CN105997582B

CN105997582B - Special filler for plant carbon black coloring cosmetics and preparation method thereof

Info

Publication number: CN105997582B
Application number: CN201610345546.XA
Authority: CN
Inventors: 林一中; 王振兴; 张骞
Original assignee: Individual
Current assignee: Shanghai Jianuova Cosmetics Co ltd
Priority date: 2016-05-20
Filing date: 2016-05-20
Publication date: 2020-05-05
Anticipated expiration: 2036-05-20
Also published as: CN105997582A

Abstract

The invention discloses a special filler for plant carbon black coloring cosmetics and a preparation method thereof. The special filler for the plant carbon black coloring cosmetics comprises a filler substrate and a plant carbon black coloring layer, wherein the plant carbon black coloring layer is prepared by a plant carbon source treating agent in situ on the surface of the filler substrate. The preparation method comprises the steps of coating the filler matrix with a plant carbon source treating agent, and then calcining at high temperature in the atmosphere of non-active gas and/or reducing gas or under the vacuum condition. The method uses plant carbon source treating agent for treatment, has high natural property, and can be applied in cosmetic formula.

Description

Special filler for plant carbon black coloring cosmetics and preparation method thereof

Technical Field

The invention belongs to the field of inorganic pigments, and particularly relates to a special filler for plant carbon black coloring cosmetics and a preparation method thereof.

Background

The filler is widely applied to cosmetics, such as cream cosmetics and pressed powder cosmetics, and a large amount of titanium dioxide, talcum powder, mica powder and the like are used. In order to be suitable for different occasions and consumer groups, the color of the formula needs to be adjusted, and the difference of the densities, surface charges and the like of the pigment and the filler in the formula can cause the flooding of the product during storage and use, thereby influencing the quality and the effect of the product. Therefore, the filler is colored, and the filler, the pigment and the pigment are combined into a whole, so that the problem of flooding of the product can be effectively solved.

According to the development of cosmetics at present, the aim of cumin of a cosmetic formulator is to replace non-renewable chemically synthesized raw materials with high pollution and high energy consumption by raw materials with high natural properties. Although it is used forCarbon black-colored fillers are used in many cosmetics, but most fillers are treated to color carbon black using synthetic treatment agents, which are complicated and cumbersome in chemical synthesis and harmful to the environment. As a method for obtaining carbon black, a process for obtaining a carbon black coating by treating an organic substance adsorbed on the surface of a filler at a high temperature under inert conditions is known. Patent application CN1826388A discloses that carbon ion coatings are alternately coated on the surface of a pigment through thermally decomposing polydiallyldimethylammonium chloride and poly (4-sodium styrene sulfonate) to obtain a carbon black coated pearlescent pigment, and the coating of the carbon ion-containing coatings needs to be carried out repeatedly, so that the operation process is complex. US6436538B1 describes the use of polymers to coat or directly polymerize on the surface to obtain N-containing polymers, followed by treatment at high temperature to obtain nitrogen-doped carbon-containing coatings, but the process is complicated, complicated and the polymerization process is not easily controlled. In the method of coloring carbon nanotubes or carbon black, a large amount of chemically synthesized solvents and treating agents are used in the process of preparing or coating the carbon nanotubes, so that the method has large environmental pollution and does not meet the requirement of green chemistry. Patent application CN104392767A discloses a method for obtaining a colored pearlescent pigment by coating graphene on the surface of the pearlescent pigment. In the method, organic solvents such as methanol, acetone, butanone and benzene are used for dispersing graphene, and the conductive pearlescent pigment is obtained by adsorbing graphene on the surface of the pearlescent pigment. In "processing and application of pearl pigment production, P46", a mixture of mica flakes and a hydrocarbon is made into a suspension, and the suspension is sprayed at a high speed, and the hydrocarbon is decomposed into ultrafine carbon black particles by thermal decomposition in a reducing atmosphere, and the ultrafine carbon black particles are attached to the surface of the mica flakes to produce a black pearl pigment colored with carbon black. (xuyanggu. manufacture, processing and application of pearlescent pigments. Beijing: chemical industry Press, 2005). It is also a common method to obtain carbon black pigmented fillers by coating pigment pastes. As for the method for coating colors such as carbon black, according to the record of the manufacturing, processing and application of pearlescent pigment, P256, a layer of aluminum hydroxide is firstly coated on the surface of the powder to be used as a lake agent, and then the aluminum hydroxide is addedThe pigment color paste enables pigment particles to be adsorbed on the surface of the alumina layer through the adsorption function of the alumina. The method makes the pigment firmly adsorbed on the surface of the pearlescent pigment through chemical bond action by the chemical reaction of metal cations in aluminum hydroxide and active functional groups with opposite charges in pigment molecules. However, when the process is used for coating carbon black, the adsorption effect of aluminum hydroxide and carbon black is difficult to control, the adhesion of carbon black is influenced, carbon black particles are easy to fall off and separate from the pearlescent pigment, and the color of the pearlescent pigment is easy to fade in the use process. Particularly, in the process of coating carbon black, heavy metals can be introduced into the coated aluminum hydroxide precursor and the used color paste to cause the heavy metals to exceed the standard, so that the special filler for the plant carbon black coloring cosmetics prepared by the method can not be applied to the fields such as cosmetics and the like with strict requirements on the heavy metals. A method for preparing composite carbon-coated pearlescent pigment is described in the literature "preparation of phthalocyanine blue-activated carbon composite mica titanium pearlescent pigment" (Houwenxiang, Tan Guozu, Pingxian, etc.. preparation of phthalocyanine blue-activated carbon composite mica titanium pearlescent pigment, paint industry, 2002 (5): 22-24.), wherein phthalocyanine blue and activated carbon are mainly considered to be difficult to disperse in water phase, and a surfactant is added to ensure that the surfaces of the activated carbon and the mica titanium pearlescent pigment can be compatible and AlCl is used₃Al (OH) formed by hydrolysis₃As a lake agent, the thickness of the carbon layer on the surface of the pearlescent pigment obtained by the method is difficult to control, and the adhesion force is poor. The plant-derived treating agent like glucose or fructose can be regenerated, so that the carbon black colored filler is obtained by treating the filler with the plant-derived treating agent, and the requirements of sustainable development are met; if the used filler base material is obtained by physical methods such as simple grinding and the like, the natural property is high; if the two are combined, the carbon black colored filler obtained by treating natural mineral substances with plant-derived treating agents has high natural attributes, and the carbon black colored filler can be applied to cosmetic formulations to obtain the cosmetic formulations with high natural attributes.

