CN102249254A - Method for preparing water glass and coproduct of sodium metasilicate nonahydrate with acid hydrolyzed alum sludge filter cake - Google Patents
Method for preparing water glass and coproduct of sodium metasilicate nonahydrate with acid hydrolyzed alum sludge filter cake Download PDFInfo
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- CN102249254A CN102249254A CN 201010598180 CN201010598180A CN102249254A CN 102249254 A CN102249254 A CN 102249254A CN 201010598180 CN201010598180 CN 201010598180 CN 201010598180 A CN201010598180 A CN 201010598180A CN 102249254 A CN102249254 A CN 102249254A
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Abstract
Belonging to the technical field of inorganic chemical "three wastes" treatment and comprehensive utilization, the invention specifically relates to a method for preparing water glass and a coproduct of sodium metasilicate nonahydrate with an acid hydrolyzed alum sludge filter cake. The method mainly comprises the steps of: hydrolyzing alum sludge fully with water, putting a filtered filter cake into a corrosion reactor for reacting with hydrochloric acid, reacting the filtrate from another filtration with sodium hydroxide, conducting one more filtration so as to obtain water glass which can be furthered processed to generate sodium metasilicate nonahydrate. With the invention, waste residues can be swallowed cleanly, and the environmental pollution of waste residues can be mitigated. Besides, valuable water glass and sodium metasilicate nonahydrate products can be prepared. With remarkable social benefit and economic benefit, the method of the invention has simple process and production equipment, thus being a practical treatment and utilization method.
Description
Technical field
The present invention relates to make the improvement and the comprehensive utilization technique field of the alum pulp waste that alum produces, particularly a kind ofly separate the method that filter cake prepares water glass coproduction non-hydrate sodium metasilicate with the alum mud acid.
Technical background
Alum claims potassium aluminium alum, arcanite and potassium alum again, and chemical formula is K
2SO
4Al
2(SO
4)
324H
2O or KAl (SO
4)
224H
2O.Alum is to contain the potassium magnesium sulfate of crystal water and the double salt of Tai-Ace S 150, and colourless octahedral crystal has sour and astringent taste; Density is 1.75, fusing point 92 degree; Soluble in water, when it is water-soluble, play hydrolysis reaction and generate the gluey precipitation of aluminium hydroxide; When it is heated, lose crystal water and form white powder abbreviation exsiccated alum.
Alum is widely used in industries such as chemical industry, food, daily use chemicals, water treatment, and China's alunite mineral products are abundant, and the alum ore deposit that economize in Zhejiang, Anhui etc. is well known.The alum ore can be obtained alum crystal after dipping, crystallization, the drying after calcining.But the production process of alum is discharged a large amount of alum slags (alum mud and alum slurry), and air storage throughout the year causes sour water loss contaminate environment.Therefore, the comprehensive utilization of alum mud and alum slurry has become alum industry urgent problem.
The alum slurry is the slurries of discharging when making alum, also is the bigger contaminating enterprises of three waste discharge in the inorganic chemical industry.Alum mud major ingredients and alum slurry produce few, mainly contain dioxide-containing silica 22.48%, ferric oxide content is that 2.29% aluminium sesquioxide content is 43.03%, and calcium oxide content is 2.97%, potassium oxide content is 4.44%, and sulfur trioxide content is 15.52%; Want not have secondary pollution must comprehensively utilize these compounds fully, even to divide independent several times technical process to handle and to fall the whole digestion of these materials, though a lot of enterprises of going together handle the improvement and the utilization of alum slurry, have occurred the phenomenon of secondary pollution after handling again.Administer and utilize the product category that processes of low grade again less, have a lot of elements and compound all not to take out; And all go up the independent several times technical process of branch basically and could fall the whole digestion of these materials; Alum mud acid also of no use is separated the relevant report that filter cake prepares the method for water glass coproduction non-hydrate sodium metasilicate at present.
Summary of the invention
The invention provides and a kind ofly separate the method that filter cake prepares water glass coproduction non-hydrate sodium metasilicate with the alum mud acid, this method not only technology is simple, and can also make multiple value product when can effectively handle waste residue.
