CN100390238C - High resisting weather pearly lustre pigment and preparation processof - Google Patents

High resisting weather pearly lustre pigment and preparation processof Download PDF

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Publication number
CN100390238C
CN100390238C CNB2006100901357A CN200610090135A CN100390238C CN 100390238 C CN100390238 C CN 100390238C CN B2006100901357 A CNB2006100901357 A CN B2006100901357A CN 200610090135 A CN200610090135 A CN 200610090135A CN 100390238 C CN100390238 C CN 100390238C
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parts
aqueous solution
minutes
drips
cecl
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CN1861701A (en
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刘景茂
谭坤
赵红芝
赵彤
庞顺星
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Hebei ook new material Limited by Share Ltd
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OUKE FINE CHEMICAL INDUSTORY CO Ltd HEBEI
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Abstract

The present invention relates to a high weather-proof pearlescent pigment and a preparation method thereof. The high weather-proof nacreous pigment is prepared from 40 to 60 portions by weight of ordinary pearlescent pigments, 6 to 8 portions by weight of AlCl3.6H2O, 3 to 4 portions by weight of CeCl3.7H2O and 3.5 to 5.5 portions by weight of ZrOCl2.8H2O. In the preparation method of the high weather-proof pearlescent pigment, on the basis of original pearlescent pigments of mica series, a transparent harmless AlCl3, CeCl3 and ZrOCl2 protective layer is coated by a chemical method; in this way, the colors and the brightness of the original pearlescent pigments are maintained, and a favorable weather-proof property can be formed; accordingly, the application requirements of high weather-proof industry can be met.

