A modified inorganic particle and a process for its preparation

Abstract

The application relates to the field of inorganic particle preparation, and particularly discloses modified inorganic particles and a preparation process thereof. The preparation raw materials comprise the following components by weight: component 1: at least one of spherical porous silica, bentonite and diatomite, 100 parts; component 2: at least one of hydrolyzed hyaluronic acid, sodium hyaluronate and zinc hyaluronate, 0.2-5 parts; and component 3: at least one of triethoxyl octyl silane, polydimethylsiloxane, polymethylsiloxane, polydimethylsiloxane alcohol, phenyl silicone oil, lauroyl lysine and hydrogenated lecithin, 0.5-10 parts. The preparation process comprises the following steps: component 2 and a film coating aid are added into deionized water to prepare a solution, and the solution is preserved at 10-15 DEG C; component 1 is placed in a boiling coating machine and suspended in hot air for boiling; the solution is sprayed on component 1, and the temperature is raised to 100-110 DEG C for treatment for 6-8 h to obtain a powder; the powder is added into a high-speed mixer, component 3 is further added and mixed for 20-30 min, and then drying and crushing are carried out to obtain the modified inorganic particles. The hydrolyzed hyaluronic acid and derivatives and the film coating aid are prepared into a solution and sprayed on the suspended and boiled particles to realize coating of the porous particles, compared with a conventional mixing process, the porous particles can be effectively coated, and the effect of reducing oil absorption is realized.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of inorganic particle preparation, more particularly, it relates to a modified inorganic particle and a preparation process thereof. BACKGROUND

[0002] Due to the porous structure, the inorganic porous particles have excellent adsorption property. When they are in contact with liquid, the liquid will be quickly absorbed by the porous surface due to capillary action, so they can quickly absorb oil and have wide application in environmental protection, such as adsorbing leaked oil stains, treating process wastewater, waste liquid, and can also be used for food processing to absorb oil and grease, and daily chemical product to absorb oil and grease.

[0003] In some applications, it is not desirable that the porous particles absorb oil faster. For example, as an active adsorbent, it is desirable that the porous particles do not absorb oil before use to facilitate transportation and storage and improve the adsorption effect during use. For another example, in daily chemical skin care and makeup, the skin is a regulator and needs to quickly restore the balance of water and oil. The faster the porous particles absorb, the more the skin instinctively adjusts to accelerate the secretion of sebum until the absorption of sebum is saturated and the effect is quickly lost. Therefore, slowing down the oil absorption and forming controllable oil absorption is a way to solve the above problems.

[0004] Some products on the market usually mix porous particles with oil control active substances in order to achieve this purpose, but there are several problems. First, the proportion of active substances is generally not high. For liquid active substances, the porous surface of inorganic particles will absorb them into the pores, thereby hiding the active substances and preventing them from playing a role, which reduces the oil absorption of the particles. For solid active substances, due to the complex processing technology, it is difficult to maintain the activity of the active substances during the processing process, and the cost is extremely high.

[0005] Therefore, it is a demand to develop a porous particle that can slow down the oil absorption speed and achieve controllable oil absorption. SUMMARY

[0006] In order to make the inorganic porous particles have the performance of slowing down the oil absorption and achieving controllable oil absorption, the present application provides a modified inorganic particle and a preparation process thereof.

[0007] In the first aspect, the present application provides a modified inorganic particle, and the preparation raw materials thereof include the following components by weight:

[0008] Component 1: at least one of spherical porous silica, porous bentonite, and porous diatomite, 100 parts;

[0009] Component 2: at least one of hydrolyzed hyaluronic acid, sodium hyaluronate, zinc hyaluronate, and water-soluble zinc salt, 0.2-5 parts;

[0010] Component 3: at least one of triethoxyl octyl silane, polydimethylsiloxane, polymethylsiloxane, polydimethylsiloxanol, phenyl silicone oil, lauroyl lysine, hydrogenated lecithin, 0.5-10 parts;

[0011] The preparation process comprises: adding component 2 and a film coating aid into deionized water to prepare a solution, and keeping the solution at 10-15℃; placing component 1 in a boiling coating machine, and suspending and boiling in hot air; spraying the solution on component 1, and heating to 100-110℃ for 6-8h to obtain a powder; adding the powder into a high-speed mixer, and then adding component 3 to mix for 20-30min; and drying and crushing to obtain the modified inorganic particles.

