CN119119598A - Antibacterial sleep-aiding latex pillow and preparation method thereof - Google Patents
Antibacterial sleep-aiding latex pillow and preparation method thereof Download PDFInfo
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
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Abstract
本发明公开了一种抗菌助眠乳胶枕及其制备方法，涉及乳胶技术领域。本发明先以4‑三甲氧硅基丁醛、间苯二胺‑4‑磺酸钠、固体光气初步改性二氧化硅，能够实现抗菌和防沾灰效果，接着利用天然丝素蛋白、胶原蛋白进一步改性，提高性能的同时，使改性二氧化硅能在天然乳胶表面形成粒子层，并借助改性二氧化硅为成核剂，通过超临界发泡、硫化，二者解封再交联，形成互穿网络结构，提高乳胶枕的力学性能；本发明在发泡过后，还掺入芳香粒子，利用石墨烯气凝胶微球固定负载助眠精油组合物，并用环糊精进行包封，使芳香粒子在使用时才会释放精油释放。The invention discloses an antibacterial sleep-aiding latex pillow and a preparation method thereof, and relates to the technical field of latex. The invention first preliminarily modifies silicon dioxide with 4-trimethoxysilyl butyraldehyde, sodium metaphenylenediamine-4-sulfonate, and solid phosgene, which can achieve antibacterial and anti-dust effects, and then further modifies with natural silk fibroin and collagen to improve the performance while enabling the modified silicon dioxide to form a particle layer on the surface of natural latex, and with the help of modified silicon dioxide as a nucleating agent, through supercritical foaming and vulcanization, the two are unsealed and then cross-linked to form an interpenetrating network structure, thereby improving the mechanical properties of the latex pillow; after foaming, the invention also incorporates aromatic particles, uses graphene aerogel microspheres to fix the load of a sleep-aiding essential oil composition, and uses cyclodextrin for encapsulation, so that the aromatic particles will release the essential oil when in use.
Description
Technical Field
The invention relates to the technical field of latex, in particular to an antibacterial sleep-aiding latex pillow and a preparation method thereof.
Background
The manufacturing process of the latex foam material or the latex pillow core mainly comprises the steps of foaming natural latex by chemical foaming, wherein the smell contained in the chemical foaming agent influences the use appearance of the latex pillow, the chemically foamed natural latex is easy to deform, and the supporting property is not high enough. With the continuous improvement of living standard, people are paying more attention to sanitary, safe and healthy products, and functionalized latex products are also becoming popular with consumers. As the current life rhythm of people is quickened, the life pressure is higher, people with poor sleep wen quality and even insomnia all night are gradually increased, and thus the sleep-aiding pillow is generated.
In addition, the yellowing trace of the pillow can appear after long use, and the reason for the phenomenon is mainly that dust is easy to accumulate on the surface of the pillow, the humidity, the temperature and the sealing degree of the pillow are all favorable for growth and propagation of bacteria and fungi, the common latex pillow does not have the antibacterial and ash-preventing effects, the latex pillow is extremely easy to yellow in the use process, the latex pillow is cleaned for a long time, the internal structure is damaged, and the service life and the use effect of the latex pillow are shortened.
Disclosure of Invention
The invention aims to provide an antibacterial sleep-aiding latex pillow and a preparation method thereof, which are used for solving the problems in the prior art.
In order to solve the technical problems, the invention provides the technical scheme that the antibacterial sleep-aiding latex pillow comprises natural latex, modified silicon dioxide, aromatic particles, a vulcanizing agent and a gelatinizing agent.
Further, the modified silicon dioxide is prepared from 4-trimethoxy silicon butyraldehyde, silicon dioxide, m-phenylenediamine-4-sodium sulfonate, solid phosgene and a protein mixture, wherein the protein mixture is natural silk fibroin and collagen.
The aromatic particles are prepared by spraying an essential oil composition on graphene aerogel microgel and then encapsulating the graphene aerogel microgel with cyclodextrin, wherein the essential oil composition is prepared by mixing tangerine peel essential oil, rose essential oil, lavender essential oil and spina date seed oil.