Description

A kind of Weather-resistant pearlescent pigments and preparation method thereof
Technical field
The present invention relates to the coating preparation field, especially relate to the preparation method of pearly pigment.
Background technology
So-called pearly pigment is to have glossy pigment as the goods of the giving pearl, it is to be nuclear with white mica or synthetic mica sheet, adopting special chemical technology to coat the powder that one or more layers titanium dioxide and other metal oxide form on its surface, is a kind of structurally very similar to natural peral sandwich body in plane.Pearly pigment can resolve into various monochromatic ray with complex light as bevelled mirror, and forms various interference color by interference of light, demonstrates extremely beautiful pearl gloss and metalluster.But its weathering resistance of common mica series pearly pigment is bad, can not satisfy coatings with high weatherability (as, automobile finish and exterior coating) requirement, people adopted on the basis of common pearly pigment afterwards, coat one deck chromic oxide again and improve its weather resistance, this pearly pigment can guarantee the color and the brightness of product, also can satisfy the weather resistance requirement.But the pearly pigment behind coating one deck chromic oxide is owing to chromic oxide is the practicality that toxic substance influences it.
Summary of the invention
The technical problem to be solved in the present invention provides bright, the nontoxic weathering resistance pearly pigment of a kind of color.
Another technical problem that the present invention will solve provides a kind of preparation method of Weather-resistant pearlescent pigments.This method is on the basis of original mica series pearly pigment; method by chemistry coats upward transparent, harmless weathering protective layer again; so both keep the color and the brightness of original pearly pigment, had the good weather energy again, therefore can satisfy the application demand of high weather-proof industry.
For solving the problems of the technologies described above, a kind of high Weather-resistant pearlescent pigments of the present invention is to be made by following materials based on weight:
40～60 parts of common pearly pigments;
AlCl 36H 26～8 parts of O;
CeCl 37H 23～4 parts of O;
ZrOCl 28H 23.5～5.5 parts of O.
For solving the problems of the technologies described above, the preparation method of a kind of Weather-resistant pearlescent pigments of the present invention comprises the steps:
1,500～700 parts of deionized waters are joined in 40～60 parts of the common pearly pigments, under 130-150 rev/min stirring velocity, are warming up to 70～80 ℃, stir, pearly pigment liquid;
2, drip gradually in the pearly pigment liquid then and contain 6～8 parts of AlCl 36H 2The aqueous solution of O, dripping 10～20% aqueous sodium hydroxide solution simultaneously, to keep the pH value constant, drips AlCl with the volume pump metering 36H 2After the O aqueous solution finishes, under 130-150 rev/min stirring velocity, stirred 10～20 minutes;
3, with dilute hydrochloric acid the 2nd step gained solution acid alkalinity is transferred to pH=2.5～3.5, dropping contains 3～4 parts of CeCl then 37H 2The aqueous solution of O, dripping 10～20% aqueous sodium hydroxide solution simultaneously, to keep the pH value constant, drips CeCl 37H 2After the O aqueous solution finishes, stirred 15 minutes;
4, with dilute hydrochloric acid the 3rd step gained solution acid alkalinity is transferred to pH=3.5～4.5, dropping contains 4.5～5.5 parts of ZrOCl then 28H 2The aqueous solution of O, dripping 10～20% aqueous sodium hydroxide solution simultaneously, to keep the pH value constant, drips ZrOCl 27H 2After the O aqueous solution finishes, stirred 15 minutes;
5, discharging, filtration, washing, oven dry 400～600 ℃ of temperature lower calcinations 15～25 minutes, promptly gets product;
Described AlCl 36H 2The concentration of aqueous solution of O is 120 grams per liters; Described CeCl 37H 2The O concentration of aqueous solution is 50 grams per liters; Described ZrOCl 27H 2The O concentration of aqueous solution is 50 grams per liters.
The protective layer of a kind of Weather-resistant pearlescent pigments of the present invention is by metal oxide Al 2O 3, Ce 2O 3And ZrO 2Form.Al wherein 2O 3, Ce 2O 3And ZrO 2Clad ratio be respectively 2-5%, preferred 3%.
Advantage such as pearly pigment of the present invention has that color is bright, nontoxic, good weatherability, preparation technology are simple.
Embodiment
Embodiment 1
A kind of Weather-resistant pearlescent pigments of the present invention is to be made by following materials based on weight:
40 parts of common pearly pigments;
AlCl 36H 26 parts of O;
CeCl 37H 23 parts of O;
ZrOCl 28H 23.5 parts of O.
The preparation method of a kind of Weather-resistant pearlescent pigments of the present invention comprises the steps:
1,500 parts of deionized waters are joined in 40 parts of the common pearly pigments, under 130 rev/mins stirring velocity, are warming up to 70 ℃, stir, pearly pigment liquid;
