CN116285429A

CN116285429A - Cosmetic-grade chameleon coloring pearlescent pigment and preparation method thereof

Info

Publication number: CN116285429A
Application number: CN202310316800.3A
Authority: CN
Inventors: 周峰; 蒋汉文
Original assignee: Hangzhou Forward Fine Chemical Co ltd
Current assignee: Hangzhou Forward Fine Chemical Co ltd
Priority date: 2023-03-23
Filing date: 2023-03-23
Publication date: 2023-06-23

Abstract

The invention belongs to the technical field of cosmetic grade pearlescent pigments, and discloses a cosmetic grade chameleon coloring pearlescent pigment and a preparation method thereof. According to the invention, the transparent flaky substrate is subjected to initial treatment, first tetravalent tin salt coating, first tetravalent titanium salt coating, silicate coating, second tetravalent tin salt coating and second tetravalent titanium salt coating in sequence to obtain the chameleon pearlescent pigment with changeable colors like running water, and then the cosmetic-grade water-soluble pigment coating is carried out on the surface of the pigment to obtain the cosmetic-grade chameleon pearlescent pigment with strong flickering sense, gorgeous color, high color saturation and colorful color variation, and the preparation process has the advantages of safe and easily obtained raw materials, simple and safe operation, environmental friendliness, low equipment cost and energy consumption.

Description

Cosmetic-grade chameleon coloring pearlescent pigment and preparation method thereof

Technical Field

The invention relates to the technical field of cosmetic grade pearlescent pigments, in particular to a cosmetic grade chameleon coloring pearlescent pigment and a preparation method thereof.

Background

In view of the unique optical properties and sparkling effect of pearlescent pigments, their use in the fields of paints, plastics, inks, automobiles, cosmetics and the like is becoming increasingly popular. Especially in the cosmetic (such as powder cake, eye shadow, nail polish, lipstick and lip glaze) industry, the pearlescent pigment has a attractive effect for cosmetics due to the rich particle size range and colorful color variation. Meanwhile, the color cosmetics are used as important components of cosmetics, and higher requirements are also put on the performances of high saturation, high flash, good dispersibility and the like of pigments.

In order to enrich the hue of pearlescent pigments, cosmetic grade water-soluble pigment coating may be performed on the surface thereof to obtain colored pearlescent pigments. The colored pearlescent pigment not only has pearlescent glossiness and sparkling effect, but also can present an attractive color which is saturated and rich like organic pigments.

In the conventional design of the colored pearlescent pigment, if the hue of the water-soluble pigment is the same as or similar to that of the original pearlescent pigment, the color purity of the obtained colored pearlescent pigment is higher; the opposite hues produce a two-color effect of changing colors.

Therefore, research is conducted on the cosmetic-grade chameleon coloring pearlescent pigment and the preparation method thereof, so that the chameleon coloring pearlescent pigment with high color saturation and gorgeous color can be obtained, and the cosmetic-grade chameleon coloring pearlescent pigment has important significance.

Disclosure of Invention

In view of the above, the invention provides a cosmetic grade chameleon coloring pearlescent pigment and a preparation method thereof, which ensures that the cosmetic grade chameleon coloring pearlescent pigment has the characteristics of safe and easily available raw materials, simple and safe operation, environmental protection, low equipment cost and energy consumption, strong flickering sense, gorgeous color, high color saturation and rich and colorful color tone.

In order to achieve the above object, the present invention provides the following technical solutions:

the invention provides a preparation method of a cosmetic-grade chameleon coloring pearlescent pigment, which comprises the following steps:

(1) Mixing the suspension of the flaky substrate with a tetravalent tin salt solution, and then reacting to prepare a first slurry;

(2) Mixing the first slurry with tetravalent titanium salt solution, and then reacting to obtain second slurry;

(3) Mixing the second slurry with silicate solution, and then reacting to obtain third slurry;

(4) Mixing the third slurry with a tetravalent tin salt solution, and then reacting to obtain a fourth slurry;

(5) Mixing the fourth slurry with tetravalent titanium salt solution, reacting, and filtering the reaction solution to obtain a filter cake;

(6) Sequentially drying and calcining the filter cake to obtain a color-changing Long Zhuguang pigment;

(7) Mixing an aqueous solution of chameleon pearlescent pigment with a pigment solution, and then reacting to obtain a fifth slurry;

(8) Mixing the fifth slurry with a trivalent aluminum salt solution, and then reacting to obtain a mother solution;

(9) Filtering the mother solution to obtain a filter cake, and drying the filter cake to obtain the chameleon-colored pearlescent pigment.

Preferably, the flaky substrate in the step (1) is a natural mica sheet, a synthetic mica sheet or a glass flake; the particle size of the flaky substrate is 5-200 mu m; the mass concentration of the flaky substrate in the suspension of the flaky substrate is 8-12%.

Preferably, the pH value of the suspension is adjusted to 1.3-1.8 before the step (1) is mixed, the pH value of the slurry is adjusted before the step (2) - (5), the pH value of the slurry is adjusted to 1.3-1.8 after the step (4), the pH value of the slurry is adjusted to 1.5-2.2 after the step (2) and the step (5), and the pH value of the slurry is adjusted to 8.0-9.0 in the step (3).

Preferably, in the steps (2) to (5) and the steps (7) to (8), the pH of the mixed solution is balanced after mixing, and the pH of the mixed solution is kept the same as the pH of the slurry before mixing or the aqueous solution of the chameleon pearlescent pigment.

