CN105778570B - High brightness and the super flash-type silvery white pearlescent pigment of high color saturation and preparation method thereof - Google Patents
High brightness and the super flash-type silvery white pearlescent pigment of high color saturation and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to pearlescent pigment technical field, it is related to a kind of high brightness and the super flash-type silvery white pearlescent pigment of high color saturation and preparation method thereof.The following steps are included: A, surface sensitizing, mica powder is placed in the hydrochloric acid mixed solution dissolved with stannous chloride and carries out surface sensitizing, it filters and washs, B, it is silver-plated, silver ammino solution and sodium hydroxide solution is added dropwise in solution after the completion of step A simultaneously while stirring, C, dispersion, agitating and heating obtains silvered mica slurry liquid, anionic surfactant is added in slurries, D, coating, under conditions of constant temperature stirring, titanium tetrachloride solution and sodium hydroxide solution are added dropwise simultaneously, water sample is added dropwise to silvery white, E, calcining, 200-600 DEG C of calcining 1-3h in air atmosphere, obtain silvery white pearlescent pigment.The present invention have many advantages, such as it is low in cost, highly-safe, be easy to implement industrialized production, be suitble to industrialization large-scale production.
Description
Technical field
The invention belongs to pearlescent pigment technical field, it is related to a kind of high brightness and the super flash-type silvery white pearly-lustre face of high color saturation
Material and preparation method thereof.
Background technique
Pearlescent pigment is a kind of decorative pigment with pearlescent, by with mica, foliated glass, sheet oxygen
Changing the sheet substrates such as aluminium is nucleome, deposits the metal oxygen of one or more layers high refractive index on its surface using special preparation process
Compound.To generate strong relief pearlescent effect under the reflection of light and refraction action, have it is nontoxic, can it is decorative it is strong, change
It learns stability and waits excellent performances well, be widely used in the fields such as cosmetics, leather, plastics, coating.
However, acceptable substrate of the natural mica as pearlescent pigment, while there is also following disadvantages: (1) natural mica sheet
Body contains some colouring ions (such as iron, chromium), there is the excitation purity for causing that product is reduced in subsequent roasting process.
(2) during wet grinding, splitting can be damaged because of the effect of mechanical shear stress, and sheet surface is made edge occur
Gradient and roughing in surface reduce the gloss of pigment product so that light be made to occur scattering and diffusing reflection.
With the improvement of people's life quality, common decorative pigment is not able to satisfy the requirement of people gradually, wherein greatly
More top grade pearlescent pigments are still needed to external import, and the especially super flash-type silvery white pearlescent pigment of high brightness, high chroma occupies very one big
Point.The method that chemical silvering is used in Chinese patent ZL201420559497.6 is plated on the surface of synthetic mica or glass flake
Silver, so that being made super dodges silver-coloured lustre pigment；But clad ratio silver-colored in the preparation process is larger, higher cost.United States Patent (USP)
2885366 disclosures coat aluminium flake by using silica to play passivation aluminium surface, to continue to coat metal oxidation
Object；The technological operation is cumbersome, and reaction process generates hydrogen, and safety is lower, is unfavorable for industrialized production.
Summary of the invention
The object of the present invention is to provide a kind of simple processes, and production cost is low, the highly-safe high brightness of production process and
The preparation method of the super flash-type silvery white pearlescent pigment of high color saturation.
It is a further object of the present invention to provide a kind of high brightness and the super flash-type silvery white pearlescent pigment of high color saturation.
In order to achieve the above objectives, present invention employs following technical proposals: a kind of high brightness and the super flash-type of high color saturation
The preparation method of silvery white pearlescent pigment, comprising the following steps:
A, mica powder is placed in the hydrochloric acid mixed solution dissolved with stannous chloride and carries out surface sensitizing by surface sensitizing, and filtering is simultaneously
Washing, sequentially adds deionized water, polyvinylpyrrolidone and glucose, stirs and adjusts pH to alkalinity,
B, silver-plated, silver ammino solution and sodium hydroxide solution is added dropwise simultaneously while stirring in solution after the completion of step A, ties up
PH is held in alkalinity, is filtered after being stirred to react and obtains filter cake, filter cake is washed with deionized to filtrate and is in neutrality, and obtains silvered mica
Powder,
C, disperse, the obtained silvered mica powder of step B is add to deionized water, agitating and heating obtains silvered mica
Anionic surfactant is added in slurry liquid in slurries, adjusts pH value to 1.0-2.5, temperature is adjusted to 40-70 DEG C, and constant temperature stirs
It mixes lower cocurrent and tin chloride solution reaction and sodium hydroxide solution is added dropwise,
D, the reaction solution of step C is warming up to 60-90 DEG C by coating, and slurry pH value is adjusted to 1.0-2.5, is stirred in constant temperature
Under conditions of mixing, while titanium tetrachloride solution and sodium hydroxide solution is added dropwise, maintains pH to stablize constant, be added dropwise to water sample to silver
It is white, stop charging, continue to stir 1-4h, be neutrality with sodium hydroxide solution regulation system pH, continues to stir 1-4h, be precipitated
Predecessor,
E, it calcines, the obtained powders from precipitated precursor of step D is washed with deionized and is dried, in air atmosphere 200-
