Preparation method of agar nanogel interface modified spray
By preparing an agar nanogel interface-modified spray, the design challenges of pore size and interface characteristics were solved, achieving low-cost and high-efficiency water evaporation and purification effects. It significantly reduces the ion concentration in seawater and removes organic pollutants, and is suitable for solar-powered seawater desalination and water evaporation management.
Patent Information
- Application Number
- CN202410635307.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-05-22
- Publication Date
- 2026-01-09
- Estimated Expiration
- 2044-05-22
AI Technical Summary
Existing technologies make it difficult to simultaneously design pore size and interface properties, resulting in complex, costly, and ineffective water evaporation processes. Furthermore, the composition and ratio of raw materials in molecular self-assembly methods affect the stability of hydrophobic mesoporous structures.
A method for preparing an agar nanogel interface-modified spray was adopted. Through molecular self-assembly technology, agarose, Tween 80 and dimethyl silicone oil were mixed, followed by ultrasonic dissolution, centrifugation and rotary drying to prepare a nanogel with a stable hydrophobic mesoporous structure, which promotes the formation and rapid extraction of water clusters.
It achieves low-cost and high-efficiency water evaporation performance. The nanogel has uniformity and high dispersibility, significantly reduces the ion concentration in seawater, improves water purification efficiency and the ability to remove organic pollutants, and meets the World Health Organization and China's drinking water hygiene standards.
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Figure CN118561358B_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the technical field of water treatment, and particularly to a preparation method of an agar nanogel interface modification spray for improving water evaporation performance and water purification efficiency. The technology can be applied to solar seawater desalination, water evaporation management in the field of agriculture, water molecule decomposition and clean energy production in environmental governance, and coating drying and environmental humidity regulation in industrial production. BACKGROUND
[0002] In view of the shortage of fresh water resources and the aggravation of water pollution, it is an urgent need to develop efficient and low-cost water purification technology. Solar interface evaporation technology, as a new and low-energy water purification technology, has shown great potential in the fields of seawater desalination and wastewater treatment due to its advantages of modularity, portability and low cost. This technology is suitable for resource-limited environments such as exploration, ships, islands and remote villages, as well as emergency drinking water supply. Reducing the heat consumption in the water evaporation process is the core problem of the research. The water cluster evaporation theory points out that the design of the pore channel of the porous material is the key. Nanoscale pores can accelerate the formation of water clusters, and mesoporous materials become the ideal choice for evaporation materials due to their moderate pore size and good water transport capacity. However, the current preparation method is difficult to simultaneously realize the design of pore size and interface properties, and has the defects of complex operation, high cost and poor effect.
[0003] Molecular self-assembly technology provides a template-free and controllable porous material preparation method, which has the advantages of adjustable pore size and channel structure, high specific surface area and pore volume. In particular, the hydrophobic self-assembly method can realize the controllable design of the hydrophobic structure of the mesoporous channel through simple operation, and has high potential in the development of low-enthalpy evaporation materials. However, the composition and ratio of each raw material in the molecular self-assembly technology can affect the stability of the hydrophobic mesoporous structure and the evaporation enthalpy and evaporation rate. Therefore, the molecular hydrophobic self-assembly method successfully constructs agar-based nanogels with uniform size, which has application prospects. SUMMARY
[0004] In view of this, the present application provides a preparation method of an agar nanogel interface modification spray.
