CN102660157B - Large-sized synthesized mica pearlescent pigment and preparation method thereof - Google Patents
Large-sized synthesized mica pearlescent pigment and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a large-sized synthesized mica pearlescent pigment, which is characterized in that large-sized synthesized mica powder with d50 being equal to 50 to 600 micrometers is adopted as a substrate, wherein a high-refraction oxide membrane is arranged on the surface of the substrate, the high-refraction oxide membrane is formed by implementing the hydrolysis enveloping adopting soluble salt which can be hydrolyzed into high-refraction oxide as a hydrolysis precursor under the existence of soluble trivalent aluminum salt which is used as a depositing agent. The invention also relates to a preparation method of the large-sized synthesized mica pearlescent pigment. The large-sized synthesized mica pearlescent pigment has strong star-like twinkling property and good decoration effect and can be widely applied to the industries such as cosmetics, synthesized leather, plastics, texture costumes, paint and the like.
Description
Technical field
The present invention relates to a kind of large particle diameter synthetic mica pearly pigment and preparation method thereof, belong to inorganic non-metallic effect pigment field.
Background technology
In recent years, the pearly pigment that the synthetic mica of take is base material, with its high whiteness (silvery white series), (iris and metallic color series) bright in luster, progressively be widely used without hazardous trace elements, the premium properties such as high temperature resistant, "dead".Especially the large particle diameter synthetic mica pearly pigment that particle diameter is 50 ~ 1000 μ m, have superpower flickering, has more special decorative effect.In this large particle size range, natural mica is variegated quality that badly influences Study On Mica inevitably; The pearly pigment that the glass flakes of take is base material, because its base material is frangible and the stimulation of skin has been limited to its use range.The large particle diameter pearly pigment of synthetic mica overcomes the shortcoming of above-mentioned two kinds of base materials, has good toughness, and fabulous whiteness, superpower flickering are arranged again simultaneously.But in the preparation of large particle diameter synthetic mica pearly pigment, a large technical barrier being arranged, is that large particle diameter compound mica is larger because of its particle diameter, and specific surface area is little, grinding time is short, and surfactivity is poor, makes the hydrolysis coating be difficult to carry out, while causing coating, produce a large amount of episome TiO
2, have a strong impact on the quality of pearly pigment, even do not produce pearl effect.Chinese patent CN200410065315.0, take natural mica as base material, adopt to add zinc salt hydrolysis coating and prepare large particle diameter natural mica pearly pigment, and identical method also is not suitable for the preparation of large particle diameter synthetic mica pearly pigment; Chinese patent CN200510020568.0 and Chinese patent CN00820062.9 disclose the preparation method of synthetic mica pearly pigment, the technology of preparing that does not relate to large particle diameter synthetic mica pearly pigment, can not solve the technology of preparing difficult problem of large particle diameter synthetic mica pearly pigment equally.
JP7157687A (06 month 20 days nineteen ninety-five) discloses the production method of flaring pearlescent pigment, it comprises at first cladding titanium dioxide on the mica substrate, then under the urea of the precipitation agent as cobalt salt and aluminium salt exists, forms from the teeth outwards cobalt-al oxide layer.
Summary of the invention
The objective of the invention is provides a kind of large particle diameter synthetic mica pearly pigment and preparation method thereof for the deficiencies in the prior art.
According to the present invention, provide following technical scheme:
1. a large particle diameter synthetic mica pearly pigment, is characterized in that, it is with d
50(corresponding particle diameter when the cumulative particle sizes percentile reaches 50%, also be meso-position radius or median particle diameter)=50 ~ 600 μ m (preferred 100 ~ 500 μ m, further preferred 200 ~ 400 μ m) large particle diameter compound mica is base material, the oxide film that has high refractive index on the surface of this base material, this film is to take soluble salt that hydrolyzable generates high refractive index oxide on base material, to form as the hydrolysis presoma coating that is hydrolyzed under base material and the existence as the solubility trivalent aluminium salt of deposition agent.
2. according to above the 1st described large particle diameter synthetic mica pearly pigment, it is characterized in that, in the hydrolysis coating, the add-on of trivalent aluminium salt is that the per kilogram compound mica adds 2 ~ 6g (preferred 3 ~ 5g, further preferably 3.5 ~ 4.5g) to press Al
3+the solubility trivalent aluminium salt of meter.