To achieve the above object, technical scheme of the present invention is:
A kind ofly separate the method that filter cake prepares water glass coproduction non-hydrate sodium metasilicate, comprise being prepared as follows step with the alum mud acid:
Steps A, alum slurry is packed in first corrosion-resistant reactor, add 1～3 times of water and fully stir, hydrolysis reaction obtains compounding substances I;
Step B, gained compounding substances I in the steps A is filtered with first strainer;
Step C, send in second corrosion-resistant reactor with the pure mass ratio of converting 1: 0.74～1.14 with hydrochloric acid, under stirring slowly, carrying out deferred reaction, the compounding substances II of reaction generation aluminum chloride, calcium chloride and silicon-dioxide filtering the gained filter cake among the step B;
Step D, gained compounding substances II among the step C is filtered with second strainer; The deep processing separately of the aluminum chloride that obtains, calcium chloride;
Step e, send in the 3rd corrosion-resistant reactor stirring that under the condition of pressurization of heating, blows slowly, reaction generation water glass mixed solution I II with the pure mass ratio of converting 1: 1.11～1.51 with sodium hydroxide with filtering the gained silica filter cake among the step D;
Step F, gained water glass mixed solution I II in the step e is carried out heat with the 3rd strainer consider, heat filters that temperature is 1100 ± 2 ℃ in the journey; Obtain the water glass product after removing impurity;
Step G, gained filtrate water glass in the step F is sent into the underpressure distillation device carry out underpressure distillation, when the solution water content reaches nine crystal water, discharge the back with water cooler, washing and spin-drying machine, moisture eliminator, pulverizer cool off, washing dries, checking the weight after drying and the pulverizing is packaged to be the non-hydrate sodium metasilicate crystal product.
Preferably, the temperature in the described step e in the 3rd corrosion-resistant reactor is 1500 ℃～2000 ℃, and pressure is 1000KPa～1500KPa.
Preferably, employed hydrochloric acid is that concentration of volume percent is 30%～60% hydrochloric acid soln among the described step C.
Preferably, employed sodium hydroxide is that concentration of volume percent is 30%～40% sodium hydroxide solution in the described step e.
Reaction principle of the present invention is:
SO
3+H
2O＝＝＝＝H
2SO
4
SiO
2+2NaOH+9H
2O＝＝＝＝Na
2SiO
3·9H
2O+H
2
Because aluminum oxide some a-Al in calcination process in the alum mud
2O
3And β-Al
2O
3Generate, this nonactive aluminium is difficult to dissolution with solvents and carries out wet processes.We propose to adopt aluminium and silicon in the acid pasting separation alum mud by experiment, the complex process and the low deficiency of aluminium recovery of the desiliconization of alkaline leaching technology have not only been overcome, and having solved in the pickling process technology the low and demanding problem of equipment material of product purity, pickling process that more outstanding is can the product of coproduction more than three kinds; Accomplish to eat to do and press warp, ensure the generation that does not have secondary pollution.
The present invention carries out abundant hydrolysis with alum mud water, etching reactor sent into by filter cake after the filtration and hydrochloric acid reacts, filtering once more filtrate and sodium hydroxide react, and filter once more and obtain water glass, and water glass further processing obtains non-hydrate sodium metasilicate; The present invention can as clean as a pennyly gulp down waste residue, alleviates the pollution of waste residue to environment; Can make valuable water glass coproduction non-hydrate sodium metasilicate product again, not only have remarkable social benefit and economic benefit, and technology and production unit are simple, be a kind of relatively actual processing and utilize method; The present invention studies invention in line with a such aim, and alum mud is divided into three decomposes digestibility and utilization, the one, by hydrolysis water miscible material is extracted as liquid phase and to administer; The 2nd, the filter cake after the water-soluble extraction is carried out sour molten extraction administer as solid phase; The 3rd, the waste residue after the sour molten extraction is re-used as the solid phase processing and utilizing.