[0005] The technical scheme of the present application is implemented as follows:
[0006] A preparation method of an agar nanogel interface modification spray, comprising the following preparation steps:
[0007] S1: the preparation method of the agarose aqueous solution is that agarose powder is weighed according to the g / ml of the material-liquid ratio (0.5-2.0):(48-50), added into deionized water, stirred for 1-1.5 h, the stirring temperature is 85-95 DEG C, the rotating speed is 450-550 rpm, the agarose aqueous solution is obtained, the agarose aqueous solution, Tween 80 and dimethyl silicone oil are mixed according to the volume ratio (1.25-3.75):(0.5-0.8):(12.5-15.0), stirred for 1-1.5 h, the stirring temperature is 85-90 DEG C, the rotating speed is 450-550 rpm, and the coarse emulsion is obtained;
[0008] S2: the coarse emulsion is dissolved into fine emulsion by ultrasonic, the dissolving time is 10-20 min, the rotating speed is 5000-5500 rpm, and the temperature is 50-55 DEG C; the upper suspension is separated, the fine emulsion is cooled to room temperature, placed in a centrifugal tube, the rotating speed is 4500-5500 rpm, and the centrifugal time is 5-10 min, the upper dimethyl silicone oil is recovered, 5-10 ml of tetrahydrofuran is added into the lower separation liquid, placed on a shaking bed and shaken for 3-5 min, mixed and centrifuged, the rotating speed is 4500-5500 rpm, and the time is 5-10 min, the upper transparent silicone oil and tetrahydrofuran mixed liquid are removed, and the agar nanogel mixed liquid is obtained
[0009] S3: the agar nanogel mixed liquid is rotary evaporated and dried, the agar nanogel mixed liquid is placed in a rotary evaporator, the rotating speed is 50-60 r / min, the temperature is 25-30 DEG C, rotary evaporation is carried out for 90-120 min, and the concentrated liquid is obtained after standing for 10-20 min, the concentrated liquid is placed in a vacuum drying oven, dried at 50-65 DEG C for 2-4 h, and the agar nanometer powder is obtained.
[0010] S4: the agar nanometer powder is added into ethanol or water, the agar nanometer powder is added into ethanol, the volume ratio of the agar nanometer powder and ethanol is (0.1-0.2):(1-2), and the amount is 0.4-0.6 kg / m 2 ; the agar nanometer powder is added into water, the volume ratio of the agar nanometer powder and water is (0.1-0.3):(1-2), and the amount is 0.3-0.5 kg / m 2 .
[0011] Preferably, the raw materials of the agar nanogel interface modification spray include the following mass parts: agarose is 35-70 parts, Tween 80 is 40-50 parts, dimethyl silicone oil is 60-150 parts, and tetrahydrofuran is 50-120 parts.
[0012] Compared with the prior art, the application has the beneficial effects that:
[0013] (1) The present application utilizes the non-homogeneous mesoporous structure of the nanogel, and by removing the dimethyl silicone oil, the super-hydrophilic nanogel obtained can maintain a stable hydrophobic mesoporous structure, which can promote the formation of water clusters, quickly guide the water clusters out through the hydrophobic mesoporous channels, and reduce the evaporation enthalpy of water.
[0014] (2) The molecular self-assembly structure of the present application can effectively control the morphology and size of the agar nanogel, and the agar nanogel is a spherical nanoparticle with uniformity and high dispersity.
[0015] (3) After solar distillation using the nanogel of the present application, the concentrations of Na + , Mg 2+ , K + and Ca 2+ in seawater are reduced to 2.16, 0, 1.54, 0.50 mgL -1 , respectively, which is far lower than the World Health Organization and the Chinese Drinking Water Health Standards, and the nanogel of the present application has the effect of purifying seawater.