Disclosure of Invention

The invention provides a special filler for plant carbon black coloring cosmetics to overcome the problems in the prior art, which comprises a filler substrate and a plant carbon black coloring layer, wherein the plant carbon black coloring layer is prepared by a plant carbon source treating agent in situ on the surface of the filler substrate,

the filler matrix is one or more matrices selected from the group consisting of: natural mineral powder and synthetic powder with particle size less than 100 μm for cosmetic.

The plant carbon source treating agent is one or more treating agents selected from the following group: a natural plant-derived organic compound containing a hydroxyl group, a natural plant-derived organic compound containing a carboxyl group, a carboxylic acid derivative of a natural plant source, and a plant-derived lecithin.

The weight of the carbon black coloring layer in the special filler for the plant carbon black coloring cosmetics accounts for 0.001 to 20 percent of the total weight of the special filler for the plant carbon black coloring cosmetics.

In another preferred example, the filler matrix is a natural mineral powder for cosmetics having a particle size of less than 100 μm.

In another preferred example, the natural mineral powder is a natural silicate mineral powder obtained by crushing using physical grinding.

In another preferred example, the natural silicate mineral powder is one or more mineral powders selected from the group consisting of: natural mica powder, natural cyanite powder, natural garnet powder, natural pyrophyllite powder, natural talcum powder, natural wollastonite powder, kaolin powder and bentonite. In another more preferred embodiment, the natural silicate mineral powder is one or more mineral powders selected from the group consisting of: natural mica powder, natural talcum powder and kaolin powder.

In another preferred embodiment, the synthetic powder is one or more powders selected from the group consisting of: synthetic mica powder, titanium dioxide, white carbon black powder, zinc oxide powder, spherical silicon dioxide, barium sulfate, calcium carbonate, magnesium carbonate, boron nitride, pearlescent pigment powder, alumina powder, glass powder and mica iron oxide powder.

In another preferred example, the white carbon black powder is selected from gas phase white carbon black and/or plant source white carbon black. In another more preferred example, the white carbon black powder is rice hull silica white carbon black.

