CN100462407C - Production of cobalt-titanium series random chromo pigment - Google Patents
Production of cobalt-titanium series random chromo pigment Download PDFInfo
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- CN100462407C CN100462407C CNB2005101054194A CN200510105419A CN100462407C CN 100462407 C CN100462407 C CN 100462407C CN B2005101054194 A CNB2005101054194 A CN B2005101054194A CN 200510105419 A CN200510105419 A CN 200510105419A CN 100462407 C CN100462407 C CN 100462407C
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Abstract
Production of cobalt-titanium series chromo pigment is carried out by pre-treating for substrate material, taking pretreated mica titanium as substrate material, depositing cobaltous hydroxide onto mica titanium surface by wet chemical method, controlling solution acidity and alkalinity, ageing, and converting cobaltous hydroxide into CoO by burning to obtain the final product. It's non-toxic, cheap and simple, has stable performance and no environmental pollution. It can be used for cosmetics, printing ink, coating, building materials and ceramics.
Description
Technical field
The present invention relates to Production of cobalt-titanium series random chromo pigment.
Background technology
Pigment changeable colors along with angle just is meant under irradiate light, and along with the color of the different pigment of viewing angle changes, perhaps viewing angle is constant and change the light source irradiation angle, and the color of pigment changes thereupon.This pigment is widely used in industries such as makeup, printing ink, coating, building materials, pottery, and the false proof markings such as currency, certificate, trade mark and Valued Securities.
According to the retrieval, the method for preparing pigment changeable colors along with angle mainly contains: (1) U.S. Pat 4705300, US4705356, US5084351 etc. adopt physical vaporous deposition, i.e. Fabry-Perot method of piling (being called for short the FP method).The pigment changeable colors along with angle that this method makes has two sandwich structures; Metal level-insulation layer-metal level-insulation layer-metal level.The intermediary metal level is an opaque total reflection layer, and outermost layer is the transparent layer that light can penetrate fully.This method needs the accurately thickness of each layer of control, could obtain good interference of light effect.(2) applied chemistry vapor phase processs such as U.S. Pat 5624468, US5401306 coated insulation layer-metal level-insulation layer successively on transparent aluminium flake finally obtains to have interference effect pigment.The preparation cost of this method is more cheap than FP method, but the apparent colour of pigment and interference effect are obvious not as the FP method.(3) European patent EP 601483, EP686674 etc. mainly are liquid crystal pigments, and it is crosslinked mesomorphic phase polymkeric substance that this pigment is mainly formed, and only has the light of a certain part wavelength to be reflected in the incident light, and the light of other wavelength is absorbed by the substrate of dead color.The gloss of this pigment is pigment changeable colors along with angle not as metal, but color changeable effect is comparatively obvious, is only applicable to the organic materials of low specific refraction.(4) U.S. Pat 6485556 grades are selected for use mica to do substrate material and are adopted chemical Vapor deposition process, coat transparent titanium dioxide at mica surface, coat chromic oxide at titanium dioxide surface again, and outermost layer coats other metals of one deck, obtains having the pigment of interference color.This method coating layer is too much, the preparation process complexity, and owing to use chromium solution, can produce environment and pollute.
Summary of the invention
The purpose of this invention is to provide a kind of method that cobalt-titanium is a pigment changeable colors along with angle for preparing.Invention is by making the pigment changeable colors along with angle of shades of colour change at the mica titanium surface clad oxide compound of different interference color.Discover, increase Co (NO
3)
2Add-on promptly increase mica titanium surface C o (OH)
2Clad ratio, the apparent colour of pigment can deepen, it is obvious that interference color are tending towards.
