A method for preparing amphiphilic oil-absorbing powder for dry hair spray

Abstract

This invention belongs to the field of surface functionalization technology of powder materials, specifically relating to a method for preparing an amphiphilic oil-absorbing powder for dry hair spray. The preparation method includes the following steps: step (1) preparing a starch / silica composite slurry; step (2) preparing a silane coupling agent grafted modified silk fibroin; step (3) preparing a starch / silica / silica composite powder; step (4) preparing a starch / silica / silica / amino acid composite material. This invention uses water-soluble silk fibroin and hydrophobic amino acids to perform dual surface treatment on the starch / silica composite. This is mainly because: silk fibroin can capture high-salt sweat on the hair, forming water-absorbing channels; hydrophobic amino acids can intercept the oil in the hair, establishing oil-absorbing channels; thus obtaining an amphiphilic oil-absorbing powder with both water-absorbing and oil-absorbing functions, which can maintain the hair's freshness, fluffiness and smoothness for a long time.

Description

Technical Field

[0001] This invention belongs to the field of surface functionalization treatment technology of powder materials, and specifically relates to a method for preparing amphiphilic oil-absorbing powder for dry hair spray. Background Technology

[0002] Dry shampoo spray is a no-rinse hair cleaning product primarily used to absorb oil and sweat from the scalp and hair, quickly restoring hair to a clean and bouncy state. It has now become a popular hair care product, on par with shampoos, conditioners, and hair oils. Currently, most dry shampoo sprays are composed primarily of a mixture of starch and silica. However, starch and silica have limited oil-absorbing capacity, so organic surface modification treatment is typically used to improve their oil absorption value.

[0003] Chinese invention patent (ZL202111510521.8) discloses a method for preparing oil-absorbing and fluffy microparticles and dry hair spray. The technical solution involves mixing rice starch granules and highly active polyether polyol, then reacting them with isocyanate to obtain oil-absorbing and fluffy microparticles. While this technical solution improves the oil absorption performance of starch to some extent, the stickiness of starch results in a lack of smoothness and slipperiness in the microparticles. To address this, Chinese invention patent (ZL202411220935.0) provides a method for preparing volumizing microspheres and oil-absorbing particles for use in dry hair spray. The technical solution is as follows: First, volumizing microspheres for use in dry hair spray are prepared using corn starch as a raw material. Then, the volumizing microspheres are mixed with lubricating silica to obtain oil-absorbing particles. However, this technical solution still has the following drawbacks: ① Only a portion of the silica is physically adsorbed onto the surface of the volumizing microspheres, resulting in low bonding force and inability to effectively support the skeletal structure of the microspheres. ① When the oil absorption of the microspheres reaches saturation, structural collapse and other problems are likely to occur; ② The oil-absorbing particles have strong hydrophobicity and poor adsorption performance for sweat on the scalp and hair, making them unsuitable for summer use and having poor universality.

[0004] Therefore, developing an amphiphilic oil-absorbing powder that combines oil and water absorption functions has become the latest development trend in the field of dry hair spray. Summary of the Invention

[0005] In view of the problems existing in the background art, the present invention provides an amphiphilic oil-absorbing powder for use in dry hair spray and its preparation method, which aims to efficiently absorb oil and sweat from the scalp while keeping the hair clean, fluffy and smooth.

[0006] To achieve the above objectives, the present invention is implemented through the following technical solution:

[0007] A method for preparing an amphiphilic oil-absorbing powder for use in dry hair spray, comprising the following preparation steps:

[0008] Step (1): At room temperature, while stirring, dissolve sodium silicate in deionized water to prepare a sodium silicate solution; then add starch to the sodium silicate solution to form a suspension; continue stirring and rapidly and continuously introduce carbon dioxide gas into the suspension to carry out the reaction. When the pH value of the system reaches 7.5 to 8.5, stop the gas introduction to obtain a starch / silica composite slurry.

[0009] Step (2): While stirring, add isocyanate silane coupling agent dropwise to water-soluble silk fibroin powder for dry modification. After the addition is complete, a silane coupling agent grafted modified silk fibroin is obtained.

[0010] Step (3): While stirring, add the silane coupling agent grafted modified silk fibroin obtained in step (2) to the starch / silica composite slurry obtained in step (1); continue stirring and reacting at a temperature of 45℃~55℃, filter, wash, dry and pulverize to obtain a starch / silica / silica composite powder.

