CN101983929A - Preparation method of low-valence titanium oxide powder - Google Patents
Preparation method of low-valence titanium oxide powder Download PDFInfo
- Publication number
- CN101983929A CN101983929A CN 201010562520 CN201010562520A CN101983929A CN 101983929 A CN101983929 A CN 101983929A CN 201010562520 CN201010562520 CN 201010562520 CN 201010562520 A CN201010562520 A CN 201010562520A CN 101983929 A CN101983929 A CN 101983929A
- Authority
- CN
- China
- Prior art keywords
- titanium oxide
- oxide powder
- low
- preparation
- titanium dioxide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Cosmetics (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention provides a preparation method of low-valence titanium oxide powder, which comprises the following steps: (1) uniformly mixing titanium dioxide powder, sodium borohydride and potassium borohydride, and then compacting and flattening the mixed materials in a drying corundum crucible; (2) heating the system prepared in step (1) in a muffle furnace, maintaining the temperature, and then cooling in the furnace; and (3) taking out deep-color powder at the lower layer of the crucible after cooling, thoroughly cleaning with distilled water, filtering, and drying the filter cake to obtain the low-valence titanium oxide powder. The low-valence titanium oxide powder prepared by the method maintains the particle diameters of titanium dioxide raw materials, and the color can be changed with the formula. The low-valence titanium oxide powder can be used as a deep-color pigment in the fields of coating, resin, paint, cosmetics and the like. Compared with the traditional low-valence titanium oxide preparation method, the invention has the advantages of low temperature, simple equipment, easy control, stable product quality, low energy consumption and easy popularization and application.
Description
Technical field
The present invention relates to a kind of preparation method of low price titanium oxide powder, belong to field of new material preparation.
Background technology
(have another name called titanium dioxide, molecular formula is TiO to titanium dioxide in recent years
2) be the popular research object of material and some other subjects always, the product of relevant titanium dioxide is applied to a lot of fields.Titanium oxide also is a titanyl compound at a low price, but because oxygen level is lacked than titanium dioxide in the low price titanium oxide, so its molecular formula is often write Ti
nO
2n-1(1≤n≤20), its character are also bigger with the titanium dioxide difference, especially aspect color, and titanium dioxide whitening look or faint yellow, and titanium oxide shows dark at a low price, even aterrimus.Titanium oxide is because its special nature has wider Application Areas at a low price.At first, titanium oxide product can compare favourably with conventional black pigment carbon black and Z 250 at a low price, even also has advantage in some aspects.Powder was easy to swim in the air when conventional black pigment carbon black used, and made troubles to use, brought certain harm also for simultaneously user's health.The compatibility of carbon black and resin is poor in addition, and the unequal shortcoming of dispersion is arranged.Z 250 also can be used as black pigment, but because it has magnetic, thermostability is also relatively poor simultaneously, also has been subjected to bigger restriction so it is used.And at a low price titanium oxide has characteristics such as nontoxic, good dispersity, thermostability height, thus at some to the black pigment performance requriements than higher field, titanium oxide more can satisfy its performance requirement as black pigment than carbon black, Z 250 at a low price.Secondly, the characteristic of, good dispersity nontoxic according to the low price titanium oxide product can be used in the cosmetic industry aspect to the low price titanium oxide, such as staining agent as hair, and the staining agent of eyelashes and eyebrow etc.Once more, titanium oxide has conductivity and antistatic effect preferably at a low price, and in electro-conductive material, antistatic material field, titanium oxide also will have application promise in clinical practice at a low price.
Preparation at present titanium oxide at a low price mainly contains methods such as ammonia reduction method, hydrogen reduction method, metallic titanium powder reduction method, methylamine reduction method, wherein the ammonia reduction method is to arrive titanium oxide at a low price at the reduction of the temperature more than 780 ℃ titanium dioxide under the ammonia atmosphere, reduction rate is slower, and ammonia is corrodibility, irritant gas, and is big to environmental hazard; Hydrogen reduction method is in 1100 ℃ high temperature titanium dioxide to be titanium oxide at a low price under nitrogen atmosphere, and reduction rate is slower, owing to use hydrogen, and to the equipment requirements height, and danger coefficient height during preparation; The metallic titanium powder reduction method is under nitrogen or argon shield atmosphere to be titanium oxide at a low price with titanium dioxide with metallic titanium powder, and cost is higher, and reduction rate is slower, and yet needs logical protective atmosphere, makes the equipment complexity; The methylamine reduction method is under 700 ℃～1000 ℃ temperature titanium dioxide to be the low price titanium oxide in methylamine atmosphere, and the methylamine reduction method is faster slightly than the ammonia reduction, but methylamine itself is a toxic gas, and is bigger to people's harm, and easy contaminate environment.In a word, more than these prepare at a low price that methods of titanium oxide have more restriction, all higher as temperature of reaction; all need use protective atmosphere, equipment and security are all had relatively high expectations, energy consumption is also high; and protective atmospheres such as hydrogen, ammonia, methylamine are also dangerous, easily harmful to human and environment etc.