Further, the preparation method of the antibacterial sleep-aiding latex pillow comprises the following preparation steps:
(1) Mixing pretreated silicon dioxide, m-phenylenediamine-4-sodium sulfonate and absolute ethyl alcohol according to the mass ratio of 0.15:0.2-0.4:15.8, stirring for 20min at 100-200 rpm, dripping 5 drops of glacial acetic acid, reacting for 1.5-2.0 h at 65-72 ℃, cooling to room temperature, carrying out suction filtration, taking a filter cake, washing 3 times with ethanol, and drying for 24h at 70 ℃ to obtain Schiff base silicon dioxide;
(2) Mixing solid phosgene particles and toluene according to a mass ratio of 1:8, stirring and dissolving, heating to 70 ℃, adding a schiff base silica mixed solution with the mass of 9.6-12.2 times of the solid phosgene particles, performing ultrasonic dispersion for 10min at a mass ratio of 1:4, 400-600W, heating to 100-110 ℃, performing heat preservation reaction for 1-3 h, performing suction filtration, and drying at 80 ℃ for 24h to obtain a modified precursor;
(3) Mixing a modified precursor, triethylamine and acetone according to a mass ratio of 5-8:1.5:11-20, stirring for 30min at 500-700 rpm, placing in an ice-water bath, cooling for 10min, adding a protein aqueous solution with 27-44 times of the modified precursor, stirring for 2h at 5000-12000 rpm, heating to 15 ℃, hydrating for 20-30 min, and distilling for 1-3 h at a vacuum degree of-0.06 MPa and a temperature of 40 ℃ to obtain modified silicon dioxide;
(4) Mixing allyl-beta-cyclodextrin, acrylic acid, 2' -azobisisobutyronitrile and N, N-dimethylformamide according to a mass ratio of 1:0.5:0.01:8, sealing and reacting for 24 hours under the protection of nitrogen to obtain a polymer solution, unsealing, adding aromatic microspheres with the mass of 0.1-0.2 times of that of the polymer solution, stirring at 400-600 rpm for 10 minutes, sealing and standing for 3 days, placing in a Soxhlet extractor, extracting with distilled water for 48 hours, placing in a refrigerator, pre-freezing for 24 hours at-50 ℃, freezing for 3-4 hours, and grinding and sieving with a 100-mesh sieve to obtain aromatic particles;
(5) Mixing natural latex and modified silicon dioxide according to a mass ratio of 50:2-5, stirring at 200-400 rpm, adding hydrochloric acid until the pH of the system is 2.7, stopping stirring, reacting at 60 ℃ for 3-5 hours, adding sulfur, potassium oleate, ricinoleic acid, coconut oleic acid and aromatic particles according to a mass ratio of 4-9:1-3:0.5-2:0.5-1:2-8, stirring at 10000rpm for 10-20 minutes, injecting into a mould, vacuumizing, filling carbon dioxide until the pressure is 10-14 MPa, foaming at 70-80 ℃ for 1-3 hours, placing into a steam box at 90-110 ℃ for vulcanization for 30 minutes, and cooling to obtain the antibacterial sleep-aiding latex pillow.
Further, the preparation method of the pretreated silicon dioxide in the step (1) comprises the steps of mixing silicon dioxide and absolute ethyl alcohol according to a mass ratio of 1:23.7, performing ultrasonic dispersion for 10min at 400-600W, adding a silane aqueous solution with a mass ratio of 10-18 times that of the silicon dioxide, uniformly stirring the mixture, reacting for 2-3 h at 60-70 ℃, washing with absolute ethyl alcohol, performing suction filtration until filtrate is clear and transparent, taking a filter cake, and drying for 24h at 70 ℃.
Further, the particle size of the silicon dioxide is 60-100 mu m.
Further, the mass ratio of the natural silk fibroin, the collagen and the ice water in the protein aqueous solution in the step (3) is 3:1:55.
Further, the preparation method of the aromatic microspheres in the step (4) comprises the steps of spraying a plant essential oil composition with the mass of 0.05-0.2 times of that of the graphene aerogel microspheres to the graphene aerogel microspheres, spraying for 3 times, placing the plant essential oil composition in a refrigerator after each spraying, freezing for 30-60 min, rolling the graphene aerogel microspheres once, continuing to spray, placing the graphene aerogel microspheres in the refrigerator after the spraying is completed, and freezing for 24h.
Further, the mass ratio of the tangerine peel essential oil to the rose essential oil to the lavender essential oil to the spine date seed oil in the plant essential oil composition is 0.3-1:1:1:0.1-0.4.
Further, the particle size of the graphene aerogel microspheres is 50-100 microns.
Compared with the prior art, the invention has the following beneficial effects:
The invention adopts natural latex, modified silicon dioxide and aromatic particles as main raw materials, and adopts the modified silicon dioxide as a nucleating agent to obtain the latex pillow through supercritical foaming so as to realize the effects of antibiosis, ash prevention, sleep aiding and allergy prevention.