Preferably, in the steps (1) and (4), the molar concentration of tetravalent tin ions in the tetravalent tin salt solution is 0.06-0.12 mol/L, tetravalent tin salt is stannic chloride, the mixing temperature is 60-70 ℃, the mass volume ratio of the flaky substrate to the tetravalent tin salt solution is 30-60 g:15-70 mL, and the reaction time is 25-35 min;

in the steps (2) and (5), the molar concentration of tetravalent titanium ions in the tetravalent titanium salt solution is 0.87-1.85 mol/L, the tetravalent titanium salt is titanium tetrachloride, the mixing temperature is 70-80 ℃, the mass-volume ratio of the flaky substrate to the tetravalent titanium salt solution in the step (2) is 30-60 g:60-180 mL, the mass-volume ratio of the flaky substrate to the tetravalent titanium salt solution in the step (5) is 30-60 g:40-135 mL, and the reaction time in the step (2) and the reaction time in the step (5) are independently 25-35 min.

Preferably, in the step (3), the mass concentration of the silicate solution is 10-30%, the silicate is sodium silicate nonahydrate, the mixing temperature is 80-90 ℃, the mass-volume ratio of the flaky substrate to the silicate solution is 30-60 g:600-2000 mL, and the reaction time is 25-35 min.

Preferably, the drying temperature in the step (6) is 90-110 ℃, and the calcination is that the calcination is carried out for 15-25 min at 500-550 ℃ and then for 15-25 min at 650-800 ℃; the temperature of the drying in the step (9) is 70-90 ℃.

Preferably, the mass concentration of the water solution of the chameleon pearlescent pigment in the step (7) is 8-12%; the temperature of the mixing in the step (7) is 15-35 ℃, the mass fraction of pigment in the pigment dispersion liquid is 8-15%, and the reaction time is 25-35 min; the pigment is water-soluble pigment.

Preferably, in the step (8), the molar concentration of trivalent aluminum ions in the trivalent aluminum salt solution is 1.25-1.95 mol/L, the trivalent aluminum salt is aluminum trichloride, the mass volume ratio of the color-changing Long Zhuguang pigment to the trivalent aluminum salt solution is 30-60 g:30-80 mL, and the reaction time is 25-35 min.

The invention also provides the cosmetic-grade chameleon coloring pearlescent pigment prepared by the preparation method of the cosmetic-grade chameleon coloring pearlescent pigment.

Compared with the prior art, the invention has the following beneficial effects:

1) According to the method, the chameleon pearlescent pigment with different colors along with angles is selected as a base material, and the surface of the chameleon pearlescent pigment is coated with the water-soluble pigment, so that the chameleon pearlescent pigment has the unique quality of stronger flickering sense, gorgeous color and colorful and changeable color tone compared with the conventional colored pearlescent pigment, and can meet the requirements of the high-end cosmetic market. The invention adopts the hydrolytic nano-deposition film-plating multilayer coating process of hydrothermal chemical sol-gel, and has the advantages of safe and easily obtained raw materials, low price, simple and safe operation, environmental friendliness and suitability for large-scale production.

2) According to the invention, firstly, a bionic principle is adopted, mica with uniform particle size and diameter-thickness ratio is selected as a base material, a complex and fine structural design is adopted, a hydrolytic nano deposition coating process of hydrothermal chemical sol gel is adopted, a multi-layer superposition coating technology is adopted, and a chameleon pearlescent pigment with changeable colors like flowing water is obtained, and then cosmetic-grade water-soluble pigment coating is carried out on the surface of the pigment, so that the chameleon colored pearlescent pigment with high color saturation and gorgeous color is obtained.

Detailed Description

In the invention, the flaky substrate in the step (1) is a natural mica sheet, a synthetic mica sheet or a glass flake; the particle diameter of the sheet-like base material is preferably 5 to 200. Mu.m, more preferably 50 to 150. Mu.m, still more preferably 80 to 120. Mu.m; the mass concentration of the flaky substrate in the suspension of the flaky substrate is preferably 8 to 12%, more preferably 9 to 11%, and still more preferably 10 to 10.5%.

In the present invention, the pH of the suspension is preferably adjusted to 1.3 to 1.8, more preferably 1.4 to 1.7, still more preferably 1.5 to 1.6, before the mixing in the steps (2) to (5), the pH of the slurry is preferably adjusted to 1.3 to 1.8, more preferably 1.4 to 1.7, still more preferably 1.5 to 1.6, the pH of the slurry is preferably adjusted to 1.5 to 2.2, still more preferably 1.6 to 2.1, still more preferably 1.8 to 1.9, and the pH of the slurry is preferably 8.0 to 9.0, still more preferably 8.2 to 8.8, still more preferably 8.4 to 8.6 after the adjustment in the step (1).

In the present invention, the mixing in step (1), step (2), step (4) and step (5) is preferably performed by pumping the salt solution into the suspension or slurry by a constant flow pump, and the pumping speed is preferably 0.5 to 1mL/min, more preferably 0.6 to 0.9mL/min, and even more preferably 0.7 to 0.8mL/min.

In the invention, in the step (3), the silicate solution is pumped into the second slurry by a constant flow pump, and the pumping speed is preferably 0.3-1 mL/min, more preferably 0.4-0.8 mL/min, and even more preferably 0.5-0.6 mL/min.

In the present invention, in steps (2) to (5) and steps (7) to (8), the pH of the mixed solution is preferably balanced after mixing, and the pH of the mixed solution is kept the same as the pH of the slurry before mixing or the aqueous solution of the chameleon pearlescent pigment.

