CN-121974361-A - Preparation method of microsphere friction type silicon dioxide colored particles for cosmetics

CN121974361ACN 121974361 ACN121974361 ACN 121974361ACN-121974361-A

Abstract

The invention discloses a preparation method of microsphere friction type silicon dioxide colored particles for cosmetics, which comprises the steps of firstly preparing silicon dioxide slurry by using sodium silicate solution and sulfuric acid solution as main and auxiliary additives, emulsifying pigments to obtain pigment slurry, coloring the silicon dioxide particles by using the pigment slurry in an atomization spraying mode, vacuumizing the slurry to store water in a special storage tank, repeatedly atomizing and coloring and vacuumizing the slurry for a plurality of times, and finally adopting centrifugal spray drying to obtain the silicon dioxide colored particles. The invention adopts a physical method to add pigment, combines a vacuum pulping process to effectively enable pigment slurry to be integrated into mesoporous silica particles, and collects and recycles the moisture in the pigment slurry to be used as discharge color liquid until reaching 0. The particle size is controlled by adopting chemical and physical mode multi-layer treatment, so that the particle shape is mainly spherical, the formation of irregular particles is effectively reduced, and the method can be used in various friction products.

Inventors

LI GANG
HUANG WEIYUAN
SUN JUNJIE
HONG YINLONG

Assignees

三明阿福硅材料有限公司

Dates

Publication Date: 20260505
Application Date: 20251230

Claims (6)

1. The preparation method of the microsphere friction type silicon dioxide colored particles for cosmetics is characterized by comprising the following steps of: Adding 5-8 cubic meters of pure water into a reaction kettle, heating to 65-95 ℃ by saturated steam, adding 1-3 cubic meters of sodium silicate solution with the concentration of 1-2.5mol/L under the condition of stirring rotation speed of 500 revolutions per minute, simultaneously adding 100-300kg of additive mixed solution A, stirring for 10-15 minutes, and controlling the pH value of materials in the reaction kettle to be in the range of 9-10.5, wherein the additive mixed solution A is prepared by emulsifying anhydrous sodium sulfate, stearate and water in a mass ratio of (0.5-1) to (0.1-0.15) to (80-100) in an emulsifying machine for 20-30 minutes at the temperature of 60-80 ℃; Step 2, dropwise adding 1-2.5mol/L sodium silicate solution into a reaction kettle at a stirring speed of 800-1000 rpm, controlling the flow rate to be 7-14 cubic meters/hour, dropwise adding dilute sulfuric acid solution with the mass concentration of 10-35% into the reaction kettle, controlling the flow rate to be 2.5-5 cubic meters/hour, controlling the pH value of materials in the reaction kettle to be 9.5-10.5 in the dropwise adding process, controlling the temperature to be 65-95 ℃ and reacting for 50-80min; step 3, after the reaction is finished, stirring for 10-15 minutes at the rotating speed of 800-1000 rpm; Continuously dripping a dilute sulfuric acid solution with the mass concentration of 10-35%, regulating the flow rate to 1-3 cubic meters per hour, dripping 30-100KG of additive mixed solution B into a reaction kettle in a dripping mode, continuously stirring at the speed of 800-1000 revolutions per minute in the dripping process, stopping dripping the dilute sulfuric acid solution when the pH value of the material acidified to the reaction kettle is within the range of 4.1-5.9, and homogenizing for 10-15 minutes at the stirring speed of 1000-1200 revolutions per minute, wherein the additive mixed solution B is prepared by emulsifying the mixture of sodium dodecyl sulfate and stearate in an emulsifying machine for 20-30 minutes at the mass ratio of (0.5-1): (0.2-0.4): (80-120) in the mass ratio of (0.2-0.4): water; step 5, pumping homogenized materials into a plate-and-frame filter press to carry out filter pressing and washing after flowing out of a cooling tank through a pump, stopping washing when the water outlet conductivity of washing water reaches 400-600 mu s/cm, extruding, and carrying out air blowing for 2-5 minutes by using dry compressed gas after extrusion to obtain silicon dioxide slurry with the solid content of 35-45%; Adding pigment into a color paste tank, wherein the mass ratio of the pigment to the pure water to the emulsifier is 1 (50-100) to 0.5-3, and emulsifying and homogenizing for 15 minutes at the stirring speed of 1000-1300 rpm to form pigment slurry of alcoholized emulsion; Step 7, conveying the silicon dioxide slurry prepared in the step 5 to a slurrying tank by a high-pressure pump, spraying the slurry into the slurrying tank by a high-pressure nozzle, stirring at a stirring rotation speed of 300-500 r/min, and synchronously spraying the pigment slurry prepared in the step 6 into the slurrying tank by an atomizing device of the slurrying tank, wherein the volume ratio of the pigment slurry to the silicon dioxide slurry is 1 (80-120); 8, when the material in the slurrying tank reaches 80% of the material level of the straight cylinder body of the tank, closing the tank opening, closing the high-pressure pump, stopping spraying the silica slurry and the pigment slurry, slurrying for 5-10 minutes, starting vacuumizing, opening the exhaust valve, controlling the vacuum negative pressure to be 0.6-0.8Mpa, vacuumizing for 3-5 minutes, and pumping water/air into a special storage tank for storage; Stopping vacuumizing, spraying the materials in the slurrying tank into the slurrying tank again through a circulating high-pressure pump, a high-pressure pump circulating pipeline and a high-pressure nozzle, stirring the materials in the slurrying tank again at the speed of 300-500 r/min, spraying pigment slurry which is equal to that in the step 7 into the slurrying tank again through an atomizing nozzle in the stirring process, slurrying for 5-10 min after spraying, starting vacuumizing, opening an exhaust valve, controlling the vacuum negative pressure to be 0.6-0.8Mpa, and vacuumizing for 3-5 min, and pumping water/air into a special storage tank for storage; Step 10, repeating the step 9 for one to five times; And 11, stopping vacuumizing, conveying the materials prepared in the slurrying tank into a drying preparation tank through a double-screw conveying device, conveying the materials in the drying preparation tank into a centrifugal spray drying tower through a high-pressure pump for atomization drying, controlling the temperature in the drying tower to be 250-350 ℃, controlling the outlet temperature to be 105-110 ℃, controlling the time of powder in the tower to be 15-25S, controlling the rotating speed of an atomization disc to be 10000-15000 r, and obtaining the dried materials, namely the silicon dioxide colored particles.
2. And 12, dedusting the dried silica colored particles by a cyclone dust collector, and sieving the dedusted silica colored particles by an ultrasonic vibration sieve to obtain a product with the particle size meeting the requirement, namely a finished product.
3. The method for producing colored silica particles according to claim 1, wherein the stearate is sodium stearate or potassium stearate.
4. The method for preparing the friction type silica colored particles for cosmetics according to claim 1, wherein the emulsifier is one or a mixture of more than one of Tween 80, polyethylene glycol, propylene glycol fatty acid ester, glycerol and span 80 in any proportion.
5. The method for preparing color particles of silica with friction type microspheres for cosmetics according to claim 1, wherein the slurrying tank is a tank body with a vacuumizing device, a double-nozzle atomizing device and a circulating device, and the vacuum degree can reach 0.4-0.9Mpa.
6. The method for producing a friction type silica colored particle for cosmetics according to claim 1, wherein said pigment is a food-grade pigment.