The invention firstly grafts the silica surface with the siloxane bond of 4-trimethoxy silicon butyraldehyde, then forms Schiff base antibacterial group by utilizing the amino reaction of aldehyde group and m-phenylenediamine-4-sodium sulfonate, then the residual unreacted amino reacts with solid phosgene, isocyanate group is introduced to make it react with active groups such as amino groups and hydroxyl groups of silk fibroin and collagen, further grafts the protein on the silica surface, and the silk fibroin and collagen have excellent biocompatibility, thus the compatibility of modified silica and natural rubber can be promoted, defects among chains can be reduced, the performance of latex molecular chains can be enhanced, in addition, silk fibroin and collagen contain a large amount of hydrophilic groups, trace moisture in the adsorption environment can be formed, molecular conductive layer can be improved, antistatic property can be prevented, dust adsorption of charges can be prevented, and the side chains are connected with sulfonic group-metal ion bonds, so that positive and negative ions can be formed for ionic conduction, and further the anti-dust adhesion capability can be improved.
Secondly, the orange peel essential oil can achieve the sedative effect, the rose essential oil has the effects of regulating qi and resolving depression, and can achieve the effect of well relieving insomnia, the lavender has the sedative effect, the semen zizyphi spinosae oil has the sedative hypnotic effect, the essential oils are mixed and sprayed on the graphene aerogel microspheres, the graphene aerogel microspheres penetrate into the inside of the microspheres along pores, the essential oil components all contain unsaturated double bonds and can form pi-pi conjugation with the unsaturated double bonds on the graphene, so that the essential oil is fixed in the graphene to play a slow release role, then the cyclodextrin is adopted to encapsulate the microspheres, the aromatic particles are not released in the natural environment, and when the cyclodextrin is used, the inclusion effect is reduced after the cyclodextrin is subjected to external pressure, so that the essential oil is released, and the sleep of a user is promoted.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In order to more clearly illustrate the method provided by the invention, the following examples are used for describing the detailed description, and the method for testing each index of the antibacterial sleep-aiding latex pillow manufactured in the following examples is as follows:
antibacterial-the same size examples and comparative examples were taken to test the antibacterial rate with reference to GB/T20944.3.
Sleep aiding, namely adopting a Pittsburgh sleep quality index PSQI to test, selecting 70 test objects, dividing the test objects into 7 groups, randomly selecting 10 persons in each group, and taking an average value after the test objects are used for 3 months, wherein the ages of men and women are 20-60 years.
The embodiment and the comparative example with the same quality are put into a communicated air duct system, standard dust simulating real ash sitting of the atmosphere is added into the air duct system at regular intervals, 20g of standard dust is added into the air duct system every 2h, the fan stops 10 minutes after running for 10 minutes, and the period is regarded as one period, the soot blowing speed is 1-2m/s for 2 days, the ash preventing effect is measured, and the larger the ash preventing effect value is, the better;
anti-dust effect= (weight of latex pillow after dust treatment-weight of latex pillow before dust treatment)/weight of latex pillow before dust treatment x 100%.
Mechanical properties were tested by taking examples and comparative examples of the same size with reference to method A in GB/T6669 at 70℃for 22h and 75% compression, and with reference to GB/T6670 for rebound.
Example 1
(1) Mixing silicon dioxide with the particle size of 60 mu m and absolute ethyl alcohol according to the mass ratio of 1:23.7, performing ultrasonic dispersion for 10min at 400W, adding a silane aqueous solution with the mass ratio of 10 times of the silicon dioxide, uniformly stirring the mixture, reacting for 2h at 60 ℃, washing with absolute ethyl alcohol, performing suction filtration until filtrate is clear and transparent, taking a filter cake, and drying for 24h at 70 ℃ to obtain pretreated silicon dioxide;
(2) Mixing pretreated silicon dioxide, m-phenylenediamine-4-sodium sulfonate and absolute ethyl alcohol according to the mass ratio of 0.15:0.2:15.8, stirring for 20min at 100rpm, dripping 5 drops of glacial acetic acid, reacting for 1.5h at 65 ℃, cooling to room temperature, suction filtering, taking a filter cake, washing 3 times with ethanol, and drying for 24h at 70 ℃ to obtain Schiff base silicon dioxide;
