CN101050316A - Method for preparing manganese doped corundum type pink coloring material - Google Patents

Method for preparing manganese doped corundum type pink coloring material Download PDF

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Publication number
CN101050316A
CN101050316A CN 200710106267 CN200710106267A CN101050316A CN 101050316 A CN101050316 A CN 101050316A CN 200710106267 CN200710106267 CN 200710106267 CN 200710106267 A CN200710106267 A CN 200710106267A CN 101050316 A CN101050316 A CN 101050316A
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manganese
coloring material
spray gun
nitrate
type pink
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CN100469842C (en
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王海
张春霞
田广
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Foshan Dowstong Technology Co ltd
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Guilin University of Technology
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Abstract

This invention discloses a method for preparing manganese-doped corundum-type pink pigment. The method utilizes aluminum nitrate, aluminum hydroxide, manganese nitrate and manganese carbonate as the raw materials, and adopts spray-pyrolysis combined with calcination to obtain manganese-doped corundum-type pink pigment with certain particle sizes and uniform morphologies. The method has such advantages as low cost and simple process. The obtained manganese-doped corundum-type pink pigment has such advantages as uniform particle sizes, controllable components and high purity.

Description

A kind of preparation method of manganese doped corundum type pink coloring material
Technical field
The present invention relates to a kind of preparation method of manganese doped corundum type pink coloring material.
Background technology
At present, the preparation technology of the industrial manganese doping Alpha-alumina corundum crystal formation pink coloring material of producing all is that the oxyhydroxide, oxide compound or the carbonate that adopt traditional processing technology to be about to manganese and aluminium carry out high-temperature calcination according to certain proportioning, will calcine the colorant of the getting well granularity by ball milling to 1～10 micron at last and promptly make needed manganese doping Alpha-alumina corundum crystal formation pink coloring material.This traditional technology has following shortcoming: be to need high calcining temperature on producing on the one hand, the metal-salt of each oxide compound, carbonate or oxyhydroxide at high temperature reacts incomplete on the other hand; In addition in order to reduce calcining temperature and to make the fully reaction at high temperature of each oxide compound, traditional processing technology has used the muriate of alkali metal containing and alkaline-earth metal, fluorochemical, nitrate, borate and carbonate, and the gas that these salt compounds are produced after at high temperature decomposing can have a strong impact on environment.
Summary of the invention
The object of the present invention is to provide the method for preparing manganese doping Alpha-alumina corundum type pink coloring material that a kind of cost is low, technological process simple, easily produce, promptly prepare manganese doping Alpha-alumina corundum type pink coloring material in conjunction with calcining process with the spraying thermolysis.
The present invention aluminum nitrate (Al (NO 3) 3.9H 2O), aluminium hydroxide (Al (OH) 3), manganous nitrate (Mn (NO 3) 2.4H 2O) and manganous carbonate (MnCO 3) four kinds of raw materials prepare burden ratio requirement: x (Al (NO 3) 3.9H 2O)+y (Al (OH) 3): z (Mn (NO 3) 2.4H 2O)+w (MnCO 3)=0.15～0.20, x wherein, y, z, w are mole number.It is to mix in 30: 70 the ethanol and the aqueous solution that raw material after preparing is together joined volume ratio, by spray gun mixed solution is atomized into drop then and in the continuous calcining stove, carries out drying and thermolysis, afterbody at continuous oven filters the glassiness strainer of powder by 16～25 micron pore size sizes by vacuumizing simultaneously, then will collecting good powder, to put into temperature be that 900～1100 ℃ calcining furnace is calcined, and cool to room temperature promptly makes manganese doping Alpha-alumina corundum type pink coloring material.
Too high and influence safety and product is collected at the stove internal gas pressure in the preparation process in order to prevent gas that spraying drying and thermolysis produce, also need vacuumize and place the glassiness strainer of one 16～25 micron pore size size at the afterbody of continuous calcining stove.
Concrete steps are as follows:
(1) with desired raw material in molar ratio the proportional meter of Mn: Al=0.15～0.20 calculate the mass ratio of used each raw material, allocating it into volume ratio is in 30: 70 the solution of second alcohol and water;
(2) mixing solutions for preparing is put into the container that is connected with the spray gun liquid-inlet pipe, and carry out violent stirring, at the inlet mouth access 0.3～0.8kg/cm of spray gun 2The pressurized air of pressure;
(3) leading portion at continuous oven is warmed up to 200 ℃, and back segment is warmed up to 550 ℃ and keep the constant of two sections temperature of continuous oven;
(4) opening spray gun sprays mixing solutions to and carries out drying and atomizing decomposition in the stove;
(5) powder that the continuous oven afterbody is collected was calcined 3～4 hours in 900～1100 ℃ of High Temperature Furnaces Heating Apparatuss, cooled to room temperature by the speed of 5～10 ℃ of per minutes and promptly obtained the needed manganese doping Alpha-alumina corundum type pink coloring material that has.
Cost of the present invention is low, process control procedure is simple, easily produce, and what make has a manganese doping Alpha-alumina corundum type pink coloring material, this colorant powder diameter evenly, controllable component, purity height.
Embodiment
Embodiment 1:
(1) takes by weighing 375 gram aluminum nitrate (Al (NO respectively 3) 3.9H 2O), 78 gram aluminium hydroxide (Al (OH) 3), 37.65 gram manganous nitrate (Mn (NO 3) 2.4H 2O) and 17.25 gram manganous carbonate (MnCO 3) four kinds of raw materials, and to allocate volume ratio into be in 30: 70 the solution of 200 milliliters of second alcohol and waters;
(2) mixing solutions for preparing is put into the container that is connected with the spray gun liquid-inlet pipe, and carry out violent stirring, at the inlet mouth access 0.4kg/cm of spray gun 2The pressurized air of pressure;
(3) leading portion at continuous oven is warmed up to 200 ℃, and back segment is warmed up to 550 ℃ and keep the constant of two sections temperature of continuous oven;
(4) opening spray gun sprays mixing solutions to and carries out drying and atomizing decomposition in the stove;
(5) powder that the continuous oven afterbody is collected was calcined 3 hours in 900 High Temperature Furnaces Heating Apparatuss, cooled to room temperature by the speed of 5 ℃ of per minutes and promptly obtained the needed manganese doping Alpha-alumina corundum type pink coloring material that has.
Embodiment 2:
(1) takes by weighing 375 gram aluminum nitrate (Al (NO respectively 3) 3.9H 2O), 78 gram aluminium hydroxide (Al (OH) 3), 50.2 gram manganous nitrate (Mn (NO 3) 2.4H 2O) and 23 gram manganous carbonate (MnCO 3) four kinds of raw materials, and to allocate volume ratio into be in 30: 70 the solution of 200 milliliters of second alcohol and waters;
(2) mixing solutions for preparing is put into the container that is connected with the spray gun liquid-inlet pipe, and carry out violent stirring, at the inlet mouth access 0.5kg/cm of spray gun 2The pressurized air of pressure;
(3) leading portion at continuous oven is warmed up to 200 ℃, and back segment is warmed up to 550 ℃ and keep the constant of two sections temperature of continuous oven;
(4) opening spray gun sprays mixing solutions to and carries out drying and atomizing decomposition in the stove;
(5) powder that the continuous oven afterbody is collected was calcined 3 hours in 1100 ℃ of High Temperature Furnaces Heating Apparatuss, cooled to room temperature by the speed of 10 ℃ of per minutes and promptly obtained the needed manganese doping Alpha-alumina corundum crystal formation pink coloring material that has.