Description

Preparation method of microsphere friction type silicon dioxide colored particles for cosmetics Technical Field The invention relates to the technical field of silica microsphere friction agents in the cosmetic industry, in particular to a preparation method of microsphere friction type silica colored particles for cosmetics such as toothpaste, facial cleanser, scrub cream and the like. Background With the continuous development of toothpaste formula technology, new toothpaste varieties are endlessly layered. An important factor for promoting the development of toothpaste formulation technology is the continuous innovation of the novel toothpaste in additives, efficacy, taste and vision, and the innovation can endow the toothpaste with novel efficacy, novel taste, novel color and appearance. Silica is a very important raw material in toothpaste and can be used as an abrasive and thickener in toothpaste. Silica particles with friction effect and bright color can be obtained through the combination of the dioxide and pigment (food grade), and the colored particles can bring new vision and good feeling to consumers. The toothpaste spherical color particles are different from conventional powdery abrasives or thickeners, have beautiful appearance, can be blended with various colors, can be prepared into various particle size particles according to requirements, have stable product properties and good compatibility under the polymerization of food-grade pigments and silicon dioxide, and increase the pleasure of brushing teeth while maintaining the friction performance. The colored particles used in the toothpaste have certain friction, and are also applied to cosmetics (such as facial cleanser and scrub cream) successively, and compared with plastic microspheres, the silica microspheres are safer to human skin, have mild friction and do not damage the skin, so that the toothpaste is widely popularized. The patent CN 105016345B provides a preparation method of suspended colored silica particles for toothpaste, which mainly adopts the technology that after polyethylene glycol, sodium dodecyl sulfate and the silica particles are combined, particles form mutual repulsion to a certain extent and are stable, so that the suspension time of the prepared silica particles in a toothpaste preparation solution system can reach at least half an hour, the suspension effect is good, the uniformity and stability of the dispersion of the silica particles in the toothpaste system can be ensured, and the suspension time is prolonged. However, this technique has the following disadvantages and problems: The process has the advantages that more pigment waste liquid is generated in the filter pressing process, and the process has pollution to the environment and is not beneficial to environmental protection. Meanwhile, the particle size and the form control mode of the particles are not clear, and when the particles are in sharp corners and water chestnut forms, the particles can damage skin or teeth after long-term use, and have larger limitation in application in cosmetics. Disclosure of Invention In order to solve the problems, the invention provides a preparation method of microsphere friction type silicon dioxide colored particles for cosmetics. In order to achieve the above purpose, the invention adopts the following technical scheme: The invention provides a preparation method of microsphere friction type silicon dioxide colored particles for cosmetics, which comprises the following steps: Adding 5-8 cubic meters of pure water into a reaction kettle, heating to 65-95 ℃ by saturated steam, adding 1-3 cubic meters of sodium silicate solution with the concentration of 1-2.5mol/L under the condition of stirring rotation speed of 500 revolutions per minute, simultaneously adding 100-300kg of additive mixed solution A, stirring for 10-15 minutes, and controlling the pH value of materials in the reaction kettle to be in the range of 9-10.5, wherein the additive mixed solution A is prepared by emulsifying anhydrous sodium sulfate, stearate and water in a mass ratio of (0.5-1) to (0.1-0.15) to (80-100) in an emulsifying machine for 20-30 minutes at the temperature of 60-80 ℃; Step 2, dropwise adding 1-2.5mol/L sodium silicate solution into a reaction kettle at a stirring speed of 800-1000 rpm, controlling the flow rate to be 7-14 cubic meters/hour, dropwise adding dilute sulfuric acid solution with the mass concentration of 10-35% into the reaction kettle, controlling the flow rate to be 2.5-5 cubic meters/hour, controlling the pH value of materials in the reaction kettle to be 9.5-10.5 in the dropwise adding process, controlling the temperature to be 65-95 ℃ and reacting for 50-80min; step 3, after the reaction is finished, stirring for 10-15 minutes at the rotating speed of 800-1000 rpm; Continuously dripping a dilute sulfuric acid solution with the mass concentration of 10-35%, regulating the flow rate to 1-3 cubic meters per hour,