(3) Mixing solid phosgene particles and toluene according to a mass ratio of 1:8, stirring and dissolving, heating to 70 ℃, adding a schiff base silica mixed solution with the mass of 9.6 times of the solid phosgene particles, performing ultrasonic dispersion for 10min with the mass ratio of 1:4 and 400W in the schiff base silica mixed solution, heating to 100 ℃, performing heat preservation reaction for 1h, performing suction filtration, and drying at 80 ℃ for 24h to obtain a modified precursor;
(4) Mixing the modified precursor, triethylamine and acetone according to the mass ratio of 5:1.5:11 at 45 ℃, stirring at 500rpm for 30min, placing in an ice-water bath, cooling for 10min, adding a protein aqueous solution with the mass ratio of 27 times of the modified precursor, stirring at 5000rpm for 2h, heating to 15 ℃ for 20min, distilling at-0.06 MPa and 40 ℃ for 1h at the vacuum degree, and performing suction filtration to obtain modified silicon dioxide;
(5) Mixing pericarpium Citri Tangerinae essential oil, flos Rosae Rugosae essential oil, lavender essential oil and semen Ziziphi Spinosae oil at a mass ratio of 0.3:1:1:0.1, stirring to obtain plant essential oil composition, spraying plant essential oil composition with a mass 0.05 times of that of graphene aerogel microsphere with particle diameter of 50 μm onto graphene aerogel microsphere, spraying for 3 times, placing in refrigerator, freezing for 30min, rolling once, spraying again, placing in refrigerator, and freezing for 24 hr to obtain aromatic microsphere;
(6) Mixing allyl-beta-cyclodextrin, acrylic acid, 2' -azobisisobutyronitrile and N, N-dimethylformamide according to a mass ratio of 1:0.5:0.01:8, sealing and reacting for 24 hours under the protection of nitrogen to obtain a polymer solution, unsealing, adding aromatic microspheres with the mass of 0.1 times of that of the polymer solution, stirring at 400rpm for 10 minutes, sealing and standing for 3 days, placing in a Soxhlet extractor, extracting with distilled water for 48 hours, placing in a refrigerator, pre-freezing for 24 hours, freezing for 3 hours at-50 ℃, grinding, and sieving with a 100-mesh sieve to obtain aromatic particles;
(7) Mixing natural latex and modified silicon dioxide according to a mass ratio of 50:2, stirring at 200rpm, adding hydrochloric acid until the pH of the system is 2.7, stopping stirring, reacting at 60 ℃ for 3 hours, adding sulfur, potassium oleate, ricinoleic acid, coconut oleic acid and aromatic particles according to a mass ratio of 4:1:0.5:0.5:2, stirring at 10000rpm for 10 minutes, injecting into a mould, vacuumizing, filling carbon dioxide until the pressure is 10MPa, foaming at 70 ℃ for 1 hour, placing in a steam box at 90 ℃ for vulcanization for 30 minutes, and cooling to obtain the antibacterial sleep-aiding latex pillow.
Example 2
(1) Mixing silicon dioxide with the particle size of 80 mu m and absolute ethyl alcohol according to the mass ratio of 1:23.7, performing ultrasonic dispersion for 10min at 50W, adding a silane aqueous solution with the mass ratio of 14 times of the silicon dioxide, uniformly stirring the mixture, reacting for 2.5h at 65 ℃, washing with absolute ethyl alcohol, performing suction filtration until filtrate is clear and transparent, taking a filter cake, and drying for 24h at 70 ℃ to obtain pretreated silicon dioxide;
(2) Mixing pretreated silicon dioxide, m-phenylenediamine-4-sodium sulfonate and absolute ethyl alcohol according to the mass ratio of 0.15:0.3:15.8, stirring for 20min at 150rpm, dripping 5 drops of glacial acetic acid, reacting for 1.8h at 65-72 ℃, cooling to room temperature, suction filtering, taking a filter cake, washing 3 times with ethanol, and drying for 24h at 70 ℃ to obtain Schiff base silicon dioxide;
(3) Mixing solid phosgene particles and toluene according to a mass ratio of 1:8, stirring and dissolving, heating to 70 ℃, adding a schiff base silica mixed solution with the mass of 10.9 times of the mass of the solid phosgene particles, performing ultrasonic dispersion for 10min with the mass ratio of the schiff base silica to the toluene of 1:4 and 500W in the schiff base silica mixed solution, heating to 105 ℃, performing heat preservation reaction for 2h, performing suction filtration, and drying at 80 ℃ for 24h to obtain a modified precursor;
(4) Mixing a modified precursor, triethylamine and acetone according to a mass ratio of 6.5:1.5:15.5 at 45 ℃, stirring at 600rpm for 30min, placing in an ice-water bath, cooling for 10min, adding a protein aqueous solution with a mass ratio of 35.5 times that of the modified precursor, stirring for 2h at 8500rpm, heating to 15 ℃, hydrating for 25min, and distilling for 2h at a vacuum degree of-0.06 MPa and 40 ℃ to obtain modified silicon dioxide;
(5) Mixing pericarpium Citri Tangerinae essential oil, flos Rosae Rugosae essential oil, lavender essential oil and semen Ziziphi Spinosae oil at a mass ratio of 0.65:1:1:0.25, stirring to obtain plant essential oil composition, spraying plant essential oil composition with a mass 0.13 times of that of graphene aerogel microsphere with particle diameter of 75 μm to graphene aerogel microsphere, spraying for 3 times, placing in refrigerator, freezing for 45min, rolling once, spraying again, placing in refrigerator, and freezing for 24 hr to obtain aromatic microsphere;