600 DEG C of calcining 1-3h are to get to silvery white pearlescent pigment.
In the preparation method of the above-mentioned super flash-type silvery white pearlescent pigment of high brightness and high color saturation, in step, table
Face sensitizing temperature is 10-30 DEG C, and the surface sensitizing time is greater than 30min, and pH value is adjusted to 10-12, and adjusts the temperature to 10-40
DEG C, the granularity of the mica powder is 10-60 μm, and female undersized easily causes plating silver content to increase, and cost improves；Mica granularity is excessive
Easily cause the peeling and mechanical damage of clad.
In the preparation method of the above-mentioned super flash-type silvery white pearlescent pigment of high brightness and high color saturation in step, cloud
The mass ratio of female powder and stannous chloride is 5-20:1, and mica powder: glucose: the mass ratio of polyvinylpyrrolidone is 1:2:0.6.
In the preparation method of the above-mentioned super flash-type silvery white pearlescent pigment of high brightness and high color saturation in stepb, institute
The production method for the silver ammino solution stated are as follows: the silver nitrate for weighing certain mass is dissolved in a certain amount of deionized water, is stirred molten
Solution, is slowly added dropwise ammonium hydroxide, until the precipitating generated is completely dissolved, solution becomes transparence, is silver ammino solution.
In the preparation method of the above-mentioned super flash-type silvery white pearlescent pigment of high brightness and high color saturation in stepb, silver-colored
The concentration of ammonia solution is 5-30g/L, and wherein the mass ratio of the additive amount of silver nitrate and mica powder is 1:1-5, keeps pH in 10-12
Between.
In the preparation method of the above-mentioned super flash-type silvery white pearlescent pigment of high brightness and high color saturation in step C, plating
Cat's silver powder, which is add to deionized water, is heated with stirring to 40-100 DEG C, and anionic surfactant constant temperature is added in slurries
Adjust pH to 1.0-2.5 again after 0.5-2h.
In the preparation method of the above-mentioned super flash-type silvery white pearlescent pigment of high brightness and high color saturation in step C, institute
The solid content of silvered mica slurry body is stated as 5-20%, the mass ratio of tin oxide and silvered mica powder is 0.005-1:1, stannic chloride
Concentration be 0.1-15mol/L.
In the preparation method of the above-mentioned super flash-type silvery white pearlescent pigment of high brightness and high color saturation in step C, institute
The anionic surfactant stated is one kind of sodium alkyl benzene sulfonate, sodium alkyl sulfate, higher fatty acids potassium or alkyl phosphoric acid potassium
Or it is several.
In the preparation method of the above-mentioned super flash-type silvery white pearlescent pigment of high brightness and high color saturation in step D, four
Titanium chloride concentration is 0.5-2mol/L, concentration of sodium hydroxide solution 0.5-2.5mol/L, the quality of titanium tetrachloride and mica powder
Than for 50-134:100.
According to silvery white pearlescent pigment made from above-mentioned preparation method.
Compared with prior art, the present invention has the advantages that (1) mica is silver-plated promotes to optical high reflection and drop
The low low scattering to light, to assign the stronger flickering of silvery white pearly-lustre, higher brightness and color saturation；(2) mica is silver-plated
The disadvantages such as surface irregularity caused by compensating for mica sheet in grinding and pretreatment process, coarse；(3) anion surface active
On the one hand the dispersibility of silvered mica powder in water can be improved in the addition of agent, it is negative on the other hand to can change powder surface electricity
Property is in order to subsequent coating；(4) be compared to aluminum current plate substrate pearlescent pigment, technique safety with higher and at
This is cheap；(5) compared to existing market silvery white pearlescent pigment calcination temperature, the technique possess under lower calcination temperature compared with
Good properties of product, have many advantages, such as it is low in cost, highly-safe, be easy to implement industrialized production, be suitble to industrialization on a large scale
Production.