In another preferred embodiment, the natural plant-derived organic compound containing a hydroxyl group is one or more compounds selected from the group consisting of: the organic compound comprises a natural plant source micromolecule organic compound containing polyhydroxy, a natural plant source polymer containing polyhydroxy and a natural plant source long-chain fatty alcohol compound with a general formula of ROH, wherein R represents a straight chain or branched chain alkyl with 2-25 carbon atoms.

In another preferred example, the natural plant-derived small-molecule organic compound containing polyhydroxy is one or more compounds selected from the group consisting of sucrose, maltose, lactose, glucose and fructose, more preferably sucrose.

In another preferred embodiment, the natural plant-derived polymer containing polyhydroxy is one or more compounds selected from the group consisting of: glucoside, hyaluronic acid, sodium alginate, soluble starch, chitosan, cyclodextrin, dextran and sodium carboxymethyl cellulose.

In another preferred example, the natural plant-derived long-chain fatty alcohol compound of the formula ROH is a long-chain fatty alcohol containing 22 to 30 carbon atoms obtained from rice bran.

In another preferred embodiment, wherein the natural plant-derived organic compound containing a carboxyl group is one or more compounds selected from the group consisting of: a phytogenic unsaturated fatty acid and/or a salt thereof, and a phytogenic amino acid and/or a salt thereof.

In another preferred example, the plant-derived unsaturated fatty acid and/or a salt thereof is one or more of an omega-9 series unsaturated fatty acid and/or a salt thereof and an omega-6 series unsaturated fatty acid and/or a salt thereof selected from the group consisting of.

In another more preferred embodiment, the plant-derived unsaturated fatty acid and/or salt thereof is one or more selected from the group consisting of: linoleic acid and/or a salt thereof, linolenic acid and/or a salt thereof, and arachidonic acid and/or a salt thereof.

In another preferred embodiment, the plant-derived amino acid is one or more selected from the group consisting of lysine and/or a salt thereof and lauroyl lysine and/or a salt thereof.

In another preferred example, the carboxylic acid derivative of natural plant source is a natural vegetable oil obtained by physical means such as pressing, which is one or more vegetable oils selected from the group consisting of: coconut oil, soybean oil, peanut oil, sunflower oil, cottonseed oil, and double sallow oil.

In another preferred embodiment, the plant-derived lecithin is soybean lecithin.

The invention also provides a preparation method of the special filler for the plant carbon black coloring cosmetics, which comprises the following steps:

(1) dispersing a filler matrix into a solvent to prepare a suspension (a) with 1-30% of solid content;

(2) heating the prepared suspension (a) to 30-120 ℃ under the condition of stirring;

(3) adding a plant carbon source treating agent into the suspension (a) in the step (2) to obtain a suspension (b), wherein the weight of the plant carbon source treating agent accounts for 0.01-50% of the weight of the filler matrix;

(4) adjusting the pH value of the suspension (b) to 1-11, stirring and reacting under heat preservation for 0.01-6 h, filtering, and drying to obtain a modified filler precursor (c);

(5) treating the modified filler precursor (c) at high temperature of 300-1200 ℃ under the atmosphere of non-active gas and/or reducing gas or under vacuum condition to obtain the special filler for the plant carbon black coloring cosmetics,

the filler is one or more matrices selected from the group consisting of: natural mineral powder and synthetic powder with particle size less than 100 μm for cosmetic,

the plant carbon source treating agent is one or more treating agents selected from the following group: natural plant source organic compounds containing hydroxyl, natural plant source organic compounds containing carboxyl, carboxylic acid derivatives of natural plant sources and plant-derived lecithin.

In another preferred example, the natural silicate mineral powder is selected from one or more of the following group: natural mica powder, natural cyanite powder, natural garnet powder, natural pyrophyllite powder, natural talcum powder, natural wollastonite powder, kaolin powder and bentonite. In another more preferred embodiment, the natural silicate mineral powder is a filler matrix selected from one or more of the following group: natural mica powder, natural talcum powder and kaolin powder.

In another preferred example, the synthetic powder is one or more mineral powders selected from the group consisting of: synthetic mica powder, titanium dioxide, white carbon black powder, zinc oxide powder, spherical silicon dioxide, barium sulfate, calcium carbonate, magnesium carbonate, boron nitride, pearlescent pigment powder, alumina powder, glass powder and mica iron oxide powder.

In another preferred embodiment, the natural plant-derived organic compound containing a hydroxyl group is one or more compounds selected from the group consisting of: the organic compound comprises a natural plant source micromolecule organic compound containing polyhydroxy, a natural plant source polymer containing polyhydroxy and a natural plant source long-chain fatty alcohol compound with a general formula of ROH.

