CN100443444C - Chemical preparation method for blue spinel type ceramic coloring material - Google Patents

Abstract

This invention discloses a chemical preparation method for blue spinel ceramic materials, which takes aluminum butoxide as the doped metal start material, ammonia as for adjusting pH value including: preparing equal mol volumes of aluminum butoxide and AlCl mixed solution, then preparing doped inorganic salt to a solution and it's necessary to penetrate nitrogen for protection in the preparation process, when the two solutions are ready, the mixture solution is poured into the inorganic salt solution to be reacted, and the deposit is centrifuged then separated in a dialyzing film to be dried and calcined under 1200deg.C to produce a spinel ceramic blue material.

Description

A kind of chemical preparation process of blue spinel type ceramic coloring material

Technical field

The present invention relates to a kind of chemical preparation process of blue spinel type ceramic coloring material, particularly adopt chemical preparation method to prepare the preparation method of the blue colorant of spinel type pottery of ferrotitanium doped aluminium.

Background technology

The production of ceramic pigment at present mainly is a large amount of the use for the decoration needs that satisfy current ceramic batch and glaze.Require it to have functions such as high mechanical endurance, high compression strength and chemical resistance because pottery uses, in ceramic batch and glaze, have performances such as color development is stable and high temperature resistant at the corresponding ceramic pigment that requires to be developed aspect the exploitation ceramic pigment.Current, ceramic pigment mainly is high-temperature oxide type ceramic pigment, spinel type ceramic coloring material and perovskite type ceramic colorant etc., the preparation technology of these colorants all adopts traditional technology, be about to each coloring oxide and silicate oxide, as aluminum oxide, quartz, zirconium white etc. mix according to certain ratio ball milling together, arrive certain fineness through high-temperature calcination and ball milling then.This traditional technology has following shortcoming: need high calcining temperature in (1) production, and make production cost improve greatly; (2) each oxide compound at high temperature reacts not exclusively, is difficult for allowing painted metal ion mixing in the stable ceramic mineral of high temperature color development; (3) used the muriate of alkali metal containing and alkaline-earth metal in the production, fluorochemical, nitrate, borate and carbonate etc., and these salt things at high temperature decompose the gas that the back produced and can have a strong impact on environment.Other synthetic route, as sol-gel method, all there is the cost height to some extent in methods such as coprecipitation method and impregnation technology, disadvantage such as the low or technology of product turnover ratio is tediously long.

Summary of the invention

The object of the present invention is to provide the chemical preparation process of the preparation blue spinel type ceramic coloring material that a kind of cost is low, technological process simple, easily produce, particularly adopt chemical preparation method to prepare the preparation method of the blue colorant of spinel type pottery of ferrotitanium doped aluminium.

The present invention is with aluminium butoxide (Al (OC ₄H ₉) ₃), aluminum chloride (AlCl ₃) as the reaction raw materials of preparation aluminum oxide, make catalyzer with nitric acid, ferrous sulfate (FeSO ₄) and titanous chloride (TiCl ₃) as the doping metals starting raw material, ammoniacal liquor is used for regulating the pH value in the preparation inorganic salt solution process.Pass through the aluminium butoxide and the aluminum chloride mixture aqueous solution of preparation equimolar amount in the preparation process earlier; Then adulterated inorganic salt are also made the aqueous solution,, in its preparation process, need to feed nitrogen protection in order to prevent the oxidation of ferrous iron and titanous.After two kinds of aqueous solution prepare, aluminium butoxide and aluminum chloride mixture aqueous solution are poured in the inorganic salt solution, mix to send out and answer, after having reacted, the gained throw out is centrifugal, change dialysis membrane then over to and separate drying, 1200 ℃ of temperature lower calcinations 3 hours, promptly make the blue colorant of spinel type pottery of ferrotitanium doped aluminium.