In the present invention, in the steps (1) to (5) and the steps (7) to (8), the pH adjustment is performed by using an acid solution or an alkali solution, the acid solution is preferably an aqueous solution of hydrogen chloride, and the alkali solution is preferably an aqueous solution of sodium hydroxide.

In the present invention, in the steps (1) and (4), the molar concentration of tetravalent tin ions in the tetravalent tin salt solution is preferably 0.06 to 0.12mol/L, more preferably 0.08 to 0.11mol/L, more preferably 0.09 to 0.1mol/L, tetravalent tin salt is preferably tin tetrachloride, the temperature of the mixing is preferably 60 to 70 ℃, more preferably 62 to 68 ℃, more preferably 64 to 67 ℃, the mass-volume ratio of the sheet-like base material to the tetravalent tin salt solution is preferably 30 to 60g:15 to 70mL, more preferably 35 to 55g:20 to 60mL, more preferably 40 to 50g:30 to 55mL, the reaction time is preferably 25 to 35min, more preferably 27 to 32min, more preferably 28 to 30min.

In the present invention, in the steps (2) and (5), the molar concentration of tetravalent titanium ions in the tetravalent titanium salt solution is preferably 0.87 to 1.85mol/L, more preferably 1 to 1.5mol/L, more preferably 1.2 to 1.3mol/L, the tetravalent titanium salt is preferably titanium tetrachloride, the temperature of the mixing is preferably 70 to 80 ℃, more preferably 73 to 78 ℃, more preferably 75 to 76 ℃, the mass-volume ratio of the sheet-like base material to the tetravalent titanium salt solution in the step (2) is preferably 30 to 60g:60 to 180mL, more preferably 35 to 50g:80 to 150mL, more preferably 40 to 45g:100 to 120mL, the mass-volume ratio of the sheet-like base material to the tetravalent titanium salt solution in the step (5) is preferably 30 to 60g:40 to 135mL, more preferably 35 to 50g:50 to 110mL, more preferably 40 to 45g:80 to 100mL, and the time of the reaction in the step (2) and the step (5) is preferably 25 to 60 min, more preferably 31 to 32min, more preferably 31 to 30min.

In the present invention, in the step (3), the mass concentration of the silicate solution is preferably 10 to 30%, more preferably 15 to 25%, more preferably 20 to 22%, the silicate is preferably sodium silicate nonahydrate, the mixing temperature is preferably 80 to 90 ℃, more preferably 82 to 86 ℃, more preferably 83 to 85 ℃, the mass/volume ratio of the sheet-like substrate to the silicate solution is preferably 30 to 60g:600 to 2000mL, more preferably 35 to 50g:800 to 1800mL, more preferably 40 to 45g:1000 to 1500mL, the reaction time is preferably 25 to 35min, more preferably 28 to 32min, more preferably 29 to 30min.

In the present invention, the filtration in the step (5) is preferably carried out after washing with water, and the number of washing times is preferably 6 to 8.

In the present invention, the drying temperature in the step (6) is preferably 90 to 110 ℃, more preferably 95 to 105 ℃, still more preferably 98 to 100 ℃, the drying temperature in the step (9) is preferably 70 to 90 ℃, still more preferably 75 to 85 ℃, still more preferably 78 to 80 ℃, the calcination in the step (6) is preferably performed by first calcining at 500 to 550 ℃ for 15 to 25min, removing hydrochloric acid generated in the hydrolysis coating process, then calcining at 650 to 800 ℃ for 15 to 25min, still more preferably calcining at 510 to 540 ℃ for 18 to 22min, then calcining at 700 to 780 ℃ for 18 to 22min, still more preferably calcining at 520 to 530 ℃ for 19 to 20min, and then calcining at 720 to 750 ℃ for 19 to 20min.

In the invention, in the step (6), the added material is converted into a metal or nonmetal oxide layer with a certain thickness from metal or nonmetal hydroxide through high-temperature calcination, and the chameleon pearlescent pigment with a multilayer coating structure, wherein the thickness of each oxide layer is precisely controlled.

In the present invention, the mass concentration of the aqueous solution of the chameleon pearlescent pigment in the step (7) is preferably 8 to 12%, more preferably 9 to 11%, still more preferably 10 to 10.5%; the temperature of the mixing in the step (7) is preferably 15 to 35 ℃, more preferably 18 to 30 ℃, more preferably 20 to 25 ℃, the mass fraction of the pigment in the pigment dispersion is preferably 8 to 15%, more preferably 10 to 13%, more preferably 11 to 12%, the reaction time is preferably 25 to 35min, more preferably 28 to 32min, more preferably 29 to 30min, and the mass ratio of the chameleon pearlescent pigment to the pigment is preferably 10:0.5 to 1.2, more preferably 10:0.6 to 1.0, more preferably 10:0.8 to 0.9.

In the present invention, the pigment in the step (7) is preferably a water-soluble pigment, and more preferably one or more of FD & cyelow No.5, FD & cyelow No.6, D & corangeno.4, FD & credno.40, D & credno.22, D & credno.28, D & cgrenno. 5, and FD & cblue No. 1.

