CN107416877A - The technique of organic matter, iron and silica in a kind of removing sodium aluminate solution - Google Patents
The technique of organic matter, iron and silica in a kind of removing sodium aluminate solution Download PDFInfo
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- CN107416877A CN107416877A CN201710332525.9A CN201710332525A CN107416877A CN 107416877 A CN107416877 A CN 107416877A CN 201710332525 A CN201710332525 A CN 201710332525A CN 107416877 A CN107416877 A CN 107416877A
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- sodium aluminate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/46—Purification of aluminium oxide, aluminium hydroxide or aluminates
- C01F7/47—Purification of aluminium oxide, aluminium hydroxide or aluminates of aluminates, e.g. removal of compounds of Si, Fe, Ga or of organic compounds from Bayer process liquors
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/46—Purification of aluminium oxide, aluminium hydroxide or aluminates
- C01F7/47—Purification of aluminium oxide, aluminium hydroxide or aluminates of aluminates, e.g. removal of compounds of Si, Fe, Ga or of organic compounds from Bayer process liquors
- C01F7/473—Removal of organic compounds, e.g. sodium oxalate
- C01F7/476—Removal of organic compounds, e.g. sodium oxalate by oxidation
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a kind of technique for removing organic matter, iron and silica in sodium aluminate solution, comprise the following steps：Sodium aluminate circulating mother liquor is heated to 80 90 DEG C, and calcium oxide is added thereto and carries out absorption displacement reaction, calcium oxide is that carbonate-free lime stone is calcined or precipitated calcium carbonate is through calcined crushed, stirring is opened after addition, the organic substance humic acid sodium in solution is set to be separated out with calcium salt forms, calcium aluminate fine particle of the sodium aluminate reaction generation with high surface area in simultaneous oxidation calcium and solution, separation of solid and liquid is carried out after completion of the reaction, the little particle to be suspended in solution after reaction is separated by filtration, solution temperature is adjusted at 45 55 DEG C, the hydrogen peroxide for adding 3 6% volumes further sloughs solution colour, processing Mother liquor is used to prepare refined liquid.The present invention has operating process simple, it is not necessary to increases extras, organic removal efficiency is high, and clean good decolorizing effect, and cost is low, has a good application prospect.
Description
Technical field
The present invention relates to organic matter, iron and two in chemical industry impurity removing technology field, more particularly to a kind of removing sodium aluminate solution
The technique of silica.
Background technology
Aluminium hydroxide micropowder is particle diameter 1-2 microns, and pattern is regular, whiteness >=95%, Fe3O2Content≤1%, SiO2Content
≤ 2%, the inorganic particle of good dispersion, it is mainly used in environmental protection flame retardant filler, on the whole, preparation method is divided into Mechanical Method and change
Method, Mechanical Method are by disintegrating apparatus such as ball mill, vibromill, airflow millings, deform upon coarse grain footpath aluminum hydroxide particles
And then rupture, finally into granularity 1-2 micro mist, but the method product, because of particle size range wider distribution, pattern is irregular, product whiteness
Aluminium hydroxide raw material is depended entirely on purity, is mainly used in some industries relatively low to purity, granularity, pattern requirement.Chemistry
Method leaches bauxite with Bayer process and saturation sodium aluminate circulating mother liquor is made, and crystallization prepares ultrafine aluminium hydroxide, has cost of material
Low, flow is simply recyclable, process produces without waste water and dregs, operation degree of controllability is high, easily realizes the advantages such as large-scale production.
Due to Bayer Process digestion bauxite sodium aluminate circulating mother liquor, impurity is more, it is necessary to which sodium aluminate circulating mother liquor purifies
Flow, increase equipment and process, to simplify micro mist production procedure, aluminium hydroxide micro powder production is more using the molten coarse aluminium hydroxide of weight
Saturated solution of sodium aluminate is made, then crystalline aluminum hydroxide is separated out production aluminium hydroxide by the stirring addition crystal seed that cools micro-
Powder, due to still containing a small amount of humic acid and ferrosilicon impurity component in coarse aluminium hydroxide, alkali soluble mother liquor is reused, can made molten
The impurity component such as organic matter, silica, iron constantly accumulates in liquid, the complexity that solution composition becomes, and solution becomes sticky, and color is in
Existing dark brown, the production capacity for causing aluminium hydroxide micro powder to produce reduce, and quality decline, product whiteness, purity reduce, the inclined reddish yellow of colour
Phase.