Specific embodiment
Reagent as used in the following examples can be commercially available unless otherwise specified from routine biochemistry reagent shop.With
Quantitative data in lower embodiment, is respectively provided with three repeated experiments, results are averaged.
Embodiment 1
A kind of preparation method of high brightness and the super flash-type silvery white pearlescent pigment of high color saturation, comprising the following steps:
Step (1): under stirring, fine mica powder is placed in carry out table in the hydrochloric acid mixed solution dissolved with stannous chloride
Face sensitization, sensitizing temperature are 10-30 DEG C, and the surface sensitizing time is greater than 30min, preferably 1hr, filters after surface sensitizing, spends
Ion water washing obtains filter cake；Add deionized water to disperse again filter cake after washing, sequentially adds polyvinylpyrrolidone and Portugal
Grape sugar, persistently stirs 0.5-2h, and by slurry pH value adjusting to 10-12, temperature is adjusted to 10-40 DEG C, under stirring conditions, together
When silver ammino solution and sodium hydroxide solution is added dropwise, maintain pH to stablize constant, after dripping silver ammino solution, be stirred to react 1-4h, take out
Filter washing to filtrate is in neutrality.The mass ratio that mica powder and stannous chloride are controlled in the step is 5-20:1, the quality of mica powder:
The quality of glucose: polyvinylpyrrolidone=1:2:0.6,
The production method of silver ammino solution are as follows: the silver nitrate for weighing certain mass is dissolved in a certain amount of deionized water, stirring
Dissolution, is slowly added dropwise ammonium hydroxide, until the precipitating generated is completely dissolved, solution becomes transparence, is silver ammino solution.Silver ammino solution
Concentration be 5-30g/L, wherein the mass ratio of the additive amount of AgNO3 and mica powder is 1:1-5, and added sodium hydroxide solution is dense
Degree is 0.5-2.5mol/L；
Step (2): the silvered mica powder filter cake that step (1) obtains is add to deionized water, and is stirred 30min and is heated
To 40-100 DEG C, add anionic surfactant, constant temperature continues 0.5-2h, and slurry pH value is adjusted to 1.0-2.5, temperature adjusting
To 40-70 DEG C, under conditions of constant temperature stirring, while tin oxide solution and sodium hydroxide solution is added dropwise, maintains pH to stablize constant,
After dripping tin oxide solution, it is stirred to react 1-4h；Wherein, the solid content of the silvered mica slurry body is 5-20%, oxidation
The additive amount of tin and the mass ratio of silvered mica powder are 0.005-1:1, and the concentration of tin oxide is 0.1-15mol/L, added hydrogen
Sodium hydroxide solution concentration is 0.5-2.5mol/L；Anionic surfactant described in the step is sodium alkyl benzene sulfonate, alkane
The one of which of base sodium sulphate, higher fatty acids potassium, alkyl phosphoric acid potassium.
Step (3): the slurry stirring that step (2) is obtained is warming up to 60-90 DEG C, and slurry pH value adjusting is arrived
Under conditions of constant temperature stirring, while titanium tetrachloride solution and sodium hydroxide solution is added dropwise in 1.0-2.5, maintains pH to stablize constant,
Water sample is added dropwise to silvery white slightly yellowing light, stops charging, continues to stir 1-4h, the hydroxide of 1.0-4.0m/L is used after completion of dropwise addition
Sodium solution regulation system pH is neutrality, continues to stir 1-4h.The powders from precipitated precursor that cladding finishes is washed with deionized, is dried
Afterwards, then 200-500 DEG C of calcining 1-3h in air atmosphere.Wherein titanium tetrachloride concentration is 0.5-2mol/L, added hydrogen-oxygen
Change sodium solution concentration is 0.5-2.5mol/L；It is high brightness and the super flash-type silvery white pearlescent pigment of high color saturation after calcining.