[0016] (4) The ultraviolet-visible light absorption spectrum analysis of Sudan III solution and methylene blue solution before and after distillation shows that the self-assembled agar nanogel of the present application has strong removal ability for organic solutions, and has the effect of purifying organic contaminated water. BRIEF DESCRIPTION OF DRAWINGS
[0017] Fig. 1 is a graph of the test results of the agar nanogel interface modification spray prepared in Example 1. Figures 1-13
[0018] Figure 1 : Optical microscope (SEM) image of agar nanogel particles;
[0019] Figure 2 : DLS particle size diagram of agar nanogel;
[0020] Figure 3 : Agar nanogel particle size distribution diagram;
[0021] Figure 4 : Schematic diagram of agar nanogel particle structure;
[0022] Figure 5 : Small-angle X-ray scattering (SAXS) diagram of agar nanogel particles;
[0023] Figure 6 : Small-angle X-ray scattering (SAXS) diagram of agar nanogel-kcl;
[0024] Figure 7 : Small-angle neutron scattering (SANS) diagram of agar nanogel;
[0025] Figure 8 : Infrared spectrum of different components of agar nanogel particles
[0026] Figure 9 : Comparison chart of evaporation performance of agar nanogel evaporator with different proportions, pure agar evaporator and pure non-woven fabric evaporator
[0027] Figure 10 : Effect of different spraying doses of agar nanogel on evaporation effect
[0028] Figure 11 : Improvement chart of water evaporation performance of self-assembled agar nanogel on different substrates
[0029] Figure 12 : Chart of concentration change of four common ions in water before and after solar seawater desalination by agar nanogel
[0030] Figure 13 : UV-Vis absorption spectrum of organic dye before and after purification by agar nanogel DETAILED DESCRIPTION
[0031] In order to better understand the technical content of the present application, specific examples are provided below to further illustrate the present application.
[0032] The experimental methods used in the embodiments of the present application are conventional methods unless otherwise specified, and the materials, reagents, etc. used in the embodiments can be obtained from commercial channels.
[0033] Agarose: brand Aladdin, purity > 99.0%;
[0034] Tetrahydrofuran: brand Greagent, purity ≥ 99.5%;
[0035] Tween 80: brand Aladdin, purity 97-100%;
[0036] Dimethicone: brand Aladdin, viscosity -10 mPa.s, neat (25℃), purity 98-99%.
[0037] Example 1
[0038] (1) Take 2.0 g of agarose powder and add it to 50 ml of deionized water, magnetically stir for 1 h, set the temperature to 90℃, and rotate at 500 rpm to obtain an agarose aqueous solution; take 1.5 mL of the agarose aqueous solution, add 0.6 mL of Tween 80 and 15.0 mL of dimethyl silicone oil, mix, heat at 90℃, and magnetically stir for 1 h at a rotation speed of 450 rpm to obtain a crude emulsion.
[0039] (2) The coarse emulsion is ultrasonically dissolved to obtain a fine emulsion, the ultrasonic dissolution time is 10 min, the rotation speed is 5000 rpm, and the temperature is 50℃; the upper suspension is separated, the fine emulsion is cooled to room temperature, placed in a centrifugal tube, the rotation speed is 5000 rpm, the centrifugal time is 10 min, the upper dimethyl silicone oil is recovered by separation, 10 ml of tetrahydrofuran is added to the lower separation liquid, placed on a shaking bed and shaken for 5 min, mixed and centrifuged for 10 min at a rotation speed of 5000 rpm, the upper transparent silicone oil and tetrahydrofuran mixed liquid are removed, and the agar nanogel mixed liquid is obtained.
[0040] (3) The agar nanogel mixed liquid is rotary evaporated and dried, the agar nanogel mixed liquid is placed in a rotary evaporator, the rotation speed is 50 r / min, the temperature is 30℃, rotary evaporation is performed for 100 min, and the concentrated liquid is placed in a vacuum drying box and dried at 50℃ for 2 h to obtain agar nanogel powder.
[0041] (4) The agar nanogel powder is added to ethanol, the volume ratio of agar nanogel powder to ethanol is 0.2:1, and the agar nanogel interface modification spray is obtained.
[0042] Example 2
[0043] (1) 1.0 g of agar powder is added to 48 ml of deionized water, magnetically stirred for 1.5 h, the temperature is set to 95℃, and the rotation speed is 550 rpm to obtain an agar aqueous solution; 1.25 mL of the agar aqueous solution is added to 0.8 mL of Tween 80 and 15.0 mL of dimethyl silicone oil, mixed, heated at 85℃, and magnetically stirred for 1 h at a rotation speed of 550 rpm to obtain a coarse emulsion.
