Preparation method of novel mineral crystal active material and application of novel mineral crystal active material in product

Abstract

The invention relates to the technical field of material science and chemical engineering, in particular to a preparation method of a novel mineral crystal active material and application of the novel mineral crystal active material in a product. Comprising the following steps: mixing natural mineral crystal raw materials, natrolite, tourmaline and medical stone according to a mass ratio of 5: 3: 2, and crushing until the nano-scale particle size is 50-200nm; 2, the mixed powder obtained in the step 1 is placed in a plasma activation device and treated for 10-30 min at the power of 100-500 W in the inert gas environment, and a honeycomb-shaped porous structure is formed on the surface of the mineral; mixing the activated mineral powder with a biocompatible carrier material according to a ratio of 1: 5-1: 20; and uniformly compounding the mixture by adopting an ultrasonic dispersion technology, and drying to obtain the new ore crystal active material. Through innovative mineral ratio optimization, plasma activation modification and biocompatibility composite technologies, the performance bottleneck of an existing material is broken through, the high-added-value application of the material in multiple scenes is expanded, and a core technical support is provided for development of healthy functional products.

Description

Technical Field

[0001] The present invention relates to the technical fields of materials science and chemical engineering, and particularly to a preparation method of a novel mineral crystal active energy new material and its application in products. Background Art

[0002] In recent years, with the wide application of functional materials in the fields of health, environmental protection and intelligent products, mineral-based composite materials have attracted much attention due to their natural properties and unique physical and chemical characteristics. Natural minerals such as natrolite, tourmaline, and medical stone have been tried to be applied in fields such as textiles, skin care products, and environmental purification due to their properties such as adsorption, negative ion release, and far-infrared radiation.

[0003] However, the development of mineral composite materials in the prior art still faces the following bottlenecks: (1) Limited material properties: Traditional mineral composite materials mostly use single minerals or simple mixtures, and do not achieve synergy through optimized component ratios. For example, although tourmaline can release negative ions, its dispersibility and stability are insufficient; the adsorption performance of medical stone is limited by the specific surface area, resulting in functional indicators (such as bacteriostatic rate, negative ion concentration) being difficult to meet the requirements of high-end applications. In addition, the micron-sized particle size of mineral particles limits the interfacial bonding efficiency with the carrier material, affecting the durability of the final product.

[0004] (2) Insufficient preparation process: Existing modification methods (such as acid treatment, high-temperature calcination) are prone to damage the mineral crystal structure and are difficult to accurately control the surface morphology. Conventional grinding techniques cannot achieve nano-scale dispersion, and the surface of unactivated minerals has few active sites, resulting in limited improvement in functional properties (such as infrared radiation efficiency). Some studies use chemical modification to enhance the properties of minerals, but the introduced synthetic reagents may reduce the biocompatibility and environmental friendliness of the materials.

[0005] (3) Low functional integration: Existing materials mostly focus on single functions (such as antibacterial or negative ion release), and lack the collaborative design of multiple effects (such as temperature control, penetration promotion, formaldehyde adsorption). For example, mineral additives for textiles are difficult to achieve both dynamic temperature control and long-term antibacterial effects; the loading efficiency and transdermal delivery ability of active ingredients by the carrier material of skin care products are insufficient, restricting their application in functional cosmetics.

[0006] (4) Poor application adaptability: The composite process of mineral materials with different substrates (such as polymers, cosmetic matrices) lacks pertinence, resulting in functional attenuation or processing difficulties. For example, directly adding mineral powder to textile fibers is likely to cause spinning breakage, and non-nano-sized mineral particles in skin care products may affect the skin feel and stability. Summary of the Invention

[0007] The present invention provides a novel mineral composite material with high activity, multi-functional adaptability and a green preparation process. Through innovative optimization of mineral ratios, plasma activation modification and biocompatible composite technology, it breaks through the performance bottlenecks of existing materials and expands its high-value-added applications in multiple scenarios, providing core technical support for the development of health functional products.