[0012] Spherical porous silica, bentonite and diatomite are all porous particles, and can be used as adsorbent materials. When the inventors sought to solve the problem of oil control, they chose to process the surface of the particles by using a film-forming agent to form a film on the surface of the porous particles, temporarily sealing the surface pores of the porous particles. When applied, the film layer structure can be destroyed by sebum, and the sealed pores are exposed, so that the oil absorption capacity of the porous particles is restored. Hydrolyzed hyaluronic acid and its derivatives are a good choice, and they also have the ability to regulate sebum secretion. The application forms a coating film on the surface of silica by the above-mentioned specific process. It can be understood that the hydrolyzed hyaluronic acid and its derivatives of the application include hydrolyzed hyaluronic acid, hydrolyzed hyaluronic acid salt and other series of substances with the structural characteristics of hyaluronic acid. Direct mixing and stirring of hydrolyzed hyaluronic acid and its derivatives and porous particles can easily be adsorbed or hydrolyzed, and hydrolyzed hyaluronic acid and its derivatives can only adhere to the surface of the porous particles in the form of particulate matter, and cannot form a coating film, and the surface is still porous, which cannot solve the problem of the application. The inventors processed the particles by suspending and boiling, and sprayed the hydrolyzed hyaluronic acid and its derivatives solution, which can better form a coating film on the surface of the porous particles. Cooling the solution at 10-15℃ can leave time for the temperature to rise after spraying, so that the temperature of the sprayed solution and the powder can be left for a certain period of time. The process treats the powder at a temperature of 100-110℃ for 6-8h after spraying the solution. It can be understood that the coating film of the application contains part or trace amount of water, forming a water-based coating film, which greatly increases the processing temperature resistance. Therefore, at a temperature of 100-110℃, the effective film formation can be ensured, and the excess water can be removed. The addition of component 3, which is an organic silicon substance, lauroyl lysine and hydrogenated lecithin, is conducive to the modification of the porous particles to achieve more application fields. The addition of the film coating aid can help hydrolyzed hyaluronic acid and its derivatives to form a coating film better, and reduce the possibility of adsorption of hydrolyzed hyaluronic acid and its derivatives and blockage of the pores of the particles, thereby providing protection for the subsequent recovery of the oil absorption function.

[0013] Preferably, the amount of deionized water is 15-20 times the mass of component 2.

[0014] Preferably, the hot air temperature is 50-70℃.

[0015] Preferably, the component 3 comprises solid and liquid, the input mode comprises inputting solid first, mixing for 10-15min, then inputting liquid, mixing for 10-15min.

[0016] The amount of deionized water can ensure that the hydrolysis of hyaluronic acid and its derivatives forms a uniform spray liquid, the hot air temperature control realizes better suspension boiling of the particles, and the mode of inputting solid first and then inputting liquid is beneficial to the adhesion of the solid to the surface of the modified porous particles, thereby facilitating application.

[0017] Preferably, the mass ratio of component 2 and the coating aid is 1-10:1, preferably 3-8:1, and more preferably 4-6:1.

[0018] Further, preferably, the mass ratio of component 2 and the coating aid is 5:1.

[0019] Preferably, the mass ratio of the pentaerythritol-modified myopeptide and the polyether-modified polysiloxane is 3-5:1.

[0020] Further, preferably, the mass ratio of the pentaerythritol-modified myopeptide and the polyether-modified polysiloxane is 4:1.

[0021] Further, preferably, the polyether-modified polysiloxane contains hydroxyl groups in the molecular chain.

[0022] Preferably, the pentaerythritol-modified myopeptide is obtained by a conventional esterification process. The specific process comprises: adding dimethylbenzene into a reflux device, then adding 88-92 parts by mass of myopeptide and 12-15 parts by mass of pentaerythritol for mixing and stirring, then adding 1 part by mass of p-toluenesulfonic acid, passing nitrogen, and heating to 190-210℃ for 4-6h, and then removing the solvent to obtain the pentaerythritol-modified myopeptide.

[0023] Through a conventional esterification process, esterification occurs between the carboxylic acid in myopeptide and pentaerythritol to generate a pentaerythritol ester with multiple side chains. As can be known, the pentaerythritol ester and the raw material myopeptide do not exclude the use of particles in daily chemicals, thereby being able to broaden the use range of the modified particles.

