CN114437565A - Preparation method of full-wavelength ultraviolet shielding pearlescent pigment - Google Patents

Preparation method of full-wavelength ultraviolet shielding pearlescent pigment Download PDF

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CN114437565A
CN114437565A CN202111675307.8A CN202111675307A CN114437565A CN 114437565 A CN114437565 A CN 114437565A CN 202111675307 A CN202111675307 A CN 202111675307A CN 114437565 A CN114437565 A CN 114437565A
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solution
reaction
stirring
pearlescent pigment
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卓仲标
唐骏
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Zhejiang Coloray Technology Development Co ltd
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Zhejiang Coloray Technology Development Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/0015—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/0015—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings
    • C09C1/0024—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings comprising a stack of coating layers with alternating high and low refractive indices, wherein the first coating layer on the core surface has the high refractive index
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/06—Treatment with inorganic compounds
    • C09C3/063—Coating
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
    • C09C2200/10—Interference pigments characterized by the core material
    • C09C2200/102—Interference pigments characterized by the core material the core consisting of glass or silicate material like mica or clays, e.g. kaolin

Abstract

The invention discloses a preparation method of a full-wavelength ultraviolet shielding pearlescent pigment, and relates to the technical field of pearlescent pigments. The method specifically comprises the following steps of S1: stirring and dissolving sodium hydroxide in water to obtain a sodium hydroxide solution, adding the pretreated base material, adding reaction auxiliary agent particles, stirring and dispersing, and heating to 50-65 ℃ to obtain a reaction base solution; s2: adding TiCl dropwise into the reaction base liquid4After the dropwise addition of the aqueous solution, heating to 80 ℃, and carrying out heat preservation and crystallization for 2 hours; s3: then ZnCl is added2Adding Na into the solution2CO3Adjusting the pH value of the solution to be neutral, performing suction filtration after the reaction is finished, and washing a filter cake by deionized water until no Cl exists in the filtrate‑Drying and crushing filter cakeAnd after removing the reaction auxiliary agent particles, calcining. The invention discloses a preparation method of full-wavelength ultraviolet shielding pearlescent pigment, which is characterized in that reaction auxiliary agent particles are added into reaction liquid, so that the pH value of the reaction liquid can be adjusted, and Cl in the reaction liquid can be removed‑And the problem of generating a large amount of chlorine-containing wastewater is avoided.

Description

Preparation method of full-wavelength ultraviolet shielding pearlescent pigment
Technical Field
The invention relates to the technical field of pearlescent pigments, in particular to a preparation method of a full-wavelength ultraviolet shielding pearlescent pigment.
Background
In recent years, with the gradual destruction of the ozone layer and the increase of ultraviolet radiation, the intensity of ultraviolet rays on the ground is continuously increased, the excessive irradiation of the ultraviolet rays can cause red swelling, peeling and aging of human bodies, and can cause skin cancer in severe cases, and the ultraviolet rays have strong penetrating power and can cause skin tanning, aging and DNA damage, so the research of ultraviolet-resistant products is gradually becoming a hot field.
The pearl pigment is named because of its pearl-like soft luster, and its main preparation method is to coat a single-layer or multi-layer metal oxide on the surface of a substrate uniformly, so that light can be reflected and refracted multiply on the surface layer and the inner layer to generate interference phenomenon, and in order to increase the ultraviolet resistance of the pearl pigment, the substrate surface is usually coated with the metal oxide with ultraviolet resistance, wherein titanium dioxide is the most commonly used coating material at the earliest.
The existing pearlescent pigment production process is mainly a liquid phase deposition method, namely, in a water solution state, a hydrolysis reaction of metal salt is utilized to generate corresponding metal oxide or hydroxide, the hydrolysis product is adsorbed on the surface of a substrate under the action of coulomb force and van der waals force, the metal salt is mainly chloride, the main byproduct generated after the chloride is hydrolyzed is HCl, the HCl can reduce the pH value of a reaction system and influence the reaction, so that in the prior art, excessive H is usually neutralized by additionally adding an alkaline substance to neutralize the excessive H+The effect of stabilizing pH is achieved, but the dripping speed of alkaline substances in the actual operation process is difficult to accurately control, and Cl in the reaction liquid cannot be controlled-The removal is carried out to generate a large amount of Cl-The wastewater of (2).