In the present invention, in the step (8), the molar concentration of trivalent aluminum ions in the trivalent aluminum salt solution is preferably 1.25 to 1.95mol/L, more preferably 1.3 to 1.8mol/L, still more preferably 1.5 to 1.7mol/L, the trivalent aluminum salt is preferably aluminum trichloride, the mass-volume ratio of the color-changing Long Zhuguang pigment to the trivalent aluminum salt solution is preferably 30 to 60g:30 to 80mL, more preferably 35 to 55g:40 to 75mL, still more preferably 40 to 50g:50 to 70mL, and the reaction time is preferably 25 to 35min, more preferably 28 to 32min, and still more preferably 29 to 30min.

In the present invention, the mixing in step (7) and step (8) is preferably to pump the pigment solution or the trivalent aluminum salt solution into the aqueous solution or the fifth slurry of the chameleon pearlescent pigment by a constant flow pump, and the pumping speed is preferably 1 to 2mL/min, more preferably 1.2 to 1.8mL/min, and even more preferably 1.4 to 1.6mL/min.

In the present invention, the filtration in the step (9) is preferably carried out after washing with water, the number of times of washing is preferably 6 to 8, and the mother liquor is washed to remove acid and salt.

The technical solutions provided by the present invention are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.

Example 1

45g of synthetic mica powder having a particle size of 35 μm was charged into a reactor, and 450mL of deionized water was added. The slurry was stirred and warmed to 65℃and the pH of the slurry was adjusted to 1.5 with 10% strength hydrochloric acid. 50mL of tin tetrachloride solution (the molar concentration of tin tetrachloride is 0.09 mol/L) was pumped into the reactor by a constant flow pump at a rate of 0.7mL/min, and the reaction was continued for 30min after the addition was completed, to obtain a first slurry.

The first slurry was stirred and warmed to 75 ℃, and the pH of the slurry was adjusted to 1.8 with 16% aqueous sodium hydroxide. 85mL of titanium tetrachloride solution (the molar concentration of tetravalent titanium ions is 1.82 mol/L) is pumped into the reactor at a speed of 0.7mL/min by a constant flow pump, the pH value of the slurry is balanced by a sodium hydroxide aqueous solution with the concentration of 16%, the pH value is kept the same as the pH value of the slurry before the titanium tetrachloride solution is added, and the reaction is continued for 30min after the addition is completed, so as to prepare a second slurry.

The second slurry was then warmed to 85 ℃ with stirring and the pH of the slurry was adjusted to 9.0 with 16% aqueous sodium hydroxide. 1200mL of sodium silicate solution (mass fraction of sodium silicate is 20%) was pumped into the reactor at a rate of 0.6mL/min using a constant flow pump, the pH of the slurry was maintained at the same value as the pH of the slurry before the sodium silicate solution was added using hydrochloric acid with a concentration of 10%, and the reaction was continued for 30min after the addition was completed, to prepare a third slurry.

The third slurry was stirred and cooled to 65℃and the pH of the slurry was adjusted to 1.5 with 10% strength hydrochloric acid. 50mL of tin tetrachloride solution (the molar concentration of tin tetrachloride is 0.09 mol/L) is pumped into the reactor by a constant flow pump at a speed of 0.7mL/min, the pH value of the slurry is balanced by a sodium hydroxide aqueous solution with the concentration of 16%, the pH value is kept the same as the pH value of the slurry before the tin tetrachloride solution is added, and the reaction is continued for 30min after the addition is finished, so as to prepare fourth slurry.

The fourth slurry was stirred and warmed to 75 ℃, and the pH of the slurry was adjusted to 1.8 with 16% aqueous sodium hydroxide. 80mL of titanium tetrachloride solution (the molar concentration of tetravalent titanium ions is 1.82 mol/L) is pumped into a reactor by a constant flow pump at the speed of 0.7mL/min, the pH value of the slurry is balanced by a sodium hydroxide aqueous solution with the concentration of 16%, the pH value is kept to be the same as that of the slurry before the titanium tetrachloride solution is added, and the reaction is continued for 30min after the addition is finished, so that a reaction liquid mother solution with the color change interval of yellow green-blue-violet red which is changed in sequence is obtained.

Filtering suspended matters of the mother solution of the reaction liquid, washing a filter cake with deionized water for 6 times to remove acid and salt, drying in a baking oven at 100 ℃, then placing in a muffle furnace to calcine for 20min at 500 ℃, and then calcining for 20min at 700 ℃ to obtain the chameleon pearlescent pigment with the color change interval of green-blue-purple-red-orange red changed in sequence.

45g of color-changing Long Zhuguang pigment is put into a reactor, 450mL of deionized water is added, and the mixture is stirred uniformly. 45mL of pigment dispersion (FD & CGrenNo.5, mass concentration 10%) was pumped into the reactor with a constant flow pump at a rate of 1mL/min, and stirring was continued for 15min after the addition was completed to prepare a fifth slurry.

The pH of the fifth slurry was adjusted to 5.8 with 10% strength hydrochloric acid. 50mL of aluminum trichloride solution (the molar concentration of trivalent aluminum ions is 1.65 mol/L) is pumped into the reactor by a constant flow pump at a speed of 1mL/min, the pH value of the slurry is balanced by a sodium hydroxide aqueous solution with the concentration of 16% so that the pH value is the same as that of the slurry before the aluminum trichloride solution is added, and the reaction is continued for 30min after the addition is finished, so that a mother solution with green stacking color is obtained.

Filtering the suspension of the mother solution, washing the filter cake with deionized water for 6 times to remove acid and salt, and drying in a 100 ℃ oven to obtain the chameleon coloring pearlescent pigment with sequentially changed green-blue-red-orange yellow color.

