CN102618932B - Method for preparing basic ammonium aluminum carbonate hydroxide whisker and aluminum oxide whisker co-production liquid sodium silicate from bentonite - Google Patents
Method for preparing basic ammonium aluminum carbonate hydroxide whisker and aluminum oxide whisker co-production liquid sodium silicate from bentonite Download PDFInfo
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- CN102618932B CN102618932B CN201210091319.0A CN201210091319A CN102618932B CN 102618932 B CN102618932 B CN 102618932B CN 201210091319 A CN201210091319 A CN 201210091319A CN 102618932 B CN102618932 B CN 102618932B
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Abstract
The invention discloses a method for preparing basic ammonium aluminum carbonate hydroxide whisker and aluminum oxide whisker co-production liquid sodium silicate from bentonite, which comprises the following steps of: adding sulfuric acid solution to bentonite mineral powder which is taken as an initial raw material; reacting; then performing filtering separation; collecting an acid-leached filtrate and acid-leached filter cakes; adding salpeter solution and isoamyl alcohol to the acid-leached filtrate; performing liquid separation and collecting an aqueous phase to obtain aluminum salt solution; adding urea and a surface active agent to the aluminum salt solution; reacting; then, separating, washing and drying to obtain basic ammonium aluminum carbonate hydroxide whiskers; and calcining the basic ammonium aluminum carbonate hydroxide whiskers to obtain aluminum oxide whiskers. Aluminum oxide and silicon dioxide which are required by the method disclosed by the invention respectively come from bentonite ore, and other industrial raw materials do not need to be adopted, so that the production cost can be effectively reduced. The method disclosed by the invention has the advantages that the recovery rate is high; the yield of the aluminum oxide in the bentonite can reach at least 90 percent; and the yield of the amorphous silicon dioxide can reach at least 95 percent.
Description
One, technical field
The present invention relates to a kind of method being produced Aluminum Carbonate Basic ammonium whisker and alumina whisker coproduction liquid sodium silicate by wilkinite, belong to bentonitic deep processing and comprehensively recycle.
Two, background technology
Wilkinite is a kind of important nonmetallic minerals, and its main valuable element is aluminium and silicon.China's bentonite resource is very abundant, and quality better, distribution are wide, have larger comprehensive utilization value.In recent years, having its comprehensive development and utilization situation of many bibliographical informations, coming the instant Starso of production daily use chemicals auxiliary agent, rubber reinforcing filler white carbon black etc. as utilized silicon wherein; Utilize aluminium wherein to produce aluminium series water purifier (as polymerize aluminum chloride, polyaluminium sulfate, poly aluminium sulfate silicate), auxiliary chemicals superfine alumina silicate etc., and be expected to obtain good economic benefit.
Whisker is a kind of filamentary material with certain length-to-diameter ratio grown into single crystal form, its diameter is little, atom high in order, intensity is close to the theoretical value of perfect crystal, thus there is excellent high temperature resistant, Nai Gaore, corrosion resistance nature, have the characteristics such as good physical strength, electrical insulating property, light weight, high strength, high elastic coefficient, high rigidity.Fire retardant be a kind of can improve inflammable substance or combustiblematerials flame retardancy, self-extinguishing or smoke elimination auxiliary agent, be one of main auxiliary agent of important fine chemical product and synthetic materials.Aluminum Carbonate Basic ammonium whisker is a kind of novel aluminium flame retardant, has the premium properties that air release amount is large, smoke effect is better, length is large.Alumina whisker is a kind of ceramic whiskers, has the mechanical property that high strength, high elastic coefficient etc. are superior, good with ceramic matrix material consistency, and application prospect is very wide, is considered to extremely rising inorganic crystal whisker material.At present, Aluminum Carbonate Basic ammonium whisker mainly with aluminum nitrate, tschermigite etc. for raw material adopt water heat transfer obtain; Alumina whisker mainly with aluminium powder, aluminum nitrate, Tai-Ace S 150 etc. for raw material adopt vapor phase process, hydrothermal method, scorification and the methods such as method of fluxing obtain, the raw material used in the above method is technical grade even SILVER REAGENT, cost of material costly, causes production cost higher.
There is not yet so far with wilkinite is the relevant report of waste Aluminum Carbonate Basic ammonium whisker and alumina whisker method.