Disclosure of Invention
Aiming at the problems, the invention aims to disclose a preparation method of full-wavelength ultraviolet shielding pearlescent pigment, which is characterized in that reaction auxiliary agent particles are added into a reaction liquid, so that the pH value of the reaction liquid can be adjusted, and Cl in the reaction liquid can be removed-And the problem of generating a large amount of chlorine-containing wastewater is avoided.
Specifically, the preparation method of the full-wavelength ultraviolet shielding pearlescent pigment specifically comprises the following steps:
a1: stirring and dissolving sodium hydroxide in water to obtain a sodium hydroxide solution, adding the pretreated base material, adding reaction auxiliary agent particles, stirring and dispersing, and heating to 50-65 ℃ to obtain a reaction base solution;
a2: dropping in the reaction base liquidAdding TiCl4After the dropwise addition of the aqueous solution, heating to 80-95 ℃, and carrying out heat preservation and crystallization for 2 hours;
a3: then ZnCl is added2Adding Na into the solution2CO3Adjusting the pH value of the solution to be neutral, completing the reaction, removing reaction auxiliary agent particles, performing suction filtration, washing a filter cake with deionized water until no Cl exists in the filtrate-And drying, crushing and calcining the filter cake to obtain the full-wavelength ultraviolet shielding pearlescent pigment.
Further, step S2, TiCl4The concentration of the aqueous solution is 2.0mol/L, and the TiCl4The dropping speed of the aqueous solution is 3.0-4.0 mL/min.
Further, the ZnCl2The concentration of the solution is 1.0mol/L, and the ZnCl is2Solution and TiCl4The volume ratio of the aqueous solution is 1 (1-6).
Further, the base material is superfine flaky mica or flaky glass flakes.
Further, the pretreatment of the substrate is as follows: weighing a base material, ultrasonically dispersing the base material in dimethyl sulfoxide, adding N- (3-sulfopropyl) -N- (acryloyloxyethyl) -N, N-dimethyl alkali, stirring and dissolving, dropwise adding a benzoyl peroxide solution, stirring and uniformly mixing, heating in an oil bath to 90-100 ℃, stirring and preserving heat for reacting for 24-48h, cooling to room temperature, filtering, washing a filter cake with absolute ethyl alcohol for 2-3 times, then washing with deionized water at 90 ℃ for 2-3 times, and performing vacuum drying.
The base material is pretreated by N- (3-sulfopropyl) -N- (acryloyloxyethyl) -N, N-dimethyl alkali, the N- (3-sulfopropyl) -N- (acryloyloxyethyl) -N, N-dimethyl alkali is used as an interface modification layer, and the N- (3-sulfopropyl) -N- (acryloyloxyethyl) -N, N-dimethyl alkali is introduced to the surface of the base material, so that the dispersibility and stability of the base material can be improved, the subsequent coating is facilitated, the affinity between the base material and titanium can be increased, and the hydrous titanium dioxide generated by titanium tetrachloride hydrolysis can be deposited and coated on the surface of the base material preferentially.
Further, the reaction auxiliary agent particles are calcined hydrotalcite particles with hydroxide intercalation.
Further, the preparation method of the reaction auxiliary agent particles comprises the following steps:
s1: stirring and dissolving magnesium nitrate hexahydrate and aluminum nitrate nonahydrate in water to prepare a mixed salt solution, adding nano ferroferric oxide particles into the mixed salt solution, stirring and dispersing at the speed of 800-1000r/min, then adding tetrapropylammonium hydroxide and urea, heating to 50 ℃, keeping the temperature and stirring for 20-30min, then placing at the temperature of 150-160 ℃, keeping the temperature and crystallizing for 24h, taking out, cooling to room temperature and filtering, washing and centrifuging a filter cake with deionized water to obtain a supernatant with the pH value of 7-8, and drying for 6-12h to obtain a hydrotalcite precursor;
s2: taking a hydrotalcite precursor, roasting for 2-12h at the temperature of 400-600 ℃ in a nitrogen atmosphere, and cooling to room temperature to obtain a composite oxide;
s3: adding the prepared composite oxide into NaOH solution, magnetically stirring for 2-12h, filtering, washing and centrifuging a filter cake with deionized water until the pH value of a supernatant is 7-8, and drying for 12-15h to obtain reaction auxiliary particles.