[0044] (2) The coarse emulsion is ultrasonically dissolved to obtain a fine emulsion, the ultrasonic dissolution time is 20 min, the rotation speed is 5500 rpm, and the temperature is 55℃; the upper suspension is separated, the fine emulsion is cooled to room temperature, placed in a centrifugal tube, the rotation speed is 4500 rpm, the centrifugal time is 10 min, the upper dimethyl silicone oil is recovered by separation, 10 ml of tetrahydrofuran is added to the lower separation liquid, placed on a shaking bed and shaken for 5 min, mixed and centrifuged for 10 min at a rotation speed of 5500 rpm, the upper transparent silicone oil and tetrahydrofuran mixed liquid are removed, and the agar nanogel mixed liquid is obtained.
[0045] (3) The agar nanogel mixed liquid is rotary evaporated and dried, the agar nanogel mixed liquid is placed in a rotary evaporator, the rotation speed is 60 r / min, the temperature is 30℃, rotary evaporation is performed for 120 min, and the concentrated liquid is placed in a vacuum drying box and dried at 65℃ for 4 h to obtain agar nanogel powder.
[0046] (4) The agar nanogel powder is added to water, the volume ratio of agar nanogel powder to water is 0.3:1, and the agar nanogel
[0047] Example 3
[0048] (1) 0.6 g of agarose powder was weighed into 48 ml of deionized water, and magnetic stirring was performed for 1 h at a temperature of 90°C and a rotation speed of 550 rpm to obtain an agarose aqueous solution; 1.25 mL of the agarose aqueous solution was added to 0.5 mL of Tween 80 and 12.5 mL of dimethyl silicone oil, mixed, heated at 85°C, and magnetic stirring was performed for 1 h at a rotation speed of 450 rpm to obtain a coarse emulsion.
[0049] (2) The coarse emulsion was ultrasonically dissolved to obtain a fine emulsion, the ultrasonic dissolution time was 10 min, the rotation speed was 5500 rpm, and the temperature was 55°C; the upper suspension was separated, the fine emulsion was cooled to room temperature, placed in a centrifugal tube, the rotation speed was 4500 rpm, and the centrifugation time was 10 min; the upper dimethyl silicone oil was recovered, 10 ml of tetrahydrofuran was added to the lower separation liquid, placed on a shaking bed and shaken for 5 min, mixed and centrifuged for 5 min at a rotation speed of 5500 rpm, and the upper transparent silicone oil and tetrahydrofuran mixture was removed to obtain an agar nanogel mixture.
[0050] (3) The agar nanogel mixture was rotary evaporated and dried, the agar nanogel mixture was placed in a rotary evaporator at a rotation speed of 50 r / min and a temperature of 30°C, rotary evaporation was performed for 120 min, and the mixture was left to stand for 20 min to obtain an agar nanogel concentrate; the concentrate was placed in a vacuum drying oven and dried at 65°C for 4 h to obtain agar nanometer powder.
[0051] (4) The agar nanometer powder was added to ethanol, and the volume ratio of agar nanometer powder to ethanol was 0.2:1 to obtain an agar nanogel interface modification spray.
[0052] Test:
[0053] The agar nanogel interface modification spray prepared in Example 1 was tested.
[0054] Test 1: Morphology analysis
[0055] The morphology and size of the obtained nanogel were observed and analyzed by scanning electron microscopy (SEM).
[0056] The SEM results showed that the self-assembled agar nanogel exhibited a relatively regular nanoparticle structure, as shown in Figure 1 These nanoparticles mainly existed in the form of spherical particles and showed good dispersibility in the SEM image. The size of the nanoparticles was measured by image analysis software, and the results showed that the average diameter of the nanoparticles was about 25 nm. The SEM image results showed that the morphology and size of the agar nanogel could be effectively controlled by molecular self-assembly, and spherical nanoparticles with uniformity and high dispersibility were prepared.
[0057] Figures 2-3The results show that the nanogels prepared by the molecular self-assembly method have very uniform nanoscale size. The size of the nanoparticles is controllable, and gel particles from tens of nanometers to hundreds of nanometers can be prepared. The nanogels have different macroscopic sizes, and except for NG2-10, the nanogels can form a hexagonal phase structure inside the nanoparticles. Figure 4 The structure of the agar nanogel is disclosed, which provides a solid structural basis for subsequent structure-activity relationship studies.
