CN100584755C - With kaolin is the method for feedstock production superfine white carbon black and nano aluminium oxide - Google Patents
With kaolin is the method for feedstock production superfine white carbon black and nano aluminium oxide Download PDFInfo
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- CN100584755C CN100584755C CN200810023208A CN200810023208A CN100584755C CN 100584755 C CN100584755 C CN 100584755C CN 200810023208 A CN200810023208 A CN 200810023208A CN 200810023208 A CN200810023208 A CN 200810023208A CN 100584755 C CN100584755 C CN 100584755C
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Abstract
A kind of is the method for feedstock production superfine white carbon black and nano aluminium oxide with kaolin.In the method, kaolin passes through the filter cake that calcining, lixiviate and filtration obtain containing the filtrate of silicon-dioxide and contain aluminum chloride.Obtain the nano alumina powder jointed and superfine white carbon black powder of the finished product by removal of impurities and aftertreatment at last to filtrate and filter cake.The present invention can make superfine white carbon black and nano aluminium oxide simultaneously, thereby has reached kaolinic integrated use, and two kinds of product indexs that make are good, the added value of product height.
Description
Technical field
The present invention relates to a kind of is the method for feedstock production superfine white carbon black and nano aluminium oxide with kaolin, belongs to preparation, purification and the crystal formation control techniques field of inorganic materials.
Background technology
Kaolin is a kind of important nonmetal mineral resource, with mica, quartz, lime carbonate and be called four big nonmetalliferous ores.Mainly by forming less than the kandite (kaolinite, dickite, nacrite, halloysite etc.) of crystal formations such as the small sheet of 2 microns, tubulose, lamination shape, the ideal chemical formula is Al to kaolin
2O
3-2SiO
2-2H
2O, its chemical constitution is mainly by a large amount of Al
2O
3, SiO
2With a spot of Fe
2O
3, TiO
2And the K of trace
2O, Na
2Compositions such as O, CaO and MgO contain SiO in the pure kaolin
2Be 46.51%, Al
2O
3Be 39.53%.
All the time, both at home and abroad majority is direct use to raw ore on the Application and Development of kaolin resource, or kaolin is carried out simple impurity elimination purification, and the added value of kaolin product is not improved significantly.Along with to kaolinic overexploitation and use, certain crisis has appearred in supply of raw material.Outstanding problem such as not enough in view of the kaolin product functionalization exploitation degree of depth, that added value is low is employed new technology, novel process, new installation are produced high quality, high-grade deep processed product becomes the inexorable trend of kaolin industry development.
The product that silicon oxide, aluminum oxide in the kaolin is separated preparation silicon or aluminium begins just to have research from the eighties of last century the eighties, and wherein some index is better.Human microwave catalysis such as Zhao Jianyu extract active carbon white from the kaolin of the southern regions of the Yunnan Province, product purity reaches more than 95%, and whiteness is 93.88%.People such as Liu Xinmei carry out the research that Coaseries kaolin is produced white carbon black, and the specific surface area of gained white carbon black is 529.6m2/g, and purity is 96.2%.But these work only limit to the single extraction to silicon in the kaolin or aluminium, fail to reach the comprehensive utilization to resource.Some reports with two kinds of products of silicon, aluminium comprehensive utilization preparation are also arranged, as being feedstock production Tai-Ace S 150, white carbon black with kaolin, perhaps aluminum chloride, two kinds of products of white carbon black.Granted publication number discloses a kind of preparation method's patent of invention of polyaluminium chloride water purification agent for the Chinese invention patent of CN1275874C, this invention is at first carried out drying treatment to the kaolin raw ore, carry out calcination processing then, 650 ℃～700 ℃ of calcining temperatures, add water again and be made into slurries, through series reaction and separating treatment, obtain water purification agent aluminum chloride and white carbon black at last.This method is with the SiO that contains in the kaolin
2And Al
2O
3Carried out comprehensive utilization, but thereby not high its range of application that has influence on of the purity of the polyaluminium chloride water purification agent of gained and white carbon black.
Summary of the invention
It is the method for feedstock production superfine white carbon black and nano aluminium oxide with kaolin that the object of the invention provides a kind of, solves the prior art problem not high to kaolinic comprehensive utilization ratio.