In the preparation process of the layered hydrotalcite, the nano ferroferric oxide is added, so that the magnetism of the prepared layered hydrotalcite is increased, the separation in the preparation process is facilitated, and meanwhile, in the process of preparing reaction auxiliary agent particles, the nano ferroferric oxide is wrapped in the reaction auxiliary agent particles, so that the stability of the ferroferric oxide can be ensured to a certain extent.
Further, the mass ratio of the magnesium nitrate hexahydrate, the aluminum nitrate nonahydrate and the nano ferroferric oxide is (1-3) to 1 (0.06-0.08).
Further, the concentration range of the magnesium nitrate hexahydrate in the mixed salt solution is 0.1-1 mol/L.
The invention has the beneficial effects that:
1. the invention discloses a preparation method of full-wavelength ultraviolet shielding pearlescent pigment, which comprises the steps of adding calcined hydrotalcite with hydroxide intercalation as reaction auxiliary agent particles into a reaction liquid, wherein hydroxide ions in the middle of the main body of the calcined hydrotalcite can adsorb and replace chloride ions in the reaction liquid, and then neutralizing the hydroxide ions in the reaction liquid, so that the purposes of adjusting the pH of the reaction liquid, adsorbing and removing the chloride ions in the reaction liquid and avoiding generating a large amount of chlorine-containing wastewater are achieved, after the reaction is finished, the reaction auxiliary agent particles can be repeatedly recycled after being resolved by magnetic separation, the aim of recycling resources is fulfilled, meanwhile, the whole adjusting process does not need artificial intervention, and the problems that in the prior art, alkali liquor is dripped, cannot be accurately controlled and the pH of the reaction liquid fluctuates are solved.
2. The invention discloses a preparation method of full-wavelength ultraviolet shielding pearlescent pigment, which is characterized in that zinc oxide and titanium dioxide are used in a composite way, the ultraviolet shielding capability of nano titanium oxide is greatly higher than that of zinc oxide in ultraviolet middle wave band, and the ultraviolet shielding capability of nano titanium oxide is not as good as that of zinc oxide in ultraviolet long wave band, so that the nano titanium oxide and zinc oxide are used in combination, the prepared product has better performance, the ultraviolet shielding capability is stronger, and the market popularization and use are facilitated
Detailed Description
The present invention will be described in detail with reference to the following specific examples, which are specifically set forth below:
example one
Preparation of reaction auxiliary particles
S1: weighing 243.1g of magnesium nitrate hexahydrate and 375.79g of aluminum nitrate nonahydrate, stirring and dissolving the magnesium nitrate hexahydrate and the aluminum nitrate nonahydrate in 2L of water to obtain a mixed salt solution, adding 30.06g of nano ferroferric oxide into the mixed salt solution, stirring and dispersing the mixture at the speed of 800-;
s2: 200g of hydrotalcite precursor was taken and heated at 2 ℃ for min under a nitrogen atmosphere-1Heating to 500 ℃, roasting for 5 hours, and cooling to room temperature to obtain a composite oxide;
s3: weighing NaOH and dissolving the NaOH in deionized water to obtain a sodium hydroxide solution with the concentration of 1mol/L, weighing 10g of composite oxide, placing the composite oxide in 800mL of sodium hydroxide solution, magnetically stirring for 2-12h, filtering, washing and centrifuging a filter cake with deionized water until the pH value of a supernatant is 7-8, and drying for 12-15h to obtain reaction auxiliary particles.
Preparation of full-wavelength ultraviolet shielding pearlescent pigment
Pretreatment of a base material: weighing 1.0g of benzoyl peroxide, stirring and dissolving in 40mL of dimethyl sulfoxide to obtain a benzoyl peroxide solution, weighing 13g of superfine flaky mica, ultrasonically dispersing in 100mL of dimethyl sulfoxide, adding 6g N- (3-sulfopropyl) -N- (acryloyloxyethyl) -N, N-dimethyl alkali, stirring and dissolving, dropwise adding the benzoyl peroxide solution, stirring and uniformly mixing, heating in an oil bath to 100 ℃, stirring and preserving heat for reacting for 48 hours, cooling to room temperature, filtering, washing a filter cake for 3 times by using absolute ethyl alcohol, then washing for 3 times by using deionized water at 90 ℃, and performing vacuum drying at 120 ℃.