2,, drip gradually in the pearly pigment liquid then and contain 6 parts of AlCl 36H 2The aqueous solution of O, dripping 10% aqueous sodium hydroxide solution simultaneously, to keep the pH value constant, and metering drips AlCl 36H 2After the O aqueous solution finishes, under 130 rev/mins stirring velocity, stirred 10 minutes;
3, with dilute hydrochloric acid the 2nd step gained solution acid alkalinity is transferred to pH=2.5, dropping contains 3 parts of CeCl then 37H 2The aqueous solution of O, dripping 10% aqueous sodium hydroxide solution simultaneously, to keep the pH value constant, drips CeCl 37H 2After the O aqueous solution finishes, stirred 10 minutes;
4, with dilute hydrochloric acid the 3rd step gained solution acid alkalinity is transferred to pH=3.5, dropping contains 4.5 parts of ZrOCl then 28H 2The aqueous solution of O, dripping 10% aqueous sodium hydroxide solution simultaneously, to keep the pH value constant, drips ZrOCl 27H 2After the O aqueous solution finishes, stirred 10 minutes;
5, discharging, filtration, washing, oven dry 400 ℃ of temperature lower calcinations 15 minutes, promptly gets product;
Described AlCl 36H 2The concentration of aqueous solution of O is 120 grams per liters; Described CeCl 37H 2The O concentration of aqueous solution is 50 grams per liters; Described ZrOCl 27H 2The O concentration of aqueous solution is 50 grams per liters.
Embodiment 2
A kind of Weather-resistant pearlescent pigments of the present invention is to be made by following materials based on weight:
60 parts of common pearly pigments;
AlCl 36H 28 parts of O;
CeCl 37H 24 parts of O;
ZrOCl 28H 25.5 parts of O.
The preparation method of a kind of Weather-resistant pearlescent pigments of the present invention comprises the steps:
1,700 parts of deionized waters are joined in 60 parts of the common pearly pigments, under 150 rev/mins stirring velocity, are warming up to 80 ℃, stir, pearly pigment liquid;
2,, drip gradually in the pearly pigment liquid then and contain 8 parts of AlCl 36H 2The aqueous solution of O, dripping 20% aqueous sodium hydroxide solution simultaneously, to keep the pH value constant, and metering drips AlCl 36H 2After the O aqueous solution finishes, under 150 rev/mins stirring velocity, stirred 20 minutes;
3, with dilute hydrochloric acid the 2nd step gained solution acid alkalinity is transferred to pH=3.5, dropping contains 4 parts of CeCl then 37H 2The aqueous solution of O, dripping 20% aqueous sodium hydroxide solution simultaneously, to keep the pH value constant, drips CeCl 37H 2After the O aqueous solution finishes, stirred 20 minutes;
4, with dilute hydrochloric acid the 3rd step gained solution acid alkalinity is transferred to pH=4.5, dropping contains 5.5 parts of ZrOCl then 28H 2The aqueous solution of O, dripping 20% aqueous sodium hydroxide solution simultaneously, to keep the pH value constant, drips ZrOCl 27H 2After the O aqueous solution finishes, stirred 20 minutes;
5, discharging, filtration, washing, oven dry 600 ℃ of temperature lower calcinations 25 minutes, promptly gets product;
Described AlCl 36H 2The concentration of aqueous solution of O is 120 grams per liters; Described CeCl 37H 2The O concentration of aqueous solution is 50 grams per liters; Described ZrOCl 27H 2The O concentration of aqueous solution is 50 grams per liters.
Embodiment 3
A kind of Weather-resistant pearlescent pigments of the present invention is to be made by following materials based on weight:
50 parts of common pearly pigments;
AlCl 36H 27 parts of O;
CeCl 37H 23.5 parts of O;
ZrOCl 28H 24.5 parts of O.
For solving the problems of the technologies described above, the preparation method of a kind of Weather-resistant pearlescent pigments of the present invention comprises the steps:
1,600 parts of deionized waters are joined in 50 parts of the common pearly pigments, under 140 rev/mins stirring velocity, are warming up to 75 ℃, stir, pearly pigment liquid;
2,, drip gradually in the pearly pigment liquid then and contain 7 parts of AlCl 36H 2The aqueous solution of O, dripping 15% aqueous sodium hydroxide solution simultaneously, to keep the pH value constant, and metering drips AlCl 36H 2After the O aqueous solution finishes, under 140 rev/mins stirring velocity, stirred 15 minutes;
3, with dilute hydrochloric acid the 2nd step gained solution acid alkalinity is transferred to pH=3, dropping contains 3.5 parts of CeCl then 37H 2The aqueous solution of O, dripping 15% aqueous sodium hydroxide solution simultaneously, to keep the pH value constant, drips CeCl 37H 2After the O aqueous solution finishes, stirred 15 minutes;
4, with dilute hydrochloric acid the 3rd step gained solution acid alkalinity is transferred to pH=4, dropping contains 5 parts of ZrOCl then 28H 2The aqueous solution of O, dripping 15% aqueous sodium hydroxide solution simultaneously, to keep the pH value constant, drips ZrOCl 27H 2After the O aqueous solution finishes, stirred 15 minutes;
5, discharging, filtration, washing, oven dry 500 ℃ of temperature lower calcinations 20 minutes, promptly gets product;
Described AlCl 36H 2The concentration of aqueous solution of O is 120 grams per liters; Described CeCl 37H 2The O concentration of aqueous solution is 50 grams per liters; Described ZrOCl 27H 2The O concentration of aqueous solution is 50 grams per liters.

