Nanosilica-free particles and method for producing same
By adding oil and emulsifier to the water glass, controlling the addition concentration of acid, and preparing nano-free silica spherical particles with a diameter of 1 to 30 μm, solving the problem of high-priced raw materials and nanoparticles in the prior art, and realizing cosmetics Low friction, improved fluidity and increased use.
Patent Information
- Application Number
- CN202280098476.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Priority Date
- 2022-07-27
- Filing Date
- 2022-09-15
- Publication Date
- 2025-02-25
AI Technical Summary
The prior art has the disadvantage of using high-priced raw materials when manufacturing silica particles. When using water glass, it has high reactivity and is difficult to adjust the particle size, resulting in rough surface, increasing friction coefficient, and deteriorating the use of cosmetics. Nanoparticles may be generated, causing nano-hazards.
By adding oil and emulsifier to the water glass, the addition concentrations of weak and strong acids are controlled and the reaction conditions are adjusted, and nano-free silica spherical particles with a diameter of 1 to 30 μm are prepared to ensure smooth surfaces of the particles and low friction coefficient.
The nano-free silica particles are manufactured to prevent nano-hazards, reduce the friction coefficient of cosmetics, improve fluidity, and enhance the sense of use of cosmetics.
Smart Images
Figure CN119522086A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to nano-free silica particles and a method for producing the same, and more particularly to spherical silica for cosmetics with a diameter of 1 to 30 μm obtained from water glass, which can prevent nano-hazards, and has a low friction coefficient for cosmetics, improved fluidity, and can enhance the feel of use of the cosmetics, and a method for producing the same. Background Art
[0002] The following description merely provides background information related to the present invention and does not constitute prior art.
[0003] Silicon dioxide is an inorganic oxide of siloxane and silane, also known as silicon dioxide and silicic anhydride, which is a combination of silicon and oxygen. As the main component of rock or soil, it exists in trace amounts in natural water in the form of ionic colloids. It is also the main component of quartz, crystal, agate, and opal.
[0004] In cosmetics, silica particles can regulate the sebum secretion of the skin, thereby helping to keep the pores clean. In addition, when the powder ingredients used in cosmetics absorb moisture, they can be used as a raw material to prevent condensation or agglomeration due to moisture. In addition, they can be used in scrub-type cosmetic compositions to achieve the effects of removing harmful substances from skin metabolism, secretions, pollutants attached to the outside, bacteria, and makeup substances; they can stimulate the nerves and blood vessels distributed in the dermis and subcutaneous tissue of the skin to promote blood flow, thereby showing the effect of preventing fine wrinkles, and preventing the stratum corneum from thickening to maintain the health of the epidermis by helping the keratinized keratin to be easily removed. The peeling effect. In addition, it can be used as a feel improver in makeup products.
[0005] In the past, when manufacturing silicon dioxide, a method of slowly adding a weak acid to tetramethyl orthosilicate (TMOS) or tetraethyl orthosilicate (TEOS) to grow silicon dioxide particles was used to prepare silicon dioxide particles. However, although this method can easily prepare silicon dioxide particles, it has the disadvantage of being more expensive than water glass.
[0006] In addition, when water glass is used instead of TMOS or TEOS and acid is added to produce silica particles, the reactivity is high and tiny nanoparticles are generated instantly. Not only is it difficult to adjust the particle size, but a large number of nanoparticles will also adhere to the surface of the generated particles (Figure 1, Figure 2), making the surface rough and increasing the friction coefficient, resulting in a poorer feel of the cosmetics. In addition, considering the adverse effects of nanoparticles on organisms, a new method for producing silica particles that does not contain nanoparticles is needed. That is, nano substances may be formed in the process of producing silica particles using sodium silicate solution. In the case of including nano substances as cosmetic ingredients, nano hazards may be induced, reducing the feel of the cosmetics.
[0007] Regarding nanomaterials, the European Cosmetic Regulations (EC Cosmetic Regulations) 1223 / 2009 stipulates that insoluble or biopersistent substances in the range of 1 to 100nm are nanomaterials, and requires that the presence of nanomaterials must be reported to the Commission before cosmetics are put on the market, and all ingredients in the form of nanomaterials must be indicated in the ingredient list. In addition, the Nanoparticle Recommendation (Recommendation 2011 / 696) issued in 2011 recommends that if the number of particles below 100nm in the results of electron microscopy (SEM) observation is less than 50%, it can be called nano-free. This means that when the average diameter of the particles is assumed to be 10 microns (μm), the content of particles below 100 nanometers is only a very small amount of less than one millionth by weight or volume.