Example 2

42g of natural mica powder having a particle size of 60 μm was charged into a reactor, and 450mL of deionized water was added. The slurry was stirred and warmed to 65℃and the pH of the slurry was adjusted to 1.5 with 10% strength hydrochloric acid. 60mL of tin tetrachloride solution (the molar concentration of tin tetrachloride is 0.09 mol/L) is pumped into the reactor by a constant flow pump at a speed of 0.7mL/min, and the reaction is continued for 28min after the addition is completed, so as to obtain a first slurry.

The first slurry was stirred and warmed to 75 ℃, and the pH of the slurry was adjusted to 1.8 with 16% aqueous sodium hydroxide. 65mL of titanium tetrachloride solution (the molar concentration of tetravalent titanium ions is 1.82 mol/L) was pumped into the reactor at a rate of 0.7mL/min by a constant flow pump, the pH value of the slurry was equilibrated with a 16% aqueous sodium hydroxide solution, the pH value was maintained to be the same as that of the slurry before adding the titanium tetrachloride solution, and the reaction was continued for 28min after the addition was completed, to prepare a second slurry.

The second slurry was then warmed to 85 ℃ with stirring and the pH of the slurry was adjusted to 9.0 with 16% aqueous sodium hydroxide. 730mL of sodium silicate solution (mass fraction of sodium silicate is 20%) is pumped into the reactor at a speed of 0.6mL/min by a constant flow pump, the pH value of the slurry is kept the same as that of the slurry before the sodium silicate solution is added by hydrochloric acid with the concentration of 10%, and the reaction is continued for 28min after the addition is finished, so as to prepare a third slurry.

The third slurry was stirred and cooled to 65℃and the pH of the slurry was adjusted to 1.5 with 10% strength hydrochloric acid. 60mL of tin tetrachloride solution (the molar concentration of tin tetrachloride is 0.09 mol/L) is pumped into the reactor by a constant flow pump at a speed of 0.7mL/min, the pH value of the slurry is balanced by a sodium hydroxide aqueous solution with the concentration of 16%, the pH value is kept the same as the pH value of the slurry before the tin tetrachloride solution is added, and the reaction is continued for 30min after the addition is finished, so as to prepare fourth slurry.

The fourth slurry was stirred and warmed to 75 ℃, and the pH of the slurry was adjusted to 1.8 with 16% aqueous sodium hydroxide. Pumping 50mL of titanium tetrachloride solution (the molar concentration of tetravalent titanium ions is 1.82 mol/L) into a reactor at a speed of 0.7mL/min by a constant flow pump, balancing the pH value of the slurry by using a sodium hydroxide aqueous solution with the concentration of 16%, keeping the pH value the same as the pH value of the slurry before adding the titanium tetrachloride solution, and continuing to react for 28min after the adding is finished to obtain a reaction liquid mother solution with the color change interval of yellow green-blue-violet red which sequentially changes.

Filtering suspended matters of the mother solution of the reaction liquid, washing a filter cake with deionized water for 7 times to remove acid and salt, drying in a baking oven at 100 ℃, then placing in a muffle furnace to calcine for 20min at 510 ℃, and then calcining for 20min at 720 ℃ to obtain the chameleon pearlescent pigment with the color change interval of blue-purple-red-orange yellow changed in sequence.

40g of color-changing Long Zhuguang pigment is put into a reactor, 450mL of deionized water is added, and the mixture is stirred uniformly. 30mL of pigment dispersion (FD & CBlueNo.1, mass concentration 8%) was pumped into the reactor with a constant flow pump at a rate of 1mL/min, and stirring was continued for 15min after the addition was completed to prepare a fifth slurry.

The pH of the fifth slurry was adjusted to 5.8 with 10% strength hydrochloric acid. 60mL of aluminum trichloride solution (the molar concentration of trivalent aluminum ions is 1.68 mol/L) is pumped into the reactor by a constant flow pump at a speed of 1mL/min, the pH value of the slurry is balanced by a sodium hydroxide aqueous solution with the concentration of 16% so that the pH value is the same as that of the slurry before the aluminum trichloride solution is added, and the reaction is continued for 28min after the addition is finished, so that mother liquor with blue stacking color is obtained.

Filtering the suspension of the mother solution, washing the filter cake with deionized water for 8 times to remove acid and salt, and drying in a 100 ℃ oven to obtain the chameleon coloring pearlescent pigment with sequentially changed spreading colors of blue, purple, red and orange red.

Example 3

50g of synthetic mica powder having a particle size of 25 μm was charged into a reactor, and 500mL of deionized water was added. The slurry was stirred and warmed to 65℃and the pH of the slurry was adjusted to 1.5 with 10% strength hydrochloric acid. 65mL of tin tetrachloride solution (the molar concentration of tin tetrachloride is 0.09 mol/L) was pumped into the reactor by a constant flow pump at a rate of 0.7mL/min, and the reaction was continued for 31min after the addition was completed, to obtain a first slurry.

The first slurry was stirred and warmed to 75 ℃, and the pH of the slurry was adjusted to 1.8 with 16% aqueous sodium hydroxide. 120mL of titanium tetrachloride solution (the molar concentration of tetravalent titanium ions is 1.82 mol/L) was pumped into the reactor at a rate of 0.7mL/min by a constant flow pump, the pH value of the slurry was equilibrated with a 16% aqueous sodium hydroxide solution, the pH value was maintained to be the same as that of the slurry before adding the titanium tetrachloride solution, and the reaction was continued for 31min after the addition was completed, to prepare a second slurry.