Organic matter can be such that induction crystal seed is poisoned by organic matter, and activity reduces, while adsorb in nucleating surface, influence hydroxide
Precipitation of the aluminium on nucleus, reduces resolution ratio, and grain growth speed reduces, and causes to produce the decline of product granularity controllability, production
Product particle diameter refines partially, filling capacity reduces.SiO2The stability of solution can be improved, makes the reduction of refined liquid degree of supersaturation degree, production
Extracting rate reduces.Fe2O3It can then make solution that yellow and red be presented, influence product whiteness.Therefore must be in sodium aluminate circulating mother liquor
Impurity content is control effectively, and solution purification is carried out in impurities accumulation solution colour dark color for a period of time.
The content of the invention
The present invention proposes a kind of technique for removing organic matter, iron and silica in sodium aluminate solution, above-mentioned to solve
The problem of being proposed in background technology.
The present invention proposes a kind of technique for removing organic matter, iron and silica in sodium aluminate solution, including following step
Suddenly：
S1, choose sodium aluminate circulating mother liquor be raw material, by sodium aluminate circulating mother liquor temperature control at 40-60 DEG C, and to its
Middle addition calcium oxide carries out absorption displacement reaction, and calcium oxide is that carbonate-free lime stone is calcined or precipitated calcium carbonate is through calcined crushed, grain
60-160 mesh is spent, CaO content 80-95%, addition 15-30g/l, stirring is opened after addition, by sodium aluminate circulating mother liquor temperature raising
To 80-90 DEG C, reaction displacement 60-180min, the organic substance humic acid sodium in solution is set to be separated out with calcium salt forms, calcium oxide and molten
Calcium aluminate particles of the sodium aluminate reaction generation with high surface area in liquid, play suction-operated to organic matter, iron, silicon impurities with
Calcium aluminosilicate hydrate crystallization separates out；
S2, separation of solid and liquid being carried out after completion of the reaction, the little particle to be suspended in solution after reaction being separated by filtration, solution is natural
Cooling or heat exchange are cooled to 45-55 DEG C, to treat to operate in next step；
S3, the hydrogen peroxide of 45-55 DEG C of addition 3-6% volume of solution further remove color, hydrogen peroxide mass fraction 25-
35%, open stirring and lift temperature to 75-85 DEG C, decolouring 60-120min, remove in decomposing solution with coloured long-chain organic matter；
S4, gained filtrate is carried out to composition detection, refined liquid is made in processing Mother liquor dilution.
Preferably, the requirement that sodium aluminate liquor alumina silica ratio is not less than 200 is met in S4.
Preferably, the shading value 0.3-0.5 of the refined sodium aluminate solution after processing, color present faint yellow.
Preferably, the hydrogen peroxide in S3 has oxidation, and colored long-chain oxidation operation in solution can break
Light small-molecular-weight organic matter is cleaved into, solution is completed and decolourizes, hydrogen peroxide will not bring other impurities, absorbance after processing into mother liquor
0.15-0.2, the limpid color of solution carry wheat, complete to decolourize.
The present invention is by adding appropriate calcium oxide into sodium aluminate liquor, and calcium oxide is main and sodium aluminate reaction generation is thin
Grain calcium aluminate, has larger surface area and stronger adsorption capacity, adsorbs organic matter, and organic matter is removed by separation of solid and liquid,
A small amount of calcium aluminate and silicon, iron reaction generation calcium aluminosilicate hydrate, reach except the purpose of silicon iron removaling, are then added into filtrated stock
Oxidant hydrogen peroxide, destruction carry dark colour long-chain organic matter, are solution colour reductions, reach the purpose of decolouring, this technology
It is simple with operating process, it is not necessary to increase extras, organic removal efficiency is high, the advantages of the good decolorizing effect that cleans, into
This is low, has a good application prospect.