3. according to above the 2nd described large particle diameter synthetic mica pearly pigment, it is characterized in that, the clad ratio of hydrolysis coating is 5 ~ 45%, preferably 6.5 ~ 30%, further preferably 10 ~ 25%.Clad ratio described here is term commonly used in prior art, the weight percent that generally refers to coating layer for the weight of the base material be wrapped by.
4. according to above the 1st described large particle diameter synthetic mica pearly pigment, it is characterized in that, above-mentioned aluminum soluble salt is selected from one or more in crystal aluminum chloride, aluminum nitrate, Tai-Ace S 150 etc.
5. according to the described large particle diameter synthetic mica pearly pigment of any one of above 1st ~ 4, it is characterized in that, above-mentioned high refractive index oxide (n>1.8) is selected from TiO
2, SnO
2, Fe
2o
3, ZnO, ZrO
2in one or more.
6. according to the described large particle diameter synthetic mica pearly pigment of any one of above 1st ~ 4, it is characterized in that, the soluble salt that above-mentioned hydrolyzable generates high refractive index oxide (refractive index n>1.8) is selected from: TiCl
4, TiOSO
4, SnCl
4, FeCl
3, FeSO
4, Zn (NO
3)
2, ZnCl
2, ZnSO
4, ZrOCl
2in one or more.
7. according to the preparation method of above the 1st described large particle diameter synthetic mica pearly pigment, it is characterized in that comprising the following steps:
(1) by particle diameter, be, d
50=50 ~ 600 μ m (preferred 100 ~ 500 μ m, further preferred 200 ~ 400 μ m) large particle diameter compound mica and the water of (detection of Ma Erwen laser particle analyzer), preferably specific conductivity is less than the reverse osmosis water of 20 μ s/cm or the deionized water that specific conductivity is less than 50 μ s/cm, stir and be made into slurry by solid-to-liquid ratio 1:5 ~ 11.5, under whipped state, slurry is warming up to 70 ~ 90 ℃;
(2), by the per kilogram compound mica, add (for example disposable adding) to press Al
3+the solubility trivalent aluminium salt of meter 2 ~ 6g (preferred 3 ~ 5g, further preferably 3.5 ~ 4.5g), the concentration of aluminum salt solution is 10 ~ 30wt%, continues constant temperature and stirs 10 ~ 30min;
(3), with dilute hydrochloric acid, the pH value is adjusted to 1.6 ~ 3.5, by per kilogram compound mica reinforced 0.1 ~ 0.8mol per hour, by concentration, be that the soluble salt solution that 0.5 ~ 4.0mol/L hydrolyzable generates high refractive index oxide (n > 1.8) slowly adds in slurry, with 2mol/L sodium hydroxide or ammoniacal liquor, keep pH constant simultaneously, under constant temperature, constant pH (i.e. 70 ~ 90 ℃ and pH 1.6 ~ 3.5), be dosed to required form and aspect, stop feeding in raw material, continue constant temperature and stir 10 ~ 30min;
(4), by step (3) gained slurries filtration, with reverse osmosis water, wash to pH=5 ~ 7, in temperature, be 100 ~ 150 ℃ of dryings, 500 ~ 900 ℃ (preferably 600 ~ 860 ℃, further preferably 700 ~ 800 ℃) calcining, obtain large particle diameter (d
50=50 ~ 600 μ m) synthetic mica pearly pigment.
8. according to the preparation method of above the 7th described large particle diameter synthetic mica pearly pigment, it is characterized in that, above-mentioned aluminum soluble salt is selected from one or more in crystal aluminum chloride, aluminum nitrate, Tai-Ace S 150 etc.; Above-mentioned high refractive index oxide (n>1.8) is selected from TiO
2, SnO
2, Fe
2o
3, ZnO, ZrO
2in one or more; The soluble salt that above-mentioned hydrolyzable generates high refractive index oxide (refractive index n>1.8) is selected from: TiCl
4, TiOSO
4, SnCl
4, FeCl
3, FeSO
4, Zn (NO
3)
2, ZnCl
2, ZnSO
4, ZrOCl
2in one or more.