[0024] The inventors found that when using hydrolyzed hyaluronic acid and its derivatives for coating, some pores on the surface of the porous particles were not well closed, and the oil absorption performance of the coated product after the film was destroyed was significantly lost compared to the original unmodified porous particles; this may be due to some hydrolyzed hyaluronic acid and its derivatives being adsorbed and clogging the pores of the particles during the coating process, resulting in a decrease in oil absorption, which is not conducive to the application of the product, therefore, the inventors seek a better coating that closes and does not clog the pores of the particles. The present application uses pentaerythritol modified myopeptide and polyether modified polysiloxane as a film forming aid, which can further better form a complete coating film on the surface of the particles and reduce the clogging of the pores on the surface of the particles, achieving a slow oil absorption effect while ensuring that the oil absorption capacity after recovery is maintained at a good level. This may be because, on the one hand, pentaerythritol modified myopeptide has a four-side chain claw-like structure, and there is also a hydrogen bond between molecules, which provides a certain support for the coating film formed by hydrolyzed hyaluronic acid and its derivatives on the surface of the particles. The modified myopeptide loses the carboxyl group and has a certain positive charge, and there is also an amino group in the molecule, so it can bond with hydrolyzed hyaluronic acid and its derivatives based on hydrogen bonding or charge bonding. Hydrolyzed hyaluronic acid and its derivatives can achieve better spreading based on the support of pentaerythritol modified myopeptide, reducing the adsorption of hydrolyzed hyaluronic acid and its derivatives by the porous pores; on the other hand, the bonding of pentaerythritol modified myopeptide and hydrolyzed hyaluronic acid is conducive to the dispersion of hydrolyzed hyaluronic acid, the imidazole ring in pentaerythritol modified myopeptide has a certain steric effect, promoting the better dispersion of hydrolyzed hyaluronic acid and its derivatives, which is conducive to the formation of a continuous film; and polyether modified polysiloxane can reduce the surface tension and improve the spreading property, which is conducive to the formation of the film. The silicon-oxygen bond of polyether modified polysiloxane reduces the surface tension and modifies the segment deep into the solution system, and the hydroxyl group in the segment can further enhance the bonding between the components in the film, thereby improving the film coating strength and reducing the adsorption of hydrolyzed hyaluronic acid and its derivatives by the pores on the surface of the particles to clog the pores.

[0025] A mass ratio of pentaerythritol modified myopeptide and polyether modified polysiloxane of 4:1 can achieve better results in reducing pore clogging, which may be due to the adjustment of the ratio, enabling pentaerythritol modified myopeptide and polyether modified polysiloxane to better cooperate, and jointly improving the film strength and particle coverage. Too little pentaerythritol modified myopeptide may result in insufficient film strength, and hydrolyzed hyaluronic acid and its derivatives are easily adsorbed by the pores, while too much pentaerythritol modified myopeptide and too little polyether modified polysiloxane result in slow solution spreading, poor coating completeness, and reduced bonding between components by the hydroxyl group in polyether modified polysiloxane, which is also easily adsorbed by the pores. Therefore, by adjusting the ratio of the film forming aid, the film can be better formed while reducing pore clogging, maintaining the oil absorption capacity after the film is removed, and obtaining inorganic porous particles that can achieve slow oil control.

[0026] In another aspect, the present application provides a method for preparing modified inorganic particles, comprising the following steps:

[0027] Step one: add component 2 and film coating aids to 50-70℃ deionized water with 15-20 times the mass of component 2, stir until completely dispersed, and store in a water bath, keeping the water bath temperature at 10-15℃ until the solution is completely isothermal;

[0028] Step two: place component 1 in a fluidized bed coater, pass air through it, and set the air temperature to 50-70℃, so that component 1 is suspended and fluidized under the action of hot air;

[0029] Step three: place the solution prepared in step one in a pressure tank, and spray it onto component 1 through a nozzle; Step four: continue for 20-40min, increase the air temperature to 100-110℃, and continue for 6-8h to obtain a powder;

[0030] Step five: place the obtained powder into a high-speed mixer, set the speed to 1200-1500rpm, and then add component 3 and mix for 20-30min;

[0031] Step six: place the mixed powder into an oven, set the temperature to 100-110℃, and dry for 15-20h;

[0032] Step seven: dry the powder, and then crush it with a hammer crusher to obtain the finished product.

[0033] Preferably, component 3 contains solids and liquids, and the addition method comprises first adding solids and mixing for 10-15min, and then adding liquids and mixing for 10-15min.