Embodiment
With reference to specific embodiment, the present invention will be further described.
Embodiment 1
The present invention proposes a kind of technique for removing organic matter, iron and silica in sodium aluminate solution, including following step
Suddenly：
S1, selection sodium aluminate circulating mother liquor are raw material, sodium aluminate circulating mother liquor are heated into 40 DEG C, and add oxygen thereto
To change calcium and carry out absorption displacement reaction, calcium oxide is that carbonate-free lime stone is calcined or precipitated calcium carbonate is through calcined crushed, the mesh of granularity 60,
CaO content 80%, addition 15g/l, stirring is opened after addition, sodium aluminate circulating mother liquor is lifted temperature to 80 DEG C, reaction displacement
60min, the organic substance humic acid sodium in solution is set to be separated out with calcium salt forms, the sodium aluminate reaction generation tool in calcium oxide and solution
There are the calcium aluminate particles of high surface area, suction-operated is played to organic matter, iron, silicon impurities and calcium aluminate reaction are with calcium aluminosilicate hydrate
Crystallization separates out；
S2, separation of solid and liquid is carried out after completion of the reaction, the little particle to be suspended in solution after reaction is separated by filtration, solution normal temperature
45 DEG C are cooled to, to treat to operate in next step；
S3, the hydrogen peroxide of 45 DEG C of 3% volumes of addition of solution further remove color, hydrogen peroxide mass fraction 25%, open and stir
Mix and lift temperature to 75 DEG C, decolouring 60min, remove in decomposing solution with coloured long-chain organic matter；
S4, gained filtrate is carried out to composition detection, processing Mother liquor is used to prepare refined liquid.
Meet the requirement that mother liquor alumina silica ratio is not less than 200 in S4.
The shading value 0.3 of refined sodium aluminate solution after processing, color present faint yellow.
Hydrogen peroxide in S3 has oxidation, colored long-chain oxidation operation in solution can be fragmented into light color
Small-molecular-weight organic matter, complete solution and decolourize, hydrogen peroxide will not bring other impurities into mother liquor, and absorbance 0.15, molten after processing
The limpid color of liquid carries wheat, completes to decolourize.
Embodiment 2
The present invention proposes a kind of technique for removing organic matter, iron and silica in sodium aluminate solution, including following step
Suddenly：
S1, selection sodium aluminate circulating mother liquor are raw material, sodium aluminate circulating mother liquor are heated into 45 DEG C, and add oxygen thereto
To change calcium and carry out absorption displacement reaction, calcium oxide is that carbonate-free lime stone is calcined or precipitated calcium carbonate is through calcined crushed, the mesh of granularity 80,
CaO content 85%, addition 20g/l, stirring is opened after addition, sodium aluminate circulating mother liquor is lifted temperature to 82 DEG C, reaction displacement
80min, the organic substance humic acid sodium in solution is set to be separated out with calcium salt forms, the sodium aluminate reaction generation tool in calcium oxide and solution
There are the calcium aluminate particles of high surface area, suction-operated is played to organic matter, iron, silicon impurities are crystallized with calcium aluminosilicate hydrate and separated out；
S2, separation of solid and liquid is carried out after completion of the reaction, the little particle to be suspended in solution after reaction is separated by filtration, solution normal temperature
47 DEG C are cooled to, to treat to operate in next step；
S3, the hydrogen peroxide of 47 DEG C of 4% volumes of addition of solution further remove color, hydrogen peroxide mass fraction 28%, open and stir
Mix and lift temperature to 78 DEG C, decolouring 80min, remove in decomposing solution with coloured long-chain organic matter；
S4, gained filtrate is carried out to composition detection, processing Mother liquor is used to prepare refined liquid.