Summary of the invention
It is reductive agent that the present invention adopts solid-state sodium borohydride and POTASSIUM BOROHYDRIDE, and the atmosphere that do not need protection is no more than in temperature of reaction under 600 ℃ the condition, titanium dioxide powder can be reduced into titanium oxide powder at a low price.This method uses equipment simple, and cost is lower, and low price titanium oxide powder good uniformity, the color and luster of prepared in reaction are good, and physicochemical property is outstanding.
The preparation method of low price titanium dioxide powder of the present invention comprises the following steps:
(1), then mixture is placed dry corundum crucible compacting, pressing with titanium dioxide powder, sodium borohydride and POTASSIUM BOROHYDRIDE uniform mixing;
(2) system of step (1) preparation is put into retort furnace and heat, under a certain temperature, be incubated for some time, then furnace cooling;
(3) take out the dark powder of the lower floor of cooling off in the crucible of back, also filter, filter cake 40 ℃～80 ℃ oven dry down, can be obtained titanium dioxide powder at a low price with the distilled water thorough washing is clean.
The size of described titanium dioxide powder both can be micron-sized, also can be nano level, and its crystalline structure both can be a rutile-type structure, also can be the duplex grain structure of anatase structures or rutile-type and anatase titanium dioxide.
The proportioning of described titanium dioxide powder, sodium borohydride and POTASSIUM BOROHYDRIDE (mass ratio) is: titanium dioxide: sodium borohydride: POTASSIUM BOROHYDRIDE=1: (0.375～1.5): (0.375～1.5).
Described holding temperature is 450 ℃～600 ℃, and soaking time is 15min～60min, and wherein optimum temps is: 520 ℃～580 ℃.
The color of the low price titanium oxide powder that the present invention is prepared presents different colours such as blueness, brown, brownish black, black, aterrimus along with the difference of the ratio between titanium dioxide, sodium borohydride and the POTASSIUM BOROHYDRIDE.The particle diameter of powder determines that by the titanium dioxide raw material raw material is a Nano titanium dioxide, and the low price titanium dioxide powder of then preparing is a nano level, and raw material is a micron order titanium dioxide, and the low price titanium dioxide powder of then preparing also is micron order.
Positively effect of the present invention is: prepared low price titanium oxide powder grain diameter keeps the raw-material particle diameter of titanium dioxide, color and luster is good, and color can change with the difference of prescription, the black low price titanium oxide powder of particularly preparing can be used as the substitute of black pigments such as carbon black and iron oxide black.In addition, temperature of reaction required for the present invention compare the traditional preparation process method low, equipment is simple, handy, the product favorable reproducibility, energy consumption is low, is easy to apply.
Embodiment
Embodiment 1
Take by weighing 2g nanometre-grade titanic-schorl type titanium dioxide powder, 1.5g sodium borohydride and the even mixing of 1.5g POTASSIUM BOROHYDRIDE, subsequently mixture is transferred to dry corundum and does compacting in the pot, pressing.Then crucible is put into retort furnace and heats, 500 ℃ the insulation 1 hour after furnace cooling.Lower floor's aterrimus powder in the cooled crucible is taken out the back clean suction filtration repeatedly with distilled water, filter cake can obtain uniform black nano level titanium oxide powder at a low price 50 ℃ of following oven dry.
Embodiment 2
Take by weighing 2g submicron order rutile titanium dioxide powder, 1g sodium borohydride and the even mixing of 1.5g POTASSIUM BOROHYDRIDE, subsequently mixture is transferred to dry corundum and does compacting in the pot, pressing.Then crucible is put into retort furnace and heats, 550 ℃ the insulation 20 minutes after furnace cooling.Lower black powder in the cooled crucible is taken out the back clean suction filtration repeatedly with distilled water, filter cake can obtain the submicron order low price titanium oxide powder of uniform black 60 ℃ of following oven dry.