Concrete preparation process may further comprise the steps:

(1) aluminium butoxide and the aluminum chloride of equimolar amount is made into mixture with distilled water the aqueous solution, be heated 65 ℃ and stir after 30 minutes and to add a small amount of nitric acid in above-mentioned solution, and continue to stir 3 hours standby, the add-on of nitric acid is 0.05 of a mixture molar weight;

(2) ferrous sulfate and titanous chloride are dissolved in the distilled water wiring solution-forming, liquor capacity is above-mentioned 50% of the preceding mixture aqueous solution volume of nitric acid, wherein the mol ratio FeSO of not adding ₄: TiCl ₃=4: 1, needing in the preparation process constantly to feed nitrogen and regulate pH with ammoniacal liquor is 8.5;

(3) mixture aqueous solution with step 1 is poured in the aqueous solution of step 2, the reaction of mixing, all the time feeding nitrogen in the reaction process and regulating pH with ammoniacal liquor is 8.5, after having reacted, the gained throw out is centrifugal, change dialysis membrane then over to and separate, dry under 80～100 ℃ of temperature, 1200 ℃ of temperature lower calcinations 3 hours, promptly make the blue colorant of spinel type pottery of ferrotitanium doped aluminium.

Embodiment

Embodiment 1:

(1) aluminium butoxides and the 266.68 gram aluminum chloride with 492.66 grams are made into the aqueous solution that volume is 100 ml mixtures with distilled water, are heated 65 ℃ and stir after 30 minutes and to add 38 gram nitric acid in above-mentioned solution, and continue to stir 3 hours standby;

(2) restrain the aqueous solution that titanous chlorides are made into mixture with 50 ml distilled waters dissolving, 121.52 gram ferrous sulfate and 30.80, needing constantly to feed nitrogen in the preparation process and regulating pH with ammoniacal liquor is 8.5;

(3) mixture aqueous solution with step 1 is poured in the aqueous solution of step 2, the reaction of mixing, all the time feeding nitrogen in the reaction process and regulating pH with ammoniacal liquor is 8.5, after having reacted, the gained throw out is centrifugal, change dialysis membrane then over to and separate, dry under 90 ℃ of temperature, 1200 ℃ of temperature lower calcinations 3 hours, promptly make the blue colorant of spinel type pottery of ferrotitanium doped aluminium.

Embodiment 2:

(1) aluminium butoxides and the 133.34 gram aluminum chloride with 246.33 grams are made into the aqueous solution that volume is 50 ml mixtures with distilled water, are heated 65 ℃ and stir after 30 minutes and to add 19 gram nitric acid in above-mentioned solution, and continue to stir 3 hours standby;

(2) restrain the aqueous solution that titanous chlorides are made into mixture with 25 ml distilled waters dissolving, 121.52 gram ferrous sulfate and 30.80, needing constantly to feed nitrogen in the preparation process and regulating pH with ammoniacal liquor is 8.5;

(3) mixture aqueous solution with step 1 is poured in the aqueous solution of step 2, the reaction of mixing, all the time feeding nitrogen in the reaction process and regulating pH with ammoniacal liquor is 8.5, after having reacted, the gained throw out is centrifugal, change dialysis membrane then over to and separate, dry under 85 ℃ of temperature, 1200 ℃ of temperature lower calcinations 3 hours, promptly make the blue colorant of spinel type pottery of ferrotitanium doped aluminium.

Claims (1)

1. the chemical preparation process of a blue spinel type ceramic coloring material is characterized in that the steps include:

(1) aluminium butoxide and the aluminum chloride of equimolar amount is made into mixture with distilled water the aqueous solution, be heated 65 ℃ and stir after 30 minutes and to add nitric acid in above-mentioned solution, and continue to stir 3 hours standby, the add-on of nitric acid is 0.05 of a mixture molar weight;

(2) ferrous sulfate and titanous chloride are dissolved in the distilled water wiring solution-forming, liquor capacity is above-mentioned 50% of the preceding mixture aqueous solution volume of nitric acid, wherein the mol ratio FeSO of not adding ₄: TiCl ₃=4: 1, needing in the preparation process constantly to feed nitrogen and regulate pH with ammoniacal liquor is 8.5;

(3) mixture aqueous solution with step 1 is poured in the aqueous solution of step 2, the reaction of mixing, all the time feeding nitrogen in the reaction process and regulating pH with ammoniacal liquor is 8.5, after having reacted, the gained throw out is centrifugal, change dialysis membrane then over to and separate, dry under 80～100 ℃ of temperature, 1200 ℃ of temperature lower calcinations 3 hours, promptly make the blue colorant of spinel type pottery of ferrotitanium doped aluminium.