Meet the requirement that mother liquor alumina silica ratio is not less than 200 in S4.
The shading value 0.35 of refined sodium aluminate solution after processing, color present faint yellow.
Hydrogen peroxide in S3 has oxidation, colored long-chain oxidation operation in solution can be fragmented into light color
Small-molecular-weight organic matter, complete solution and decolourize, hydrogen peroxide will not bring other impurities into mother liquor, and absorbance 0.16, molten after processing
The limpid color of liquid carries wheat, completes to decolourize.
Embodiment 3
The present invention proposes a kind of technique for removing organic matter, iron and silica in sodium aluminate solution, including following step
Suddenly：
S1, selection sodium aluminate circulating mother liquor are raw material, sodium aluminate circulating mother liquor are heated into 50 DEG C, and add oxygen thereto
To change calcium and carry out absorption displacement reaction, calcium oxide is that carbonate-free lime stone is calcined or precipitated calcium carbonate is through calcined crushed, the mesh of granularity 100,
CaO content 90%, addition 25g/l, stirring is opened after addition, sodium aluminate circulating mother liquor is lifted temperature to 85 DEG C, reaction displacement
100min, the organic substance humic acid sodium in solution is set to be separated out with calcium salt forms, the sodium aluminate reaction generation in calcium oxide and solution
Calcium aluminate particles with high surface area, suction-operated is played to organic matter, and iron, silicon impurities are crystallized with calcium aluminosilicate hydrate and separated out；
S2, separation of solid and liquid is carried out after completion of the reaction, the little particle to be suspended in solution after reaction is separated by filtration, solution normal temperature
50 DEG C are cooled to, to treat to operate in next step；
S3, the hydrogen peroxide of 50 DEG C of 5% volumes of addition of solution further remove color, hydrogen peroxide mass fraction 30%, open and stir
Mix and lift temperature to 80 DEG C, decolouring 100min, remove in decomposing solution with coloured long-chain organic matter；
S4, gained filtrate is carried out to composition detection, processing Mother liquor is used to prepare refined liquid.
Mother liquor alumina silica ratio is not less than 200 requirement in S4.
The shading value 0.4 of refined sodium aluminate solution after processing, color present faint yellow.
Hydrogen peroxide in S3 has oxidation, colored long-chain oxidation operation in solution can be fragmented into light color
Small-molecular-weight organic matter, complete solution and decolourize, hydrogen peroxide will not bring other impurities into mother liquor, and absorbance 0.17, molten after processing
The limpid color of liquid carries wheat, completes to decolourize.
Embodiment 4
The present invention proposes a kind of technique for removing organic matter, iron and silica in sodium aluminate solution, including following step
Suddenly：
S1, selection sodium aluminate circulating mother liquor are raw material, sodium aluminate circulating mother liquor are heated into 55 DEG C, and add oxygen thereto
To change calcium and carry out absorption displacement reaction, calcium oxide is that carbonate-free lime stone is calcined or precipitated calcium carbonate is through calcined crushed, the mesh of granularity 120,
CaO content 92%, addition 28g/l, stirring is opened after addition, sodium aluminate circulating mother liquor is lifted temperature to 88 DEG C, reaction displacement
130min, the organic substance humic acid sodium in solution is set to be separated out with calcium salt forms, the sodium aluminate reaction generation in calcium oxide and solution
Calcium aluminate particles with high surface area, suction-operated is played to organic matter, and iron, silicon impurities are crystallized with calcium aluminosilicate hydrate and separated out；
S2, separation of solid and liquid is carried out after completion of the reaction, the little particle to be suspended in solution after reaction is separated by filtration, solution normal temperature
52 DEG C are cooled to, to treat to operate in next step；
S3, the hydrogen peroxide of 52 DEG C of 5% volumes of addition of solution further remove color, hydrogen peroxide mass fraction 32%, open and stir
Mix and lift temperature to 82 DEG C, decolouring 110min, remove in decomposing solution with coloured long-chain organic matter；
S4, gained filtrate is carried out to composition detection, refined liquid is made in processing Mother liquor dilution.