[0008] The technical solution adopted by the present invention is: a preparation method of a novel mineral crystal active energy new material, comprising the following steps:

[0009] Step 1: Mix natural mineral crystal raw materials of natrolite, tourmaline and picrite in a mass ratio of 5:3:2, and crush them to a nanoscale particle size (50 - 200 nm);

[0010] Step 2: Place the mixed powder obtained in Step 1 in a plasma activation device, and treat it for 10 - 30 minutes at a power of 100 - 500 W in an inert gas environment to form a honeycomb-like porous structure on the surface of the mineral;

[0011] Step 3: Mix the activated mineral powder with a biocompatible carrier material in a ratio of 1:5 - 1:20, and the carrier material is selected from at least one of chitosan, polylactic acid, and cellulose derivatives;

[0012] Step 4: Use ultrasonic dispersion technology to uniformly compound the mixture, and obtain the mineral crystal active energy new material after drying.

[0013] As a further improvement of the present invention, the mineral crystal raw materials in Step 1 contain rare earth element doping, and the doping amount is 0.1% - 1.5% of the total mass.

[0014] As a further improvement of the present invention, the plasma treatment in Step 2 adopts a radio frequency glow discharge mode, with a frequency of 13.56 MHz, and the treatment temperature is controlled at 25 - 60 °C.

[0015] As a further improvement of the present invention, a natural plant antioxidant with a mass fraction of 0.05% - 0.5% is further added in Step 3, and the antioxidant is selected from at least one of tea polyphenols, rosemary extract, and grape seed proanthocyanidins.

[0016] The mineral crystal active energy new material prepared according to the above method has an infrared radiation emissivity ≥ 0.88 (in the 8 - 14 μm band), a negative ion release amount ≥ 1500 pieces / cm 3 , and an antibacterial rate against Staphylococcus aureus ≥ 99%.

[0017] An application of the above-mentioned ore crystal active energy new material in products, where the products include clothing, textiles, skin care products, cosmetics, automotive interiors, and bedding, and the functionalization is achieved in the following ways: in clothing and textile products, the material is melt-spun and coating-finished at a mass ratio of 3-15%; in skin care and cosmetic products, the material is added to the matrix in the form of a nano-dispersion, with a concentration of 0.1-5%; in automotive interior and bedding products, the material is compounded with a polymer, granulated, and then injection-molded.

[0018] As a further improvement of the present invention, in clothing and textile products, the ore crystal active energy new material is compounded with phase change energy storage microcapsules to form intelligent textiles with dual functions of temperature control and negative ion release.

[0019] As a further improvement of the present invention, in skin care and cosmetic products, the ore crystal active energy new material is used as an active carrier to load vitamin C derivatives, and the transdermal penetration rate is increased by more than 40% compared with conventional carriers.

[0020] As a further improvement of the present invention, in automotive interior products, the ore crystal active energy new material is compounded with polyurethane foaming materials, so that the formaldehyde adsorption efficiency of interior components reaches 90% / 24h.

[0021] As a further improvement of the present invention, in bedding products, the ore crystal active energy new material is made into a porous fiber membrane by electrospinning technology and compounded with memory foam to form a sleep-promoting functional layer.

[0022] The beneficial effects of the present invention are as follows: (1) By optimizing the mass ratio of natrolite, tourmaline, and pyrophyllite at 5:3:2, combining nano-scale crushing (50-200nm) and plasma activation technology, the specific surface area and surface active site density of the mineral composite material are significantly improved. The formation of a honeycomb-like porous structure increases the infrared radiation emissivity of the material to ≥0.88 (in the 8-14μm band), and the negative ion release amount reaches ≥1500 ions / cm 3 , and at the same time, the nano-scale particle size enhances the interfacial binding force with the carrier, making the antibacterial rate stably ≥99%, and the durability of the material is increased by more than 30%, overcoming the problems of scattered functions and poor stability of traditional mineral composite materials.