For achieving the above object, the technical solution used in the present invention is: a kind of is the method for feedstock production superfine white carbon black and nano aluminium oxide with kaolin, is made up of successively following process steps:
(1) calcining
Kaolin calcined under 600 ℃～630 ℃ conditions make the kaolinite dehydration that contains in the kaolin generate metakaolinite, its reaction formula is: Al
2O
32SiO
22H
2O → Al
2O
3SiO
2+ H
2O;
(2) lixiviate
Kaolin after the calcining is joined in 90 ℃～98 ℃ the hydrochloric acid soln, the Sodium hexametaphosphate 99 that adds kaolin quality 0.8%～1.1% then, and it is stirred, chemical ingredients aluminum oxide and hydrochloric acid that metakaolinite is contained fully react the generation aluminum chloride, and its reaction formula is: Al
2O
3+ 6HCl=2AlCl
3+ 3H
2O, silicon-dioxide is stripping from metakaolinite; Wherein, the mass percent concentration of hydrochloric acid soln is 18～23%, and aluminum oxide is 1: 6.8～7.2 with the ratio of the mole number of hydrochloric acid;
(3) filter
Vat liquor after the lixiviate is filtered, obtain to contain the filter cake of silicon-dioxide; Contain aluminum chloride, anionic impurity metasilicic acid radical ion, silicic acid sol, the filtrate of cation impurity potassium ion, sodium ion, calcium ion, magnesium ion, iron ion and titanium ion;
(4) aftertreatment
Aftertreatment is made of processing two portions of filtrate that step (3) is obtained and filter cake:
The concrete steps that filtrate is handled are:
A, in filtrate, add the barium chloride solution of 0.8～1.2mol/l, and to its stirring barium ion and silicic acid sol and sulfate ion are fully reacted to generate barium silicate, barium sulfate precipitate, the back to its filter clear filtrate, wherein the volume ratio of filtrate and barium chloride solution is 1: 3.5～4.5;
B, add sodium hydroxide solution in the filtrate that the A step obtains, be heated to 75～85 ℃ then, make aluminum chloride and sodium hydroxide fully react the generation sodium metaaluminate under the condensing reflux condition, its reaction formula is: AlCl
3+ 4NaOH=NaAlO
2+ 3NaCl+2H
2O gets sodium metaaluminate filtrate after the filtration;
C, the sodium metaaluminate filtrate that the B step is obtained are heated to 50～60 ℃ of formation colloidal solution, and evenly dripping hydrochloric acid makes sodium metaaluminate and hydrochloric acid fully react the generation aluminum chloride, dropwise splashes into ammonium hydrogencarbonate then to generating aluminium carbonate ammonia gel fully; With deionized water aluminium carbonate ammonia gel is carried out at least the once washing operation to remove foreign ion, said washing operation is: aluminium carbonate ammonia gel is added the filter cake that the even after-filtration of deionized water and stirring obtains to contain aluminium carbonate ammonia gel;
D, the aluminium carbonate ammonia gel filter cake after will washing are with ethanol or acetone dehydration, and the dehydration back gets xerogel in 105 ℃～115 ℃ vacuum-dryings;
E, calcine nano alumina powder jointedly in 1100 ℃～1200 ℃ xerogel;
Processing concrete steps to the filter cake that contains silicon-dioxide are:
A, the filter cake that contains silicon-dioxide is carried out at least the once washing operation to remove foreign ion, described washing operation is: the filter cake that will contain silicon-dioxide and the water after-filtration acquisition silica filter cake that stirs;
B, the silica filter cake that a step is obtained is mixed with sodium hydroxide solution makes silicon-dioxide fully be converted into water glass, and its reaction formula is: 2NaOH+SiO
2=Na
2SiO
3+ H
2O adds hydrochloric acid then and makes water glass fully be converted into silicic acid gel in this solution, its reaction formula is: Na
2SiO
3+ 2HCl=H
2SiO
3↓+2NaCl;
C, silicic acid gel is carried out at least the once washing operation to remove impurity, described washing operation is: with silicic acid gel and the water after-filtration acquisition silicic acid gel filter cake that stirs;
D, with the silicic acid gel filter cake at 105 ℃～115 ℃ dryings, porphyrize then;
Silicic acid gel behind e, the porphyrize obtains the superfine white carbon black powder at 550 ℃～600 ℃ calcined dehydrations.