(6) Mixing allyl-beta-cyclodextrin, acrylic acid, 2' -azobisisobutyronitrile and N, N-dimethylformamide according to a mass ratio of 1:0.5:0.01:8, sealing and reacting for 24 hours under the protection of nitrogen to obtain a polymer solution, unsealing, adding aromatic microspheres with the mass of 0.15 times of that of the polymer solution, stirring at 500rpm for 10 minutes, sealing and standing for 3 days, placing in a Soxhlet extractor, extracting with distilled water for 48 hours, placing in a refrigerator, pre-freezing for 24 hours, freezing for 3.5 hours at-50 ℃, grinding, and sieving with a 100-mesh sieve to obtain aromatic particles;
(7) Mixing natural latex and modified silicon dioxide according to a mass ratio of 50:3.5, stirring at 300rpm, adding hydrochloric acid until the pH of the system is 2.7, stopping stirring, reacting at 60 ℃ for 4 hours, adding sulfur, potassium oleate, ricinoleic acid, coconut oleic acid and aromatic particles according to a mass ratio of 6.5:2:1.3:0.7:5, stirring at 10000rpm for 15 minutes, injecting into a mould, vacuumizing, filling carbon dioxide until the pressure is 12MPa, foaming at 75 ℃ for 2 hours, placing into a 100 ℃ steam box, vulcanizing for 30 minutes, and cooling to obtain the antibacterial sleep-aiding latex pillow.
Example 3
(1) Mixing silicon dioxide with the particle size of 100 mu m and absolute ethyl alcohol according to the mass ratio of 1:23.7, performing ultrasonic dispersion for 10min at 600W, adding a silane aqueous solution with the mass of 18 times of the silicon dioxide, uniformly stirring the mixture, performing reaction for 3h at 70 ℃, washing with absolute ethyl alcohol, performing suction filtration until filtrate is clear and transparent, taking a filter cake, and drying for 24h at 70 ℃ to obtain pretreated silicon dioxide;
(2) Mixing pretreated silicon dioxide, m-phenylenediamine-4-sodium sulfonate and absolute ethyl alcohol according to the mass ratio of 0.15:0.4:15.8, stirring for 20min at 200rpm, dripping 5 drops of glacial acetic acid, reacting for 2h at 72 ℃, cooling to room temperature, carrying out suction filtration, taking a filter cake, washing 3 times with ethanol, and drying for 24h at 70 ℃ to obtain Schiff base silicon dioxide;
(3) Mixing solid phosgene particles and toluene according to a mass ratio of 1:8, stirring and dissolving, heating to 70 ℃, adding a schiff base silica mixed solution with the mass of 12.2 times of that of the solid phosgene particles, ultrasonically dispersing for 10min with the mass ratio of 1:4,600W of the schiff base silica in the schiff base silica mixed solution, heating to 110 ℃, carrying out heat preservation reaction for 3h, carrying out suction filtration, and drying at 80 ℃ for 24h to obtain a modified precursor;
(4) Mixing the modified precursor, triethylamine and acetone according to the mass ratio of 8:1.5:20 at 45 ℃, stirring at 700rpm for 30min, placing in an ice-water bath, cooling for 10min, adding a protein aqueous solution with the mass ratio of 44 times of the modified precursor, stirring for 2h at 12000rpm, heating to 15 ℃ for 30min, distilling at-0.06 MPa and 40 ℃ for 3h at vacuum degree, and performing suction filtration to obtain modified silicon dioxide;
(5) Mixing pericarpium Citri Tangerinae essential oil, flos Rosae Rugosae essential oil, lavender essential oil and semen Ziziphi Spinosae oil at a mass ratio of 1:1:1:0.4, stirring to obtain plant essential oil composition, spraying plant essential oil composition with a mass 0.2 times of that of graphene aerogel microsphere with a particle diameter of 100 μm onto graphene aerogel microsphere, spraying for 3 times, placing in refrigerator after each spraying, freezing for 60min, rolling graphene aerogel microsphere once, continuing spraying, placing in refrigerator after spraying, and freezing for 24 hr to obtain aromatic microsphere;
(6) Mixing allyl-beta-cyclodextrin, acrylic acid, 2' -azobisisobutyronitrile and N, N-dimethylformamide according to a mass ratio of 1:0.5:0.01:8, sealing and reacting for 24 hours under the protection of nitrogen to obtain a polymer solution, unsealing, adding aromatic microspheres with the mass of 0.2 times of that of the polymer solution, stirring at 600rpm for 10 minutes, sealing and standing for 3 days, placing in a Soxhlet extractor, extracting with distilled water for 48 hours, placing in a refrigerator, pre-freezing for 24 hours, freezing for 4 hours at-50 ℃, grinding, and sieving with a 100-mesh sieve to obtain aromatic particles;
(7) Mixing natural latex and modified silicon dioxide according to a mass ratio of 50:5, stirring at 400rpm, adding hydrochloric acid until the pH of the system is 2.7, stopping stirring, reacting at 60 ℃ for 5 hours, adding sulfur, potassium oleate, ricinoleic acid, coconut oleic acid and aromatic particles according to a mass ratio of 9:3:2:1:8, stirring at 10000rpm for 20 minutes, injecting into a mould, vacuumizing, filling carbon dioxide until the pressure is 14MPa, foaming at 80 ℃ for 3 hours, placing into a steaming box at 110 ℃ for vulcanization for 30 minutes, and cooling to obtain the antibacterial sleep-aiding latex pillow.