[0011] Step (4): Disperse the hydrophobic amino acid in ethanol solvent to prepare an ethanol solution containing amino acid with a mass percentage concentration of 25% to 35%; under the condition of 45℃ to 55℃, while stirring, add the ethanol solution of amino acid dropwise to the starch / silica / silk fibroin composite powder obtained in step (3); after the addition is completed, a starch / silica / silk fibroin / amino acid composite material is obtained.

[0012] Preferably, in step (1) of the present invention, the mass ratio of sodium silicate to deionized water is (0.1-0.2):1, the mass ratio of starch to deionized water is (0.15-0.3):1, and the flow rate of carbon dioxide gas is controlled at 5-10 L / min.

[0013] Preferably, in step (1) of the present invention, the starch particle size is 10-15 μm.

[0014] More preferably, the starch described in this invention is selected from one of cereal starch, potato starch, or legume starch.

[0015] More preferably, the starch described in this invention is selected from one of rice starch, wheat starch, potato starch, corn starch, cassava starch, pea starch, or mung bean starch.

[0016] Preferably, in step (2) of the present invention, the mass ratio of the isocyanate silane coupling agent to the silk fibroin powder is (0.5-1):1.

[0017] Preferably, in step (2) of the present invention, the isocyanate silane coupling agent is selected from one of 3-propyl isocyanatetriethoxysilane, 3-isocyanatepropyltrimethoxysilane or 3-isocyanatepropylmethyldimethoxysilane.

[0018] Preferably, in step (3) of the present invention, the ratio of the total mass of the silane coupling agent grafted modified silk fibroin to the total mass of sodium silicate and starch in step (1) is (0.05-0.1):1.

[0019] Preferably, in step (4) of the present invention, the mass ratio of the hydrophobic amino acid to the starch / silica / silk fibroin composite powder is (0.05~0.15):1.

[0020] More preferably, the hydrophobic amino acid described in this invention is selected from one of alanine, valine, leucine, isoleucine, or proline.

[0021] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0022] 1. This invention utilizes the gas-liquid reaction of carbon dioxide and sodium silicate solution to deposit silica (SiO2·H2O) on the surface of micron-sized starch in a liquid phase. Its advantages are: ① Carbon dioxide first dissolves in water to form carbonic acid, which slowly lowers the pH of the reaction system, allowing silica to precipitate and deposit uniformly on the surface of the micron-sized starch substrate, avoiding the problem of particle agglomeration caused by localized over-acidity; ② Natural starch has disadvantages such as soft texture, high viscosity, and low smoothness. By loading silica onto the surface of the starch substrate, not only can the smoothness of the starch be improved and the stickiness reduced, but it also acts as a supporting framework for the starch, preventing structural collapse due to saturation from oil absorption; ③ Unlike a simple physical mixture of starch and silica, loading silica onto the surface of the starch substrate forms an integral composite, effectively reducing the risk of inhaling small particles such as silica.

[0023] 2. This invention employs an isocyanate silane coupling agent to first graft and modify water-soluble silk fibroin, and then performs organic surface modification with a starch / silica complex. On the one hand, the isocyanate groups in the isocyanate silane coupling agent undergo a chemical grafting reaction with the amino and hydroxyl groups in the water-soluble silk fibroin. On the other hand, the silanol groups generated by the hydrolysis of the isocyanate silane coupling agent undergo a condensation reaction with the silanol groups on the surface of the starch / silica complex to generate Si-O-Si bonds. Ultimately, the water-soluble silk fibroin is chemically bonded to the surface of the starch / silica complex, which can effectively prevent the water-soluble silk fibroin from being in a free state.

[0024] 3. This invention employs water-soluble silk fibroin and hydrophobic amino acids to perform dual surface treatment on the starch / silica complex. This is mainly because: silk fibroin can capture high-salt sweat on the hair, forming water-absorbing channels; hydrophobic amino acids can intercept the hair's oil, establishing oil-absorbing channels; thus obtaining an amphiphilic oil-absorbing powder with both water-absorbing and oil-absorbing functions, which can maintain the hair's freshness, fluffiness, and smoothness for a long time. Attached Figure Description

[0025] Figure 1 This is a polarized microscope image of corn starch from Example 4.

[0026] Figure 2 The image shows a polarized light microscope image of the corn starch / silica composite in step (2) of Example 4.