Weighing sodium hydroxide, stirring and dissolving the sodium hydroxide in water to prepare a sodium hydroxide aqueous solution with the concentration of 1.5mol/L, weighing 53.0mL of the sodium hydroxide aqueous solution, adding 5g of the pretreated base material, adding 1g of the reaction auxiliary agent particles, stirring and dispersing, heating in a water bath to 50 ℃ to obtain a reaction base solution, and adding 20.0mL of 2.0mol/L TiCl4The aqueous solution is dripped into the reaction base liquid at the speed of 3.0mL/min, after the dripping is finished, the temperature is raised to 80 ℃, the temperature is kept for crystallization for 2 hours, and then 60mL of 1.0mol/L ZnCl is added2Adding 1.0mol/L Na into the solution2CO3Neutralizing the system to neutrality, removing reaction assistant particles by magnetic separation, vacuum filtering, washing with deionized water until the filtrate is free of Cl-(1.0mol/L AgNO3Detecting no white precipitate in the solution), drying the filter cake at 80 ℃, crushing, and calcining at 500 ℃ to obtain the full-wavelength ultraviolet shielding pearlescent pigment.
Example two
Preparation of reaction auxiliary particles
S1: weighing 534.83g of magnesium nitrate hexahydrate and 750.26g of aluminum nitrate nonahydrate, stirring and dissolving in 2L of water to obtain a mixed salt solution, adding 45.06g of nano ferroferric oxide into the mixed salt solution, stirring and dispersing at the speed of 800-;
s2: taking 150g of hydrotalcite precursor, and heating at 10 ℃ for min in nitrogen atmosphere-1Heating to 400 ℃ at the heating rate, roasting for 12 hours, and cooling to room temperature to obtain a composite oxide;
s3: weighing NaOH and dissolving the NaOH in deionized water to obtain a sodium hydroxide solution with the concentration of 1mol/L, weighing 15g of composite oxide, placing the composite oxide in 1200mL of sodium hydroxide solution, magnetically stirring for 2-12h, filtering, washing and centrifuging a filter cake with deionized water until the pH value of a supernatant is 7-8, and drying for 12-15h to obtain reaction auxiliary particles.
Preparation of full-wavelength ultraviolet shielding pearlescent pigment
Pretreatment of a base material: weighing 0.85g of benzoyl peroxide, stirring and dissolving in 30mL of dimethyl sulfoxide to obtain a benzoyl peroxide solution, weighing 10g of superfine flaky mica, ultrasonically dispersing in 100mL of dimethyl sulfoxide, adding 4g N- (3-sulfopropyl) -N- (acryloyloxyethyl) -N, N-dimethyl base, stirring and dissolving, dropwise adding the benzoyl peroxide solution, stirring and uniformly mixing, heating in an oil bath to 90 ℃, stirring and preserving heat for reacting for 40 hours, cooling to room temperature, filtering, washing a filter cake for 2 times by using absolute ethyl alcohol, then washing for 3 times by using deionized water at 90 ℃, and performing vacuum drying at 110 ℃.
Weighing sodium hydroxide, stirring and dissolving the sodium hydroxide in water to prepare a sodium hydroxide aqueous solution with the concentration of 1.5mol/L, weighing 53.0mL of the sodium hydroxide aqueous solution, adding 5g of the pretreated base material, adding 1.2g of the reaction auxiliary agent particles, stirring and dispersing, heating in a water bath to 50 ℃ to obtain a reaction base solution, and adding 20.0mL of TiCl with the concentration of 2.0mol/L4The aqueous solution is dripped into the reaction base liquid at the speed of 3.0mL/min, after the dripping is finished, the temperature is raised to 80 ℃, the temperature is kept for crystallization for 2 hours, and then 20mL of 1.0mol/L ZnCl is added2Adding 1.0mol/L Na into the solution2CO3Neutralizing the system to neutrality, removing reaction assistant particles by magnetic separation, vacuum filtering, washing with deionized water until the filtrate is free of Cl-(1.0mol/L AgNO3Detecting no white precipitate in the solution), drying the filter cake at 80 ℃, crushing, and calcining at 400 ℃ to obtain the full-wavelength ultraviolet shielding pearlescent pigment.