9. according to the preparation method of above the 7th described large particle diameter synthetic mica pearly pigment, it is characterized in that, the feeding quantity of soluble salt is generally 0.625mol ~ 5.625mol/ per kilogram mica powder, and the coating clad ratio formed after calcining is about 5 ~ 45%, preferably 6.5 ~ 30%, further preferably 10 ~ 25%.
10. the purposes for makeup, synthetic leather, plastics, textile garment or paint according to any one described large particle diameter synthetic mica pearly pigment in above 1st ~ 6 or the method for any one obtains in above 7 ~ 9 large particle diameter synthetic mica pearly pigment.
The large particle diameter synthetic mica powder raw material used as base material in the application can adopt any product be purchased.In general, d
50(corresponding particle diameter when the cumulative particle sizes percentile reaches 50%, also be meso-position radius or median particle diameter)=50 ~ 600 μ m, preferred 100 ~ 500 μ m, further preferred 200 ~ 400 μ m.
After the large particle diameter synthetic mica of gained pearly pigment card-coating, adopt the CIE LCH color model of Ai Seli x-rite to detect form and aspect colourity.
That this large particle diameter synthetic mica pearly pigment has is superpower, the flickering as star, has fabulous decorative effect, can be widely used in the industries such as makeup, synthetic leather, plastics, textile garment, paint.
The present invention has the following advantages:
1, utilize " the multivalent metal cation effect " of aluminium salt, changed the electronegativity on large particle diameter compound mica surface, accelerate the sedimentation of hydrolysis presoma material, solved the technical barrier that can not prepare the synthetic pearly pigment of the large particle diameter of high-quality because large particle diameter compound mica specific surface area is little, surfactivity is poor;
2, the Al of aluminium salt
3+have and make titanium dioxide crystal form be converted to the brilliant effect of leading of rutile-type by anatase titanium dioxide, in the pearly pigment preparation of using titanium salt as hydrolysis coating presoma, rutile titanium dioxide has higher specific refractory power, better weathering resistance, corrosion-resistant, make its pearly pigment brightness better, have more and have been widely used.
3, through the check of Ai Seli (x-rite) color measurement instrument, adopt CIE LCH color model to estimate, the large particle diameter pearly pigment of gained of the present invention has higher whiteness, fullness of shade and purer tone.
Embodiment
Further illustrate by the following examples the present invention, wherein said raw material umber, except specified otherwise, is parts by weight or weight percent.
Embodiment 1
(1) take d
50the compound mica 100g of=50 μ m, add by solid-liquid 1:11.5 the reverse osmosis water 1150ml that specific conductivity is 20 μ s/cm, and it is 70 ℃ that intensification limit, limit is stirred to temperature;
(2) in step (1) gained suspension, by the per kilogram compound mica, add 2 gram Al
3+count, add the crystal aluminum chloride (AlCl of concentration 20wt%
3h
2o) solution 9 grams, 70 ℃ of constant temperature stir 10min;
(3) under temperature 70 C, regulating the pH value with dilute hydrochloric acid is 1.6, the titanium tetrachloride that is 4mol/L by concentration is 20ml/h with 0.8mol/kg synthetic mica h() feed rate evenly add lentamente in step (2) suspension, drip the sodium hydroxide solution that concentration is 20wt%, to keep the constant in 1.6 left and right of pH value simultaneously.While being dosed to silvery white pearly pigment standard specimen form and aspect, stop feeding in raw material (for the 100g compound mica, at this moment having added the 0.225mol soluble salt), continue constant temperature and stir 10min;
(4) by step (3) gained slurries filtration, with reverse osmosis water, washing to pH=5 ~ 7, is dry under 100 ± 5 ℃ of conditions in temperature, and 900 ℃ of calcinings, obtain a kind of large particle diameter (d
50=50 μ m) silvery white synthetic mica pearly pigment, the TiO of formation
2coating is about 15% with respect to the clad ratio of compound mica.
After the large particle diameter synthetic mica of gained pearly pigment card-coating, adopt the CIE LCH color model of Ai Seli x-rite to detect form and aspect colourity.Detected result is in Table 1.