Comparative example 1
The difference between the comparative example 1 and the example 2 is that steps (1) - (4) are not needed, the step (7) is changed into that natural latex and silicon dioxide are mixed according to the mass ratio of 50:3.5, hydrochloric acid is added until the pH value of the system is 2.7 under the stirring of 300rpm, stirring is stopped, after the reaction is carried out for 4 hours under the temperature of 60 ℃, sulfur, potassium oleate, ricinoleic acid, coconut oleic acid and aromatic particles are added according to the mass ratio of 6.5:2:1.3:0.7:5, the mass ratio of the sulfur to the natural latex is 3:50 and 10000rpm, stirring is carried out for 15 minutes, the mixture is injected into a die, vacuumizing and filling carbon dioxide until the pressure is 12MPa and 75 ℃ are carried out for foaming for 2 hours, and then the mixture is placed in a 100 ℃ steam box for vulcanization for 30 minutes, and the antibacterial sleep-aiding latex pillow is prepared after cooling. The rest of the procedure is the same as in example 2.
Comparative example 2
The difference between comparative example 2 and example 2 is that step (2) is not included, step (3) is changed into that solid phosgene particles and toluene are mixed according to the mass ratio of 1:8, stirred and dissolved, then heated to 70 ℃, pretreated silicon dioxide mixed solution with the mass ratio of 10.9 times of the mass of the solid phosgene particles is added, the pretreated silicon dioxide and toluene in the pretreated silicon dioxide mixed solution are subjected to ultrasonic dispersion for 10min at the mass ratio of 1:4,500W, then heated to 105 ℃, subjected to heat preservation reaction for 2h, subjected to suction filtration, and dried at 80 ℃ for 24h to obtain a modified precursor. The rest of the procedure is the same as in example 2.
Comparative example 3
The difference between comparative example 3 and example 2 is that in the absence of step (3), in the step (4), at 45 ℃, schiff base silicon dioxide, triethylamine and acetone are mixed according to the mass ratio of 6.5:1.5:15.5, stirred at 600rpm for 30min, placed in an ice-water bath, cooled for 10min, a protein aqueous solution with the mass ratio of 35.5 times of the mass of the Schiff base silicon dioxide is added, the natural silk fibroin, collagen and ice water in the protein aqueous solution are stirred for 2h at 3:1:55, and then heated to 15 ℃ for hydration for 25min, and then distilled for 2h at 40 ℃ under the vacuum degree of-0.06 MPa, and the modified silicon dioxide is obtained by suction filtration. The rest of the procedure is the same as in example 2.
Comparative example 4
The difference between comparative example 4 and example 2 is that there is no step (6), step (7) is changed to mixing natural latex and modified silicon dioxide according to the mass ratio of 50:3.5, stirring at 300rpm, adding hydrochloric acid until the pH of the system is 2.7, stopping stirring, reacting at 60 ℃ for 4 hours, adding sulfur, potassium oleate, ricinoleic acid, coconut oleic acid and aromatic microspheres according to the mass ratio of 6.5:2:1.3:0.7:5, stirring at 10000rpm for 15 minutes, injecting into a mould, vacuumizing and filling carbon dioxide until the pressure is 12MPa and 75 ℃ for foaming for 2 hours, then placing into a 100 ℃ steam box for vulcanization for 30 minutes, and cooling to obtain the antibacterial sleep-aiding latex pillow. The rest of the procedure is the same as in example 2.