EXAMPLE III
Preparation of reaction auxiliary particles
S1: weighing 769.20g of magnesium nitrate hexahydrate and 1125.39g of aluminum nitrate nonahydrate, stirring and dissolving in 2L of water to obtain a mixed salt solution, adding 78.78g of nano ferroferric oxide into the mixed salt solution, stirring and dispersing at the speed of 800-;
s2: 100g of hydrotalcite precursor was taken and heated at 8 ℃ for min under a nitrogen atmosphere-1Heating to 600 ℃, roasting for 2h, and cooling to room temperature to obtain a composite oxide;
s3: weighing NaOH and dissolving the NaOH in deionized water to obtain a sodium hydroxide solution with the concentration of 1mol/L, weighing 2g of composite oxide, placing the composite oxide in 500mL of sodium hydroxide solution, magnetically stirring for 2-12h, filtering, washing and centrifuging a filter cake with deionized water until the pH value of a supernatant is 7-8, and drying for 12-15h to obtain reaction auxiliary particles.
Preparation of full-wavelength ultraviolet shielding pearlescent pigment
Pretreatment of a base material: weighing 0.85g of benzoyl peroxide, stirring and dissolving in 30mL of dimethyl sulfoxide to obtain a benzoyl peroxide solution, weighing 11g of flaky glass flakes, ultrasonically dispersing in 100mL of dimethyl sulfoxide, adding 5g N- (3-sulfopropyl) -N- (acryloyloxyethyl) -N, N-dimethyl alkali, stirring and dissolving, dropwise adding the benzoyl peroxide solution, stirring and uniformly mixing, heating in an oil bath to 95 ℃, stirring and preserving heat for reacting for 24 hours, cooling to room temperature, filtering, washing a filter cake with absolute ethyl alcohol for 2-3 times, then washing with deionized water at 90 ℃ for 2-3 times, and vacuum drying at 100 ℃
Weighing sodium hydroxide, stirring and dissolving the sodium hydroxide in water to prepare a sodium hydroxide aqueous solution with the concentration of 1.5mol/L, weighing 53.0mL of the sodium hydroxide aqueous solution, adding 5g of the pretreated base material, adding 1.5g of reaction auxiliary agent particles, stirring and dispersing, heating in a water bath to 50 ℃ to obtain the sodium hydroxide aqueous solutionTo the reaction base, 20.0mL of 2.0mol/L TiCl was added4The aqueous solution is dripped into the reaction base liquid at the speed of 4.0mL/min, after the dripping is finished, the temperature is raised to 80 ℃, the temperature is kept for crystallization for 2 hours, and then 120mL of 1.0mol/L ZnCl is added2Adding 1.0mol/L Na into the solution2CO3Neutralizing the system to neutrality, removing reaction assistant particles by magnetic separation, vacuum filtering, washing with deionized water until the filtrate is free of Cl-(1.0mol/L AgNO3Detecting no white precipitate in the solution), drying the filter cake at 80 ℃, crushing, and calcining at 550 ℃ to obtain the full-wavelength ultraviolet shielding pearlescent pigment.
Comparative example 1
The comparative example is different from the first example in that the substrate of the comparative example is not pretreated.
Comparative example No. two
The comparative example is different from the first example in that no reaction aid particles are added during the reaction.
Experiment-coating rate detection
The coating rates of the pearlescent pigments prepared in the first to third examples and the first comparative example were measured, and the measurement results are shown in table 1:
TABLE 1
Example one Example two EXAMPLE III Comparative example 1
Coating rate 99％ 99.1％ 98％ 76％
As can be seen from the data in the table above, after the base material is pretreated by the method of the present invention, the coating rate of the titanium dioxide/zinc oxide composite material on the base material is high in the subsequent preparation process, while the coating rate of the comparative example I is greatly reduced.
Experimental chloride ion detection
The concentrations of chloride ions in the reaction solutions obtained by adding the sodium carbonate solution to the reaction solutions of the first to third examples and the second comparative example were measured, and the measurement results are shown in the following table 2:
TABLE 2
Example one Example two EXAMPLE III Comparative example No. two
Cl-Concentration (mol/L) 0.25 0.30 0.33 1.89
As can be seen from the data in Table 2, the reaction auxiliary agent particles can remove chloride ions in the reaction solution, effectively reduce the content of chloride ions in the waste liquid, and are beneficial to ensuring the stability of the reaction and the reaction effect.
Although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the invention as defined in the appended claims. The techniques, shapes, and configurations not described in detail in the present invention are all known techniques.