Embodiment 2
(1) take d
50the compound mica 100g of=325 μ m, add specific conductivity to be less than the deionized water 825ml of 50 μ s/cm by solid-liquid 1:8.25, and it is 80 ℃ that intensification limit, limit is stirred to temperature;
(2) in step (1) gained suspension, by the per kilogram compound mica, add 4 gram Al
3+count, add the crystal aluminum chloride (AlCl of concentration 10wt%
3h
2o) solution 36 grams, 80 ℃ of constant temperature stir 20min;
(3) at 80 ℃ of temperature, regulating the pH value with dilute hydrochloric acid is 1.9, the titanium tetrachloride that is 2.25mol/L by concentration is 20ml/h with 0.45mol/kg synthetic mica h() feed rate evenly add lentamente in step (2) suspension, drip the sodium hydroxide solution that concentration is 20%, to keep the constant in 1.9 left and right of pH value simultaneously.(for the 100g compound mica, at this moment added the 0.1mol soluble salt) while being dosed to silvery white pearly pigment standard specimen form and aspect, stopped feeding in raw material, continued constant temperature and stir 20min;
(4) by step (3) gained slurries filtration, with reverse osmosis water, washing to pH=5 ~ 7, is dry under 125 ± 5 ℃ of conditions in temperature, and 700 ℃ of calcinings, obtain a kind of large particle diameter (d
50=325 μ m) silvery white synthetic mica pearly pigment, the TiO of formation
2coating is about 7% with respect to the clad ratio of compound mica.
After the large particle diameter synthetic mica of gained pearly pigment card-coating, adopt the CIE LCH color model of Ai Seli x-rite to detect form and aspect colourity.Detected result is in Table 1.
Embodiment 3
(1) take d
50the compound mica 100g of=600 μ m, add by solid-liquid 1:5 the reverse osmosis water 500ml that specific conductivity is 20 μ s/cm, and it is 90 ℃ that intensification limit, limit is stirred to temperature;
(2) in step (1) gained suspension, by the per kilogram compound mica, add 6 gram Al
3+meter, add concentration 30wt% crystal aluminum chloride (AlCl
3h
2o) solution 18 grams, 90 ℃ of constant temperature stir 30min;
(3) at 90 ℃ of temperature, regulating the pH value with dilute hydrochloric acid is 2.2, the titanium tetrachloride that is 0.5mol/L by concentration is 20ml/h with 0.1mol/kg synthetic mica h() feed rate evenly add lentamente in step (2) suspension, drip the sodium hydroxide solution that concentration is 20%, to keep the constant in 2.2 left and right of pH value simultaneously.(for the 100g compound mica, at this moment added the 0.0625mol soluble salt) while being dosed to silvery white pearly pigment standard specimen form and aspect, stopped feeding in raw material, continued constant temperature and stir 30min;
(4) by step (3) gained slurries filtration, with reverse osmosis water, washing to pH=5 ~ 7, is dry under 150 ℃ of conditions in temperature, and 500 ℃ of calcinings, obtain a kind of large particle diameter (d
50=600 μ m) silvery white synthetic mica pearly pigment, the TiO of formation
2coating is about 4.55% with respect to the clad ratio of compound mica.
After the large particle diameter synthetic mica of gained pearly pigment card-coating, adopt the CIE LCH color model of Ai Seli x-rite to detect form and aspect colourity.Detected result is in Table 1.
Embodiment 4
(1) take d
50the compound mica 100g of=50 μ m, add specific conductivity to be less than the deionized water 1150ml of 50 μ s/cm by solid-liquid 1:11.5, and it is 70 ℃ that intensification limit, limit is stirred to temperature;
(2) in step (1) gained suspension, by the per kilogram compound mica, add 2 gram Al
3+count, add the crystal aluminum chloride (AlCl of concentration 20wt%
3h
2o) solution 9 grams, 70 ℃ of constant temperature stir 10min;
(3) under temperature 70 C, regulating the pH value with dilute hydrochloric acid is 3.5, the iron trichloride that is 1mol/L by concentration is 20ml/h with 0.8mol/kg synthetic mica h() feed rate evenly add lentamente in step (2) suspension, drip the sodium hydroxide solution that concentration is 20%, to keep the constant in 3.5 left and right of pH value simultaneously.While being dosed to bronze-colored pearly pigment standard specimen form and aspect, stop feeding in raw material (for the 100g compound mica, at this moment having added the 0.3mol soluble salt), continue constant temperature and stir 10min;
(4) by step (3) gained slurries filtration, with reverse osmosis water, washing to pH=5 ~ 7, is dry under 100 ± 5 ℃ of conditions in temperature, and 550 ℃ of calcinings, obtain a kind of large particle diameter (d
50=50 μ m) bronze-colored synthetic mica pearly pigment, the Fe of formation
2o
3coating is 18% with respect to the clad ratio of compound mica.