Embodiment 3
Take by weighing 2g submicron order anatase titanium dioxide powder, 0.75g sodium borohydride and the even mixing of 1.5g POTASSIUM BOROHYDRIDE, subsequently mixture is transferred to dry corundum and does compacting in the pot, pressing.Then crucible is put into retort furnace and heats, 550 ℃ the insulation half an hour after furnace cooling.Lower floor's brownish black powder taking-up in the cooled crucible is cleaned suction filtration repeatedly with distilled water, and filter cake can obtain the submicron order low price titanium oxide powder of uniform brownish black 50 ℃ of following oven dry.
Claims (4)
1. the preparation method of a low price titanium oxide powder comprises the following steps:
(1), then mixture is placed dry corundum crucible compacting, pressing with titanium dioxide powder, sodium borohydride and POTASSIUM BOROHYDRIDE uniform mixing;
(2) system of step (1) preparation is put into retort furnace and heat, under a certain temperature, be incubated for some time, then furnace cooling;
(3) take out the dark powder of the lower floor of cooling off in the crucible of back, also filter, filter cake 40 ℃～80 ℃ oven dry down, can be obtained titanium oxide powder at a low price with the distilled water thorough washing is clean.
2. the preparation method of a kind of low price titanium oxide powder according to claim 1, it is characterized in that: the size of described titanium dioxide powder both can be micron-sized, also can be nano level, its crystalline structure both can be a rutile-type structure, also can be the duplex grain structure of anatase structures or rutile-type and anatase titanium dioxide.
3. the preparation method of a kind of low price titanium oxide powder according to claim 1 is characterized in that: the proportioning of titanium dioxide powder, sodium borohydride and POTASSIUM BOROHYDRIDE (mass ratio) is: titanium dioxide: sodium borohydride: POTASSIUM BOROHYDRIDE=1: (0.375～1.5): (0.375～1.5).
4. the preparation method of a kind of low price titanium oxide powder according to claim 1 is characterized in that: described holding temperature is 450 ℃～600 ℃, and soaking time is 15min～60min, and wherein optimum temperature range is: 520 ℃～580 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105625203A CN101983929B (en) | 2010-11-29 | 2010-11-29 | Preparation method of low-valence titanium oxide powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105625203A CN101983929B (en) | 2010-11-29 | 2010-11-29 | Preparation method of low-valence titanium oxide powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101983929A true CN101983929A (en) | 2011-03-09 |
| CN101983929B CN101983929B (en) | 2012-04-25 |
Family
ID=43641098
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010105625203A Expired - Fee Related CN101983929B (en) | 2010-11-29 | 2010-11-29 | Preparation method of low-valence titanium oxide powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101983929B (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104016411A (en) * | 2014-05-14 | 2014-09-03 | 周振平 | Convenient and simple method for increasing high-temperature reaction preparation efficiency of complex inorganic color pigment (CICP) |
| CN106467316A (en) * | 2016-10-13 | 2017-03-01 | 哈尔滨工业大学 | A kind of method of the oxide with sodium borohydride for raw material preparation hydrogenation |
| CN109772380A (en) * | 2019-02-25 | 2019-05-21 | 江苏大学 | Hydrogenate titanium dioxide complex three-dimensional bouquet chlorine oxygen bismuth photochemical catalyst and preparation method |
| CN110790305A (en) * | 2019-11-27 | 2020-02-14 | 湖南科莱新材料有限公司 | Preparation method of black titanium dioxide powder |
| CN111573721A (en) * | 2020-05-21 | 2020-08-25 | 攀枝花学院 | Preparation method of black titanium dioxide |
| CN114349037A (en) * | 2022-01-02 | 2022-04-15 | 广西师范大学 | Preparation method and application of black calcium carbonate |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4668501A (en) * | 1981-11-27 | 1987-05-26 | Mitsubishi Kinzoku Kabushiki Kaisha | Process for preparing a titanium oxide powder |
| CN1169956A (en) * | 1996-07-08 | 1998-01-14 | 同济大学 | Manufacture of black titanium oxide |
| US5711798A (en) * | 1994-10-11 | 1998-01-27 | Shiseido Co., Ltd. | Pigment containing low-order titanium oxide and method of manufacturing the same |
-
2010