The method that the present invention adopts U.S. Pat 5611851 to introduce is earlier carried out pre-treatment to mica titanium, to remove mineral substance such as the sodium that influences illumination effect in the mica substrate, potassium, makes the mica titanium substrate material become the part hollow structure.The air that is full of in the hollow structure, its specific refractory power (Rf=1.00) are lower than the specific refractory power (Rf=1.58) of mica substrate.Replace the mica medium with air, can utilize the high refractive index (Rf=2.60～2.80) of titanium dioxide to greatest extent, make the refraction of titanium dioxide more true, to obtain bigger secondary reflection gloss and more pure colourity.Adopt wet chemistry method then, take by weighing a certain amount of mica titanium, be configured to slurries about 6% with deionized water, under 70～80 ℃ of continuous stirrings, pH value with the weak ammonia regulator solution approximates 10, slowly drips 10～15% Co (NO of certain volume in the mica titanium slurries with the speed of 1～2/2min
3)
2Solution, the pH value with weak ammonia and sodium hydroxide solution conditioned reaction system is controlled between 9.0～10.0 it.Co
2+The Co (OH) that continuous hydrolysis generates
2Be deposited on the mica titanium surface uniformly, ageing 40～60min uses deionized water wash 2～3 times, and 120 ℃ of down dry 60～100min put into 850～1000 ℃ of roasting 40～60min of retort furnace, hot discharging, and naturally cooling obtains the powdery pigment changeable colors along with angle.
The mica titanium that can use different interference color instead among the present invention is done substrate material, and the clad ratio that changes cobalt oxide prepares the pigment changeable colors along with angle of different colours change.
Embodiment
Embodiment 1
Take by weighing 3g titanium dioxide massfraction and be 30% mica titanium and put into reactor, add the 6g vitriol oil and 6g strong phosphoric acid mixed solution, approximate 2 with deionized water wash to elutant pH value in 85 ℃ of following backflow 4h.Moist, directly add 10ml 10% NaOH solution at 80 ℃ of following backflow 2h, washing, drying.Take by weighing pretreated mica titanium 1g, add the 25ml deionized water, 74 ℃ of recirculated water heating reflux, and use the pH value of extremely rare ammoniacal liquor regulator solution to approximate 10.0, add the Co (NO of 1.6ml 10% with the speed of 1～2/2min
3)
2Solution with 10% the NaOH solution and the pH value of weak ammonia regulator solution, remains between 9.5～10.5 it simultaneously.It is constant to keep temperature of reaction, ageing 40min, and washing is filtered, and 120 ℃ of following dry 1h put into retort furnace in 900 ℃ of roasting 60min, and hot discharging naturally cools to room temperature.Obtain the powder apparent colour for green, the pigment changeable colors along with angle that interference color are changed by the colour of loess-green.
Embodiment 2
Take by weighing 3g titanium dioxide massfraction and be 40% mica titanium and put into reactor, add 4g hydrofluoric acid and 4g strong phosphoric acid mixed solution, approximate 2 with deionized water wash to elutant pH value in 85 ℃ of following backflow 4h.Moist, directly add 10ml 10% NaOH solution at 80 ℃ of following backflow 2h, washing, drying.Take by weighing pretreated mica titanium 1g, add the 25ml deionized water, 74 ℃ of recirculated water heating reflux, and use the pH value of extremely rare ammoniacal liquor regulator solution to approximate 9.5, add the Co (NO of 1ml 10% with the speed of 1～2/2min
3)
2Solution with 10% the NaOH solution and the pH value of weak ammonia regulator solution, remains between 9.5～10.5 it simultaneously.It is constant to keep temperature of reaction, ageing 40min, and washing is filtered, and 120 ℃ of following dry 1h put into retort furnace in 900 ℃ of roasting 40min, and hot discharging naturally cools to room temperature.Obtaining clad ratio is that apparent colour is red, and interference color are by the pigment changeable colors along with angle of red-green variation.