[0008] The present inventors have obtained "Nano free silica" by controlling important process variables in a method for producing silica particles using water glass (Na2SiO3 aqueous solution). Summary of the invention
[0009] Technical issues
[0010] The technical problem to be achieved by the present invention is to solve the previous problems, and the purpose is to provide a nano-silica-free spherical particle and a method for manufacturing the same, which can use water glass to manufacture spherical silica particles for cosmetics with a diameter of 1 to 30 μm, while preventing nano-hazards, and the friction coefficient of the cosmetics is low, the fluidity is improved, and the use feeling of the cosmetics can be improved.
[0011] Solution to the problem
[0012] The present invention provides a silica particle, characterized in that it is a spherical silica for cosmetics with a diameter of 1 to 30 μm obtained by using water glass.
[0013] The result of measurement using a scanning electron microscope (SEM) was that the particles were nano-free.
[0014] Preferably, the friction coefficient (gf) of the silica particles is 160 gf or less or the avalanche energy (Avalanche Energy) is 20 mj / kg or less.
[0015] In addition, the present invention provides a method for producing silicon dioxide particles, characterized by comprising:
[0016] In the first step, oil and an emulsifier are added to water glass or a mixture of water glass and water and stirred to prepare a mixed solution;
[0017] The second step is to add a weak acid or a weak acid aqueous solution to the mixed solution to react;
[0018] The third step is to add a strong acid aqueous solution to the reactant in the second step to carry out a reaction; and
[0019] In the fourth step, the product of the third step is dried and crushed.
[0020] Preferably, the oil is liquid paraffin, light oil or kerosene.
[0021] Preferably, the hydrophilic lipophilic balance (HLB) of the emulsifier is 4 to 6.
[0022] Specifically, the weak acid may be one or more selected from the group consisting of acetic acid, carbonic acid, citric acid, and lactic acid.
[0023] Preferably, the strong acid aqueous solution is added until the pH of the final aqueous solution reaches 5 to 7.
[0024] Preferably, the weak acid aqueous solution is added by sequentially adding two or more aqueous solutions with different concentrations starting from the lowest concentration.
[0025] Preferably, the strong acid aqueous solution is added by sequentially adding two or more aqueous solutions with different concentrations starting from a low concentration.
[0026] Furthermore, the present invention provides silica particles produced by the above-described method for producing silica particles.
[0027] The present invention also provides a cosmetic comprising the above-described silica particles.
[0028] Effects of the Invention
[0029] According to the present invention, nano-free silica particles and a method for producing the same can be provided. The nano-free silica particles are spherical silica particles for cosmetics with a diameter of 1 to 30 μm obtained using water glass, which can prevent nano-hazards, and the friction coefficient of the cosmetics is low, the fluidity is improved, and the use feel of the cosmetics can be improved. BRIEF DESCRIPTION OF THE DRAWINGS
[0030] FIG. 1 is an electron microscope photograph of particles of water glass after weak acid treatment according to the prior art.
[0031] FIG. 2 is an electron microscope photograph of broken particles during acid treatment using a strong acid according to the prior art.
[0032] FIG. 3 is a flow chart showing a silicon dioxide manufacturing process according to an embodiment of the present invention. DETAILED DESCRIPTION
[0033] Hereinafter, the embodiments of the present invention will be described in detail with reference to the accompanying drawings so that those skilled in the art can easily implement the present invention. However, the present invention can be implemented in various different ways and is not limited to the embodiments described here.
[0034] Throughout this specification, when a certain part is said to “comprise” a certain constituent element, unless there is a special description to the contrary, it means that other constituent elements may also be included, rather than excluding other constituent elements.
[0035] The present invention provides silica particles, characterized in that the silica particles are spherical silica for cosmetics with a diameter of 1 to 30 μm obtained by using water glass.
[0036] The result of measurement using a scanning electron microscope (SEM) was that the particles were nano-free.
[0037] In the present invention, the so-called "Nano free" observed by electron microscopy (SEM) means that the product complies with the nano free standard established by the European Cosmetics Council, and the number of particles below 100 nm in the results of electron microscopy observation is less than 50%, and the content of particles below 100 nanometers is only a very small amount of less than one millionth by weight or volume.
[0038] Preferably, the silica particles of the present invention have a friction coefficient (gf) of 160 gf or less, or an avalanche energy of 20 mj / kg or less. In this case, the friction coefficient of the cosmetic is low, the fluidity is improved, and the feel of the cosmetic during use can be improved.