Meet the requirement that mother liquor alumina silica ratio is not less than 200 in S4.
The shading value 0.45 of refined sodium aluminate solution after processing, color present faint yellow.
Hydrogen peroxide in S3 has oxidation, colored long-chain oxidation operation in solution can be fragmented into light color
Small-molecular-weight organic matter, complete solution and decolourize, hydrogen peroxide will not bring other impurities into mother liquor, and absorbance 0.18, molten after processing
The limpid color of liquid carries wheat, completes to decolourize.
Embodiment 5
The present invention proposes a kind of technique for removing organic matter, iron and silica in sodium aluminate solution, including following step
Suddenly：
S1, selection sodium aluminate circulating mother liquor are raw material, sodium aluminate circulating mother liquor are heated into 60 DEG C, and add oxygen thereto
To change calcium and carry out absorption displacement reaction, calcium oxide is that carbonate-free lime stone is calcined or precipitated calcium carbonate is through calcined crushed, the mesh of granularity 160,
CaO content 95%, addition 30g/l, stirring is opened after addition, sodium aluminate circulating mother liquor is lifted temperature to 90 DEG C, reaction displacement
180min, the organic substance humic acid sodium in solution is set to be separated out with calcium salt forms, the sodium aluminate reaction generation in calcium oxide and solution
Calcium aluminate particles with high surface area, suction-operated is played to organic matter, and iron, silicon impurities are crystallized with calcium aluminosilicate hydrate and separated out；
S2, separation of solid and liquid is carried out after completion of the reaction, the little particle to be suspended in solution after reaction is separated by filtration, solution normal temperature
55 DEG C are cooled to, to treat to operate in next step；
S3, the hydrogen peroxide of 55 DEG C of 6% volumes of addition of solution further remove color, hydrogen peroxide mass fraction 35%, open and stir
Mix and lift temperature to 85 DEG C, decolouring 120min, remove in decomposing solution with coloured long-chain organic matter；
S4, gained filtrate is carried out to composition detection, refined liquid is made in processing Mother liquor dilution.
Meet the requirement that mother liquor alumina silica ratio is not less than 200 in S4.
The shading value 0.5 of refined sodium aluminate solution after processing, color present faint yellow.
Hydrogen peroxide in S3 has oxidation, colored long-chain oxidation operation in solution can be fragmented into light color
Small-molecular-weight organic matter, complete solution and decolourize, hydrogen peroxide will not bring other impurities into mother liquor, absorbance 0.2, solution after processing
Limpid color carries wheat, completes to decolourize.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art the invention discloses technical scope in, technique according to the invention scheme and its
Inventive concept is subject to equivalent substitution or change, should all be included within the scope of the present invention.
Claims (4)
1. a kind of technique for removing organic matter, iron and silica in sodium aluminate solution, it is characterised in that comprise the following steps：
S1, selection sodium aluminate circulating mother liquor are raw material, sodium aluminate circulating mother liquor are heated into 40-60 DEG C, and add oxygen thereto
Change calcium and carry out absorption displacement reaction, calcium oxide is that carbonate-free lime stone is calcined or precipitated calcium carbonate is through calcined crushed, granularity 60-160
Mesh, CaO content 80-95%, addition 15-30g/l, stirring is opened after addition, sodium aluminate circulating mother liquor is lifted temperature into 80-90
DEG C, reaction displacement 60-180min, the organic substance humic acid sodium in solution is separated out with calcium salt forms, in calcium oxide and solution
Calcium aluminate particulate of the sodium aluminate reaction generation with high surface area, suction-operated, iron, silicon impurities and calcium aluminate are played to organic matter
Reaction is crystallized with calcium aluminosilicate hydrate and separated out；
S2, separation of solid and liquid is carried out after completion of the reaction, the little particle to be suspended in solution after reaction is separated by filtration, the cooling of solution normal temperature
To 45-55 DEG C, to treat to operate in next step；
S3, the hydrogen peroxide of 45-55 DEG C of solution addition 3-6% volumes further remove color, hydrogen peroxide mass fraction 25-35%,
Open stirring and lift temperature to 75-85 DEG C, decolouring 60-120min, remove in decomposing solution with coloured long-chain organic matter；
S4, gained filtrate is carried out to composition detection, processing Mother liquor is used to prepare refined liquid.