In another preferred embodiment, the natural plant-derived small-molecule organic compound containing polyhydroxy is one or more compounds selected from the group consisting of: glucose, fructose, sucrose, maltose and lactose, more preferably sucrose.

In another preferred embodiment, the natural plant-derived polymer containing polyhydroxy is one or more polymers selected from the group consisting of: cyclodextrin, glucoside, chitosan, dextran, hyaluronic acid, sodium alginate, soluble starch and sodium carboxymethylcellulose.

In another preferred embodiment, the natural plant-derived organic compound containing a carboxyl group is one or more compounds selected from the group consisting of: a phytogenic unsaturated fatty acid and/or a salt thereof, and a phytogenic amino acid and/or a salt thereof.

In another preferred example, the plant-derived unsaturated fatty acid and/or salt thereof is one or more compounds selected from the group consisting of: an omega-9 series unsaturated fatty acid and/or a salt thereof and an omega-6 series unsaturated fatty acid and/or a salt thereof.

In another more preferred embodiment, the plant-derived unsaturated fatty acid and/or salt thereof is one or more compounds selected from the group consisting of: linoleic acid and/or salts thereof, linolenic acid and/or salts thereof, and arachidonic acid and/or salts thereof; (ii) a

In another preferred embodiment, the plant-derived amino acid and/or salt thereof is one or more compounds selected from the group consisting of: lysine and/or a salt thereof and lauroyl lysine and/or a salt thereof.

In another preferred embodiment, the solvent in step (1) is one or more solvents selected from the group consisting of: water and an alcohol solvent with a boiling point of 60-200 ℃; more preferably the solvent is one or more solvents selected from the group consisting of: the solvent water and ethanol; most preferably the solvent is water.

In another preferred embodiment, the prepared suspension (a) is heated to a preferred temperature of 50 to 100 ℃, more preferably 60 to 90 ℃ in step (2).

In another preferred example, the weight of the plant carbon source treating agent in the step (3) accounts for 0.1-50% of the weight of the filler matrix; more preferably 1% to 30%.

In another preferred embodiment, the reaction time in step (4) is 0.05 to 5 hours, and more preferably 0.1 to 3 hours.

In another preferred example, the drying may be performed by heating under normal pressure, heating under reduced pressure, drying under reduced pressure at room temperature, or vacuum freeze-drying.

In another preferred embodiment, the high temperature treatment temperature is 400 to 1000 ℃, and more preferably 500 to 900 ℃. In another preferred embodiment, the time of the high temperature treatment is 0.1 to 10 hours, more preferably 0.1 to 5 hours, and most preferably 0.5 to 3 hours.

In another preferred embodiment, the nonreactive gas is one or more gases selected from the group consisting of: nitrogen (N)₂) Carbon dioxide (CO)₂) Argon (Ar), helium (He), neon (Ne), krypton (Kr), and xenon (Xe).

In another preferred example, the reducing gas is one or more gases selected from the group consisting of: hydrogen (H)₂) Carbon monoxide (CO) and ammonia (NH)₃)。

In another preferred example, the atmosphere of the inert gas and/or the reducing gas is a positive pressure state in which the system pressure is maintained to be equal to or higher than the external system pressure.

In another preferred example, the reducing atmosphere is obtained by partial oxidation of the precursor under the condition of oxygen deficiency in a closed condition; in another preferred embodiment, the reducing atmosphere is generated by incomplete combustion generated by adding additional organic matter and/or water to the system.

In another preferred embodiment, in the mixed atmosphere of the inert gas and the reducing gas, the volume content of the inert gas is controlled to be 0% to 100%, more preferably 90% to 100%, and the volume content of the reducing gas is controlled to be 0% to 100%, more preferably 0% to 10%. In another preferred embodiment, the gas flow rate is controlled to be 0.1 to 100L/h, more preferably 5 to 30L/h.

In another preferred embodiment, the vacuum condition is an absolute pressure of 10-³～10-¹Pa. In another preferred embodiment, the vacuum condition is to pump the system to a system absolute pressure of 10-⁵～10-¹And after Pa, introducing an inactive gas and/or a reducing gas into the system to keep the absolute pressure of the system lower than the external pressure of the gas so as to keep the system in a negative pressure state.