[0058] Test 2: Scattering test
[0059] Small-angle X-ray scattering (SAXS) and agar nanogel small-angle neutron scattering (SANS) are used to observe the internal structure of agar microgel micelles (see Figure 5 、 Figure 7 ), and the injection liquid is a potassium chloride solution and a deuterium water solution.
[0060] According to the small-angle X-ray scattering data, the internal structure of the agar microgel micelles is a hexagonal phase structure, the hexagonal phase column is filled with dimethyl silicone oil, and the continuous phase is a gel network of agar and water (q ratio = 1:3:4), with a d-spacing of 7.25 nm, see Figure 5 . Figure 6 The results show that the small-angle X-ray scattering SAXS scattering curve of the self-assembled agar nanogel shows a typical peak merging feature, which indicates that the potassium chloride solution can enter the internal structure of the columnar phase and the continuous phase at the same time, and the columnar phase channel is in an open state. The small-angle neutron scattering SANS curve of NG1-10 with different deuterium solvent contents can be fitted with a columnar structure model, and the inner diameter of the hexagonal phase cylinder is determined to be about 6.2 nm, see Figure 7 . With the decrease of deuterium water content, the scattering intensity of the columnar phase gradually decreases, indicating that deuterium water can enter the internal channel of the columnar phase, and the scattering contrast difference between the deuterium water and the agar hydrogel gradually decreases until it approaches zero.
[0061] Test 3: Infrared spectrum analysis
[0062] Fourier transform infrared spectroscopy (FTIR) is used to analyze the infrared spectrum of the self-assembled agar nanogel to evaluate the effect of the oil removal treatment.
[0063] The results of the infrared spectrum analysis show that the absorption peaks at specific wave numbers of the agar nanogel before and after the removal of dimethyl silicone oil change, see Figure 8 . After the removal of dimethyl silicone oil, the intensity of the corresponding wave peak in the infrared spectrum of the nanogel decreases. The decrease in wave peak intensity indicates that the content of dimethyl silicone oil in the agar nanogel is significantly reduced during the dimethyl silicone oil removal process. Therefore, the residual amount of silicone oil in the agar nanogel after the removal of dimethyl silicone oil is below the detection level, and it is considered to be completely removed.
[0064] Test 4: Evaporation rate analysis
[0065] Agar nanogel evaporators with different proportions were prepared, with proportions of 0.5wt% 1.25ml, 1.0wt% 1.25ml, 2.0wt% 1.25ml. A control group (without spraying agar nanogel) was set up, and the evaporation efficiency of the test group and the control group was tested.
[0066] The experimental results show that the evaporation rate of the evaporator sprayed with self-assembled agar nanogel is significantly better than that of the control group, as shown in Figure 9 This result shows that the introduction of self-assembled agar nanogel significantly enhances the evaporation efficiency of the evaporator. The spraying of nanogel changes the properties of the evaporator surface, thereby promoting the evaporation of water.
[0067] Test 5: Spraying dosage test
[0068] In order to explore the influence of spraying dosage on evaporation performance, this experiment systematically studied the spraying dosage of self-assembled agar nanogel, as shown in Figure 10 . In the experiment, three different spraying dosages were selected: 0.2kg / m 2 , 0.4kg / m 2 , 0.6kg / m 2 , and the evaporation rate of the corresponding evaporator was measured. The experimental results show that with the increase of spraying dosage, the evaporation rate of the evaporator shows a trend of first increasing and then tending to be stable. Among the three dosages tested, the spraying dosage of 0.4kg / m 2 shows the best evaporation performance, which can achieve an evaporation rate of 3.2kg / m 2 .
[0069] Test 6: Agar nanogel spray universality test
[0070] Agar nanogel was sprayed onto a series of different material substrates (PVA hydrogel, wood, nylon film, fiber paper, non-woven fabric, etc.), and compared with pure agar gel.