2. a kind of technique for removing organic matter, iron and silica in sodium aluminate solution according to claim 1, its feature
It is：Aluminium meets the requirement that mother liquor alumina silica ratio is not less than 200 in S4.
3. a kind of technique for removing organic matter, iron and silica in sodium aluminate solution according to claim 1, its feature
It is：The shading value 0.3-0.5 of refined sodium aluminate solution after processing, color present faint yellow.
4. a kind of technique for removing organic matter, iron and silica in sodium aluminate solution according to claim 1, its feature
It is：Hydrogen peroxide in S3 has oxidation, and it is small that colored long-chain oxidation operation in solution can be fragmented into light color
Molecular weight organics, to complete solution and decolourize, hydrogen peroxide will not bring other impurities into mother liquor, absorbance 0.15-0.2 after processing,
The limpid color of solution carries wheat, completes to decolourize.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109502609A (en) * | 2018-11-23 | 2019-03-22 | 宜宾海丰和锐有限公司 | The method and apparatus of silica in salt water is reduced in ionic membrane method alkali-chloride technique |
| CN110436494A (en) * | 2019-08-30 | 2019-11-12 | 贵州大学 | A kind of alumina producing circulating mother liquor hydrogen peroxide method of modifying |
| CN111217384A (en) * | 2020-02-24 | 2020-06-02 | 中南大学 | Method for removing organic matters in sodium aluminate solution by foam separation |
| CN112194160A (en) * | 2020-09-30 | 2021-01-08 | 洛阳中超新材料股份有限公司 | Method for decoloring sodium aluminate solution for superfine aluminum hydroxide |
| CN113184873A (en) * | 2021-04-23 | 2021-07-30 | 内蒙古超牌新材料股份有限公司 | Preparation method of molecular sieve, low-nitrogen-adsorption hollow glass drying agent and preparation method thereof |
| CN113526535A (en) * | 2021-09-07 | 2021-10-22 | 淄博鹏丰新材料科技有限公司 | Method for producing aluminum hydroxide micropowder at high concentration, high temperature and micro-positive pressure |
| CN114180604A (en) * | 2020-12-11 | 2022-03-15 | 安徽金禾实业股份有限公司 | Comprehensive utilization method of waste residues in spice production and synthetic ammonia purge gas |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111217384A (en) * | 2020-02-24 | 2020-06-02 | 中南大学 | Method for removing organic matters in sodium aluminate solution by foam separation |
| CN112194160A (en) * | 2020-09-30 | 2021-01-08 | 洛阳中超新材料股份有限公司 | Method for decoloring sodium aluminate solution for superfine aluminum hydroxide |
| CN114180604A (en) * | 2020-12-11 | 2022-03-15 | 安徽金禾实业股份有限公司 | Comprehensive utilization method of waste residues in spice production and synthetic ammonia purge gas |
| CN113184873A (en) * | 2021-04-23 | 2021-07-30 | 内蒙古超牌新材料股份有限公司 | Preparation method of molecular sieve, low-nitrogen-adsorption hollow glass drying agent and preparation method thereof |
| CN113184873B (en) * | 2021-04-23 | 2022-12-02 | 内蒙古超牌新材料股份有限公司 | Preparation method of molecular sieve, low-nitrogen-adsorption hollow glass drying agent and preparation method thereof |
| CN113526535A (en) * | 2021-09-07 | 2021-10-22 | 淄博鹏丰新材料科技有限公司 | Method for producing aluminum hydroxide micropowder at high concentration, high temperature and micro-positive pressure |
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