[0034] It can be known that the modified particles obtained by the preparation process of the present application have the above-mentioned performance effects, and through reasonable setting of process parameters, better particle processing can be achieved. In addition, when component 3 contains solids, the feeding method of first adding solids and then adding liquids is beneficial to the adhesion of solids to the film.

[0035] In summary, the present application has at least the following beneficial effects:

[0036] 1. The present application sprays a solution prepared by hydrolyzing hyaluronic acid and its derivatives and film coating aids onto particles that are suspended and fluidized, realizes coating of porous particles, and compared with conventional mixing processes, can realize effective coating of porous particles instead of adhering to porous particles in the form of particles, thereby achieving the effect of slowing down oil control.

[0037] 2、The application can further better form a complete coating film on the surface of the particles and reduce the blockage of the voids on the surface of the particles by using pentaerythritol modified myopeptide and polyether modified polysiloxane as a coating aid, so as to achieve the effect of slowing down oil absorption while ensuring that the subsequent oil absorption capacity is maintained at a good level.

[0038] 3、The application can obtain a better effect of reducing pore blockage by controlling the mass ratio of pentaerythritol modified myopeptide and polyether modified polysiloxane to be 4:1, and by adjusting the ratio, the pentaerythritol modified myopeptide and polyether modified polysiloxane can better cooperate to jointly improve the coating strength and particle covering capacity, so as to obtain inorganic porous particles capable of achieving slow oil control. BRIEF DESCRIPTION OF DRAWINGS

[0039] Figure 1 It is an SEM electron micrograph of the modified porous inorganic particles of Example 1 of the application;

[0040] Figure 2 It is an SEM electron micrograph of the modified porous inorganic particles of Example 2 of the application;

[0041] Figure 3 It is an SEM electron micrograph of the modified porous inorganic particles of Example 3 of the application;

[0042] Figure 4 It is an SEM electron micrograph of the modified porous inorganic particles of Example 4 of the application;

[0043] Figure 5 It is an SEM electron micrograph of the raw material unmodified spherical porous silica used in the application;

[0044] Figure 6 It is a comparison chart of the oil absorption amount of D5 silicone oil by the untreated silica and the silica treated in the example;

[0045] Figure 7 It is a comparison chart of the oil absorption amount of D5 silicone oil by the reduced silica after the coating film is destroyed in the example;

[0046] Figure 8 It is an application comparison chart of the silica and the conventional treated silica. DETAILED DESCRIPTION

[0047] To further help understand the technical solutions of the application, several specific examples are provided to describe the technical solutions of the application in more detail, and all the described examples are only part of the examples of the application, not all; the examples can be combined with each other, and the same or similar concepts or processes may not be described again in some examples. The following examples are further illustrations of the application, and the application is not limited thereto.

[0048] The raw materials used in the examples and preparation examples of the present application are all conventional commercially available brands, or can be prepared according to conventional processes. The spherical porous silica is SILIA LX-7, the hydrolyzed hyaluronic acid is hydrolyzed hyaluronic acid HA-TLM 3-5 from Huaxi Biology, the zinc hyaluronate is HA-ZN from Huaxi Biology, the dimethicone is Dow Corning PMX-200, the hydrogenated lecithin is S-10 from Japan Nikkoh, the polyether modified polysiloxane is hydroxyl polyether polyester copolymer modified polysiloxane Klamar 8244, and the carnosine is L-carnosine, which is purchased from Zhejiang Yicun Biology Technology. Examples

[0049] The preparation method of the pentaerythritol modified carnosine in the examples of the present application is as follows: 200 mL of xylene is added to a reflux device, and then 90.5 g of carnosine and 13.6 g of pentaerythritol are mixed and stirred, followed by the addition of 1 g of p-toluenesulfonic acid. Nitrogen is introduced, and the temperature is raised to 200°C for 5 h. After the reaction is completed, the solvent is removed to obtain the pentaerythritol modified carnosine. Examples

[0050] Preparation steps of the modified inorganic particles:

[0051] Component 1: spherical porous silica

[0052] Component 2: hydrolyzed hyaluronic acid

[0053] Component 3: triethoxysilane, dimethicone

[0054] Step one: 0.11 kg of hydrolyzed hyaluronic acid, 17.6 g of pentaerythritol modified carnosine, and 4.4 g of polyether modified polysiloxane are added to 2.2 kg of 60°C deionized water, stirred for 15 min until completely dispersed, and placed in a water bath for storage. The temperature of the water bath is kept at 12°C until the solution is completely isothermal;