[0023] (2) The present invention uses radio frequency glow discharge plasma activation (13.56MHz, 25-60°C) to precisely control the surface morphology of minerals under the protection of inert gas, avoiding the damage of the crystal structure caused by high temperature or chemical treatment, and reducing the process energy consumption by 40%. By introducing rare earth element doping (0.1%-1.5%) and natural plant antioxidants (such as tea polyphenols), while improving the far-infrared radiation efficiency of the material, long-term antioxidant performance is imparted, realizing the multi-functional synergy of antibacterial, negative ion release, and free radical scavenging, and meeting the composite requirements of high-end health products.

[0024] (3) The present invention designs customized composite solutions for different application scenarios: when compounded with phase change energy storage microcapsules in textiles, it realizes dual functions of temperature control (phase change enthalpy ≥ 80 J / g) and negative ion release, solving the limitation of single performance of traditional functional textiles; as a nano-carrier in skin care products to load vitamin C derivatives, the percutaneous penetration rate is increased by 40%, breaking through the bottleneck of the delivery efficiency of active ingredients; when compounded with polyurethane in automotive interiors, the formaldehyde adsorption efficiency reaches 90% / 24h, with both long-term purification and material mechanical strength (tensile strength ≥ 15 MPa), significantly superior to commercially available adsorption materials.

[0025] (4) The present invention uses biocompatible carriers (such as chitosan and polylactic acid) to replace traditional petrochemical substrates. The material degradation rate is ≥ 70% (180 days), and through ultrasonic dispersion technology, uniform compounding of minerals and carriers is achieved, and the processing yield is increased to more than 95%. The sleep-promoting functional layer formed by compounding an electrospun porous fiber membrane (porosity ≥ 85%) with memory foam realizes the balance of material light weight (density ≤ 0.3 g / cm 3 ) and air permeability (air permeability ≥ 500 L / m 2 / s), reducing production costs by 20% - 30%, and having the potential for large-scale industrialization. Detailed implementation manners

[0026] In order to make the technical problems, technical solutions and beneficial effects to be solved by the present application clearer, the present application will be further described in detail below in conjunction with embodiments. It should be understood that the embodiments described herein are only used to explain the present application and are not used to limit the present application.

[0027] The present invention provides a preparation method of a new type of mineral crystal active energy material, including the following steps:

[0028] Step 1: Mix natural mineral crystal raw materials, natrolite, tourmaline and medallion stone, in a mass ratio of 5:3:2, and crush them to a nano-scale particle size (50 - 200 nm). The mineral crystal raw materials contain rare earth element doping, and the doping amount is 0.1% - 1.5% of the total mass;

[0029] Step 2: Place the mixed powder obtained in Step 1 in a plasma activation device, and process it for 10 - 30 minutes in an inert gas environment at a power of 100 - 500 W to form a honeycomb-like porous structure on the surface of the mineral. The plasma treatment adopts a radio frequency glow discharge mode, with a frequency of 13.56 MHz, and the treatment temperature is controlled at 25 - 60 °C;

[0030] Step 3: Mix the activated mineral powder with the biocompatible carrier material in a ratio of 1:5 - 1:20. The carrier material is selected from at least one of chitosan, polylactic acid, and cellulose derivatives. Further add a natural plant antioxidant with a mass fraction of 0.05% - 0.5%, which is selected from at least one of tea polyphenols, rosemary extract, and grape seed proanthocyanidins;

[0031] Step 4: Use ultrasonic dispersion technology to uniformly compound the mixture, and obtain a new mineral crystal active energy material after drying.

[0032] For the new mineral crystal active energy material prepared according to the above method, the infrared radiation emissivity of the new mineral crystal active energy material is ≥0.88 (in the 8 - 14μm band), the negative ion release amount is ≥1500 pieces / cm 3 , and the antibacterial rate against Staphylococcus aureus is ≥99%.

[0033] An application of the new mineral crystal active energy material as described above in products, the products include clothing, textiles, skin care products, cosmetics, automotive interiors, and bedding, and the functions are realized in the following ways: in clothing and textile products, the material is melt - spun and coated at a mass ratio of 3 - 15%; in skin care and cosmetic products, the material is added to the matrix in the form of a nano - dispersion, with a concentration of 0.1 - 5%; in automotive interior and bedding products, the material is compounded with a polymer and granulated, and then injection - molded.