Three, summary of the invention
The present invention aims to provide a kind of method being produced Aluminum Carbonate Basic ammonium whisker and alumina whisker coproduction liquid sodium silicate by wilkinite, there is low production cost, technique be easy to control, the useful component rate of recovery comparatively high.Simultaneously for improving bentonitic comprehensive utilization value, silicon is wherein used for producing liquid sodium silicate.
Technical solution problem of the present invention adopts following technical scheme:
The present invention produces the method for Aluminum Carbonate Basic ammonium whisker and alumina whisker coproduction liquid sodium silicate by wilkinite, is be initial feed with bentonite, comprises acidleach, purification, synthesis, calcining and alkali and soak each unit process, it is characterized in that:
Described acidleach is less than in the bentonite of 200 μm to particle diameter that to add bentonite quality 2.5-5.5 concentration be doubly the sulphuric acid soln of 15-60wt%, at 80-105 DEG C, react filtering separation after 2-6 hour collect acidleach filtrate and acidleach filter cake, by described acidleach filter cake clear water washing to neutral;
Described purification is the mass concentration adding acidleach filtrate volume 0.5-1% in described acidleach filtrate is the salpeter solution of 60-70%, and add acidleach filtrate volume 0.5-2.0 primary isoamyl alcohol doubly after stirring reaction 10min again, separatory is collected aqueous phase and is aluminum salt solution;
Described synthesis adds urea and tensio-active agent in described aluminum salt solution, 100-140 DEG C reaction 18-36 hour, with after through be separated, washing and drying after obtain Aluminum Carbonate Basic ammonium whisker; Wherein in aluminum salt solution, the molar weight of aluminium is 1: 1.5-2.5 with the ratio of the molar weight of urea; Described tensio-active agent is selected from polyoxyethylene glycol (PEG, number-average molecular weight is 200-6000), cetyl trimethylammonium bromide (CTAB) or sodium lauryl sulphate (SDS), addition is the 0.1-1.8% of aluminium quality in described aluminum salt solution;
Described calcining is that described Aluminum Carbonate Basic ammonium whisker is calcined 2-5 hour at 800-1200 DEG C, obtains alumina whisker;
The leaching of described alkali is that in described acidleach filter cake, add acidleach filter cake quality 2.5-4.5 concentration be doubly the sodium hydroxide solution of 6-25wt%, and filter after 0.5-2 hour 60-95 DEG C of reaction, gained filtrate is liquid sodium silicate.
The each step reaction equation of the inventive method is:
1, bentonitic acidleach
Al
2O
3·4SiO
2·3H
2O+3H
2SO
4+(4n-6)H
2O→4SiO
2·nH
2O+Al
2(SO
4)
3
Fe
2O
3+3H
2SO
4→Fe
2(SO
4)
3+3H
2O
2, the preparation of Aluminum Carbonate Basic ammonium whisker
Al
2(SO
4)
3+8CO(NH
2)
2+4H
2O→2NH
4[Al(OH)
2CO
3]↓+3(NH
4)
2SO
4+8NH
4HCO
3
3, the preparation of alumina whisker
2NH
4[Al(OH)
2CO
3]→Al
2O
3+2CO
2↑+2NH
3↑+3H
2O
4, the alkali leaching of wilkinite acidleach filter cake
m(SiO
2·nH
2O)+2NaOH→Na
2O·mSiO
2+(nm+1)H
2O
Concrete steps prepared by the present invention are as follows:
Step 1: bentonitic acidleach
Being less than to particle diameter in the bentonite of 200 μm and adding bentonite quality 2.5-5.5 concentration is doubly the sulphuric acid soln of 15-60wt%, acidleach filter cake and acidleach filtrate is filtered to obtain react 2-6 hour at 80-105 DEG C after, by described acidleach filter cake clear water washing to neutral, collect acidleach filter cake, acidleach filtrate and washings respectively.
Step 2: pickling liquor purifies
Mixed solution is obtained by after step 1 gained acidleach filtrate and washing lotion mixing, the mass concentration adding mixeding liquid volume 0.5-1% in mixed solution is the salpeter solution of 60-70%, mixeding liquid volume 0.5-2.0 primary isoamyl alcohol is doubly added again after stirring reaction 5-10min, at room temperature repeatedly shake 10-20min, after leaving standstill phase-splitting, gained aqueous phase is aluminum salt solution.