- 2010-11-29 CN CN2010105625203A patent/CN101983929B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4668501A (en) * | 1981-11-27 | 1987-05-26 | Mitsubishi Kinzoku Kabushiki Kaisha | Process for preparing a titanium oxide powder |
| US5711798A (en) * | 1994-10-11 | 1998-01-27 | Shiseido Co., Ltd. | Pigment containing low-order titanium oxide and method of manufacturing the same |
| CN1169956A (en) * | 1996-07-08 | 1998-01-14 | 同济大学 | Manufacture of black titanium oxide |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104016411A (en) * | 2014-05-14 | 2014-09-03 | 周振平 | Convenient and simple method for increasing high-temperature reaction preparation efficiency of complex inorganic color pigment (CICP) |
| CN106467316A (en) * | 2016-10-13 | 2017-03-01 | 哈尔滨工业大学 | A kind of method of the oxide with sodium borohydride for raw material preparation hydrogenation |
| CN109772380A (en) * | 2019-02-25 | 2019-05-21 | 江苏大学 | Hydrogenate titanium dioxide complex three-dimensional bouquet chlorine oxygen bismuth photochemical catalyst and preparation method |
| CN109772380B (en) * | 2019-02-25 | 2022-07-05 | 江苏大学 | Hydrogenated titanium dioxide composite three-dimensional flower ball bismuth oxychloride photocatalyst and preparation method thereof |
| CN110790305A (en) * | 2019-11-27 | 2020-02-14 | 湖南科莱新材料有限公司 | Preparation method of black titanium dioxide powder |
| CN111573721A (en) * | 2020-05-21 | 2020-08-25 | 攀枝花学院 | Preparation method of black titanium dioxide |
| CN111573721B (en) * | 2020-05-21 | 2022-10-18 | 攀枝花学院 | Preparation method of black titanium dioxide |
| CN114349037A (en) * | 2022-01-02 | 2022-04-15 | 广西师范大学 | Preparation method and application of black calcium carbonate |
| CN114349037B (en) * | 2022-01-02 | 2023-09-15 | 广西师范大学 | Preparation method and application of black calcium carbonate |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101983929B (en) | 2012-04-25 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101983929B (en) | Preparation method of low-valence titanium oxide powder | |
| JP6124496B2 (en) | Multicolored glossy pearlescent pigment | |
| CN100548888C (en) | Titanium particles that character is useful and manufacture method thereof | |
| JP2728294B2 (en) | Particularly, a method for producing a bluish pearlescent pigment | |
| CN1826388B (en) | Carbon coated high luster materials | |
| US7850775B2 (en) | Multi-colored lustrous pearlescent pigments | |
| EP2688961B1 (en) | High-gloss silver-colored pigments having high covering power and a metal appearance, method for the production thereof and use of the same | |
| WO2007040206A1 (en) | Pearlescent pigment, process for producing the same, coating material composition and coating film composition | |
| Tawiah et al. | Polymer-encapsulated colorful Al pigments with high NIR and UV reflectance and their application in textiles | |
| EP1986595A1 (en) | Cosmetic comprising coloured effect pigments and method of producing it | |
| EP2599838A1 (en) | Color metallic pigment, method for producing same, and coating composition and cosmetic containing same | |
| JPH0351645B2 (en) | ||
| CN107163294A (en) | A kind of far infrared composite powder | |
| WO2014019639A1 (en) | Effect pigments | |
| CN105254337A (en) | Method for preparing high-color-developing zirconium-silicate-coated carbon black pigment by taking plant fiber as carbon source | |
| CN106189519A (en) | One can photochromic water-based ultraviolet (UV) curable ceramic ink jet ink and preparation method thereof | |
| CN100482753C (en) | Composite resin type electromagnetic wave shielding coating and its preparation method | |
| JPH09255533A (en) | Flaky metal oxide and cosmetic mixed with the same | |
| CN106349814A (en) | Antibacterial and antistatic water- borne UV light curing ceramic ink jet ink and preparing method thereof | |
| CN109535771A (en) | Cobalt blue palygorskite nano composite pigment, preparation method and application | |
| JPH04144918A (en) | Production of titanium dioxide flake | |
| JP2697611B2 (en) | Flake glass, method for producing the same, and cosmetics incorporating the same | |
| JPH06116510A (en) | Production of iridescent luster pigment | |
| JPH08239310A (en) | Flaky powder, its production, and cosmetic formulated therewith | |
| CN104559329A (en) | Multi-Colored Lustrous Pearlescent Pigments |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20120425 Termination date: 20141129 |
|
| EXPY | Termination of patent right or utility model |