[0039] The silicon dioxide particles of the present invention are obtained from water glass and are nano-free silicon dioxide particles. When added to cosmetics, the silicon dioxide particles can fundamentally prevent nano-hazards and improve the feeling of use.
[0040] The silica particles of the present invention can be produced by a method for producing silica particles characterized by comprising the following steps:
[0041] In the first step, oil and an emulsifier are added to water glass or a mixture of water glass and water and stirred to prepare a mixed solution;
[0042] The second step is to add a weak acid or a weak acid aqueous solution to the mixed solution to react;
[0043] The third step is to add a strong acid aqueous solution to the reactant in the second step to carry out a reaction; and
[0044] In the fourth step, the product of the third step is dried and crushed.
[0045] Hereinafter, the technical structure of each production step of the above-mentioned method for producing silica particles will be described in more detail with reference to FIG. 1 .
[0046] The method for manufacturing silicon dioxide particles of the present invention can use only water glass as raw material, or can be used after diluting with water as needed. At this time, the amount of water can be arbitrarily adjusted, and preferably, the amount used in the mixed solution with water glass can be 1 to 50 weight %. As the amount of water increases, the porosity of the manufactured silicon dioxide also increases.
[0047] In the present invention, oil and emulsifier are added to water glass or a mixture of water glass and water to prepare an oleophilic emulsion (first step). At this time, the oil that can be used is preferably hydrocarbon oil, specifically, various types such as liquid paraffin, light oil, kerosene or polybutene can be used, preferably liquid paraffin or kerosene. In this case, safety issues such as fire and economy can be improved.
[0048] In addition, as the above-mentioned emulsifier, the hydrophilic lipophilic balance (HLB) is preferably 4 to 6. As a specific example, it is preferably selected from the group consisting of sorbitan stearate, sorbitan isostearate, sorbitan oleate, sorbitan linoleate and polyglycerol polylinoleate. The amount of the above-mentioned emulsifier can be 0.1 to 20 parts by weight relative to 100 parts by weight of oil. If the amount of the emulsifier is too small, a sufficiently uniform emulsion cannot be prepared, resulting in a deterioration in the uniformity of the particles. In addition, if the amount of the emulsifier is too large, the particle size is too small and the silica particles of the desired size cannot be obtained.
[0049] When the oil is mixed, the ratio of the water phase to the oil phase can be adjusted arbitrarily. Preferably, the content of the water phase as the inner phase is 30 to 80 parts by weight, more preferably 50 to 70 parts by weight. The productivity and homogeneity of the silica particles can be satisfied at the same time.
[0050] The method for producing silica particles of the present invention includes a second step of adding a weak acid or a weak acid aqueous solution to the mixed solution of the first step to carry out a reaction.
[0051] The above-mentioned weak acid is not particularly limited, and specifically, one or more selected from the group consisting of acetic acid, carbonic acid, citric acid, and lactic acid can be used. When used with a weak acid aqueous solution, the concentration of the aqueous solution can be arbitrarily adjusted, and specifically, a 1 to 50% by weight, preferably a 1 to 30% by weight aqueous solution can be made for use. The addition amount of the above-mentioned weak acid or weak acid aqueous solution can be used with a weight of 0.5 to 10 times the above-mentioned oil input amount. Preferably, the above-mentioned weak acid aqueous solution can be made into two or more concentrations and a high-concentration aqueous solution is added successively after adding a low-concentration weak acid aqueous solution. In this case, the surface of the manufactured silicon dioxide particles is smoother, and the friction coefficient is low, and fluidity can be further improved.
[0052] The method for producing silica particles of the present invention includes a third step of adding a strong acid aqueous solution to the reactants of the second step to carry out a reaction.
[0053] The above-mentioned strong acid can specifically be sulfuric acid, hydrochloric acid or nitric acid. When used in the form of a strong acid aqueous solution, the concentration of the aqueous solution can be made into 1 to 20 weight % for use. The addition amount of the above-mentioned strong acid aqueous solution is preferably added until the pH of the final aqueous solution reaches 5 to 7. In this case, the situation in which the manufactured silicon dioxide particles are broken and nanoparticles are generated can be prevented. Preferably, the above-mentioned strong acid aqueous solution can be made into two or more concentrations and high-concentration aqueous solutions are added in sequence after adding a low-concentration strong acid aqueous solution. In this case, the surface of the manufactured silicon dioxide particles is smoother and has a low friction coefficient, which can further improve fluidity.
[0054] The method for producing silica particles of the present invention includes a fourth step of drying and pulverizing the silica obtained in the third step. The drying and pulverizing can be performed by known methods.