Related content in the technique scheme is explained as follows:
1, in the such scheme, calcining (calcination) is meant in suitable atmosphere and is lower than the hot-work of carrying out under the temperature condition of kaolinite (soil) fusing point, makes the process of kaolin component generation physicochemical change.This calcination process is the gas-solid interface heterogeneous chemical reaction, mainly is based on redox reaction.The incinerating purpose is to reach the product that high whiteness, high chemically reactive, recrystallization and high porosity etc. require.Kaolinic calcining can make its changes in crystal structure, chemically reactive change; And these variations are with the kind of calcining temperature, the crystallization degree of order, association component and calcination atmosphere etc. confidential relation to be arranged.Kaolin is calcined the effect of being played is: dehydration, decarburization, removal of impurities, separate out new crystal etc.And these complicated physicochemical change have crucial influence to kaolinic calcination product character and quality etc.The main chemical reactions of calcination process generation in the present invention is specially:
Al
2O
3·2SiO
2·2H
2O→Al
2O
3·SiO
2+H
2O
(kaolinite) (metakaolinite)
Al
2O
32SiO
22H
2O (kaolinite) calcines under 600 ℃～630 ℃ conditions and generates metakaolinite (Al
2O
3SiO
2).
2, in the such scheme, AlCl
3+ 3NaOH=Al (OH)
3↓+3NaCl (NaOH is in shortage), NaOH is excessive can to continue reaction: NaOH+Al (OH)
3=NaAlO
2+ 2H
2O, so net reaction is:
AlCl
3+4NaOH＝NaAlO
2+3NaCl+2H
2O
Therefore dropping sodium solution is that first adularescent precipitation generates until excessive phenomenon in the aluminum trichloride solution, and postprecipitation dissolves disappearance gradually.
3, in the such scheme, white carbon black is the general name of white powder X-ray amorphous silicic acid and silicate product, mainly be meant precipitated silica, aerosil, superfine silicon dioxide gel and aerogel, also comprise Powdered synthetic aluminium silicate and Calucium Silicate powder etc.White carbon black is a porous material, and it forms available SiO
2NH
2O represents, wherein nH
2O is that the form with surface hydroxyl exists.Can be dissolved in caustic alkali and hydrofluoric acid, water insoluble acid (except for hydrofluoric acid).High temperature resistant, do not fire, tasteless, do not have and to smell, to have good electrical insulating property.
4, in the such scheme, nano aluminium oxide (Nanometer Aluminium oxide, molecular formula: Al
2O
3, molecular weight: 101.96).Nano aluminium oxide is white crystalline powder, has confirmed that aluminum oxide has 11 kinds of crystal such as α, β, γ, δ, η, θ, κ and χ.Different preparation methods and processing condition can obtain the nano aluminium oxide of different structure.χ, β, η and γ type nano aluminium oxide are characterized in porousness, and high dispersive, high reactivity belong to activated alumina.α-Al2O3, its specific surface is low, has resistant to elevated temperatures inertia, but does not belong to activated alumina, does not almost have catalytic activity.
5, in the such scheme, described kaolin refers to the kaolin concentrate that the kaolin raw ore obtains after separation and purification.
Because the technique scheme utilization, the present invention compared with prior art has following advantage and effect:
1, kaolin of the present invention only needs can reach processing requirement 600 ℃～630 ℃ calcinings.Changed traditional technology and be uisng kaolin decomposing process prepare white carbon black usually need be in the shortcoming of high-temperature calcination more than 800 ℃.Do not need to add alkali during this technology calcining and activating kaolin, thereby reduced corrosion and infringement equipment.
2, the present invention compares with the traditional preparation process white carbon black technique, only need acidleach to handle once, reaction times 70～90min, need not repeatedly acidleach, white carbon black gel after the acidleach is used the NaOH solution-treated once at normal temperatures, generates silicic acid gel with the titration of 15%-18% hydrochloric acid soln then, with gel detergent, filtration totally, drying and calcining get final product finished product, purity reaches more than 98.5%.The purified back of aluminum trichloride solution reaches nano level with ammonium hydrogencarbonate volumetry gained aluminum oxide particle diameter.
3, the present invention can make superfine white carbon black and nano aluminium oxide simultaneously, thereby has reached kaolinic integrated use, and two kinds of product indexs that make are good, the added value of product height.