The invention also provides a preparation method of the special filler for the plant carbon black coloring cosmetics, which comprises the following steps: (1) dispersing a filler matrix into a solvent to prepare a suspension (a) with 1-50% of solid content; (2) under the condition of stirring, heating the prepared suspension (a) to 30-150 ℃, and adjusting the pH value of the suspension (a) to 1-11; (3) adding a plant carbon source treating agent into the suspension (a) to obtain a suspension (b), wherein the weight of the plant carbon source treating agent accounts for 0.01-80% of the weight of the filler matrix, and the pH is maintained as in the step (2) during the adding of the plant carbon source treating agent; (4) stirring and reacting under heat preservation for 0.01-10 h, filtering, and drying to obtain a modified pearlescent pigment precursor (c); (5) treating the modified pearlescent pigment precursor (c) at high temperature of 300-1200 ℃ in the atmosphere of non-active gas and/or reducing gas or under vacuum condition to obtain the special filler for the plant carbon black coloring cosmetic, wherein the filler matrix is one or more of the following matrixes: natural mineral powder and synthetic powder with particle diameter less than 100 μm for cosmetic; the plant carbon source treating agent is one or more treating agents selected from the following group: natural plant source organic compounds containing hydroxyl, natural plant source organic compounds containing carboxyl, carboxylic acid derivatives of natural plant sources and plant-derived lecithin.

The invention also provides a preparation method of the special filler for the plant carbon black coloring cosmetics, which comprises the following steps: (1) dispersing a filler matrix into a solvent to prepare a suspension (a) with 1-50% of solid content; (2) under the condition of stirring, heating the prepared suspension (a) to 30-150 ℃, and adjusting the pH value of the suspension (a) to 1-11; (3) adding a plant carbon source treating agent into the suspension (a) to obtain a suspension (b), wherein the weight of the plant carbon source treating agent accounts for 0.01-80% of the weight of the filler, and the pH is maintained as in the step (2) during the adding of the plant carbon source treating agent; (4) stirring and reacting under heat preservation for 0.01-10 h, and directly performing vacuum freeze drying without filtering to obtain a modified pearlescent pigment precursor (c); (5) treating the modified pearlescent pigment precursor (c) at high temperature of 300-1200 ℃ in the atmosphere of non-active gas and/or reducing gas or under vacuum condition to obtain the special filler for the plant carbon black coloring cosmetic, wherein the filler matrix is one or more of the following matrixes: natural mineral powder and synthetic powder with particle size less than 100 μm for cosmetic. The plant carbon source treating agent is one or more treating agents selected from the following group: natural plant source organic compounds containing hydroxyl, natural plant source organic compounds containing carboxyl, carboxylic acid derivatives of natural plant sources and plant-derived lecithin.

The surface of the filler matrix of the invention contains hydroxyl groups in different forms, such as silicon hydroxyl (Si-OH) and aluminum hydroxyl (Al-OH) of natural mica, and titanium hydroxyl contained on the surface of titanium dioxide, and the groups can react with carboxyl of a plant carbon source treating agent to generate ester-like substances, namely, the treating agent molecules are tightly bonded on the surface of the filler through the firm chemical bonds. The schematic is as follows:

therein, the

Representing a filler matrix, the surface of which contains a varying number of hydroxyl groups, R-representing an organic molecular group.

When the natural plant source organic compound containing hydroxyl is used as the treating agent, the hydroxyl of the natural plant source organic compound and the hydroxyl on the surface of the filler matrix form hydrogen bonds, and a plurality of hydroxyl of the polyhydroxy compound and a plurality of hydroxyl on the surface of the filler matrix form a plurality of hydrogen bonds, so that the treating agent is firmly attached to the surface of the filler matrix.

The invention is to modify the surface of the filler matrix by using a treating agent which can form strong chemical adsorption (hydrogen bond) or stable chemical bond with the surface of the filler matrix. And then carbonizing the surface-modified filler matrix at high temperature under the protection of vacuum or non-active gas and/or reducing gas atmosphere to generate a compact carbon black coloring layer in situ. Therefore, the filler special for the vegetable carbon black coloring cosmetics uses the natural plant source treating agent and the filler matrix obtained by natural minerals in a physical mode, has high natural property and is suitable for cosmetic fillers.

Detailed Description

The method for measuring the glossiness (brightness) adopts a method of an internal detection standard of Zhejiang Angel new material company Limited, and specifically comprises the following steps: adding commercially available polyurethane resin 2g into pearlescent pigment 0.2g, stirring, knife coating two comparative pearlescent pigment polyurethane resin pastes on the same black and white cardboard with 100 μm wet film preparation device, oven drying at 110 deg.C for 1min, and using

The BGO519GLOSSMETER gloss Meter measures gloss at 60 ℃ on a white background.