Comparative example 5
The difference between comparative example 5 and example 2 is that step (5) is not included, and step (6) is modified by dissolving beta-cyclodextrin in distilled water with the mass of 50 times that of beta-cyclodextrin, adding a plant essential oil composition according to a wall-core ratio of 3:1, mixing pericarpium citri reticulatae essential oil, rose essential oil, lavender essential oil and spine date seed oil according to a mass ratio of 0.3:1:1:0.1, stirring at 40 ℃ and 400rpm for 3 hours, standing and precipitating for 12 hours, filtering, and drying at 60 ℃ for 5 hours to obtain aromatic particles.
Effect example
The results of performance analysis of the antibacterial sleep-aiding latex pillows using examples 1 to 3 of the present invention and comparative examples 1 to 5 are given in table 1 below.
TABLE 1
As can be found from comparison of rebound experimental data of the embodiment and the comparative example, the modified silicon dioxide is adopted to wrap natural latex particles, and in the vulcanization and foaming processes, the modified silicon dioxide and the natural latex particles are unsealed and crosslinked to form an interpenetrating network structure, so that the mechanical property of the latex pillow is improved; according to comparison of experimental data of the antibacterial rate of the embodiment and the comparative example, the antibacterial capacity of the latex pillow is improved by adopting raw materials such as 4-trimethoprim-butyraldehyde, m-phenylenediamine-4-sodium sulfonate, protein mixture and the like to modify silicon dioxide, leading take seat f alkali and silk fibroin to the surface of the silicon dioxide, and according to comparison of experimental data of the embodiment and the comparative example, the antibacterial capacity of the latex pillow is improved, meanwhile, the silk fibroin and the collagen contain a large amount of hydrophilic groups, the hydrophilic groups can be improved, the slow release effect is enhanced, the cyclodextrin is utilized to encapsulate, the essential oil is prevented from being volatilized at high temperature in the vulcanization process, the sleep-aiding and slow release effects are improved, and according to comparison of experimental data of the embodiment and the comparative example, positive and negative ions are generated on the surface of the silicon dioxide to conduct ionic conduction, the anti-ash-staining capacity is improved, meanwhile, the silk fibroin and the collagen contain a large amount of hydrophilic groups, the natural latex can be improved, the absorption effect of moisture in the natural latex can be effectively improved, the electric conductive layer is prevented from forming dust absorption by electric resistance.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (10)
1. An antibacterial sleep-aiding latex pillow is characterized by comprising natural latex, modified silicon dioxide, aromatic particles, a vulcanizing agent and a gelatinizing agent.
2. The antibacterial sleep-aiding latex pillow according to claim 1, wherein the modified silicon dioxide is prepared from 4-trimethoxy silicon butyraldehyde, silicon dioxide, m-phenylenediamine-4-sodium sulfonate, solid phosgene and a protein mixture, wherein the protein mixture is natural silk fibroin and collagen.
3. The antibacterial sleep-aiding latex pillow according to claim 1, wherein the aromatic particles are prepared by spraying an essential oil composition on graphene aerogel microgel and then encapsulating the graphene aerogel microgel with cyclodextrin, and the essential oil composition is prepared by mixing dried orange peel essential oil, rose essential oil, lavender essential oil and spina date seed oil.