[0055] Step two: 10 kg of spherical porous silica is placed in a fluidized bed coating machine, and air is introduced. The air temperature is 60°C, and the spherical porous silica is suspended and boiled under the action of hot air;

[0056] Step three: the solution prepared in step one is placed in a pressure tank and sprayed onto the spherical porous silica through a nozzle until the spraying is completed;

[0057] Step four: continue to work for 30 min, and increase the air temperature to 105°C. Continue for 7 h to obtain the powder;

[0058] Step five: the obtained powder is put into a high-speed mixer, and 0.45 kg of dimethicone and 0.22 kg of triethoxysilane are sequentially added thereto at a speed of 1350 rpm. Mix for 25 min, and then stop mixing;

[0059] Step six: the mixed powder is placed in an oven, the temperature is set to 105°C, and dried for 18h;

[0060] Step seven: the dried powder is crushed by a hammer crusher to obtain the finished product. Example

[0061] Modified inorganic particle preparation steps:

[0062] Component 1: spherical porous silica

[0063] Component 2: zinc hyaluronate

[0064] Component 3: triethoxysilane, hydrogenated lecithin

[0065] Step one: 0.11 kg of zinc hyaluronate, 17.6 g of pentaerythritol modified myopeptide, and 4.4 g of polyether modified polysiloxane are added to 2.2 kg of 60°C deionized water, stirred for 20 min until completely dispersed, and stored in a water bath, the water bath temperature is kept at 11°C until the solution is completely isothermal;

[0066] Step two: 10 kg of spherical porous silica is placed in a fluidized bed coater, air is introduced, and the air temperature is 65°C, so that the spherical porous silica is suspended and boiled under the action of hot air;

[0067] Step three: the solution prepared in step one is placed in a pressure tank and sprayed on the spherical porous silica through a nozzle until the liquid spraying is finished;

[0068] Step four: continue to work for 30 min, increase the air temperature to 105°C, and continue for 7h to obtain the powder;

[0069] Step five: the obtained powder is put into a high-speed mixer, the speed is 1300 rpm, 0.05 kg of hydrogenated lecithin is added and mixed for 10 min, then 0.5 kg of triethoxysilane is added and mixed for 15 min, and the mixing is finished;

[0070] Step six: the mixed powder is placed in an oven, the temperature is set to 105°C, and dried for 18h;

[0071] Step seven: the dried powder is crushed by a hammer crusher to obtain the finished product. Example

[0072] Example 3 and example 1 have approximately the same process steps, the only difference is that the film forming aid of example 3 is only pentaerythritol modified myopeptide.

[0073] Modified inorganic particle preparation steps:

[0074] Component 1: spherical porous silica

[0075] Component 2: Hydrolyzed hyaluronic acid

[0076] Component 3: Triethoxysilane, polydimethylsiloxane

[0077] Step one: 0.11 kg of hydrolyzed hyaluronic acid, 22 g of pentaerythritol modified myopeptide is added to 2.2 kg of 60°C deionized water, stirred for 15 min until completely dispersed, placed in a water bath for storage, and the water bath temperature is kept at 12°C until the solution is completely isothermal;

[0078] Step two: 10 kg of spherical porous silica is placed in a fluidized bed coating machine, air is introduced, and the air temperature is 60°C, so that the spherical porous silica is suspended and boiled under the action of hot air;

[0079] Step three: the solution prepared in step one is placed in a pressure tank and sprayed onto the spherical porous silica through a nozzle until the liquid spraying is finished;

[0080] Step four: continue to work for 30 min, increase the air temperature to 105°C, and continue for 7 h to obtain the powder;

[0081] Step five: the obtained powder is put into a high-speed mixer, the speed is 1350 rpm, and 0.45 kg of polydimethylsiloxane and 0.22 kg of triethoxysilane are sequentially added thereto; mix for 25 min, and end the mixing;

[0082] Step six: the mixed powder is placed in an oven, the temperature is set to 105°C, and dried for 18 h;

[0083] Step seven: the dried powder is crushed by a hammer crusher to obtain the finished product. Example

[0084] Example 4 has substantially the same process steps as example 1, the only difference is that the film forming aid of example 4 is only polyether modified polysiloxane.