[0055] The method for producing silica particles of the present invention can use water glass to produce spherical silica particles for cosmetics with a size of 1 to 30 μm, and can prevent the generation of nanoparticles and thus prevent nano-hazards. The method also has a low friction coefficient and improved fluidity, which can improve the feel of cosmetics during use, and can produce silica particles with high productivity.
[0056] Hereinafter, the present invention will be described in detail by way of examples, which are as follows. However, the following examples are merely illustrative of the present invention, and the present invention is not limited to the following examples.
[0057] [Example 1]
[0058] 300 kg of sodium silicate and 30 kg of water were mixed and stirred at room temperature to make them uniform. A mixed solution of 200 kg of liquid paraffin and 20 kg of sorbitan isostearate as an emulsifier was added thereto and stirred at room temperature to form a water-in-oil emulsion. 700 kg of a 5 wt % aqueous solution of acetic acid was slowly added thereto to form particles, while being careful not to break the particles.
[0059] 10 wt % hydrochloric acid aqueous solution was slowly added thereto to adjust the pH of the final solution to 5 to 7, thereby hardening the particles. Only the precipitated silica particles were extracted and washed, then dried and sieved to produce nano-free silica. Electron microscope photos were taken of the produced silica particles, and the results showed a nano-free state.
[0060] [Example 2]
[0061] 300 kg of sodium silicate and 30 kg of water were mixed and stirred at room temperature to make them uniform. A mixed solution of 200 kg of liquid paraffin and 20 kg of sorbitan isostearate as an emulsifier was added thereto and stirred at room temperature to form a water-in-oil emulsion.
[0062] 200 kg of 1%, 2%, 5%, and 10% aqueous solutions of acetic acid on a weight basis were slowly added thereto to generate particles, while taking care not to break the particles.
[0063] 1%, 2%, 5%, 10%, 20% hydrochloric acid aqueous solution by weight was slowly added thereto to adjust the pH of the final solution to 5 to 7, thereby hardening the particles. Only the precipitated silica particles were extracted and washed, and then dried and sieved to produce nano-free silica. Electron microscope photos were taken of the produced silica particles, and the results showed a nano-free state.
[0064] [Table 1]
[0065]
[0066] As shown in Table 1, the silica particles produced according to the present invention were found to be free of nanoparticles. In addition, Example 2, in which weak acid and strong acid were added at successively higher concentrations, was found to have more excellent physical properties than Example 1.
[0067] Industrial Applicability
[0068] The technical problem to be achieved by the present invention is to solve the previous problems, and the purpose is to provide a nano-silica-free spherical particle and a method for manufacturing the same, which can use water glass to manufacture spherical silica particles for cosmetics with a diameter of 1 to 30 μm, while preventing nano-hazards, and the friction coefficient of the cosmetics is low, the fluidity is improved, and the use feeling of the cosmetics can be improved.
Claims
1. A silicon dioxide particle, characterized in that It is a spherical silica for cosmetics with a diameter of 1 to 30 μm obtained from water glass. The results of measurement using an electron microscope (SEM) showed that there was no nanoparticles. 2 . The silica particles according to claim 1 , wherein the friction coefficient gf of the silica particles is 160 gf or less or the avalanche energy is 20 mj / kg or less.
3. A method for producing silicon dioxide particles, characterized in that: include: In the first step, oil and an emulsifier are added to water glass or a mixture of water glass and water and stirred to prepare a mixed solution; The second step is to add a weak acid or a weak acid aqueous solution to the mixed solution for reaction; The third step is to add a strong acid aqueous solution to the reactant in the second step to react; as well as The fourth step is to dry and pulverize the product of the third step.
4. The method for producing silicon dioxide particles according to claim 3, characterized in that: The oil is liquid paraffin, light oil or kerosene.
5. The method for producing silicon dioxide particles according to claim 3, wherein: The hydrophilic-lipophilic balance (HLB) of the emulsifier is 4 to 6.
6. The method for producing silicon dioxide particles according to claim 3, wherein: The weak acid is one or more selected from the group consisting of acetic acid, carbonic acid, citric acid and lactic acid.
7. The method for producing silicon dioxide particles according to claim 3, wherein: The weak acid aqueous solution is added by sequentially adding two or more aqueous solutions with different concentrations starting from the lowest concentration.
8. The method for producing silicon dioxide particles according to claim 3, characterized in that: The strong acid aqueous solution is added by sequentially adding two or more aqueous solutions with different concentrations starting from the lowest concentration. 9 . Silica particles produced by the method for producing silica particles according to claim 3 . 10 . A cosmetic comprising the silica particles according to claim 1 .