Claims (2)

1. the preparation method of a manganese doped corundum type pink coloring material is characterized in that the steps include:
(1) with required aluminum nitrate, aluminium hydroxide, manganous nitrate and four kinds of raw materials of manganous carbonate in molar ratio the proportional meter of Mn: Al=0.15～0.20 calculate the quality of used each raw material, allocating it into volume ratio is in 30: 70 the solution of second alcohol and water;
(2) mixing solutions for preparing is put into the container that is connected with the spray gun liquid-inlet pipe, and carry out violent stirring, at the inlet mouth access 0.3～0.8kg/cm of spray gun 2The pressurized air of pressure;
(3) leading portion at continuous oven is warmed up to 200 ℃, and back segment is warmed up to 550 ℃ and keep the constant of two sections temperature of continuous oven;
(4) opening spray gun sprays mixing solutions to and carries out drying and atomizing decomposition in the stove;
(5) powder that the continuous oven afterbody is collected was calcined 3～4 hours in 900～1100 ℃ of High Temperature Furnaces Heating Apparatuss, cooled to room temperature by the speed of 5～10 ℃ of per minutes and promptly obtained the needed manganese doping Alpha-alumina corundum type pink coloring material that has.
2. preparation method as claimed in claim 1, the molecular formula that it is characterized in that described aluminum nitrate, aluminium hydroxide, manganous nitrate and manganous carbonate is Al (NO 3) 3.9H 2O, Al (OH), Mn (NO 3) 2.4H 2O and MnCO 3
CNB2007101062679A 2007-05-14 2007-05-14 Method for preparing manganese doped corundum type pink coloring material Active CN100469842C (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105586005A (en) * 2016-01-14 2016-05-18 洛阳三睿宝纳米科技有限公司 Nano corundum abrasive and preparation method thereof
CN105778566A (en) * 2016-02-29 2016-07-20 三祥新材股份有限公司 Method for preparing pigment with manganese carbonate

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH08505175A (en) * 1992-12-23 1996-06-04 ミネソタ・マイニング・アンド・マニュファクチュアリング・カンパニー Abrasive grains containing manganese oxide
CN1093072A (en) * 1993-04-01 1994-10-05 山东省硅酸盐研究设计院 Corundum ceramic material and method for making thereof and purposes
CN100572281C (en) * 2005-11-28 2009-12-23 中国铝业股份有限公司 A kind of preparation method of red alumina powder

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105586005A (en) * 2016-01-14 2016-05-18 洛阳三睿宝纳米科技有限公司 Nano corundum abrasive and preparation method thereof
CN105586005B (en) * 2016-01-14 2018-02-23 洛阳三睿宝纳米科技有限公司 A kind of preparation method of Nano Alumina Abrasive
CN105778566A (en) * 2016-02-29 2016-07-20 三祥新材股份有限公司 Method for preparing pigment with manganese carbonate
CN108864762A (en) * 2016-02-29 2018-11-23 三祥新材股份有限公司 A kind of method for preparing colorant using manganese carbonate for keeping coloring force of color strong
CN108864761A (en) * 2016-02-29 2018-11-23 三祥新材股份有限公司 It is a kind of to make the bright-coloured method for preparing colorant using manganese carbonate of colorant tone
CN108864762B (en) * 2016-02-29 2020-06-02 三祥新材股份有限公司 Method for preparing pigment by using manganese carbonate and capable of enabling pigment to have strong coloring power
CN108864761B (en) * 2016-02-29 2020-09-01 三祥新材股份有限公司 Method for preparing pigment by using manganese carbonate and capable of enabling pigment to be bright in color tone

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