Claims (1)

1. the preparation method of a Weather-resistant pearlescent pigments comprises the steps:
A, select following portions by weight for use material as raw material:
40～60 parts of common pearly pigments;
AlCl 36H 26～8 parts of O;
CeCl 37H 23～4 parts of O;
ZrOCl 28H 23.5～5.5 parts of O;
B, reactions steps are as follows:
1) 500～700 parts of deionized waters are joined in 40～60 parts of the common pearly pigments, under 130-150 rev/min stirring velocity, are warming up to 70～80 ℃, stir, pearly pigment liquid;
2) drip gradually in the pearly pigment liquid then and contain 6～8 parts of AlCl 36H 2The aqueous solution of O drips 10～20% aqueous sodium hydroxide solution simultaneously, and it is constant to keep the pH value, and metering drips AlCl 36H 2After the O aqueous solution finishes, under 130-150 rev/min stirring velocity, stirred 10～20 minutes;
3) with dilute hydrochloric acid the 2nd step gained solution acid alkalinity is transferred to pH=2.5～3.5, dropping contains 3～4 parts of CeCl then 37H 2The aqueous solution of O, dripping 10～20% aqueous sodium hydroxide solution simultaneously, to keep the pH value constant, drips CeCl 37H 2After the O aqueous solution finishes, stirred 15 minutes;
4) with dilute hydrochloric acid the 3rd step gained solution acid alkalinity is transferred to pH=3.5～4.5, dropping contains 4.5～5.5 parts of ZrOCl then 28H 2The aqueous solution of O, dripping 10～20% aqueous sodium hydroxide solution simultaneously, to keep the pH value constant, drips ZrOCl 27H 2After the O aqueous solution finishes, stirred 15 minutes;
5) discharging, filtration, washing, oven dry 400～600 ℃ of temperature lower calcinations 15～25 minutes, promptly gets product.
CNB2006100901357A 2006-06-23 2006-06-23 High resisting weather pearly lustre pigment and preparation processof Active CN100390238C (en)

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Publication number Priority date Publication date Assignee Title
CN103771900B (en) * 2014-01-27 2016-01-13 汕头市龙华珠光颜料有限公司 A kind of spangles and preparation method thereof, purposes
CN104327552B (en) * 2014-09-25 2016-08-24 广西七色珠光材料股份有限公司 A kind of high temperature resistant pearlescent pigment and preparation method thereof
CN105295449A (en) * 2015-11-10 2016-02-03 温州维特利颜料科技有限公司 Environment-friendly pearlescent pigment
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

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB384473A (en) * 1931-02-07 1932-12-08 Ig Farbenindustrie Ag Manufacture of inorganic coloured pigments
GB1192788A (en) * 1966-06-27 1970-05-20 Du Pont Process for Surface Coating TiO2 Pigments
GB1340045A (en) * 1971-04-19 1973-12-05 Laporte Industries Ltd Treatment of titanium dioxide pigments
JPS532164B2 (en) * 1973-07-25 1978-01-26
CN1217736A (en) * 1997-02-27 1999-05-26 科尔－麦克基化学有限责任公司 Inorganic pigment coated with inorganic oxides
TW419809B (en) * 1997-05-16 2001-01-21 Toshiba Corp Non-volatile semiconductor memory
CN1353145A (en) * 2000-11-06 2002-06-12 默克专利股份有限公司 Stabilization of pearl light luster pigment

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB384473A (en) * 1931-02-07 1932-12-08 Ig Farbenindustrie Ag Manufacture of inorganic coloured pigments
GB1192788A (en) * 1966-06-27 1970-05-20 Du Pont Process for Surface Coating TiO2 Pigments
GB1340045A (en) * 1971-04-19 1973-12-05 Laporte Industries Ltd Treatment of titanium dioxide pigments
JPS532164B2 (en) * 1973-07-25 1978-01-26
CN1217736A (en) * 1997-02-27 1999-05-26 科尔－麦克基化学有限责任公司 Inorganic pigment coated with inorganic oxides
TW419809B (en) * 1997-05-16 2001-01-21 Toshiba Corp Non-volatile semiconductor memory
CN1353145A (en) * 2000-11-06 2002-06-12 默克专利股份有限公司 Stabilization of pearl light luster pigment

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
银白色珠光颜料. 连加松.湖南化工，第2期. 1988
银白色珠光颜料. 连加松.湖南化工，第2期. 1988 *

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Address after: 065001 south side of Hongrun Road, Langfang economic and Technological Development Zone, Hebei

Patentee after: Hebei ook new material Limited by Share Ltd

Address before: 065001 south side of Hongrun Road, Langfang Development Zone, Hebei

Patentee before: Ouke Fine Chemical Industory Co., Ltd., Hebei