Embodiment 3
Take by weighing 3g titanium dioxide massfraction and be 60% mica titanium and put into reactor, add 4g concentrated nitric acid and 4g strong phosphoric acid mixed solution, approximate 2 with deionized water wash to elutant pH value in 85 ℃ of following backflow 4h.Moist, directly add 10ml 10% NaOH solution at 80 ℃ of following backflow 2h, washing, drying.Take by weighing pretreated mica titanium 1g, add the 25ml deionized water, 80 ℃ of recirculated water heating reflux, and use the pH value of extremely rare ammoniacal liquor regulator solution to approximate 10, add the Co (NO of 2.0ml 10% with the speed of 1～2/2min
3)
2Solution remains between 9.0～10 with 10% the NaOH solution and the pH value of ammoniacal liquor regulator solution simultaneously.It is constant to keep temperature of reaction, ageing 40min, and washing is filtered, and 120 ℃ of following dry 1h put into retort furnace in 900 ℃ of roasting 60min, and hot discharging naturally cools to room temperature.Obtaining the powder look is the pigment changeable colors along with angle that the golden red color changes from gold-green.
Claims (4)
1. cobalt-titanium series random chromo pigment, it is characterized in that: the preparation process of this pigment comprises: 1) the mica substrate is carried out pre-treatment, the molten mica titanium substrate material that goes part mica substrate to obtain the part hollow structure with acid, alkaline solution successively; Used mica substrate is the coated by titanium dioxide mica substrate of Detitanium-ore-type, becomes rutile-type through the crystal conversion of titanium dioxide after the roasting, and the titanium dioxide massfraction and has interference color between 10～60%; Used acid is phosphoric acid and is selected from the vitriol oil, hydrofluoric acid, the concentrated nitric acid one or both; Used alkaline solution is sodium hydroxide or potassium hydroxide aqueous solution; 2) be 9.0～10.0 in the pH value, 70～80 ℃ of temperature of reaction in the slurries of the described mica titanium substrate material of concentration between 5%～10%, slowly drip 10%～15% Co (NO with the speed of 1～2/2min
3)
2Solution adds sig water and promotes Co
2+Hydrolysis reaction, the Co (OH) that hydrolysis generates
2Be coated on mica titanium substrate material surface equably; 3) make Co (OH) through ageing, washing, drying, roasting
2Be transformed into CoO, finally obtain pigment changeable colors along with angle.
2. cobalt-titanium series random chromo pigment as claimed in claim 1 is characterized in that: described mica substrate is a white mica.
3. cobalt-titanium series random chromo pigment as claimed in claim 1 is characterized in that: described sig water is weak ammonia or diluted sodium hydroxide solution.
4. cobalt-titanium series random chromo pigment as claimed in claim 1 is characterized in that: digestion time 40～60min, use deionized water wash 2～3 times, and at 120 ℃ of dry 1h, 850～1000 ℃ of maturing temperatures, roasting time 40～60min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005101054194A CN100462407C (en) | 2005-09-28 | 2005-09-28 | Production of cobalt-titanium series random chromo pigment |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005101054194A CN100462407C (en) | 2005-09-28 | 2005-09-28 | Production of cobalt-titanium series random chromo pigment |
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| CN1939984A CN1939984A (en) | 2007-04-04 |
| CN100462407C true CN100462407C (en) | 2009-02-18 |
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| CNB2005101054194A Active CN100462407C (en) | 2005-09-28 | 2005-09-28 | Production of cobalt-titanium series random chromo pigment |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN108752977A (en) * | 2018-06-29 | 2018-11-06 | 林中 | There is the pigment and preparation method thereof of high brightness, excitation purity and covering effect simultaneously |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4192691A (en) * | 1978-10-26 | 1980-03-11 | The Mearl Corporation | Metal oxide platelets as nacreous pigments |