Step 3: the preparation of Aluminum Carbonate Basic ammonium whisker
To step 2 prepare aluminum salt solution in add urea and tensio-active agent, 100-140 DEG C reaction 18-36 hour, with after through be separated, washing and drying after obtain Aluminum Carbonate Basic ammonium whisker; Wherein in aluminum salt solution, the molar weight of aluminium is 1: 1.5-2.5 with the ratio of the molar weight of urea; Described tensio-active agent is selected from PEG, CTAB or SDS, and addition is the 0.1-1.8% of aluminium quality in described aluminum salt solution.
Step 4: the preparation of alumina whisker
By the Aluminum Carbonate Basic ammonium whisker of gained in step 3 at 800-1200 DEG C of calcining 2-5 hour, obtain alumina whisker.
Step 5: the alkali leaching of wilkinite acidleach filter cake
In step 1 gained acidleach filter cake, add acidleach filter cake quality 2.5-4.5 concentration is doubly the sodium hydroxide solution of 6-25wt%, and filter after 0.5-2 hour 60-95 DEG C of reaction, gained filtrate is liquid sodium silicate.
Compared with the prior art, beneficial effect of the present invention is embodied in:
1, the inventive method produces Aluminum Carbonate Basic ammonium whisker, alumina whisker and liquid sodium silicate, and take full advantage of the aluminum oxide in wilkinite and silicon-dioxide useful component, production technique is closed cycle, basic three-waste free discharge.
2, the inventive method raw Aluminum Carbonate Basic ammonium whisker, alumina whisker and the aluminum oxide needed for liquid sodium silicate and silicon-dioxide all come from bentonite ore, without the need to adopting other industrial raw material, its production cost can be made effectively to be reduced.
3, the present invention utilizes primary isoamyl alcohol to extract method for removing iron purification aluminum salt solution, and de-ironing efficiency is high, and aluminium salt loses hardly.
4, the rate of recovery of the present invention is high, and in wilkinite, the yield of aluminum oxide can reach more than 90%, the yield of amorphous silica can reach more than 95%.
The present invention is further illustrated below by specific embodiment.
Four, accompanying drawing explanation
Fig. 1 is the SEM figure of Aluminum Carbonate Basic ammonium whisker prepared by the embodiment of the present invention 1.
Fig. 2 is the SEM figure of alumina whisker prepared by the embodiment of the present invention 1.
Fig. 3 is the SEM figure of Aluminum Carbonate Basic ammonium whisker prepared by the embodiment of the present invention 2.
Fig. 4 is the SEM figure of alumina whisker prepared by the embodiment of the present invention 2.
Fig. 5 is the SEM figure of Aluminum Carbonate Basic ammonium whisker prepared by the embodiment of the present invention 3.
Fig. 6 is the SEM figure of alumina whisker prepared by the embodiment of the present invention 3.
Five, embodiment
Embodiment 1:
1, in the bentonite of particle diameter≤75 μm, the sulphuric acid soln that concentration is 20wt% is added, the mass ratio of bentonite and sulphuric acid soln is 1: 5, acidleach filter cake and acidleach filtrate is filtered to obtain react 3h at 100 DEG C of temperature after, by described acidleach filter cake clear water washing to neutral, collect acidleach filter cake, acidleach filtrate and washing lotion respectively;
2, step 1 gained acidleach filtrate and washing lotion are mixed to obtain mixed solution, the mass concentration adding mixeding liquid volume 0.5% in mixed solution is the salpeter solution of 66%, stirring reaction 10min, add isopyknic primary isoamyl alcohol with mixed solution again, shake 15min, stratification, collects aqueous phase and is alum liquor;
3, in 75mL reactor, add 45mL step 2 gained alum liquor, urea is added in the molar weight of aluminium in alum liquor and the ratio of the ratio 1: 1.5 of urea molar weight, the CTAB of 0.5% of aluminium quality in alum liquor is added again after dissolving, at 120 DEG C of reaction 24h after dissolving, filter, washing, at 105 DEG C of dry 2h, obtains Aluminum Carbonate Basic ammonium whisker.
Aluminum Carbonate Basic ammonium crystal whisker products is accredited as pure phase through X-ray diffraction.The SEM figure of Aluminum Carbonate Basic ammonium whisker is shown in Fig. 1.Fig. 1 shows: it is 12 μm that whisker is about, and diameter is about 0.8 μm; Aluminum Carbonate Basic ammonium yield is 91.2%.
4, step 3 gained Aluminum Carbonate Basic ammonium whisker is placed in retort furnace, in 900 DEG C of calcining 5h, obtains alumina whisker product.