[0034] In the clothing and textile products of the present invention, the new mineral crystal active energy material is compounded with phase - change energy - storage microcapsules to form an intelligent textile with dual functions of temperature control and negative ion release.

[0035] In the skin care and cosmetic products of the present invention, the new mineral crystal active energy material is used as an active carrier to load vitamin C derivatives, and the percutaneous penetration rate is increased by more than 40% compared with conventional carriers.

[0036] In the automotive interior products of the present invention, the new mineral crystal active energy material is compounded with polyurethane foaming material, so that the formaldehyde adsorption efficiency of interior parts reaches 90% / 24h.

[0037] In the bedding products of the present invention, the new mineral crystal active energy material is made into a porous fiber membrane by electrospinning technology and compounded with memory foam to form a sleep - promoting functional layer.

[0038] Example 1 (Preparation of intelligent textile):

[0039] (I) Raw material ratio: Natrolite: 50g (purity ≥98%); Tourmaline: 30g (particle size D50 = 10μm); Clinochlore: 20g (containing 0.8% lanthanide rare - earth doping); Phase - change energy - storage microcapsules: 15g (phase - change temperature 28 - 32°C, shell material is polymethyl methacrylate); Chitosan: 150g (deacetylation degree ≥90%)

[0040] (II) Preparation steps: (1) Mix natrolite, tourmaline, and medical stone in a ratio of 5:3:2, and pulverize them to an average particle size of 120 nm by high-energy ball milling (rotation speed 1200 rpm, zirconia ball milling medium) to obtain nano-mineral powder; (2) Place the powder in a radio frequency plasma device (frequency 13.56 MHz, argon gas flow rate 50 sccm), and treat it at a power of 300 W and a temperature of 40 °C for 20 minutes to form a honeycomb structure with a surface pore size of 50 - 200 nm; (3) Mix the activated mineral powder and chitosan in a ratio of 1:10, add phase change microcapsules and 0.3% rosemary extract, and treat them by ultrasonic dispersion (frequency 40 kHz, power 500 W) for 1 hour to form a uniform slurry; (4) The slurry is made into fibers by melt spinning (temperature 220 °C), and the proportion of mineral crystal materials in the fibers is 10%. After coating finishing, intelligent textiles are obtained.

[0041] (III) Performance testing:

[0042] Negative ion release amount: Tested according to GB / T 30128-2013, the initial value is 1800 ions / cm 3 , and ≥1550 ions / cm after 50 times of washing 3 ;

[0043] Temperature control performance: The phase change enthalpy measured by differential scanning calorimetry (DSC) is 85 J / g, and the enthalpy retention rate is ≥95% after 100 cycles;

[0044] Bacteriostatic rate: Tested according to GB / T 20944.3-2008, the bacteriostatic rate against Staphylococcus aureus is 99.8%, and the bacteriostatic rate against Escherichia coli is 99.5%.

[0045] Example 2 (Preparation of functional skin care products):

[0046] (I) Raw material ratio: Mineral crystal active energy material: 2 g (particle size 80 nm, modified with 0.5% tea polyphenols); Ethyl ether of vitamin C: 5 g (purity ≥99%); Aqueous phase matrix: 10 g of glycerol, 0.5 g of hyaluronic acid, 82.5 g of deionized water

[0047] (II) Preparation steps: (1) Ultrasonically disperse the mineral crystal material and ethyl ether of vitamin C in an ethanol solution in a ratio of 1:2.5 (30 kHz, 30 minutes), and obtain drug-loaded mineral crystals after vacuum drying; (2) Add the drug-loaded mineral crystals to the aqueous phase matrix and homogenize and emulsify (rotation speed 10000 rpm, 15 minutes) to form a nano-dispersion (average particle size 150 nm, PDI = 0.12); (3) After filling, an essence product is obtained, and the final concentration of the mineral crystal material is 2%.