| US5137575A (en) * | 1989-06-02 | 1992-08-11 | Tayca Corporation | Chromatic pigments comprising a coloring metal oxide coating on transparent titanium oxide core particles of 0.01 to 0.1 micron size |
| JPH07157688A (en) * | 1993-12-08 | 1995-06-20 | Dainichiseika Color & Chem Mfg Co Ltd | Green nacreous pigment |
| JPH07157689A (en) * | 1993-12-08 | 1995-06-20 | Dainichiseika Color & Chem Mfg Co Ltd | Production of green nacreous pigment |
| US5611851A (en) * | 1995-12-13 | 1997-03-18 | The Mearl Corporation | Process for preparing unsupported metal oxide nacreous pigments |
| JP2000336284A (en) * | 1999-03-23 | 2000-12-05 | Shiseido Co Ltd | Mica coated with titanium-cobalt-aluminum compound oxide and product coated therewith |
| US6290766B1 (en) * | 1999-02-24 | 2001-09-18 | Engelhard Corporation | Lustrous interference pigments with black absorption color |
| CN1563210A (en) * | 2004-04-19 | 2005-01-12 | 付建生 | Pigment changed color as changing angle, and fabricating method |
| CN1597793A (en) * | 2004-08-10 | 2005-03-23 | 汕头市龙华珠光颜料有限公司 | Pigment of multi-gradition discolour at diffierent direction and production process thereof |
-
2005
- 2005-09-28 CN CNB2005101054194A patent/CN100462407C/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4192691A (en) * | 1978-10-26 | 1980-03-11 | The Mearl Corporation | Metal oxide platelets as nacreous pigments |
| US5137575A (en) * | 1989-06-02 | 1992-08-11 | Tayca Corporation | Chromatic pigments comprising a coloring metal oxide coating on transparent titanium oxide core particles of 0.01 to 0.1 micron size |
| JPH07157688A (en) * | 1993-12-08 | 1995-06-20 | Dainichiseika Color & Chem Mfg Co Ltd | Green nacreous pigment |
| JPH07157689A (en) * | 1993-12-08 | 1995-06-20 | Dainichiseika Color & Chem Mfg Co Ltd | Production of green nacreous pigment |
| US5611851A (en) * | 1995-12-13 | 1997-03-18 | The Mearl Corporation | Process for preparing unsupported metal oxide nacreous pigments |
| US6290766B1 (en) * | 1999-02-24 | 2001-09-18 | Engelhard Corporation | Lustrous interference pigments with black absorption color |
| JP2000336284A (en) * | 1999-03-23 | 2000-12-05 | Shiseido Co Ltd | Mica coated with titanium-cobalt-aluminum compound oxide and product coated therewith |
| CN1563210A (en) * | 2004-04-19 | 2005-01-12 | 付建生 | Pigment changed color as changing angle, and fabricating method |
| CN1597793A (en) * | 2004-08-10 | 2005-03-23 | 汕头市龙华珠光颜料有限公司 | Pigment of multi-gradition discolour at diffierent direction and production process thereof |
Non-Patent Citations (4)
| Title |
|---|
| 蓝色云母钛珠光颜料的制备. 张德文，孙淑清.辽宁化工，第3期. 1996 |
| 蓝色云母钛珠光颜料的制备. 张德文，孙淑清.辽宁化工，第3期. 1996 * |
| 表面包覆制备云母系珠光颜料研究现状. 郭萌萌，杜海燕，孙家跃.国外建材科技，第25卷第4期. 2004 |
| 表面包覆制备云母系珠光颜料研究现状. 郭萌萌，杜海燕，孙家跃.国外建材科技，第25卷第4期. 2004 * |
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| CN1939984A (en) | 2007-04-04 |
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Assignee: Jinchen Xikeni Safety Printing Co., Ltd., Beijing Assignor: Beijing Technology and Business University Contract fulfillment period: 2006.5.10 to 2025.5.9 contract change Contract record no.: 2009990001036 Denomination of invention: Production of cobalt-titanium series random chromo pigment Granted publication date: 20090218 License type: Exclusive license Record date: 2009.9.17 |
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| LIC | Patent licence contract for exploitation submitted for record |
Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2006.5.10 TO 2025.5.9; CHANGE OF CONTRACT Name of requester: BEIJING JINCHEN CICCONE SECURITY PRINTING CO., LTD Effective date: 20090917 |