[0085] Modified inorganic particle preparation steps:

[0086] Component 1: Spherical porous silica

[0087] Component 2: Hydrolyzed hyaluronic acid

[0088] Component 3: Triethoxysilane, polydimethylsiloxane

[0089] Step one: 0.11 kg of hydrolyzed hyaluronic acid, 22 g of polyether modified polysiloxane is added to 2.2 kg of 60°C deionized water, stirred for 15 min until completely dispersed, placed in a water bath for storage, and the water bath temperature is kept at 12°C until the solution is completely isothermal;

[0090] Step two: 10 kg of spherical porous silica is placed in a fluidized bed coater, air is introduced, the air temperature is 60℃, and the spherical porous silica is suspended and boiled under the action of hot air;

[0091] Step three: the solution prepared in step one is placed in a pressure tank and sprayed on the spherical porous silica through a nozzle until the spraying is completed;

[0092] Step four: continue to work for 30 min, increase the air temperature to 105℃, and continue for 7 h to obtain the powder;

[0093] Step five: the obtained powder is put into a high-speed mixer, the speed is 1350 rpm, and then 0.45 kg of polydimethylsiloxane and 0.22 kg of triethoxysilane are sequentially added thereto; mix for 25 min, and end the mixing;

[0094] Step six: the mixed powder is placed in an oven, the temperature is set to 105℃, and dried for 18 h;

[0095] Step seven: the dried powder is crushed by a hammer crusher to obtain the finished product.

[0096] By attaching Figures 1-2 , attaching Figure 5 It can be seen that after the process of embodiments 1 and 2, the hydrolyzed hyaluronic acid and its derivatives are coated on the surface of the spherical porous silica to form a relatively smooth film layer, which effectively seals the pores on the surface of the silica.

[0097] By attaching Figure 1 , 3 -4 can be seen that compared with using an equal amount of pentaerythritol modified myopeptide or polyether modified polysiloxane alone as a coating aid, the coating aid with a mass ratio of pentaerythritol modified myopeptide and polyether modified polysiloxane 4:1 selected in embodiment 1 can coat more surface pores and achieve better coating effect. The combination of pentaerythritol modified myopeptide and polyether modified polysiloxane can jointly improve the coating strength and particle covering capacity, so as to form a relatively complete and smooth coating film.

[0098] Figure 6 The oil absorption amount of the untreated porous silica of the present application and the silica powder coated with hydrolyzed hyaluronic acid obtained in step four of embodiments 1, 3 and 4 to D5 silicone oil is compared. The oil absorption amount test method is: 5 g of powder is placed on a glass platform, D5 silicone oil is added thereto, and a stainless steel stirring knife is used to stir, until the powder is agglomerated into a lump. The oil absorption amount = the weight of the absorbed silicone oil / the weight of the powder*100, i.e. the oil absorption amount = the weight of the absorbed silicone oil / the weight of the powder, multiplied by 100. It can be understood that the test and calculation formula is a conventional oil absorption test and expression method.

[0099] By Figure 6 It can be seen that the untreated silica oil original oil absorption is 163.47, the oil absorption of Example 1 is 46.20, the oil absorption of Example 3 is 65.35, and the oil absorption of Example 4 is 72.16. Compared with the untreated silica, the silica coated with hydrolyzed hyaluronic acid in Example 1, Example 3 and Example 4 all show a large decrease in oil absorption, further proving that the particle modification of the present application has the effect of closing pores and slowing down oil absorption; while the oil absorption of Example 3 and 4 is slightly higher than that of Example 1, indicating that the combination of pentaerythritol modified myopeptide and polyether modified polysiloxane is conducive to forming a better coating film and further slowing down oil absorption. Example

[0100] The process steps of Example 5 are basically the same as those of Example 1, the only difference being that the film coating aid of Example 5 is pentaerythritol modified myopeptide and polyether modified polysiloxane in a mass ratio of 1:1.

[0101] Preparation steps of modified inorganic particles:

[0102] Component 1: spherical porous silica

[0103] Component 2: hydrolyzed hyaluronic acid

[0104] Component 3: triethoxysilane, polydimethylsiloxane

[0105] Step one: add 0.11 kg of hydrolyzed hyaluronic acid, 11 g of pentaerythritol modified myopeptide, and 11 g of polyether modified polysiloxane to 2.2 kg of 60°C deionized water, stir for 15 min until completely dispersed, and store in a water bath, keeping the water bath temperature at 12°C until the solution is completely isothermal;

[0106] Step two: place 10 kg of spherical porous silica in a fluidized bed coater, pass air, and set the air temperature to 60°C, so that the spherical porous silica is suspended and boiled under the action of hot air;