The second slurry was then warmed to 85 ℃ with stirring and the pH of the slurry was adjusted to 9.0 with 16% aqueous sodium hydroxide. 980mL of sodium silicate solution (the mass fraction of sodium silicate is 20%) is pumped into the reactor at a speed of 0.6mL/min by a constant flow pump, the pH value of the slurry is kept the same as that of the slurry before the sodium silicate solution is added by hydrochloric acid with the concentration of 10%, and the reaction is continued for 31min after the addition is finished, so as to prepare the third slurry.

The third slurry was stirred and cooled to 65℃and the pH of the slurry was adjusted to 1.5 with 10% strength hydrochloric acid. 65mL of tin tetrachloride solution (the molar concentration of tin tetrachloride is 0.09 mol/L) was pumped into the reactor by a constant flow pump at a rate of 0.7mL/min, the pH value of the slurry was equilibrated with a 16% aqueous sodium hydroxide solution, the pH value was maintained to be the same as the pH value of the slurry before the addition of the tin tetrachloride solution, and the reaction was continued for 31min after the addition was completed, to prepare a fourth slurry.

The fourth slurry was stirred and warmed to 75 ℃, and the pH of the slurry was adjusted to 1.8 with 16% aqueous sodium hydroxide. 105mL of titanium tetrachloride solution (the molar concentration of tetravalent titanium ions is 1.82 mol/L) is pumped into the reactor by a constant flow pump at the speed of 0.7mL/min, the pH value of the slurry is balanced by a sodium hydroxide aqueous solution with the concentration of 16 percent, the pH value is the same as that of the slurry before adding the titanium tetrachloride solution, and the reaction is continued for 31min after the addition is finished, so as to obtain a reaction liquid mother solution with the color change interval of orange yellow-yellow green-blue green.

Filtering suspended matters of the mother solution of the reaction liquid, washing a filter cake with deionized water for 8 times to remove acid and salt, drying in a baking oven at 100 ℃, then placing in a muffle furnace to calcine for 20min at 520 ℃, and then calcining for 20min at 750 ℃ to obtain the chameleon pearlescent pigment with the color change interval of which yellow, green and blue are changed in sequence.

50g of color-changing Long Zhuguang pigment is put into a reactor, 500mL of deionized water is added, and the mixture is stirred uniformly. 60mL of pigment dispersion (FD & CYellowNo.5, mass concentration 10%) was pumped into the reactor at a rate of 1mL/min using a constant flow pump, and stirring was continued for 15min after the completion of the addition, to prepare a fifth slurry.

The pH of the fifth slurry was adjusted to 5.8 with 10% hydrochloric acid. 60mL of aluminum trichloride solution (the molar concentration of trivalent aluminum ions is 1.68 mol/L) is pumped into the reactor by a constant flow pump at a speed of 1.3mL/min, the pH value of the slurry is balanced by a sodium hydroxide aqueous solution with the concentration of 16% so that the pH value is the same as that of the slurry before the aluminum trichloride solution is added, and the reaction is continued for 31min after the addition is finished, so that a mother solution with yellow stacking color is obtained.

Filtering the suspension of the mother solution, washing the filter cake with deionized water for 7 times to remove acid and salt, and drying in a 100 ℃ oven to obtain the chameleon coloring pearlescent pigment with yellow-green-blue-green sequentially changed spreading color.

Example 4

60g of synthetic mica powder having a particle size of 120 μm was charged into a reactor, and 600mL of deionized water was added. The slurry was stirred and warmed to 65℃and the pH of the slurry was adjusted to 1.5 with 10% strength hydrochloric acid. 70mL of tin tetrachloride solution (the molar concentration of tin tetrachloride is 0.09 mol/L) is pumped into the reactor by a constant flow pump at a speed of 0.7mL/min, and the reaction is continued for 30min after the addition is completed, so as to obtain first slurry.

The first slurry was stirred and warmed to 75 ℃, and the pH of the slurry was adjusted to 1.8 with 16% aqueous sodium hydroxide. 90mL of titanium tetrachloride solution (the molar concentration of tetravalent titanium ions is 1.82 mol/L) is pumped into the reactor at a speed of 0.7mL/min by a constant flow pump, the pH value of the slurry is balanced by a sodium hydroxide aqueous solution with the concentration of 16%, the pH value is kept the same as the pH value of the slurry before the titanium tetrachloride solution is added, and the reaction is continued for 30min after the addition is completed, so that a second slurry is prepared.

The second slurry was then warmed to 85 ℃ with stirring and the pH of the slurry was adjusted to 9.0 with 16% aqueous sodium hydroxide. 760mL of sodium silicate solution (the mass fraction of sodium silicate is 20%) is pumped into the reactor at a speed of 0.6mL/min by a constant flow pump, the pH value of the slurry is kept the same as that of the slurry before the sodium silicate solution is added by hydrochloric acid with the concentration of 10%, and the reaction is continued for 30min after the addition is finished, so as to prepare a third slurry.

The third slurry was stirred and cooled to 65℃and the pH of the slurry was adjusted to 1.5 with 10% strength hydrochloric acid. 70mL of tin tetrachloride solution (the molar concentration of tin tetrachloride is 0.09 mol/L) is pumped into the reactor by a constant flow pump at a speed of 0.7mL/min, the pH value of the slurry is balanced by a sodium hydroxide aqueous solution with the concentration of 16%, the pH value is kept the same as the pH value of the slurry before the tin tetrachloride solution is added, and the reaction is continued for 30min after the addition is finished, so as to prepare fourth slurry.