The bonding firmness of the conductive coating and the pearlescent pigment matrix in the invention is determined by the following method: weighing two parts of pearlescent pigment with the same weight, respectively dispersing in water (1g of sample is dispersed in 50mL of water), respectively pouring the pearlescent pigment into two identical measuring cylinders after stirring for 30min at 300rpm, standing for 2h, and observing the color of upper water in the two measuring cylinders (the more transparent the upper water is, the less carbon particles of the conductive coating fall off); the sample after stirring and standing in a measuring cylinder is filtered and dried to be measured for glossiness and compared with the conductive pearlescent pigment which is not stirred and washed with water (the closer the glossiness is, the less the carbon particles in the conductive coating are separated); the sample after stirring and standing in the other graduated cylinder was carefully cleaned of the upper water layer, the remaining 1/5 lower slurry was filtered, washed and dried, and the sample was analyzed for carbon content versus the change in carbon content before and after stirring (smaller change in carbon content indicates less shedding of carbon particles in the conductive coating).

The present invention is further illustrated by the following examples, which are not to be construed as limiting the invention.

Example 1

10g of natural mica powder with the particle size of less than 80 mu m is weighed and placed in a reactor, and 100g of water is added to prepare suspension. Stirring until the suspension is uniformly dispersed, heating the suspension to 80 ℃, adding 2.5g of glucose into the suspension, adjusting the pH value to 2.5, stirring for reaction for 3 hours, filtering, and drying to obtain a precursor.

And placing the dried precursor in a vacuum furnace, vacuumizing until the absolute pressure is 0.001Pa, heating to 400 ℃, and preserving heat for 3 hours. Furnace cooling in vacuum state to obtain the special filler for plant carbon black coloring cosmetics. The prepared pearlescent pigment coated with carbon black is subjected to heavy metal detection, and the result is shown in table 1:

TABLE 1

The method has heavy metal content meeting the relevant regulations of cosmetic use.

Example 2

Weighing 10g of natural talcum powder with the particle size of less than 5 mu m, placing the natural talcum powder into a reactor, adding 100g of water to prepare a suspension, stirring the suspension until the suspension is uniformly dispersed, heating the suspension to 85 ℃, adding 2g of cane sugar into the suspension, adjusting the pH value to 2.0 by using acetic acid, stirring the suspension for reaction for 1 hour, filtering the reaction product, and drying the reaction product to obtain the precursor.

Placing the dried precursor in an atmosphere furnace, and introducing carbon dioxide (CO)₂) Heating to 700 deg.C, and maintaining for 0.5 h. Under nitrogen (N)₂) Cooling with the furnace under the protection to obtain the special filler for the plant carbon black coloring cosmetics.

The gloss and firmness of the cosmetic-specific filler prepared as described above were measured and compared with a product prepared by a conventional method in which aluminum hydroxide was used as a lake agent to coat carbon black. Compared with the traditional method, the method has the advantages that the prepared product has higher glossiness, the glossiness is reduced a little after stirring, the upper layer of water is transparent and colorless after stirring, and the carbon content is reduced a little after stirring. The traditional process has obvious reduction of gloss after stirring, the upper layer has black turbid substances after stirring, and the carbon content is reduced more after stirring. See table 2 for details.

Example 3

10g of kaolin having a particle size of <5 μm are weighed into a reactor, and 200g of water are added thereto to prepare a suspension. Stirring until the suspension is uniformly dispersed, heating the suspension to 80 ℃, adding 1.2g of fructose into the suspension, adjusting the pH value to 4.0, stirring for reaction for 3.5h, filtering, and drying to obtain a precursor.

Placing the dried precursor in an atmosphere furnace, and introducing 90% N₂+10％H₂Heating to 900 deg.C, and maintaining for 0.3 h. In N₂Cooling with the furnace under the protection to obtain the special filler for the plant carbon black coloring cosmetics.

Example 4

10g of natural wollastonite powder with a particle size range of less than 10 μm are weighed into a reactor, and 100g of water +20g of ethanol are added thereto to prepare a suspension. Stirring until the suspension is uniformly dispersed, heating the suspension to 75 ℃, adjusting the pH value to 4.0, adding 2g of fructose into the suspension, stirring and reacting for 0.4h, filtering, and drying to obtain a precursor.