Embodiment
Below in conjunction with embodiment the present invention is further described:
Embodiment: a kind of is the method for feedstock production superfine white carbon black and nano aluminium oxide with kaolin, is made up of successively following process steps:
(1) calcining
Kaolin calcined under 610 ℃ of conditions make the kaolinite dehydration that contains in the kaolin generate metakaolinite, its reaction formula is: Al
2O
32SiO
22H
2O → Al
2O
3SiO
2+ H
2O;
(2) lixiviate
Kaolin after the calcining is joined in 95 ℃ the hydrochloric acid soln, the Sodium hexametaphosphate 99 that adds kaolin quality 0.95% then, and it is stirred, chemical ingredients aluminum oxide and hydrochloric acid that metakaolinite is contained fully react the generation aluminum chloride, and its reaction formula is: Al
2O
3+ 6HCl=2AlCl
3+ 3H
2O, thus make silicon-dioxide stripping from metakaolinite become amorphous silica, and described amorphous silica major part is colloidal state and exists; Wherein, the mass percent concentration of hydrochloric acid soln is 20%, and aluminum oxide is 1: 7 with the ratio of the mole number of hydrochloric acid;
(3) filter
Vat liquor after the lixiviate is filtered, obtain to contain the filter cake of silicon-dioxide; Contain aluminum chloride, anionic impurity metasilicic acid radical ion, a small amount of silicic acid impurity, the filtrate of cation impurity potassium ion, sodium ion, calcium ion, magnesium ion, iron ion and titanium ion;
(4) aftertreatment
Aftertreatment is made of processing two portions of filtrate that step (3) is obtained and filter cake, to obtain white carbon black and nano aluminium oxide product:
The concrete steps that filtrate is handled are:
A, in filtrate, add the barium chloride solution of 1.0mol/l, and to its stirring barium ion and silicic acid sol and sulfate ion are fully reacted to generate barium silicate, barium sulfate precipitate, the back to its filter clear filtrate, wherein the volume ratio of filtrate and barium chloride solution is 1: 4;
B, add excessive sodium hydrate solution in the filtrate that the A step obtains, be heated to 80 ℃ then, make aluminum chloride and sodium hydroxide fully react the generation sodium metaaluminate under the condensing reflux condition, its reaction formula is: AlCl
3+ 4NaOH=NaAlO
2+ 3NaCl+2H
2O has red Fe (OH) simultaneously
3Precipitation generates, and gets sodium metaaluminate filtrate after the filtration;
C, the sodium metaaluminate filtrate that the B step is obtained are heated to 55 ℃ of formation colloidal solution, and evenly dripping hydrochloric acid makes sodium metaaluminate and hydrochloric acid fully react the generation aluminum chloride, dropwise splashes into ammonium hydrogencarbonate then to generating aluminium carbonate ammonia gel fully; With deionized water aluminium carbonate ammonia gel is carried out at least the once washing operation to remove foreign ion, said washing operation is: aluminium carbonate ammonia gel is added the filter cake that the even after-filtration of deionized water and stirring obtains to contain aluminium carbonate ammonia gel;
D, the aluminium carbonate ammonia gel filter cake after will washing are with ethanol or acetone dehydration, and the dehydration back gets xerogel in 110 ℃ of vacuum-dryings;
E, calcine nano alumina powder jointedly in 1150 ℃ xerogel;
Processing concrete steps to the filter cake that contains silicon-dioxide are:
A, the filter cake that contains silicon-dioxide is carried out at least the once washing operation to remove foreign ion, described washing operation is: the filter cake that will contain silicon-dioxide and the water after-filtration acquisition silica filter cake that stirs;
B, the silica filter cake that a step is obtained is mixed with sodium hydroxide solution makes silicon-dioxide fully be converted into water glass, and its reaction formula is: 2NaOH+SiO
2=Na
2SiO
3+ H
2O adds hydrochloric acid then and makes water glass fully be converted into silicic acid gel in this solution, its reaction formula is: Na
2SiO
3+ 2HCl=H
2SiO
3↓+2NaCl;
C, silicic acid gel is carried out at least the once washing operation to remove impurity, described washing operation is: with silicic acid gel and the water after-filtration acquisition silicic acid gel filter cake that stirs;
D, with the silicic acid gel filter cake at 110 ℃ of dryings, porphyrize then;
Silicic acid gel behind e, the porphyrize obtains the superfine white carbon black powder at 576 ℃ of calcined dehydrations.
The foregoing description only is explanation technical conceive of the present invention and characteristics, and its purpose is to allow the personage who is familiar with this technology can understand content of the present invention and enforcement according to this, can not limit protection scope of the present invention with this.All equivalences that spirit is done according to the present invention change or modify, and all should be encompassed within protection scope of the present invention.