[0027] Figure 3 A scanning electron microscope (SEM) image of the corn starch / silica composite in step (2) of Example 4 ( Figure 2 (A magnified view of a portion of the image). Detailed Implementation

[0028] The present invention will be further described in detail below with reference to specific embodiments, but the implementation of the present invention is not limited thereto. For process parameters not specifically noted, conventional techniques can be referred to.

[0029] Example 1

[0030] (1) At room temperature, while stirring, 1.0 kg of sodium silicate (Na2SiO3·9H2O, molecular weight 284.2) was dissolved in 10.0 kg of deionized water to prepare a sodium silicate solution. Then, 1.5 kg of rice starch was added to the sodium silicate solution to form a suspension. Stirring continued, and carbon dioxide gas was continuously and rapidly introduced into the suspension to carry out the reaction. The carbon dioxide flow rate was controlled at 5 L / min. When the pH value of the system reached 7.5, the gas was stopped, and a starch / silica composite slurry was obtained.

[0031] (2) While stirring, 0.5 kg of 3-propyltriethoxysilane (Hangzhou Jessica Chemical Co., Ltd.) was added dropwise to 1.0 kg of water-soluble silk fibroin powder (a high molecular weight polypeptide, purchased from Aladdin Chemical Reagent) for dry modification. After the addition was completed, a silane coupling agent grafted modified silk fibroin was obtained.

[0032] (3) While stirring, take 0.25 kg of the silane coupling agent grafted modified silk fibroin obtained in step (2) and add it to the starch / silica composite slurry obtained in step (1). Continue stirring and reacting at a temperature of 45℃ for 6 hours. Filter, wash, dry and pulverize to obtain a starch / silica / silica composite powder.

[0033] (4) Disperse alanine in ethanol solvent to prepare an ethanol solution containing alanine with a mass percentage concentration of 25%. Under the condition of 50°C, while stirring, take 1.0 kg of starch / silica / silk fibroin composite powder obtained in step (3) and add 0.2 kg of ethanol solution containing alanine dropwise; after the addition is completed, a starch / silica / silk fibroin / amino acid composite material is obtained.

[0034] Example 2

[0035] (1) At room temperature, while stirring, 2.0 kg of sodium silicate (Na2SiO3·9H2O, molecular weight 284.2) was dissolved in 10.0 kg of deionized water to prepare a sodium silicate solution. Then, 3.0 kg of wheat starch was added to the sodium silicate solution to form a suspension. Stirring continued, and carbon dioxide gas was continuously and rapidly introduced into the suspension to carry out the reaction. The carbon dioxide flow rate was controlled at 10 L / min. When the pH value of the system reached 8.5, the gas was stopped, and a starch / silica composite slurry was obtained.

[0036] (2) While stirring, 1.0 kg of 3-isocyanate-propyltrimethoxysilane (Hangzhou Jessica Chemical Co., Ltd.) was added dropwise to 1.0 kg of water-soluble silk fibroin powder (a high molecular weight polypeptide, purchased from Aladdin Chemical Reagent) for dry modification. After the addition was completed, a silane coupling agent grafted modified silk fibroin was obtained.

[0037] (3) While stirring, take 0.25 kg of the silane coupling agent grafted modified silk fibroin obtained in step (2) and add it to the starch / silica composite slurry obtained in step (1). Continue stirring and reacting at a temperature of 55℃ for 2 hours. Filter, wash, dry and pulverize to obtain a starch / silica / silica composite powder.

[0038] (4) Disperse valine in ethanol solvent to prepare an ethanol solution containing valine with a mass percentage concentration of 35%. Under the condition of 45℃, while stirring, take 1.0 kg of starch / silica / silk fibroin composite powder obtained in step (3) and add 0.43 kg of valine-containing ethanol solution dropwise; after the addition is completed, a starch / silica / silk fibroin / amino acid composite material is obtained.

[0039] Example 3

[0040] (1) At room temperature, while stirring, 1.5 kg of sodium silicate (Na2SiO3·9H2O, molecular weight 284.2) was dissolved in 10.0 kg of deionized water to prepare a sodium silicate solution. Then, 2.25 kg of cassava starch was added to the sodium silicate solution to form a suspension. Stirring continued, and carbon dioxide gas was continuously and rapidly introduced into the suspension to carry out the reaction. The carbon dioxide flow rate was controlled at 7.5 L / min. When the pH value of the system reached 8.0, the gas was stopped, and a starch / silica composite slurry was obtained.