And (3) placing the dried precursor in an atmosphere furnace, introducing argon (Ar), heating to 450 ℃, and preserving heat for 3 hours. In N₂Cooling with the furnace under the protection to obtain the special filler for the plant carbon black coloring cosmetics.

The gloss of the cosmetic-specific filler prepared as described above was measured and compared with a product prepared by a conventional method in which carbon black was coated using aluminum hydroxide as a lake agent. It was found that the gloss of the product prepared by the method was higher and the gloss reduction after stirring was less than that of the product prepared by the conventional method. See table 2 for details.

Example 5

10g of plant-derived white carbon black having a particle size of less than 5 μm was weighed in a reactor, and 200g of water was added thereto to prepare a suspension. Stirring until the suspension is uniformly dispersed, heating the suspension to 60 ℃, adding 0.1g of sodium palmitate into the suspension, adjusting the pH value to 3.0, stirring for reaction for 0.5h, filtering, and drying to obtain the precursor.

Placing the dried precursor in an atmosphere furnace, and introducing N₂Heating to 1000 deg.C, and maintaining for 0.2 h. In N₂Cooling with the furnace under the protection to obtain the special filler for the plant carbon black coloring cosmetics.

The firmness of the cosmetic-specific filler prepared as described above was determined and compared with a product prepared by a conventional method in which carbon black was coated using aluminum hydroxide as a lake agent. Compared with the traditional method, the product prepared by the method has the advantages that the upper layer water is transparent and colorless after stirring, and the carbon content is reduced little after stirring. The upper layer of the traditional process has black turbid matters after stirring, and the carbon content is reduced more after stirring. See table 2 for details.

Example 6

10g of titanium dioxide powder with the particle size of less than 0.5 μm is weighed and placed in a reactor, and 100g of water is added to prepare suspension. Stirring until the suspension is uniformly dispersed, heating the suspension to 80 ℃, adding 1.5g of magnesium oleate into the suspension, adjusting the pH value to 1.5, reacting for 2h, filtering, and drying to obtain a precursor.

And (3) placing the dried precursor in an atmosphere furnace, introducing Ar, heating to 600 ℃, and preserving heat for 2.5 hours to obtain the treated special filler for the plant carbon black coloring cosmetics.

Example 7

10g of natural mica powder (particle size <25 μm) was weighed into a reactor, and 100g of water was added thereto to prepare a suspension. Stirring until the suspension is uniformly dispersed, heating the suspension to 90 ℃, adding 0.2g of linoleic acid into the suspension, adjusting the pH value to 3, reacting for 2h, then adding 1.0g of castor oil, stirring for 1h, filtering, and drying to obtain the precursor.

The dried precursor is placed in an atmosphere furnace, and 99.9 percent N is introduced₂+0.1％H₂Heating to 400 ℃ and preserving the heat for 3 h. In N₂Cooling with the furnace under the protection to obtain the special filler for the plant carbon black coloring cosmetics.

Example 8

Weighing 10g of precipitated barium sulfate with the particle size of less than 0.5 mu m, placing the precipitated barium sulfate into a reactor, adding 100g of water, stirring until the barium sulfate is uniformly dispersed, keeping the suspension at 40 ℃, adjusting the pH to 3.5, adding a mixed solution of 0.1g of oleic acid and 10g of ethanol, reacting for 2 hours, and carrying out vacuum freeze drying to obtain a precursor.

And placing the dried precursor in a vacuum furnace, vacuumizing until the absolute pressure is 0.01Pa, heating to 550 ℃, and preserving heat for 2 hours. Cooling along with the furnace under the condition of not reducing the vacuum degree to obtain the special filler for the plant carbon black coloring cosmetics.

Example 9

Weighing 10g of flaky alumina powder with the particle size of less than 2 mu m, adding 100g of ethanol, stirring until the mixture is uniformly dispersed, maintaining the suspension at 40 ℃, adjusting the pH to 3.5, adding a mixed solution of 0.1g of lysine and 10g of ethanol, reacting for 2 hours, and then directly freezing and drying to obtain the precursor.

And placing the dried precursor in a vacuum furnace, vacuumizing until the absolute pressure is 0.01Pa, heating to 500 ℃, and preserving heat for 2.75 h. Cooling along with the furnace under the condition of not reducing the vacuum degree to obtain the special filler for the plant carbon black coloring cosmetics.

