid silica gel material and preparation method and application thereof Technical Field A liquid silica gel material and a preparation method and application thereof belong to the technical field of functional polymer composite materials. Background Liquid silicone gum (Liquid Silicone Rubber, LSR) is a class of silicone elastomer materials based on vinyl polysiloxanes that are vulcanizable and cross-linked by a platinum catalyzed addition reaction. The liquid silica gel has the processing advantages of good fluidity, high vulcanization speed, injection molding and the like, has excellent high and low temperature resistance (-60 to 200 ℃ for long-term use), excellent biocompatibility and chemical inertness, and has been widely applied to the fields of food-grade products, medical devices, infant products, electronic seals and the like. In industrial practice, the liquid silica gel can balance the relation between fluidity and mechanical strength by adjusting the molecular weight and vinyl content of the base polymer, and the viscosity is usually controlled in the range of tens of thousands to hundreds of thousands of millipascal seconds, and the liquid silica gel is suitable for automatic processing technologies such as injection molding, casting molding and the like. The molecular framework of the liquid silica gel isThe main chain has excellent heat stability and ultraviolet resistance, so that the main chain is particularly suitable for long-term outdoor use or application scenes where the main chain frequently contacts human skin. The lignum Aquilariae Resinatum (Agarwood) is resin-containing wood aggregate formed by long-term biochemical transformation of plants of Aquilaria of Thymelaeaceae after being infected or physically damaged by specific fungi, and is Chinese traditional rare spice and Chinese medicinal material. The lignum Aquilariae Resinatum contains rich sesquiterpenoids (such as agalloch eaglewood spirool),Agarofuran, agalloch eaglewood tetrol), chromone compounds (such as 2- (2-phenethyl) chromone derivatives) and various aromatic compounds, which not only endow agalloch eaglewood with unique elegant and durable fragrance, but also show various biological activities of anti-inflammatory, analgesic, tranquilizing, antioxidant, antibacterial, bacteriostatic and the like. In the practice of traditional Chinese medicine systems and modern aromatherapy, agilawood is widely used to alleviate anxiety, improve sleep quality and create a pleasant living atmosphere. In recent years, with the continuous increase of the demands of consumers for natural perfume products and functional health materials, the introduction of agilawood active ingredients into daily-contact functional materials to realize continuous slow release has become an important research direction and industrialization hot spot in the field. The main active molecular agalloch eaglewood screw alcohol in the agalloch eaglewood volatile oil has the physical and chemical characteristics of molecular weight 222.37 and boiling point about 260 ℃, and the molecular diameter is about 0.65nm, and belongs to typical small and medium molecular organic matters. The molecular weight of chromone compounds is usually between 250 and 350, the boiling point is higher, the volatility is weaker, and the chromone compounds are important contribution components for the durability of the agilawood fragrance. However, the effective introduction of the active ingredient of agilawood into a liquid silica gel system and the realization of sustained release face three major technical hurdles. First, the volatilization loss problem is that the platinum-catalyzed addition vulcanization process of liquid silica gel is usually carried out at a high temperature of 120-160 ℃ for 5-30min, the vapor pressure of sesquiterpenes volatile components (boiling point range of 180-280 ℃) in agilawood extracts is remarkably increased at the temperature, the vapor pressure of the agilawood spirool at 140 ℃ is about 100-200 times of the vapor pressure of the agilawood spirool at room temperature according to an Antoine equation, a large amount of volatilization dissipation is caused, and the residual quantity of effective aroma components in the vulcanized product is seriously insufficient, and the retention rate is usually lower than 30%. Second, compatibility problems are that the eaglewood extract is a natural organic mixture containing a large amount of hydroxyl and carbonyl polar groups, and a large difference in solubility parameter exists between the eaglewood extract and the nonpolar polysiloxane matrix (the solubility parameter of the eaglewood extract is about 18-22The polydimethyl siloxane was about 15.1) Direct blending is extremely easy to cause macroscopic phase separation caused by Flory-Huggins thermodynamic instability, and the macroscopic phase separation is manifested in that oil spots ooze out of the surface of the product, agilawood enrichment phase domain