Embodiment 2
A kind of preparation method of high brightness and the super flash-type silvery white pearlescent pigment of high color saturation, comprising the following steps:
A, mica powder is placed in the hydrochloric acid mixed solution dissolved with stannous chloride and carries out surface sensitizing by surface sensitizing, and filtering is simultaneously
Washing, sequentially adds deionized water, polyvinylpyrrolidone and glucose, stirs and adjusts pH to alkalinity,
B, silver-plated, silver ammino solution and sodium hydroxide solution is added dropwise simultaneously while stirring in solution after the completion of step A, stirs
Suction filtration obtains filter cake after mixing reaction, and filter cake is washed with deionized to filtrate and is in neutrality, and obtains silvered mica powder,
C, disperse, the obtained silvered mica powder of step B is add to deionized water, agitating and heating obtains silvered mica
Anionic surfactant is added in slurry liquid in slurries, adjusts pH value to 1.0-2.5, preferably pH=2, temperature is adjusted to 40-70
DEG C, it preferably 55 DEG C, stirs the lower tin oxide solution that is added dropwise and reacts,
D, the reaction solution of step C is warming up to 60-90 DEG C, preferably 75 DEG C by coating, and slurry pH value is adjusted to 1.0-2.5,
It is preferred that pH=2, under conditions of constant temperature stirring, while being added dropwise titanium tetrachloride solution and sodium hydroxide solution, pH is maintained to stablize not
Become, is added dropwise to water sample to silvery white, stops charging, continue to stir 1-4h, preferably stirring 2h, with sodium hydroxide solution regulation system pH
For neutrality, continue to stir 1-4h, preferably stirring 2h, obtain powders from precipitated precursor,
E, it calcines, the obtained powders from precipitated precursor of step D is washed with deionized and is dried, in air atmosphere 200-
500 DEG C of calcining 1-3h calcine 2h preferably at 300 DEG C to get silvery white pearlescent pigment is arrived.
In step, surface sensitizing temperature is 10-30 DEG C, and preferably 20 DEG C, the surface sensitizing time is greater than 30min, this reality
It applies in example, the surface sensitizing time is 1-3h, and pH value is adjusted to 10-12, is preferably adjusted to 11, and adjust the temperature to 10-40 DEG C, excellent
Section recruit to 30 DEG C, the mass ratio of mica powder and stannous chloride is 5-20:1, preferably 8:1, mica powder: glucose: polyethylene
The mass ratio of pyrrolidones is 1:2:0.6, preferably 1:1:0.5.
In stepb, the production method of the silver ammino solution are as follows: the silver nitrate for weighing certain mass is dissolved in a certain amount of
Deionized water in, ammonium hydroxide is slowly added dropwise in stirring and dissolving, until generate precipitating be completely dissolved, solution becomes transparence, is
Silver ammino solution, the concentration of silver ammino solution are 5-30g/L, preferably 10g/L, wherein the quality of the additive amount of silver nitrate and mica powder
Than for 1:1-5, preferably 1:2.
In step C, silvered mica powder, which is add to deionized water, is heated with stirring to 40-100 DEG C, is preferably heated to 60
DEG C, adjust pH to 1.0-2.5, preferably constant temperature 1h, ph to be adjusted to again after anionic surfactant constant temperature 0.5-2h is added in slurries
2, the solid content of the silvered mica slurry body is 5-20%, and preferably solid content is 15%, the matter of tin oxide and silvered mica powder
For amount than being 0.005-1:1, preferred mass ratio is 0.1:1, and the concentration of tin oxide is 0.1-15mol/L, preferably 10mol/L, described
Anionic surfactant be sodium alkyl benzene sulfonate, sodium alkyl sulfate, higher fatty acids potassium or alkyl phosphoric acid potassium one kind or
It is several.
In step D, titanium tetrachloride concentration is 0.5-2mol/L, preferably 1mol/L, and concentration of sodium hydroxide solution is
0.5-2.5mol/L, preferably 1mol/L.
Specific embodiment described herein is only an example for the spirit of the invention.The neck of technology belonging to the present invention
The technical staff in domain can make various modifications or additions to the described embodiments or replace by a similar method
In generation, however, it does not deviate from the spirit of the invention or beyond the scope of the appended claims.