[0048] (III) Performance testing:

[0049] Transdermal permeability: Franz diffusion cell method (ex vivo porcine skin), the cumulative permeation amount reached 45 μg / cm² in 24 hours 2 , which was 40.6% higher than that of the blank carrier (32 μg / cm² 2 );

[0050] Antioxidant property: The DPPH free radical scavenging rate was 92% (1% concentration), which was higher than that of the control group without added mineral crystals (68%);

[0051] Stability: After 3 months of accelerated test at 40°C / 75% RH, no crystal precipitation occurred, and the retention rate of the active ingredient was ≥90%.

[0052] Example 3 (Formaldehyde adsorption material for automotive interior):

[0053] (I) Raw material ratio: Mineral crystal active energy material: 8 kg (doped with 1.2% cerium element); Polyurethane prepolymer: 100 kg (NCO content 12%); Blowing agent: Cyclopentane 3 kg

[0054] (II) Preparation steps: (1) The mineral crystal material and the polyurethane prepolymer were blended in a twin-screw extruder (temperature 180°C, rotation speed 200 rpm), and compound masterbatch was obtained after pelletizing; (2) The masterbatch and the blowing agent were injected into the mold, and high-pressure foaming (pressure 8 MPa, temperature 60°C) was carried out to form automotive seat foam; (3) The proportion of mineral crystals in the material was 7.5%, and the finished product density was 45 kg / m³ 3 .

[0055] (III) Performance testing:

[0056] Formaldehyde adsorption: Referring to GB / T 27632-2011, the adsorption efficiency in 24 hours was 91.3% (initial formaldehyde concentration 1.0 mg / m³ 3 );

[0057] Mechanical properties: Tensile strength 16.2 MPa, tear strength 4.8 kN / m, which were better than those of unmodified polyurethane (12.5 MPa, 3.5 kN / m);

[0058] Durability: After 500 hours of thermal aging at 50°C, the attenuation rate of the adsorption efficiency was ≤5%.

[0059] Example 4 (Sleep-promoting memory foam mattress):

[0060] (I) Raw material ratio: Mineral crystal porous fiber membrane: 10 m² 2 (porosity 88%, thickness 0.2 mm); Memory foam: thickness 5 cm (density 80 kg / m³ 3 )

[0061] (2) Preparation steps: (1) The ore crystal material is dissolved in an 8% polyvinyl alcohol solution, and electrospun (voltage 25 kV, receiving distance 15 cm) to form a fiber membrane; (2) The fiber membrane and memory foam are thermally pressed and compounded (temperature 110 °C, pressure 0.5 MPa, time 5 minutes) to form a multi-layer structure; (3) The proportion of the ore crystal layer in the finished mattress is 15%, and the density is 0.28 g / cm 3 .

[0062] (3) Performance testing:

[0063] Negative ion release: Continuously release ≥1600 ions / cm under a sleep simulation environment (temperature 25 °C, humidity 60%); 3 ;

[0064] Air permeability: Tested according to GB / T 5453-1997, the air permeability rate is 620 L / m 2 / s;

[0065] Sleep-promoting effect: After 30 subjects used it, the average sleep onset time was shortened by 22% (the control group was shortened by 8%), and the deep sleep duration increased by 35%.

[0066] The above embodiments show that through process innovation and structural design, the present invention has achieved a significant improvement in functional performance in multiple application fields, and has excellent processing stability and market competitiveness.

[0067] In summary, the preparation method of a novel ore crystal active energy new material of the present invention and its application in products not only effectively solve the problems of scattered functions and poor stability of traditional mineral composite materials, but also meet the specific requirements of different application scenarios through a customized composite scheme. In the field of intelligent textiles, this material realizes the dual functions of temperature control and negative ion release, significantly increasing the added value of textiles. In the fields of skin care products and cosmetics, the ore crystal active energy new material as an active carrier significantly improves the transdermal penetration rate of active ingredients, providing new ideas for the development of functional skin care products. In the fields of automotive interiors and bedding, this material exhibits excellent formaldehyde adsorption capacity and sleep-promoting effect, providing strong protection for consumers' health. In addition, the material preparation process of the present invention is environmentally friendly and energy-saving, and the use of biocompatible carrier materials makes the products safer and more environmentally friendly, with the potential for large-scale industrialization.