Alumina whisker product is accredited as pure phase through XRD.The SEM figure of alumina whisker is shown in Fig. 2.As seen from the figure, diameter of whiskers is about 0.5 μm, mean length about 8 μm; Aluminum oxide yield is 91.0%.
5, the mass concentration adding acidleach filter cake quality 4.5 times in the acidleach filter cake of step 1 collection is the sodium hydroxide solution of 8%, and heated and stirred reaction 1h under the temperature condition of 90 DEG C, filter, gained filtrate is liquid sodium silicate.
Analytical results shows, the modulus of this liquid sodium silicate is about 3.50, meets the requirement of liquid-1 product standard.Gained filter cake, mainly containing unreacted wilkinite, can be back in acid-leaching reaction after cleaning.The yield of amorphous silica is 95.5%.
Embodiment 2:
1, in the bentonite of particle diameter≤100 μm, the sulphuric acid soln that concentration is 40wt% is added, the mass ratio of bentonite and sulphuric acid soln is 1: 4, acidleach filter cake and acidleach filtrate is filtered to obtain react 4h at 95 DEG C of temperature after, by described acidleach filter cake clear water washing to neutral, collect acidleach filter cake, acidleach filtrate and washing lotion respectively.
2, step 1 gained acidleach filtrate and washing lotion are mixed to obtain mixed solution, the mass concentration adding mixeding liquid volume 0.8% in mixed solution is the salpeter solution of 60%, stirring reaction 8min, add the primary isoamyl alcohol of mixeding liquid volume 0.5 times again, shake 20min, stratification, collects aqueous phase and is alum liquor.
3, in 75mL reactor, add 45mL step 2 gained alum liquor, urea is added in the molar weight of aluminium in alum liquor and the ratio of the ratio 1: 2.0 of urea molar weight, the SDS of 1.0% of aluminium quality in alum liquor is added again after dissolving, at 140 DEG C of reaction 18h after dissolving, filter, washing, at 105 DEG C of dry 2h, obtains Aluminum Carbonate Basic ammonium whisker.
Aluminum Carbonate Basic ammonium crystal whisker products is accredited as pure phase through X-ray diffraction.The SEM figure of Aluminum Carbonate Basic ammonium whisker is shown in Fig. 3.Fig. 3 shows: it is 15 μm that whisker is on average about, and diameter is about 1 μm; Aluminum Carbonate Basic ammonium yield is 91.6%.
4, step 3 gained Aluminum Carbonate Basic ammonium whisker is placed in retort furnace, in 1100 DEG C of calcining 3h, obtains alumina whisker product.
Alumina whisker product is accredited as pure phase through X-ray diffraction.The SEM figure of alumina whisker is shown in Fig. 4.As seen from the figure, diameter of whiskers is about 0.6 μm, mean length about 8 μm; Aluminum oxide yield is 91.5%.
5, the mass concentration adding acidleach filter cake quality 3.3 times in the acidleach filter cake of step 1 collection is the sodium hydroxide solution of 13%, and heated and stirred reaction 1.5h under the temperature condition of 80 DEG C, filter, gained filtrate is liquid sodium silicate.
Analytical results shows, the modulus of this liquid sodium silicate is about 2.75, meets the requirement of liquid-3 product standard.Gained filter cake, mainly containing unreacted wilkinite, can be back in acid-leaching reaction after cleaning.The yield of amorphous silica is 96.0%;
Embodiment 3:
1, in the bentonite of particle diameter≤125 μm, the sulphuric acid soln that concentration is 50wt% is added, the mass ratio of bentonite and sulphuric acid soln is 1: 3, acidleach filter cake and acidleach filtrate is filtered to obtain react 5h at 85 DEG C of temperature after, by described acidleach filter cake clear water washing to neutral, collect acidleach filter cake, acidleach filtrate and washing lotion respectively.
2, step 1 gained acidleach filtrate and washing lotion are mixed to obtain mixed solution, the mass concentration adding mixeding liquid volume 1% in mixed solution is the salpeter solution of 66%, stirring reaction 5min, add the primary isoamyl alcohol of mixeding liquid volume 2 times again, shake 10min, stratification, collects aqueous phase and is alum liquor.
3, in 75mL reactor, add 45mL step 2 gained alum liquor, urea is added in the molar weight of aluminium in alum liquor and the ratio of the ratio 1: 2.5 of urea molar weight, the PEG2000 of 1.5% of aluminium quality in alum liquor is added again after dissolving, at 100 DEG C of reaction 36h after dissolving, filter, washing, at 105 DEG C of dry 2h, obtains Aluminum Carbonate Basic ammonium whisker.