Claims (1)
1, a kind of is the method for feedstock production superfine white carbon black and nano aluminium oxide with kaolin, it is characterized in that: be made up of successively following process steps:
(1) calcining
Kaolin calcined under 600 ℃～630 ℃ conditions make the kaolinite dehydration that contains in the kaolin generate metakaolinite, its reaction formula is: Al
2O
32SiO
22H
2O → Al
2O
3SiO
2+ H
2O;
(2) lixiviate
Kaolin after the calcining is joined in 90 ℃～98 ℃ the hydrochloric acid soln, the Sodium hexametaphosphate 99 that adds kaolin quality 0.8%～1.1% then, and it is stirred, chemical ingredients aluminum oxide and hydrochloric acid that metakaolinite is contained fully react the generation aluminum chloride, and its reaction formula is: Al
2O
3+ 6HCl=2AlCl
3+ 3H
2O, silicon-dioxide is stripping from metakaolinite; Wherein, the mass percent concentration of hydrochloric acid soln is 18～23%, and aluminum oxide is 1: 6.8～7.2 with the ratio of the mole number of hydrochloric acid;
(3) filter
Vat liquor after the lixiviate is filtered, obtain to contain the filter cake of silicon-dioxide; Contain aluminum chloride, anionic impurity metasilicic acid radical ion, silicic acid sol, the filtrate of cation impurity potassium ion, sodium ion, calcium ion, magnesium ion, iron ion and titanium ion;
(4) aftertreatment
Aftertreatment is made of processing two portions of filtrate that step (3) is obtained and filter cake:
The concrete steps that filtrate is handled are:
A, in filtrate, add the barium chloride solution of 0.8～1.2mol/l, and to its stirring barium ion and silicic acid sol and sulfate ion are fully reacted to generate barium silicate, barium sulfate precipitate, the back to its filter clear filtrate, wherein the volume ratio of filtrate and barium chloride solution is 1: 3.5～4.5;
B, add sodium hydroxide solution in the filtrate that the A step obtains, be heated to 75～85 ℃ then, make aluminum chloride and sodium hydroxide fully react the generation sodium metaaluminate under the condensing reflux condition, its reaction formula is: AlCl
3+ 4NaOH=NaAlO
2+ 3NaCl+2H
2O gets sodium metaaluminate filtrate after the filtration;
C, the sodium metaaluminate filtrate that the B step is obtained are heated to 50～60 ℃ of formation colloidal solution, and evenly dripping hydrochloric acid makes sodium metaaluminate and hydrochloric acid fully react the generation aluminum chloride, dropwise splashes into ammonium hydrogencarbonate then to generating aluminium carbonate ammonia gel fully; With deionized water aluminium carbonate ammonia gel is carried out at least the once washing operation to remove foreign ion, said washing operation is: aluminium carbonate ammonia gel is added the filter cake that the even after-filtration of deionized water and stirring obtains to contain aluminium carbonate ammonia gel;
D, the aluminium carbonate ammonia gel filter cake after will washing are with ethanol or acetone dehydration, and the dehydration back gets xerogel in 105 ℃～115 ℃ vacuum-dryings;
E, calcine nano alumina powder jointedly in 1100 ℃～1200 ℃ xerogel;
Processing concrete steps to the filter cake that contains silicon-dioxide are:
A, the filter cake that contains silicon-dioxide is carried out at least the once washing operation to remove foreign ion, described washing operation is: the filter cake that will contain silicon-dioxide and the water after-filtration acquisition silica filter cake that stirs;
B, the silica filter cake that a step is obtained is mixed with sodium hydroxide solution makes silicon-dioxide fully be converted into water glass, and its reaction formula is: 2NaOH+SiO
2=Na
2SiO
3+ H
2O adds hydrochloric acid then and makes water glass fully be converted into silicic acid gel in this solution, its reaction formula is: Na
2SiO
3+ 2HCl=H
2SiO
3↓+2NaCl;
C, silicic acid gel is carried out at least the once washing operation to remove impurity, described washing operation is: with silicic acid gel and the water after-filtration acquisition silicic acid gel filter cake that stirs;
D, with the silicic acid gel filter cake at 105 ℃～115 ℃ dryings, porphyrize then;
Silicic acid gel behind e, the porphyrize obtains the superfine white carbon black powder at 550 ℃～600 ℃ calcined dehydrations.
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