After the large particle diameter synthetic mica of gained pearly pigment card-coating, adopt the CIE LCH color model of Ai Seli x-rite to detect form and aspect colourity.Detected result is in Table 1.
Comparative Examples 1: do not add aluminium salt, other is identical with embodiment 3.
(1) take d
50the compound mica 100g of=600 μ m, add by solid-liquid 1:5 the reverse osmosis water 500ml that specific conductivity is 20 μ s/cm, and it is 90 ℃ that intensification limit, limit is stirred to temperature;
(2) at 90 ℃ of temperature, regulating the pH value with dilute hydrochloric acid is 2.2, the titanium tetrachloride that is 0.5mol/L by concentration is 20ml/h with 0.1mol/kg synthetic mica h() feed rate evenly add lentamente in step (2) suspension, drip the sodium hydroxide solution that concentration is 20%, to keep the constant in 2.2 left and right of pH value simultaneously.While being dosed to silvery white pearly pigment standard specimen form and aspect, stop feeding in raw material (for the 100g compound mica, at this moment having added the 0.0625mol soluble salt), continue constant temperature and stir 30min;
(3) by step (2) gained slurries filtration, with reverse osmosis water, washing to pH=5 ~ 7, is dry under 150 ℃ of conditions in temperature, and 500 ℃ of calcinings, obtain a kind of large particle diameter (d
50=600 μ m) silvery white synthetic mica pearly pigment, the TiO of formation
2coating is 4.5% with respect to the clad ratio of compound mica.
After the large particle diameter synthetic mica of gained pearly pigment card-coating, adopt the CIE LCH color model of Ai Seli x-rite to detect form and aspect colourity.Detected result is in Table 1.
CIE LCH color model detected result (x-rite) table 1
From table 1 embodiment 3 and Comparative Examples 1 relatively can find out to there is the embodiment 3 that forms the high refractive index oxide film under the existence of the solubility trivalent aluminium salt as deposition agent and obviously be better than not using the Comparative Examples 1 of solubility trivalent aluminium salt as deposition agent on colourimetric number.
Claims (12)
1. a large particle diameter synthetic mica pearly pigment, is characterized in that, it is with d
50the large particle diameter compound mica of=50 ~ 600 μ m is base material, the oxide film that there is high refractive index on the surface of this base material, this film is to take soluble salt that hydrolyzable generates high refractive index oxide on base material, to form as the hydrolysis presoma coating that is hydrolyzed under base material and the existence as the solubility trivalent aluminium salt of deposition agent
Wherein, in the hydrolysis coating, the add-on of trivalent aluminium salt is that the per kilogram compound mica adds by Al
3+the solubility trivalent aluminium salt of meter 2 ~ 6g.
2. large particle diameter synthetic mica pearly pigment according to claim 1, is characterized in that, the clad ratio of hydrolysis coating is 5 ~ 45%.
3. large particle diameter synthetic mica pearly pigment according to claim 2, is characterized in that, the clad ratio of hydrolysis coating is 6.5 ~ 30%.
4. large particle diameter synthetic mica pearly pigment according to claim 1, is characterized in that, described aluminum soluble salt is selected from one or more in crystal aluminum chloride, aluminum nitrate, Tai-Ace S 150.
5. according to the described large particle diameter synthetic mica pearly pigment of any one of claim 1 ~ 4, it is characterized in that, the oxide compound of described high refractive index is selected from TiO
2, SnO
2, Fe
2o
3, ZnO, ZrO
2in one or more.
6. according to the described large particle diameter synthetic mica pearly pigment of any one of claim 1 ~ 4, it is characterized in that, the soluble salt that described hydrolyzable generates high refractive index oxide is selected from: TiCl
4, TiOSO
4, SnCl
4, FeCl
3, FeSO
4, Zn (NO
3)
2, ZnCl
2, ZnSO
4, ZrOCl
2in one or more.