[0068] The above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, those of ordinary skill in the art should understand that they can still modify the technical solutions described in the foregoing embodiments, or perform equivalent replacements for some of the technical features; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims

1. A preparation method of a new type of mineral crystal active energy new material, characterized in that, It includes the following steps: Step 1: Mix natrolite, tourmaline and medical stone as natural mineral crystal raw materials in a mass ratio of 5:3:2, and crush them to a nanoscale particle size (50 - 200 nm); Step 2: Place the mixed powder obtained in Step 1 in a plasma activation device, and treat it for 10 - 30 minutes at a power of 100 - 500 W in an inert gas environment to form a honeycomb-like porous structure on the mineral surface; Step 3: Mix the activated mineral powder with a biocompatible carrier material in a ratio of 1:5 - 1:20, and the carrier material is selected from at least one of chitosan, polylactic acid, and cellulose derivatives; Step 4: Use ultrasonic dispersion technology to uniformly compound the mixture, and obtain the new mineral crystal active energy material after drying.

2. The preparation method of a new type of mineral crystal active energy new material according to claim 1, characterized in that, The mineral crystal raw material in Step 1 contains rare earth element doping, and the doping amount is 0.1% - 1.5% of the total mass.

3. The preparation method of a new type of mineral crystal active energy new material according to claim 1, characterized in that, In Step 2, the plasma treatment adopts the radio frequency glow discharge mode, with a frequency of 13.56 MHz, and the treatment temperature is controlled at 25 - 60 °C.

4. The preparation method of a new type of mineral crystal active energy new material according to claim 1, characterized in that In Step 3, a natural plant antioxidant with a mass fraction of 0.05% - 0.5% is further added, and it is selected from at least one of tea polyphenols, rosemary extract, and grape seed proanthocyanidins.

5. The new mineral crystal active energy material prepared by the method according to any one of claims 1-4, characterized in that, The infrared radiation emissivity of the new mineral crystal active energy material is ≥ 0.88 (in the 8 - 14 μm band), the negative ion release amount is ≥ 1500 ions / cm 3 , and the antibacterial rate against Staphylococcus aureus is ≥ 99%.

6. The application of the new ore crystal active energy material as described in claim 5 in a product, characterized in that, The products include clothing, textiles, skin care products, cosmetics, automotive interiors, and bedding, and the functions are realized in the following ways: In clothing and textile products, the material is melt-spun and coated at a mass ratio of 3 - 15%; In skin care and cosmetic products, the material is added to the matrix in the form of a nano-dispersion, with a concentration of 0.1 - 5%; In automotive interior and bedding products, the material is compounded with a polymer and granulated, and then injection molded.

7. The application of the new mineral crystal active energy material according to claim 6 in a product, characterized in that, In clothing and textile products, the new mineral crystal active energy material is compounded with phase change energy storage microcapsules to form an intelligent textile with dual functions of temperature control and negative ion release.

8. The application of the new mineral crystal active energy material according to claim 6 in a product, characterized in that, In skin care and cosmetic products, the new mineral crystal active energy material is used as an active carrier to load vitamin C derivatives, and the transdermal penetration rate is increased by more than 40% compared with conventional carriers.

9. The application of the new mineral crystal active energy material according to claim 6 in a product, characterized in that, In automotive interior products, the new mineral crystal active energy material is compounded with polyurethane foaming material, so that the formaldehyde adsorption efficiency of interior parts reaches 90% / 24 h.

10. The application of the new mineral crystal active energy material according to claim 6 in a product, characterized in that, In bedding products, the new mineral crystal active energy material is made into a porous fiber membrane by electrospinning technology and compounded with memory foam to form a sleep-promoting functional layer.