[0041] (2) While stirring, 0.75 kg of 3-isocyanate-propylmethyldimethoxysilane (Hangzhou Jessica Chemical Co., Ltd.) was added dropwise to 1.0 kg of water-soluble silk fibroin powder (a high molecular weight polypeptide, purchased from Aladdin Chemical Reagent) for dry modification. After the addition was completed, a silane coupling agent grafted modified silk fibroin was obtained.

[0042] (3) While stirring, take 0.28 kg of the silane coupling agent grafted modified silk fibroin obtained in step (2) and add it to the starch / silica composite slurry obtained in step (1). Continue stirring and reacting at 50°C for 4 hours. Filter, wash, dry and pulverize to obtain a starch / silica / silica composite powder.

[0043] (4) Disperse proline in ethanol solvent to prepare an ethanol solution containing proline with a mass percentage concentration of 30%. Under the condition of 55°C, while stirring, take 1.0 kg of starch / silica / silk fibroin composite powder obtained in step (3) and add 0.33 kg of ethanol solution containing proline dropwise; after the addition is completed, a starch / silica / silk fibroin / amino acid composite material is obtained.

[0044] Example 4

[0045] (1) At room temperature, while stirring, 1.8 kg of sodium silicate (Na2SiO3·9H2O, molecular weight 284.2) was dissolved in 10.0 kg of deionized water to prepare a sodium silicate solution. Then, 2.0 kg of corn starch was added to the sodium silicate solution to form a suspension. Stirring continued, and carbon dioxide gas was continuously and rapidly introduced into the suspension to carry out the reaction. The carbon dioxide flow rate was controlled at 8 L / min. When the pH value of the system reached 7.5, the gas was stopped, and a starch / silica composite slurry was obtained.

[0046] (2) While stirring, 0.6 kg of 3-propyltriethoxysilane (Hangzhou Jessica Chemical Co., Ltd.) was added dropwise to 1.0 kg of water-soluble silk fibroin powder (a high molecular weight polypeptide, purchased from Aladdin Chemical Reagent) for dry modification. After the addition was completed, a silane coupling agent grafted modified silk fibroin was obtained.

[0047] (3) While stirring, take 0.25 kg of the silane coupling agent grafted modified silk fibroin obtained in step (2) and add it to the starch / silica composite slurry obtained in step (1). Continue stirring and reacting at a temperature of 50°C for 3 hours. Filter, wash, dry and pulverize to obtain a starch / silica / silica composite powder.

[0048] (4) Leucine was dispersed in ethanol solvent to prepare an ethanol solution containing 28% leucine by mass. At a temperature of 50°C, while stirring, 0.3 kg of the ethanol solution containing leucine was added dropwise to 1.0 kg of the starch / silica / silk fibroin composite powder obtained in step (3); after the addition was completed, a starch / silica / silk fibroin / amino acid composite material was obtained.

[0049] Comparative Example 1

[0050] In Comparative Example 1, the "carbon dioxide gas introduction process" in step (1) of Example 4 was replaced with the "dilute hydrochloric acid addition process". The specific operation steps are as follows:

[0051] (1) At room temperature, while stirring, 1.8 kg of sodium silicate (Na2SiO3·9H2O, molecular weight 284.2) was dissolved in 10.0 kg of deionized water to prepare a sodium silicate solution. Then, 2.0 kg of corn starch was added to the sodium silicate solution to form a suspension. Stirring continued, and hydrochloric acid solution with a molar concentration of 0.5 mol / L was rapidly added dropwise to the suspension to carry out the reaction. When the pH value of the system reached 7.5, the dropwise addition was stopped, and a starch / silica composite slurry was obtained.

[0052] (2) While stirring, 0.6 kg of 3-propyltriethoxysilane (Hangzhou Jessica Chemical Co., Ltd.) was added dropwise to 1.0 kg of water-soluble silk fibroin powder (a high molecular weight polypeptide, purchased from Aladdin Chemical Reagent) for dry modification. After the addition was completed, a silane coupling agent grafted modified silk fibroin was obtained.

[0053] (3) While stirring, take 0.25 kg of the silane coupling agent grafted modified silk fibroin obtained in step (2) and add it to the starch / silica composite slurry obtained in step (1). Continue stirring and reacting at a temperature of 50°C for 3 hours. Filter, wash, dry and pulverize to obtain a starch / silica / silica composite powder.