[0071] The experimental results show that the evaporation performance of samples sprayed with self-assembled agar nanogel is generally better than that of samples without spraying self-assembled agar nanogel. As shown in Figure 11 , the application of self-assembled agar nanogel spray leads to a significant improvement in the evaporation performance of the substrate material. For the nylon substrate, the evaporation rate after spraying increases from 1.4 to 2.5, with an increase of 74.6%. This improvement effect is verified on different substrate materials, indicating the universality and effectiveness of the technology.
[0072] Test 7: Application of agar nanogel modified evaporator in actual water treatment
[0073] Liquid UV absorption tests of pure water and methyl blue solvent and Sudan III solvent after water purification by using the evaporator modified by agar nanogel particles were carried out. In order to consider the application potential of the self-assembled agar nanogel in real seawater, seawater collected from Yongxing Island of Sansha in the South China Sea was used to collect and test the actual distilled water, and the actual desalination effect was detected.
[0074] In Figure 9 , it can be seen that the contents of the main four ions (Na + , Mg 2+ , K + and Ca 2+ ) in seawater after solar distillation are obviously decreased to 2.16, 0, 1.54 and 0.50 mg / L -1 , respectively, and the concentrations are far lower than the standards of the World Health Organization and the Chinese drinking water health standards. In addition, in order to explore the removal ability of the self-assembled agar nanogel spray on organic dyes in sewage, the UV-visible absorption spectrum analysis of Sudan III solution and methylene blue solution before and after distillation was carried out, as shown in Figures 10-13 , the solution after distillation presents a clear and transparent state, and the characteristic absorption peaks of the methylene blue and methyl orange solutions completely disappear, indicating that the self-assembled agar nanogel has a strong removal ability on organic solutions, which widens the application environment of water treatment in the future practical application.
[0075] Summary Figures 1-13 , through the index determination of the agar nanogel interface modification spray prepared in the embodiment of the present application, it can be known that the agar nanogel interface modification spray has good evaporation performance, has a hexagonal phase columnar structure, and improves the light-heat conversion efficiency and water transmission performance. The agar nanogel interface modification spray prepared in the embodiment of the present application shows good dispersibility in the SEM image, the average diameter of the nanometer particles is about 25 nm, the morphology and size of the agar nanogel can be effectively controlled through molecular self-assembly, and the spherical nanometer particles have uniformity and high dispersibility. The scattering test shows that the agar nanogel micelle is of a hexagonal phase structure, and the inner diameter of the hexagonal phase column is about 6.2 nm, indicating that the pore structure of the agar nanogel interface modification spray is relatively uniform and the property is relatively stable. The evaporation rate analysis result shows that the evaporation rate of the evaporator sprayed with the self-assembled agar nanogel is significantly better than that of the control test without spraying, indicating that the agar nanogel of the embodiment significantly enhances the evaporation efficiency, and the spraying of the nanogel can change the characteristics of the liquid surface, thereby promoting the evaporation of water. The spraying dose test proves that the spraying dose of 0.4 kg / m 2 shows the best evaporation performance and can achieve an evaporation rate of 3.2 kg / m 2 . The seawater test shows that after solar distillation using the nanogel of the present application, the Na+ Mg 2 + K + and Ca 2+ respectively dropped to 2.16, 0, 1.54, 0.50mgL -1 , the concentration is far lower than the World Health Organization and China drinking water health standards. Through the Sudan three solution and methylene blue solution before and after distillation of UV-visible absorption spectrum analysis, using the present application nanogel after distillation solution shows clear and transparent state, and the characteristic absorption peak of methylene blue and methyl orange solution completely disappeared, indicating that the self-assembly agar nanogel on the organic solution strong ability to remove. In summary, the raw materials and methods of the present application prepared agar nanogel interface modification spray has a hexagonal phase column hole stable structure, improve the water surface light heat conversion efficiency, evaporation rate and water transport performance, a large number of tests show that the present application self-assembly agar nanogel on the organic solution strong ability to remove, with simple operation, low cost and good effect of application advantage.