Aluminum Carbonate Basic ammonium crystal whisker products is accredited as pure phase through X-ray diffraction.The SEM figure of Aluminum Carbonate Basic ammonium whisker is shown in Fig. 5.Fig. 5 shows: it is 18 μm that whisker is about, and diameter is about 1.1 μm; Aluminum Carbonate Basic ammonium yield is 92.1%.
4, step 3 gained Aluminum Carbonate Basic ammonium whisker is placed in retort furnace, in 1000 DEG C of calcining 4h, obtains alumina whisker product.
Alumina whisker product is accredited as pure phase through X-ray diffraction.The SEM figure of alumina whisker is shown in Fig. 6.Diameter of whiskers is about 0.5 μm as seen from the figure, mean length about 10 μm; Aluminum oxide yield is 92.0%.
5, the mass concentration adding acidleach filter cake quality 2.5 times in the acidleach filter cake of step 1 collection is the sodium hydroxide solution of 18%, and heated and stirred reaction 2h under the temperature condition of 70 DEG C, filter, gained filtrate is liquid sodium silicate.
Analytical results shows, the modulus of this liquid sodium silicate is about 2.40, meets the requirement of liquid-4 product standard.Gained filter cake, mainly containing unreacted wilkinite, can be back in acid-leaching reaction after cleaning.The yield of amorphous silica is 98.0%.
Claims (1)
1. produced a method for Aluminum Carbonate Basic ammonium whisker and alumina whisker coproduction liquid sodium silicate by wilkinite, detailed process is as follows:
1) in the bentonite of particle diameter≤125 μm, the sulphuric acid soln that concentration is 50wt% is added, the mass ratio of bentonite and sulphuric acid soln is 1:3, acidleach filter cake and acidleach filtrate is filtered to obtain react 5h at 85 DEG C of temperature after, by described acidleach filter cake clear water washing to neutral, collect acidleach filter cake, acidleach filtrate and washing lotion respectively;
2) step 1) gained acidleach filtrate and washing lotion are mixed to obtain mixed solution, the mass concentration adding mixeding liquid volume 1% in mixed solution is the salpeter solution of 66%, stirring reaction 5min, add the primary isoamyl alcohol of mixeding liquid volume 2 times again, shake 10min, stratification, collects aqueous phase and is alum liquor;
3) in 75mL reactor, 45mL step 2 is added) gained alum liquor, urea is added in the molar weight of aluminium in alum liquor and the ratio of the ratio 1: 2.5 of urea molar weight, the PEG2000 of 1.5% of aluminium quality in alum liquor is added again after dissolving, at 100 DEG C of reaction 36h after dissolving, filter, washing, at 105 DEG C of dry 2h, obtain Aluminum Carbonate Basic ammonium whisker, Aluminum Carbonate Basic ammonium yield is 92.1%;
4) step 3) gained Aluminum Carbonate Basic ammonium whisker is placed in retort furnace, in 1000 DEG C of calcining 4h, obtain alumina whisker product, aluminum oxide yield is 92.0%;
5) mass concentration adding acidleach filter cake quality 2.5 times in the acidleach filter cake of step 1) collection is the sodium hydroxide solution of 18%, heated and stirred reaction 2h under the temperature condition of 70 DEG C, and filter, gained filtrate is liquid sodium silicate; The modulus of liquid sodium silicate is 2.40, and the yield of amorphous silica is 98.0%.
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| CN104449097A (en) * | 2014-12-11 | 2015-03-25 | 江门市绿茵环保科技有限公司 | Novel fireproof thermal insulation coating and preparation method thereof |
| CN105749946B (en) * | 2016-04-15 | 2018-02-13 | 盐城工学院 | A kind of solid base catalyst NH4Al(OH)2CO3, preparation method and its catalyzed conversion glucose method |
| CN106518117A (en) * | 2016-10-07 | 2017-03-22 | 常州市鼎日环保科技有限公司 | Superhard ceramic abrasive material preparation method |
| CN108217702B (en) * | 2018-01-10 | 2020-09-01 | 中国石油大学(华东) | Synthesis of ultramicropore basic ammonium aluminum carbonate and method for preparing aluminum oxide by pyrolysis of ultramicropore basic ammonium aluminum carbonate |
| CN108484132B (en) * | 2018-02-06 | 2021-11-02 | 淮北特旭信息科技有限公司 | Preparation method of compact composite bulletproof plate |
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