Example 10

Weighing 10g of pearl powder AG6126 with the particle size range of 5-25 mu m, adding a mixed solution of 50g of water and 50g of ethanol, stirring until the mixture is uniformly dispersed, keeping the suspension at 55 ℃, adjusting the pH value to be 2.5, adding 1g of maltose, reacting for 3h, and then directly freezing and drying to obtain the precursor.

And placing the dried precursor in a vacuum furnace, vacuumizing until the absolute pressure is 0.001Pa, heating to 700 ℃, and preserving heat for 0.75 h. Cooling along with the furnace under the condition of not reducing the vacuum degree to obtain the special filler for the plant carbon black coloring cosmetics.

TABLE 2

All documents mentioned in the present application are incorporated by reference in the present application. Furthermore, it should be understood that various changes and modifications of the present invention can be made by those skilled in the art after reading the above teachings of the present invention, and these equivalents also fall within the scope of the present invention as defined by the appended claims.

Claims

1. A preparation method of a special filler for vegetable carbon black coloring cosmetics comprises the following steps:

(3) adding a plant carbon source treating agent into the suspension (a) in the step (2) to obtain a suspension (b), wherein the weight of the treating agent accounts for 0.01-50% of the weight of the filler matrix;

(4) adjusting the pH value of the suspension (b) to 1-4, stirring and reacting under heat preservation for 0.01-6 h, filtering, and drying to obtain a modified filler precursor (c);

the filler matrix is one or more matrices selected from the group consisting of: natural mineral powder and synthetic powder with particle size less than 100 μm for cosmetic,

the plant carbon source treating agent is one or more treating agents selected from the following group: natural plant source organic compound containing hydroxyl, natural plant source organic compound containing carboxyl, carboxylic acid derivative of natural plant source and plant source lecithin,

the carboxylic acid derivative of natural plant source is natural vegetable oil obtained by squeezing,

the solvent in the step (1) is water and an alcohol solvent with a boiling point of 30-200 ℃.

2. The production method according to claim 1, wherein the natural mineral powder is a natural silicate mineral powder obtained by crushing using physical grinding, which is selected from one or more mineral powders of the following group: natural mica powder, natural cyanite powder, natural garnet powder, natural pyrophyllite powder, natural talcum powder, natural wollastonite powder, kaolin powder and bentonite.

3. The method of claim 1, wherein the synthetic powder is one or more powders selected from the group consisting of: synthetic mica powder, titanium dioxide, white carbon black powder, zinc oxide powder, spherical silicon dioxide, barium sulfate, calcium carbonate, magnesium carbonate, boron nitride, pearlescent pigment powder, alumina powder, glass powder and mica iron oxide powder.

4. The production method according to claim 1, wherein the natural plant-derived organic compound containing a hydroxyl group is one or more compounds selected from the group consisting of: the organic compound comprises a natural plant source micromolecule organic compound containing polyhydroxy, a natural plant source polymer containing polyhydroxy and a natural plant source long-chain fatty alcohol compound with a general formula of ROH, wherein R represents a straight chain or branched chain alkyl with 2-25 carbon atoms.

5. The production method according to claim 1, wherein the natural plant-derived organic compound having a carboxyl group is one or more compounds selected from the group consisting of: phytogenic unsaturated fatty acid and/or salt thereof and phytogenic amino acid and/or salt thereof.

6. The production method according to claim 1, wherein the carboxylic acid derivative of natural plant origin is a natural vegetable oil obtained by physical means, which is selected from one or more vegetable oils of the following group: coconut oil, soybean oil, peanut oil, sunflower oil, cottonseed oil, and double sallow oil.

7. The method of claim 1, wherein the vegetal lecithin is soybean lecithin.

8. The production method according to any one of claims 1 to 7, wherein the nonreactive gas is selected from the group consisting of

One or more gases: nitrogen (N)₂) Carbon dioxide (CO)₂) Argon (Ar), helium (He), neon (Ne), krypton (Kr), and xenon (Xe).

9. The production method according to any one of claims 1 to 7, wherein the reducing gas is one or more gases selected from the group consisting of: hydrogen (H)₂₎Carbon monoxide (CO) and ammonia (NH)₃₎。

10. The production method according to any one of claims 1 to 7, wherein the vacuum condition is an absolute pressure of 10^-5～10^- ¹Pa。

11. A vegetable carbon black coloring cosmetic-specific filler prepared according to the preparation method of any one of the preceding claims.