The fourth slurry was stirred and warmed to 75 ℃, and the pH of the slurry was adjusted to 1.8 with 16% aqueous sodium hydroxide. 70mL of titanium tetrachloride solution (the molar concentration of tetravalent titanium ions is 1.82 mol/L) is pumped into a reactor by a constant flow pump at the speed of 0.7mL/min, the pH value of the slurry is balanced by a sodium hydroxide aqueous solution with the concentration of 16%, the pH value is kept to be the same as that of the slurry before the titanium tetrachloride solution is added, and the reaction is continued for 30min after the addition is finished, so that a reaction liquid mother solution with the color change interval of blue-green-blue-purple-orange-red which is changed in sequence is obtained.

Filtering suspended matters of the mother solution of the reaction liquid, washing a filter cake with deionized water for 6 times to remove acid and salt, drying in a baking oven at 100 ℃, then placing in a muffle furnace to calcine for 20min at 540 ℃, and then calcining for 20min at 680 ℃ to obtain the chameleon pearlescent pigment with the color change interval of blue-purple-red-orange changed in sequence.

60g of color-changing Long Zhuguang pigment is put into a reactor, 450mL of deionized water is added, and the mixture is stirred uniformly. 60mL of pigment dispersion (FD & CBlueNo.1, mass concentration 8%) was pumped into the reactor with a constant flow pump at a rate of 1mL/min, and stirring was continued for 15min after the addition was completed to prepare a fifth slurry.

The pH of the fifth slurry was adjusted to 5.8 with 10% strength hydrochloric acid. 60mL of aluminum trichloride solution (the molar concentration of trivalent aluminum ions is 1.65 mol/L) is pumped into the reactor by a constant flow pump at a speed of 1mL/min, the pH value of the slurry is balanced by a sodium hydroxide aqueous solution with the concentration of 16% so that the pH value is the same as that of the slurry before the aluminum trichloride solution is added, and the reaction is continued for 30min after the addition is finished, so that mother liquor with blue stacking color is obtained.

Filtering the suspension of the mother solution, washing the filter cake with deionized water for 7 times to remove acid and salt, and drying in a 100 ℃ oven to obtain the chameleon coloring pearlescent pigment with the color of blue-purple-red-orange red sequentially changed.

Example 5

35g of synthetic mica powder having a particle size of 15 μm was charged into a reactor, and 400mL of deionized water was added. The slurry was stirred and warmed to 65℃and the pH of the slurry was adjusted to 1.5 with 10% strength hydrochloric acid. 55mL of tin tetrachloride solution (the molar concentration of tin tetrachloride is 0.09 mol/L) was pumped into the reactor by a constant flow pump at a rate of 0.7mL/min, and the reaction was continued for 30min after the addition was completed, to obtain a first slurry.

The first slurry was stirred and warmed to 75 ℃, and the pH of the slurry was adjusted to 1.8 with 16% aqueous sodium hydroxide. Pumping 135mL of titanium tetrachloride solution (the molar concentration of tetravalent titanium ions is 1.82 mol/L) into a reactor at a speed of 0.7mL/min by a constant flow pump, balancing the pH value of the slurry by using a sodium hydroxide aqueous solution with the concentration of 16%, keeping the pH value the same as the pH value of the slurry before adding the titanium tetrachloride solution, and continuing to react for 30min after the adding is finished to prepare second slurry.

The second slurry was then warmed to 85 ℃ with stirring and the pH of the slurry was adjusted to 9.0 with 16% aqueous sodium hydroxide. 1850mL of sodium silicate solution (the mass fraction of sodium silicate is 20%) is pumped into the reactor at a speed of 0.6mL/min by a constant flow pump, the pH value of the slurry is kept stable by hydrochloric acid with the concentration of 10%, the pH value is kept the same as the pH value of the slurry before the sodium silicate solution is added, and the reaction is continued for 30min after the addition is finished, so as to prepare a third slurry.

The third slurry was stirred and cooled to 65℃and the pH of the slurry was adjusted to 1.5 with 10% strength hydrochloric acid. 55mL of tin tetrachloride solution (the molar concentration of tin tetrachloride is 0.09 mol/L) is pumped into the reactor by a constant flow pump at a speed of 0.7mL/min, the pH value of the slurry is balanced by a sodium hydroxide aqueous solution with the concentration of 16%, the pH value is kept the same as the pH value of the slurry before the tin tetrachloride solution is added, and the reaction is continued for 30min after the addition is completed, so as to prepare fourth slurry.

The fourth slurry was stirred and warmed to 75 ℃, and the pH of the slurry was adjusted to 1.8 with 16% aqueous sodium hydroxide. 120mL of titanium tetrachloride solution (the molar concentration of tetravalent titanium ions is 1.82 mol/L) is pumped into a reactor by a constant flow pump at the speed of 0.7mL/min, the pH value of the slurry is balanced by a sodium hydroxide aqueous solution with the concentration of 16 percent, the pH value is the same as that of the slurry before adding the titanium tetrachloride solution, and the reaction is continued for 30min after the addition is finished, so that a reaction liquid mother solution with the color change interval of yellow-green-blue-violet-red which is changed in sequence is obtained.

Filtering suspended matters of the mother solution of the reaction liquid, washing a filter cake with deionized water for 8 times to remove acid and salt, drying in a baking oven at 100 ℃, then placing in a muffle furnace to calcine for 20min at 550 ℃, and then calcining for 20min at 800 ℃ to obtain the chameleon pearlescent pigment with the color change interval of green-blue-purple-red-orange changed in sequence.