[0054] (4) Leucine was dispersed in ethanol solvent to prepare an ethanol solution containing 28% leucine by mass. At a temperature of 50°C, while stirring, 0.3 kg of the ethanol solution containing leucine was added dropwise to 1.0 kg of the starch / silica / silk fibroin composite powder obtained in step (3); after the addition was completed, a starch / silica / silk fibroin / amino acid composite material was obtained.

[0055] Comparative Example 2

[0056] In Comparative Example 2, the "corn starch surface coated with silica process" in step (1) of Example 4 was deleted. The specific operation steps are as follows:

[0057] (1) At room temperature, while stirring, add 2.0 kg of corn starch to 10.0 kg of deionized water to form a suspension, and control the pH value of the system to 7.5 to obtain a starch slurry.

[0058] (2) While stirring, 0.6 kg of 3-propyltriethoxysilane (Hangzhou Jessica Chemical Co., Ltd.) was added dropwise to 1.0 kg of water-soluble silk fibroin powder (a high molecular weight polypeptide, purchased from Aladdin Chemical Reagent) for dry modification. After the addition was completed, a silane coupling agent grafted modified silk fibroin was obtained.

[0059] (3) While stirring, take 0.25 kg of the silane coupling agent grafted modified silk fibroin obtained in step (2) and add it to the starch slurry obtained in step (1). Continue stirring and reacting at a temperature of 50°C for 3 hours. Filter, wash, dry and pulverize to obtain a starch / silk fibroin complex powder.

[0060] (4) Disperse leucine in ethanol solvent to prepare an ethanol solution containing leucine with a mass percentage concentration of 28%. Under the condition of 50°C, while stirring, add 0.3 kg of ethanol solution containing leucine to 1.0 kg of starch / silk fibroin composite powder obtained in step (3); after the addition is completed, a starch / silk fibroin / amino acid composite material is obtained.

[0061] Comparative Example 3

[0062] In Comparative Example 3, the "process of coating corn starch with silica" in step (1) of Example 4 is replaced with the "physical mixing process of corn starch and silica". The specific operation steps are as follows:

[0063] (1) At room temperature, while stirring, add 0.38 kg of silica (the mass of silica here is the same as the mass of silica generated by adding 1.8 kg of sodium silicate in the original process, with a particle size of 200 nm) to 10.0 kg of deionized water, then add 2.0 kg of corn starch to form a suspension, continue stirring, and control the pH value of the system to 7.5 to obtain a starch / silica composite slurry;

[0064] (2) While stirring, 0.6 kg of 3-propyltriethoxysilane (Hangzhou Jessica Chemical Co., Ltd.) was added dropwise to 1.0 kg of water-soluble silk fibroin powder (a high molecular weight polypeptide, purchased from Aladdin Chemical Reagent) for dry modification. After the addition was completed, a silane coupling agent grafted modified silk fibroin was obtained.

[0065] (3) While stirring, take 0.25 kg of the silane coupling agent grafted modified silk fibroin obtained in step (2) and add it to the starch / silica composite slurry obtained in step (1). Continue stirring and reacting at a temperature of 50°C for 3 hours. Filter, wash, dry and pulverize to obtain a starch / silica / silica composite powder.

[0066] (4) Leucine was dispersed in ethanol solvent to prepare an ethanol solution containing 28% leucine by mass. At a temperature of 50°C, while stirring, 0.3 kg of the ethanol solution containing leucine was added dropwise to 1.0 kg of the starch / silica / silk fibroin composite powder obtained in step (3); after the addition was completed, a starch / silica / silk fibroin / amino acid composite material was obtained.

[0067] Comparative Example 4

[0068] In Comparative Example 4, step (2) of Example 4 was deleted (i.e., the "isocyanate modification process" was deleted). The specific operation steps are as follows:

[0069] (1) At room temperature, while stirring, 1.8 kg of sodium silicate (Na2SiO3·9H2O, molecular weight 284.2) was dissolved in 10.0 kg of deionized water to prepare a sodium silicate solution. Then, 2.0 kg of corn starch was added to the sodium silicate solution to form a suspension. Stirring continued, and carbon dioxide gas was continuously and rapidly introduced into the suspension to carry out the reaction. The carbon dioxide flow rate was controlled at 8 L / min. When the pH value of the system reached 7.5, the gas was stopped, and a starch / silica composite slurry was obtained.