[0076] The above description is only the preferred embodiment of the present application, and is not intended to limit the present application, any modification, equivalent replacement, improvement, etc. within the spirit and principle of the present application should be included in the protection scope of the present application.
Claims
1. A method for preparing an agar nanogel interfacial modification spray, characterized by, The preparation steps include the following: S1: Put agarose into heated deionized water to obtain an agarose aqueous solution, and add a mixture of Tween 80 and dimethyl silicone oil into the aqueous solution to form a coarse emulsion; S2: ultrasonically dissolve the coarse emulsion to obtain a fine emulsion, cool the fine emulsion to room temperature, place it in a centrifuge tube, centrifuge, separate and recover the upper layer of dimethyl silicone oil, add tetrahydrofuran to the lower layer of the separated liquid, place it on a shaking bed and shake, then mix and centrifuge, and then remove the upper layer of transparent dimethyl silicone oil and tetrahydrofuran mixture to obtain an agar nanogel mixture; S3: rotary evaporate and dry the agar nanogel mixture to obtain agar nanometer powder; S4: add ethanol or water to the agar nanometer powder to obtain an agar nanogel interface modified spray.
2. A method of preparing an agar nanogel interfacial modification spray as claimed in claim 1, wherein, By weight: agarose is 35-70 parts, Tween 80 is 40-50 parts, dimethyl silicone oil is 60-150 parts, and tetrahydrofuran is 50-120 parts.
3. A method of preparing an agar nanogel interface-modified spray according to claim 1, characterized by, S1, the preparation method of the agarose aqueous solution is as follows: weigh agarose powder according to the ratio of g / ml of (0.5-2.0):(48-50), add it into deionized water, stir for 1-1.5 h, and the stirring temperature is 85-95℃ and the stirring speed is 450-550 rpm to obtain the agarose aqueous solution.
4. A method of preparing an agar nanogel interface-modified spray according to claim 1, characterized by, S1, the preparation method of the coarse emulsion is as follows: mix the agarose aqueous solution, Tween 80 and dimethyl silicone oil according to the volume ratio of (1.25-3.75):(0.5-0.8):(12.5-15.0), stir for 1-1.5 h, and the stirring temperature is 85-90℃ and the stirring speed is 450-550 rpm to obtain the coarse emulsion.
5. A method of preparing an agar nanogel interface-modified spray according to claim 1, characterized by, S2, the ultrasonic dissolution of the coarse emulsion is performed for 10-20 min at a temperature of 50-55℃; cool the fine emulsion to room temperature, place it in a centrifuge tube, centrifuge at a speed of 4500-5500 rpm for 5-10 min, separate and recover the upper layer of dimethyl silicone oil, add 5-10 ml of tetrahydrofuran to the lower layer of the separated liquid, place it on a shaking bed and shake for 3-5 min, mix and centrifuge at a speed of 4500-5500 rpm for 5-10 min, and then remove the upper layer of transparent dimethyl silicone oil and tetrahydrofuran mixture to obtain the agar nanogel mixture.
6. A method of preparing an agar nanogel interface-modified spray of claim 1, characterized by, S3, the method of rotary evaporation and drying is as follows: place the agar nanogel mixture into a rotary evaporator at a speed of 50-60 r / min and a temperature of 25-30℃, rotary evaporate for 90-120 min, stand for 10-20 min, obtain a gel concentrate, and place the gel concentrate into a vacuum drying oven and dry at 50-65℃ for 2-4 h.
7. A method of preparing an agar nanogel interface-modified spray according to claim 1, wherein S4, add ethanol to the agar nanometer powder, and the volume ratio of the agar nanometer powder to ethanol is (0.1-0.2):(1-2).
8. A method of preparing an agar nanogel interface-modified spray according to claim 1, characterized by, S4, add water to the agar nanometer powder, and the volume ratio of the agar nanometer powder to water is (0.1-0.3):(1-2).
Citation Information
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