4. The preparation method of the antibacterial sleep-aiding latex pillow is characterized by comprising the following preparation steps:
(1) Mixing pretreated silicon dioxide, m-phenylenediamine-4-sodium sulfonate and absolute ethyl alcohol according to the mass ratio of 0.15:0.2-0.4:15.8, stirring for 20min at 100-200 rpm, dripping 5 drops of glacial acetic acid, reacting for 1.5-2.0 h at 65-72 ℃, cooling to room temperature, carrying out suction filtration, taking a filter cake, washing 3 times with ethanol, and drying for 24h at 70 ℃ to obtain Schiff base silicon dioxide;
(2) Mixing solid phosgene particles and toluene according to a mass ratio of 1:8, stirring and dissolving, heating to 70 ℃, adding a schiff base silica mixed solution with the mass of 9.6-12.2 times of the solid phosgene particles, performing ultrasonic dispersion for 10min at a mass ratio of 1:4, 400-600W, heating to 100-110 ℃, performing heat preservation reaction for 1-3 h, performing suction filtration, and drying at 80 ℃ for 24h to obtain a modified precursor;
(3) Mixing a modified precursor, triethylamine and acetone according to a mass ratio of 5-8:1.5:11-20, stirring for 30min at 500-700 rpm, placing in an ice-water bath, cooling for 10min, adding a protein aqueous solution with 27-44 times of the modified precursor, stirring for 2h at 5000-12000 rpm, heating to 15 ℃, hydrating for 20-30 min, and distilling for 1-3 h at a vacuum degree of-0.06 MPa and a temperature of 40 ℃ to obtain modified silicon dioxide;
(4) Mixing allyl-beta-cyclodextrin, acrylic acid, 2' -azobisisobutyronitrile and N, N-dimethylformamide according to a mass ratio of 1:0.5:0.01:8, sealing and reacting for 24 hours under the protection of nitrogen to obtain a polymer solution, unsealing, adding aromatic microspheres with the mass of 0.1-0.2 times of that of the polymer solution, stirring at 400-600 rpm for 10 minutes, sealing and standing for 3 days, placing in a Soxhlet extractor, extracting with distilled water for 48 hours, placing in a refrigerator, pre-freezing for 24 hours at-50 ℃, freezing for 3-4 hours, and grinding and sieving with a 100-mesh sieve to obtain aromatic particles;
(5) Mixing natural latex and modified silicon dioxide according to a mass ratio of 50:2-5, adding hydrochloric acid to a system pH of 2.7 under stirring at 200-400 rpm, stopping stirring, reacting for 3-5 h at 60 ℃, and mixing according to a mass ratio
Adding sulfur, potassium oleate, ricinoleic acid, coconut acid and aromatic particles into the mixture in a mass ratio of 4-9:1-3:0.5-2:0.5-1:2:2:8, stirring the mixture at 10000rpm for 10-20 min, injecting the mixture into a mold, vacuumizing and filling carbon dioxide to a pressure of 10-14 MPa, foaming the mixture at 70-80 ℃ for 1-3 h, then placing the mixture into a steam box at 90-110 ℃ for vulcanization for 30min, and cooling the mixture to obtain the antibacterial sleep-aiding latex pillow.
5. The preparation method of the antibacterial sleep-aiding latex pillow according to claim 4 is characterized in that the preparation method of the pretreated silicon dioxide in the step (1) comprises the steps of mixing silicon dioxide and absolute ethyl alcohol according to a mass ratio of 1:23.7, performing ultrasonic dispersion for 10min at 400-600W, adding a silane aqueous solution with a mass ratio of 10-18 times that of the silicon dioxide, reacting the silane aqueous solution with 4-trimethoxy silicon butyraldehyde and deionized water for 2-3 h at 60-70 ℃ after stirring uniformly, washing with absolute ethyl alcohol, performing suction filtration until filtrate is clear and transparent, taking a filter cake, and drying for 24h at 70 ℃.
6. The method for preparing the antibacterial sleep-aiding latex pillow according to claim 5, wherein the particle size of the silicon dioxide is 60-100 μm.
7. The method for preparing the antibacterial sleep-aiding latex pillow according to claim 4, wherein the mass ratio of the natural silk fibroin, the collagen and the ice water in the protein aqueous solution in the step (3) is 3:1:55.
8. The preparation method of the antibacterial sleep-aiding latex pillow is characterized by comprising the steps of spraying a plant essential oil composition with the mass of 0.05-0.2 times of that of graphene aerogel microspheres onto the graphene aerogel microspheres in the step (4), spraying for 3 times, placing the plant essential oil composition in a refrigerator after each spraying, freezing for 30-60 min, rolling the graphene aerogel microspheres once, continuing spraying again, placing the graphene aerogel microspheres in the refrigerator after the spraying is completed, and freezing for 24h.
9. The method for preparing the antibacterial sleep-aiding latex pillow according to claim 8, wherein the mass ratio of the tangerine peel essential oil, the rose essential oil, the lavender essential oil and the spina date seed oil in the plant essential oil composition is 0.3-1:1:1:0.1-0.4.
10. The preparation method of the antibacterial sleep-aiding latex pillow according to claim 8, wherein the particle size of the graphene aerogel microspheres is 50-100 microns.
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| US20080213191A1 (en) * | 2007-03-01 | 2008-09-04 | Timothy Alan Scavone | Composition and/or articles comprising cyclodextrin complexing material |
| CN112280118A (en) * | 2020-10-20 | 2021-01-29 | 山东贝隆新材料科技有限公司 | Foaming material prepared by using eucommia ulmoides latex and natural latex together, method and application |
| CN112940359A (en) * | 2021-03-16 | 2021-06-11 | 宁波恩派新材料科技有限公司 | Preparation method of long-acting sleep-aiding latex pillow |
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