Claims (2)
1. the preparation method of a kind of high brightness and the super flash-type silvery white pearlescent pigment of high color saturation, which is characterized in that including following
Step:
A, mica powder is placed in the hydrochloric acid mixed solution dissolved with stannous chloride and carries out surface sensitizing by surface sensitizing, filters and washs,
Deionized water, polyvinylpyrrolidone and glucose are sequentially added, stir and adjusts pH to alkalinity,
B, silver-plated, silver ammino solution and sodium hydroxide solution is added dropwise in solution after the completion of step A simultaneously while stirring, maintains pH
In alkalinity, being filtered after being stirred to react and obtain filter cake, filter cake is washed with deionized to filtrate and is in neutrality, silvered mica powder is obtained,
C, disperse, the obtained silvered mica powder of step B is add to deionized water, agitating and heating obtains silvered mica slurry
Anionic surfactant is added in liquid in slurries, adjusts pH value to 1.0-2.5, and temperature is adjusted to 40-70 DEG C, under constant temperature stirring
Tin chloride solution reaction and sodium hydroxide solution is added dropwise in cocurrent,
D, the reaction solution of step C is warming up to 60-90 DEG C by coating, and slurry pH value is adjusted to 1.0-2.5, in constant temperature stirring
Under the conditions of, while titanium tetrachloride solution and sodium hydroxide solution is added dropwise, it maintains pH to stablize constant, is added dropwise to water sample to silvery white, stops
It only feeds, continues to stir 1-4h, be neutrality with sodium hydroxide solution regulation system pH, continue to stir 1-4h, obtain precipitating forerunner
Object,
E, it calcines, the obtained powders from precipitated precursor of step D is washed with deionized and is dried, 200-600 DEG C in air atmosphere
1-3h is calcined to get to silvery white pearlescent pigment,
In step, surface sensitizing temperature is 10-30 DEG C, and the surface sensitizing time is greater than 30min, and pH value is adjusted to 10-12, and
10-40 DEG C is adjusted the temperature to, the granularity of the mica powder is 10-60 μm,
In step, the mass ratio of mica powder and stannous chloride is 5-20:1, mica powder: glucose: polyvinylpyrrolidone
Mass ratio is 1:2:0.6,
In stepb, the production method of the silver ammino solution are as follows: the silver nitrate for weighing certain mass is dissolved in a certain amount of go
In ionized water, ammonium hydroxide is slowly added dropwise in stirring and dissolving, until the precipitating generated is completely dissolved, solution becomes transparence, is silver-colored ammonia
Solution,
In stepb, the concentration of silver ammino solution is 5-30g/L, and wherein the mass ratio of the additive amount of silver nitrate and mica powder is 1:
1-5 keeps pH between 10-12,
In step C, silvered mica powder, which is add to deionized water, is heated with stirring to 40-100 DEG C, and anion is added in slurries
PH to 1.0-2.5 is adjusted again after surfactant constant temperature 0.5-2h,
In step C, the solid content of the silvered mica slurry body is 5-20%, and the mass ratio of tin oxide and silvered mica powder is
0.005-1:1, the concentration of stannic chloride are 0.1-15mol/L,
In step C, the anionic surfactant be sodium alkyl benzene sulfonate, sodium alkyl sulfate, higher fatty acids potassium or
The one or more of alkyl phosphoric acid potassium,
In step D, titanium tetrachloride concentration is 0.5-2mol/L, concentration of sodium hydroxide solution 0.5-2.5mol/L, four chlorinations
The mass ratio of titanium and mica powder is 50-134:100.
2. silvery white pearlescent pigment made from preparation method according to claim 1.
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| CN106833030A (en) * | 2017-01-13 | 2017-06-13 | 爱乐彩（天津）新材料科技有限公司 | A kind of preparation method of the artificial synthesized base material pearlescent pigment of super large particle diameter |
| CN108864757A (en) * | 2018-05-31 | 2018-11-23 | 深圳市绚图新材科技有限公司 | A kind of preparation method of conductive silver packet pearl powder |
| CN109266042B (en) * | 2018-11-13 | 2020-12-11 | 南阳市凌宝珠光颜料有限公司 | Preparation method of pure silver crystal pearlescent pigment |
| CN114426780A (en) * | 2021-12-29 | 2022-05-03 | 浙江凯色丽科技发展有限公司 | Preparation method of barium sulfate-based conductive composite pearlescent pigment |
| CN115895293A (en) * | 2022-11-16 | 2023-04-04 | 福建坤彩材料科技股份有限公司 | Pearlescent pigment suitable for powder coating and preparation method and application thereof |
| CN115852511A (en) * | 2022-12-15 | 2023-03-28 | 烟台泰和新材料股份有限公司 | Cool-feeling antistatic spandex and preparation method thereof |
| CN116875082A (en) * | 2023-07-10 | 2023-10-13 | 江苏贝丽得新材料有限公司 | A kind of preparation method of high flash and high whiteness pearlescent pigment |
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Denomination of invention: Super shiny silver white pearlescent pigment with high brightness and color saturation and its preparation method Effective date of registration: 20221201 Granted publication date: 20190419 Pledgee: Zhejiang Deqing rural commercial bank Limited by Share Ltd. Pledgor: ZHEJIANG COLORAY TECHNOLOGY DEVELOPMENT Co.,Ltd. Registration number: Y2022330003356 |
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