35g of color-changing Long Zhuguang pigment is put into a reactor, 400mL of deionized water is added, and the mixture is stirred uniformly. 70mL of pigment dispersion (FD & CBlueNo.1, 5% by mass, FD & CGreen No. 5) was pumped into the reactor with a constant flow pump at a rate of 1mL/min, and stirring was continued for 15min after the addition was completed to prepare a fifth slurry.

The pH of the fifth slurry was adjusted to 5.8 with 10% strength hydrochloric acid. 45mL of aluminum trichloride solution (the molar concentration of trivalent aluminum ions is 1.65 mol/L) is pumped into the reactor by a constant flow pump at a speed of 1mL/min, the pH value of the slurry is balanced by a sodium hydroxide aqueous solution with the concentration of 16% so that the pH value is the same as that of the slurry before the aluminum trichloride solution is added, and the reaction is continued for 30min after the addition is finished, so that a mother solution with a blue-green stacking color is obtained.

Filtering the suspension of the mother solution, washing the filter cake with deionized water for 6 times to remove acid and salt, and drying in a 100 ℃ oven to obtain the chameleon coloring pearlescent pigment with the color of green-blue-purple-red-orange changed in sequence.

The method of the invention uses the chameleon pearlescent pigment with different colors along with angles as a base material, and the surface of the chameleon pearlescent pigment is coated with the water-soluble pigment, so that the chameleon pearlescent pigment has the unique quality of stronger flickering sense, gorgeous color and colorful color change compared with the conventional colored pearlescent pigment, and can better meet the demands of the high-end cosmetic market. The invention adopts the hydrolytic nano-deposition film-plating multilayer coating process of hydrothermal chemical sol-gel, and has the advantages of safe and easily obtained raw materials, low price, simple and safe operation, environmental friendliness and suitability for large-scale production.

The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.

Claims

1. The preparation method of the cosmetic-grade chameleon coloring pearlescent pigment is characterized by comprising the following steps of:

2. The method for preparing cosmetic grade chameleon colored pearlescent pigment of claim 1, wherein the flaky substrate in step (1) is a natural mica sheet, a synthetic mica sheet or a glass flake; the particle size of the flaky substrate is 5-200 mu m; the mass concentration of the flaky substrate in the suspension of the flaky substrate is 8-12%.

3. The method for preparing the cosmetic-grade chameleon-colored pearlescent pigment according to claim 1, wherein the pH value of the suspension is adjusted to 1.3-1.8 before the mixing in the steps (1), the pH value of the slurry is adjusted to 1.3-1.8 before the mixing in the steps (2) - (5), the pH value of the slurry is adjusted to 1.5-2.2 after the adjusting in the steps (4), and the pH value of the slurry is adjusted to 8.0-9.0 after the adjusting in the steps (3).

4. The method of producing a cosmetic-grade chameleon pearlescent pigment according to claim 3, wherein in steps (2) to (5) and steps (7) to (8), the pH of the mixture is equilibrated after mixing, and the pH of the mixture is kept the same as the pH of the slurry before mixing or the aqueous solution of chameleon pearlescent pigment.

5. The method for preparing a cosmetic grade chameleon coloring pearlescent pigment according to claim 1, wherein in the steps (1) and (4), the molar concentration of tetravalent tin ions in the tetravalent tin salt solution is 0.06-0.12 mol/L, tetravalent tin salt is stannic chloride, the mixing temperature is 60-70 ℃, the mass-volume ratio of the flaky substrate and the tetravalent tin salt solution is 30-60 g:15-70 mL, and the reaction time is 25-35 min;

6. The method for preparing a cosmetic grade chameleon coloring pearlescent pigment according to claim 3 or 4, wherein in the step (3), the mass concentration of the silicate solution is 10-30%, the silicate is sodium silicate nonahydrate, the mixing temperature is 80-90 ℃, the mass volume ratio of the flaky substrate to the silicate solution is 30-60 g:600-2000 mL, and the reaction time is 25-35 min.

7. The method for preparing a cosmetic-grade chameleon-colored pearlescent pigment according to claim 1, wherein the drying temperature in the step (6) is 90-110 ℃, and the calcining is carried out for 15-25 min at 500-550 ℃ and then for 15-25 min at 650-800 ℃; the temperature of the drying in the step (9) is 70-90 ℃.

8. The method for producing a cosmetic-grade chameleon-colored pearlescent pigment according to claim 3 or 4, wherein the mass concentration of the aqueous solution of chameleon-colored pearlescent pigment in step (7) is 8 to 12%; the temperature of the mixing in the step (7) is 15-35 ℃, the mass fraction of pigment in the pigment dispersion liquid is 8-15%, and the reaction time is 25-35 min; the pigment is water-soluble pigment.

9. The method for preparing the cosmetic-grade chameleon coloring pearlescent pigment according to claim 8, wherein in the step (8), the molar concentration of trivalent aluminum ions in the trivalent aluminum salt solution is 1.25-1.95 mol/L, the trivalent aluminum salt is aluminum trichloride, the mass-volume ratio of the chameleon Long Zhuguang pigment to the trivalent aluminum salt solution is 30-60 g:30-80 mL, and the reaction time is 25-35 min.

10. The cosmetic-grade chameleon-colored pearlescent pigment produced by the process for producing the cosmetic-grade chameleon-colored pearlescent pigment of any one of claims 1 to 9.