[0070] (2) While stirring, take 0.25 kg of silk fibroin and add it to the starch / silica composite slurry prepared in step (1). Continue stirring and reacting at a temperature of 50°C for 3 hours. Filter, wash, dry and pulverize to obtain a starch / silica / silica composite powder.

[0071] (3) Leucine was dispersed in ethanol solvent to prepare an ethanol solution containing 28% leucine by mass. At a temperature of 50°C, while stirring, 0.3 kg of the ethanol solution containing leucine was added dropwise to 1.0 kg of the starch / silica / silk fibroin composite powder prepared in step (3); after the addition was completed, a starch / silica / silk fibroin / amino acid composite material was obtained.

[0072] Comparative Example 5

[0073] In Comparative Example 5, steps (2) and (3) of Example 4 were deleted (i.e., the "water-soluble silk fibroin" component was removed). The specific operation steps are as follows:

[0074] (1) At room temperature, while stirring, 1.8 kg of sodium silicate (Na2SiO3·9H2O, molecular weight 284.2) was dissolved in 10.0 kg of deionized water to prepare a sodium silicate solution. Then, 2.0 kg of corn starch was added to the sodium silicate solution to form a suspension. Stirring continued, and carbon dioxide gas was continuously and rapidly introduced into the suspension to carry out the reaction. The carbon dioxide flow rate was controlled at 8 L / min. When the pH value of the system reached 7.5, the gas was stopped, and a starch / silica composite slurry was obtained. Then, the reaction was continued to be stirred at 50℃ for 3 hours. After filtration, washing, drying and pulverizing, a starch / silica composite powder was obtained.

[0075] (2) Leucine was dispersed in ethanol solvent to prepare an ethanol solution containing 28% leucine by mass. Under the condition of 50°C, while stirring, 0.3 kg of ethanol solution containing leucine was added dropwise to 1.0 kg of starch / silica composite powder obtained in step (1); after the addition was completed, a starch / silica / amino acid composite material was obtained.

[0076] Comparative Example 6

[0077] In Comparative Example 6, step (4) of Example 4 was deleted (i.e., the "hydrophobic amino acid" component was removed). The specific operation steps are as follows:

[0078] (1) At room temperature, while stirring, 1.8 kg of sodium silicate (Na2SiO3·9H2O, molecular weight 284.2) was dissolved in 10.0 kg of deionized water to prepare a sodium silicate solution. Then, 2.0 kg of corn starch was added to the sodium silicate solution to form a suspension. Stirring continued, and carbon dioxide gas was continuously and rapidly introduced into the suspension to carry out the reaction. The carbon dioxide flow rate was controlled at 8 L / min. When the pH value of the system reached 7.5, the gas was stopped, and a starch / silica composite slurry was obtained.

[0079] (2) While stirring, 0.6 kg of 3-propyltriethoxysilane (Hangzhou Jessica Chemical Co., Ltd.) was added dropwise to 1.0 kg of water-soluble silk fibroin powder (a high molecular weight polypeptide, purchased from Aladdin Chemical Reagent) for dry modification. After the addition was completed, a silane coupling agent grafted modified silk fibroin was obtained.

[0080] (3) While stirring, take 0.25 kg of the silane coupling agent grafted modified silk fibroin obtained in step (2) and add it to the starch / silica composite slurry obtained in step (1). Continue stirring and reacting at a temperature of 50°C for 3 hours. Filter, wash, dry and pulverize to obtain a starch / silica / silica composite powder.

[0081] Microstructure analysis and characterization:

[0082] Figure 1 This is a polarized light microscope image of corn starch from Example 4. (Source: [Insert source here]) Figure 1 As can be seen, pure corn starch has a particle size in the micrometer range and a smooth surface.

[0083] Figure 2 This is a polarized light microscope image of corn starch coated with silica in step (2) of Example 4. Figure 2 It is evident that the particle size of corn starch does not change significantly before and after being coated with silica.

[0084] Figure 3 This is a scanning electron microscope (SEM) image of corn starch coated with silica from step (2) of Example 4. From... Figure 3 As can be seen, nano-silica is uniformly attached to the surface of micron-sized starch and stacked together to form a rough silica film.

[0085] Performance evaluation:

[0086] The performance of the samples prepared in the examples and comparative examples was evaluated by performance tests, and the test results are shown in Table 1.