7. the preparation method of the large particle diameter synthetic mica pearly pigment of claim 1 is characterized in that comprising the following steps:
(1) by particle diameter, be, d
50large particle diameter compound mica and the water of=50 ~ 600 μ m, stir and be made into slurry by solid-to-liquid ratio 1:5 ~ 11.5, under whipped state, slurry is warming up to 70 ~ 90 ℃;
(2), by the per kilogram compound mica, add by Al
3+the solubility trivalent aluminium salt of meter 2 ~ 6g, wherein the concentration of aluminum salt solution is 10 ~ 30wt%, continues constant temperature and stirs 10 ~ 30min;
(3), with dilute hydrochloric acid, the pH value is adjusted to 1.6 ~ 3.5, by per kilogram compound mica reinforced 0.1 ~ 0.8mol per hour, the soluble salt solution that is 0.5 ~ 4.0mol/L hydrolyzable generation high refractive index oxide by concentration slowly adds in slurry, with 2mol/L sodium hydroxide or ammoniacal liquor, keep pH constant simultaneously, under constant temperature, constant pH, be dosed to required form and aspect, stop feeding in raw material, continue constant temperature and stir 10 ~ 30min;
(4), by step (3) gained slurries filtration, with reverse osmosis water, wash to pH=5 ~ 7, in temperature, be 100 ~ 150 ℃ of dryings, 500 ~ 900 ℃ of calcinings, obtain large particle diameter synthetic mica pearly pigment.
8. the preparation method of large particle diameter synthetic mica pearly pigment according to claim 7, is characterized in that, described water is that specific conductivity is less than the reverse osmosis water of 20 μ s/cm or the deionized water that specific conductivity is less than 50 μ s/cm.
9. according to the preparation method of the described large particle diameter synthetic mica pearly pigment of claim 7 or 8, it is characterized in that, described aluminum soluble salt is selected from one or more in crystal aluminum chloride, aluminum nitrate, Tai-Ace S 150; Described high refractive index oxide is selected from TiO
2, SnO
2, Fe
2o
3, ZnO, ZrO
2in one or more; The soluble salt that described hydrolyzable generates high refractive index oxide is selected from: TiCl
4, TiOSO
4, SnCl
4, FeCl
3, FeSO
4, Zn (NO
3)
2, ZnCl
2, ZnSO
4, ZrOCl
2in one or more.
10. according to the preparation method of the described large particle diameter synthetic mica pearly pigment of claim 7 or 8, it is characterized in that, be dosed to the clad ratio of the high refractive index oxide that obtains 5 ~ 45% after calcining step in step (3).
11. the preparation method according to the described large particle diameter synthetic mica pearly pigment of claim 7 or 8, is characterized in that, is dosed to the clad ratio of the high refractive index oxide that obtains 6.5 ~ 30% after calcining step in step (3).
12. the purposes according to the large particle diameter synthetic mica pearly pigment of any one of claim 1 ~ 6 or the large particle diameter synthetic mica pearly pigment that obtained by any one described method in claim 7 ~ 11 for makeup, synthetic leather, plastics, textile garment or paint.
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| CN103540171B (en) * | 2013-10-11 | 2015-05-13 | 南京理工大学 | Preparation method of single-coating cobalt titanate green/mica pearlescent composite pigment |
| CN104263017B (en) * | 2014-09-24 | 2016-01-27 | 南阳市凌宝珠光颜料有限公司 | A kind of preparation method of iron series crystal effect pigment |
| CN105504889A (en) * | 2016-01-14 | 2016-04-20 | 广西七色珠光材料股份有限公司 | Gold-series low-glossiness laminated pigment and preparation method thereof |
| CN107325589A (en) * | 2017-07-05 | 2017-11-07 | 江苏贝丽得新材料有限公司 | A kind of glittering Gold production effect pearlescent pigment of high-purity titanium ferroalloy and preparation method thereof |
| CN107641339A (en) * | 2017-10-27 | 2018-01-30 | 河北欧克精细化工股份有限公司 | Changeable colors along with angle stereoscopic series feature pearlescent pigment and its preparation technology and purposes |
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