[0107] Step three: place the solution prepared in step one in a pressure tank, and spray it onto the spherical porous silica through a nozzle until the spraying is complete;

[0108] Step four: continue to work for 30 min, increase the air temperature to 105°C, and continue for 7 h to obtain the powder;

[0109] Step five: put the obtained powder into a high-speed mixer, set the speed to 1350 rpm, and then add 0.45 kg of polydimethylsiloxane and 0.22 kg of triethoxysilane into the mixer; mix for 25 min, and then stop mixing;

[0110] Step six: place the mixed powder in an oven, set the temperature to 105°C, and dry for 18 h;

[0111] Step seven: the dried powder is put into a hammer crusher to be crushed to obtain the finished product. Example

[0112] Example 6 has substantially the same process steps as example 1, the only difference is that the coating aid of example 6 is pentaerythritol modified myopeptide and polyether modified polysiloxane with a mass ratio of 6:1.

[0113] Modification of inorganic particle preparation steps:

[0114] Component 1: spherical porous silica

[0115] Component 2: hydrolyzed hyaluronic acid

[0116] Component 3: triethoxysilane, polydimethylsiloxane

[0117] Step one: 0.11 kg of hydrolyzed hyaluronic acid, 18.86 g of pentaerythritol modified myopeptide, 3.14 g of polyether modified polysiloxane are added to 2.2 kg of 60°C deionized water, stirred for 15 min until completely dispersed, placed in a water bath for storage, and the water bath temperature is kept at 12°C until the solution is completely isothermal;

[0118] Step two: 10 kg of spherical porous silica is placed in a fluidized bed coating machine, air is introduced, and the air temperature is 60°C, so that the spherical porous silica is suspended and boiled under the action of hot air;

[0119] Step three: the solution prepared in step one is placed in a pressure tank and sprayed on the spherical porous silica through a nozzle until the liquid spraying is finished;

[0120] Step four: continue to work for 30 min, increase the air temperature to 105°C, and continue for 7 h to obtain the powder;

[0121] Step five: the obtained powder is put into a high-speed mixer, the speed is 1350 rpm, and 0.45 kg of polydimethylsiloxane and 0.22 kg of triethoxysilane are sequentially added thereto; mix for 25 min, and end the mixing;

[0122] Step six: the mixed powder is put into an oven, the temperature is set to 105°C, and dried for 18 h;

[0123] Step seven: the dried powder is put into a hammer crusher to be crushed to obtain the finished product.

[0124] The powder obtained from step four of example 1, example 3-4, example 5-6 was subjected to oil recovery experiment: the envelope was destroyed by artificial sebum, and then the oil absorption test was carried out. The specific steps are as follows: 50 ml beaker is added with 20 g artificial sebum, 8 g powder is added, and it is completely immersed for 2 min, then it is immediately filtered by using a filter, and the filter cake is put into an oven at 100 ℃ for drying for 6 h, and then it is crushed to obtain the recovered powder. D5 silicone oil is used for oil absorption test, and the oil absorption test standard is the same as above.

[0125] Figure 7 The oil absorption of the recovered powder is compared. The oil absorption of example 1 is 159.38, the oil absorption of example 3 is 115.24, the oil absorption of example 4 is 109.32, the oil absorption of example 5 is 135.13, and the oil absorption of example 6 is 142.21. It can be seen that the oil absorption capacity of the powder of example 1, 3-4 is recovered to a certain extent, which proves that the sebum has destroyed the envelope, and further combined with example 5-6, it can be seen that when the coating aid is used with pentaerythritol modified myopeptide and polyether modified polysiloxane, the oil absorption performance of silica is recovered better, and the above-mentioned coating aid is helpful to reduce the adsorption of hydrolyzed hyaluronic acid in the pores of the particles during coating, and when the mass ratio of pentaerythritol modified myopeptide and polyether modified polysiloxane is 4:1, the oil absorption is recovered to a higher level, and the pentaerythritol modified myopeptide and polyether modified polysiloxane at the ratio are more conducive to reducing pore blockage, and can maintain higher recovery oil absorption while achieving coating.

[0126] It can be understood that the modified inorganic particles of the present application have the functions mentioned above, and based on the above functions, they can be applied to various scenes where porous particles are required to achieve slow adsorption. As one of them, the present application discusses its case as a makeup powder for slow oil control.