[0087] Oil absorption value determination: The oil absorption value of the test samples was determined using the Anton Paar Brabender fully automatic oil absorption instrument and reagent-grade refined flaxseed oil. A certain amount of powder was weighed and added to the fully automatic oil absorption instrument for oil absorption capacity testing. An excessively high oil absorption value will result in rapid oil absorption, leading to dry and frizzy hair; an excessively low oil absorption value will not achieve the desired oil control effect.

[0088] Contact angle: The contact angle of the sample was measured using a KRUSS DSA25 optical water contact angle analyzer from Germany. After the sample was prepared into a disc, water droplets were slowly and controlled to fall onto the sample from the syringe. Each sample was measured three times, and the average value was taken.

[0089] Loose packing density: Refer to GB / T 31057.1-2014 "Physical Properties Test of Particulate Materials - Part 1: Measurement of Loose Packing Density". The lower the loose packing density, the higher the bulkiness of the sample.

[0090] Friction performance testing: The surface friction coefficient of the samples was tested using a KES-SE friction coefficient tester from KATO Corporation of Japan. A fingerprint simulator with an interval of 0.5 mm was used, with a traction force of 0.5 N and a simulator speed of 1 mm / s. The lower the friction coefficient of the sample, the lower the powder roughness, the higher the smoothness, and the better the comfort.

[0091] Table 1

[0092]

[0093]

[0094] As shown in Table 1, the starch / silica / silk fibroin / amino acid composite material prepared by the present invention has a moderate contact angle and certain amphiphilic properties; at the same time, the composite material has better oil absorption, fluffiness and smoothness, and can maintain the hair's freshness and smoothness for a long time.

Claims

1. A method for preparing an amphiphilic oil-absorbing powder for use in dry hair spray, characterized in that: The preparation steps are as follows: Step (1): At room temperature, while stirring, dissolve sodium silicate in deionized water to prepare a sodium silicate solution; then add starch to the sodium silicate solution to form a suspension; continue stirring and rapidly and continuously introduce carbon dioxide gas into the suspension to carry out the reaction. When the pH value of the system reaches 7.5~8.5, stop the gas introduction to obtain a starch / silica composite slurry. Step (2): While stirring, add isocyanate silane coupling agent dropwise to water-soluble silk fibroin powder for dry modification. After the addition is complete, a silane coupling agent grafted modified silk fibroin is obtained. Step (3): While stirring, add the silane coupling agent grafted modified silk fibroin obtained in step (2) to the starch / silica composite slurry obtained in step (1); continue stirring and reacting at a temperature of 45℃~55℃, filter, wash, dry and pulverize to obtain a starch / silica / silica composite powder. Step (4): Disperse the hydrophobic amino acid in ethanol solvent to prepare an ethanol solution containing amino acid with a mass percentage concentration of 25%~35%; under the condition of 45℃~55℃, while stirring, add the ethanol solution of amino acid dropwise to the starch / silica / silk fibroin composite powder obtained in step (3); after the addition is completed, a starch / silica / silk fibroin / amino acid composite material is obtained. In step (1), the mass ratio of sodium silicate to deionized water is (0.1~0.2):1, and the mass ratio of starch to deionized water is (0.15~0.3):1; the flow rate of carbon dioxide gas is controlled at 5~10 L / min. In step (2), the mass ratio of the isocyanate silane coupling agent to the silk fibroin powder is (0.5~1):1; The isocyanate silane coupling agent is selected from one of 3-propyl isocyanatetriethoxysilane, 3-isocyanatepropyltrimethoxysilane, or 3-isocyanatepropylmethyldimethoxysilane; In step (3), the ratio of the total mass of the silane coupling agent-grafted modified silk fibroin to that of sodium silicate and starch in step (1) is (0.05~0.1):1; In step (4), the mass ratio of the hydrophobic amino acid to the starch / silica / silk fibroin composite powder is (0.05~0.15):1; The hydrophobic amino acid is selected from one of alanine, valine, leucine, isoleucine, or proline.

2. The preparation method according to claim 1, characterized in that: In step (1), the starch particle size is 10~15m.

3. The preparation method according to claim 2, characterized in that: The starch is selected from one of cereal starch, potato starch, or legume starch.

4. The preparation method according to claim 3, characterized in that: The starch is selected from one of rice starch, wheat starch, potato starch, corn starch, cassava starch, pea starch, or mung bean starch.

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