Claims (9)

1. A preparation method of full-wavelength ultraviolet shielding pearlescent pigment is characterized by comprising the following steps:
a1: stirring and dissolving sodium hydroxide in water to obtain a sodium hydroxide solution, adding the pretreated base material, adding reaction auxiliary agent particles, stirring and dispersing, and heating to 50-65 ℃ to obtain a reaction base solution;
a2: adding TiCl dropwise into the reaction base liquid4After the dropwise addition of the aqueous solution, heating to 80-95 ℃, and carrying out heat preservation and crystallization for 2 hours;
a3: then ZnCl is added2Adding Na into the solution2CO3Adjusting the pH value of the solution to be neutral, completing the reaction, removing reaction auxiliary agent particles, performing suction filtration, washing a filter cake with deionized water until no Cl exists in the filtrate-And drying, crushing and calcining the filter cake to obtain the full-wavelength ultraviolet shielding pearlescent pigment.
2. The method for preparing full-wavelength UV-screening pearlescent pigment according to claim 1, wherein the step S2 is TiCl4The concentration of the aqueous solution is 2.0mol/L, and the TiCl4Dropping speed of aqueous solutionThe degree is 3.0-4.0 mL/min.
3. The method for preparing full-wavelength ultraviolet-shielding pearlescent pigment according to claim 2, wherein the ZnCl is used as a main component2The concentration of the solution is 1.0mol/L, and the ZnCl is2Solution and TiCl4The volume ratio of the aqueous solution is 1 (1-6).
4. The method for preparing full-wavelength ultraviolet-shielding pearlescent pigment according to claim 3, wherein the base material is ultrafine flaky mica or flaky glass flakes.
5. The method for preparing full-wavelength ultraviolet shielding pearlescent pigment according to claim 4, wherein the pretreatment of the substrate is as follows: weighing a base material, ultrasonically dispersing the base material in dimethyl sulfoxide, adding N- (3-sulfopropyl) -N- (acryloyloxyethyl) -N, N-dimethyl alkali, stirring and dissolving, dropwise adding a benzoyl peroxide solution, stirring and uniformly mixing, heating in an oil bath to 90-100 ℃, stirring and preserving heat for reacting for 24-48h, cooling to room temperature, filtering, washing a filter cake with absolute ethyl alcohol for 2-3 times, then washing with deionized water at 90 ℃ for 2-3 times, and performing vacuum drying.
6. The method for preparing full-wavelength UV-screening pearlescent pigment according to any one of claims 1-5, wherein the reaction promoter particles are hydroxide-intercalated calcined hydrotalcite particles.
7. The method for preparing full-wavelength ultraviolet shielding pearlescent pigment according to claim 6, wherein the reaction auxiliary particles are prepared by the following steps:
s1: stirring and dissolving magnesium nitrate hexahydrate and aluminum nitrate nonahydrate in water to prepare a mixed salt solution, adding nano ferroferric oxide particles into the mixed salt solution, stirring and dispersing at the speed of 800-1000r/min, then adding tetrapropylammonium hydroxide and urea, heating to 50 ℃, keeping the temperature and stirring for 20-30min, then placing at the temperature of 150-160 ℃, keeping the temperature and crystallizing for 24h, taking out, cooling to room temperature and filtering, washing and centrifuging a filter cake with deionized water to obtain a supernatant with the pH value of 7-8, and drying for 6-12h to obtain a hydrotalcite precursor;
s2: taking a hydrotalcite precursor, roasting for 2-12h at the temperature of 400-600 ℃ in a nitrogen atmosphere, and cooling to room temperature to obtain a composite oxide;
s3: adding the prepared composite oxide into NaOH solution, magnetically stirring for 2-12h, filtering, washing and centrifuging a filter cake with deionized water until the pH value of a supernatant is 7-8, and drying for 12-15h to obtain reaction auxiliary particles.
8. The preparation method of the full-wavelength ultraviolet shielding pearlescent pigment according to claim 7, wherein the mass ratio of the magnesium nitrate hexahydrate, the aluminum nitrate nonahydrate and the nano ferroferric oxide is (1-3) to 1 (0.06-0.08).
9. The method for preparing a full-wavelength ultraviolet-screening pearlescent pigment according to claim 8, wherein the concentration of magnesium nitrate hexahydrate in the mixed salt solution is in the range of 0.1-1 mol/L.
CN202111675307.8A 2021-12-31 2021-12-31 Preparation method of full-wavelength ultraviolet shielding pearlescent pigment Pending CN114437565A (en)

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