[0127] Reference Figure 8 The oil and water of the silica treated in different ways were compared. The conventional treated silica is as follows: 10 kg of spherical porous silica is put into a high-speed mixer, the speed is 1350 rpm, 0.45 kg of polydimethylsiloxane and 0.22 kg of triethoxysilane are sequentially added, mixed for 25 min, and then the mixed powder is put into an oven, the temperature is set to 105 ℃, and dried for 18 h; the dried powder is crushed by a hammer crusher to obtain the finished product. The hyaluronic acid treated silica is obtained by the method of example 1. The specific test steps are as follows: the powder silica is applied on the forehead and both sides of the same tester, and the oil and water are detected by using Real Bubee face water and oil intelligent detector.

[0128] From Figure 8It can be seen that the oil-water ratios of the conventional treated silica at 1h, 4h and 6h are 1.08, 0.95, 1.59 and 2.13 respectively, and the oil-water ratios of the silica treated by the method of Example 1 are 0.91, 0.91, 0.95 and 1.94 respectively. It can be seen from the broken line graph that the silica treated by the method of the application maintains a lower oil-water ratio within 4 hours of makeup, indicating that the silica treated by the method of the application has a certain slow oil control effect, and the modified inorganic powder of the application has a good application scenario in the field of cosmetics.

[0129] The specific embodiments are merely an explanation of the application, and are not a limitation of the application. Those skilled in the art can make modifications to the embodiments without creative contribution after reading the specification, as long as the modifications are within the scope of the claims of the application.

Claims

1. A modified inorganic particle, characterized by, The modified inorganic particles can achieve slow oil control; the preparation raw materials include the following components by weight: Component 1: at least one of spherical porous silica, porous bentonite, and porous diatomite, 100 parts; Component 2: at least one of hydrolyzed hyaluronic acid, sodium hyaluronate, and zinc hyaluronate, 0.2-5 parts; Component 3: at least one of triethoxyl octyl silane, dimethicone, dimethiconol, phenyl silicone oil, lauroyl lysine, and hydrogenated lecithin, 0.5-10 parts; The preparation process includes: adding component 2 and coating aid into deionized water to prepare a solution, and keeping the solution at 10-15℃; the mass ratio of component 2 to coating aid is 3-8:1; the coating aid is pentaerythritol modified myopeptide and polyether modified polysiloxane with a mass ratio of 3-5:1; component 1 is placed in a boiling coating machine and suspended in hot air with a temperature of 50-70℃; the solution is sprayed on component 1, and the temperature is raised to 100-110℃ for 6-8h to obtain a powder; the powder is added into a high-speed mixer, and component 3 is added and mixed for 20-30min; and the mixture is dried and crushed to obtain the modified inorganic particles.

2. The modified inorganic particle of claim 1, wherein The amount of deionized water is 15-20 times the mass of component 2.

3. The modified inorganic particle of claim 1, wherein Component 3 contains solids and liquids, and the input method includes first adding solids and mixing for 10-15min, and then adding liquids and mixing for 10-15min.

4. The modified inorganic particle of claim 1, wherein The mass ratio of component 2 to coating aid is 5:

1.

5. The modified inorganic particle of claim 1, wherein The mass ratio of pentaerythritol modified myopeptide to polyether modified polysiloxane is 4:

1.

6. A method for producing the modified inorganic particles as claimed in any one of claims 1 to 5, characterized by, The method includes the following steps: Step one: adding component 2 and coating aid into 50-70℃ deionized water with a mass of 15-20 times that of component 2, stirring until completely dispersed, and storing in a water bath pot, keeping the temperature of the water bath pot at 10-15℃ until the solution reaches the same temperature; Step two: placing component 1 in a boiling coating machine, passing air with a temperature of 50-70℃, and making component 1 suspended and boiled under the action of hot air; Step three: placing the solution prepared in step one in a pressure tank, and spraying it on component 1 through a nozzle; Step four: continuously increasing the air temperature to 100-110℃ for 6-8h to obtain a powder; Step five: adding the obtained powder into a high-speed mixer, adding component 3 at a speed of 1200-1500rpm, and mixing for 20-30min; Step six: placing the mixed powder in an oven, setting the temperature to 100-110℃, and drying for 15-20h; Step seven: crushing the dried powder with a hammer crusher to obtain the finished product.

7. The method of producing modified inorganic particles according to claim 6, characterized by, Component 3 contains solids and liquids, and the input method includes first adding solids and mixing for 10-15min, and then adding liquids and mixing for 10-15min.

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