Description of drawings
Fig. 1 separates the process flow sheet that filter cake prepares the method for water glass coproduction non-hydrate sodium metasilicate with the alum mud acid;
Wherein:
1-first corrosion-resistant reactor, 2-first strainer, 3-second corrosion-resistant reactor, 4-second strainer, 5-the 3rd corrosion-resistant reactor, 6-the 3rd strainer, 7-water glass product, 8-underpressure distillation device, the 9-water cooler, 10-washing and spin-drying machine, 11-moisture eliminator, the 12-pulverizer, 13-non-hydrate sodium metasilicate crystal product.
Concrete embodiment
Embodiment 1
A kind ofly separate the method that filter cake prepares water glass coproduction non-hydrate sodium metasilicate, comprise being prepared as follows step with the alum mud acid:
Steps A, alum is starched pack into 1 li of first corrosion-resistant reactor of 1000Kg, add 1～3 times of water and fully stir, hydrolysis reaction obtains compounding substances I; Wherein calculate by pure 155.2Kg sulphur trioxide, 224.8Kg silicon-dioxide in the alum slurry;
Step B, gained compounding substances I in the steps A is filtered with first strainer 2;
Step C, send into 3 li of second corrosion-resistant reactors with hydrochloric acid at 1: 0.74 with the pure mass ratio of converting, under stirring slowly, carrying out deferred reaction, the compounding substances II of reaction generation aluminum chloride, calcium chloride and silicon-dioxide filtering the gained filter cake among the step B;
Step D, gained compounding substances II among the step C is filtered with second strainer 4; The deep processing separately of the aluminum chloride that obtains, calcium chloride;
Step e, send into 5 li of the 3rd corrosion-resistant reactors at 1: 1.11 with the pure mass ratio of converting with filtering gained silica filter cake and sodium hydroxide among the step D, the stirring that under the condition of pressurization of heating, blows slowly, reaction generates water glass mixed solution I II, wherein temperature is 1500 ℃, pressure is 1000KPa, and wherein sodium hydroxide is that concentration of volume percent is 30% sodium hydroxide solution;
Step F, gained mixed solution I II in the step e is carried out heat with the 3rd strainer 6 consider, heat filters that temperature is 1100 ± 2 ℃ in the journey; Obtain 380.72Kg water glass product 7 after removing impurity;
Step G, gained filtrate water glass in the step F is sent into underpressure distillation device 8 carry out underpressure distillation, when the solution water content reaches nine crystal water, discharge the back and cool off, wash to check the weight after drying, drying and the pulverizing with water cooler 9, washing and spin-drying machine 10, moisture eliminator 11, pulverizer 12 and be packaged to be 886.14Kg non-hydrate sodium metasilicate crystal product 13.
Embodiment 2
A kind ofly separate the method that filter cake prepares water glass coproduction non-hydrate sodium metasilicate, comprise being prepared as follows step with the alum mud acid:
Steps A, alum is starched pack into 1 li of first corrosion-resistant reactor of 1000Kg, add 1～3 times of water and fully stir, hydrolysis reaction obtains compounding substances I; Wherein calculate by pure 155.2Kg sulphur trioxide, 224.8Kg silicon-dioxide in the alum slurry;
Step B, gained compounding substances I in the steps A is filtered with first strainer 2;
Step C, send into 3 li of second corrosion-resistant reactors with hydrochloric acid at 1: 0.94 with the pure mass ratio of converting, under stirring slowly, carrying out deferred reaction, the compounding substances II of reaction generation aluminum chloride, calcium chloride and silicon-dioxide filtering the gained filter cake among the step B;
Step D, gained compounding substances II among the step C is filtered with second strainer 4; The deep processing separately of the aluminum chloride that obtains, calcium chloride;
Step e, send into 5 li of the 3rd corrosion-resistant reactors at 1: 1.31 with the pure mass ratio of converting with filtering gained silica filter cake and sodium hydroxide among the step D, the stirring that under the condition of pressurization of heating, blows slowly, reaction generates water glass mixed solution I II, wherein temperature is 1800 ℃, pressure is 1400KPa, and wherein sodium hydroxide is that concentration of volume percent is 38% sodium hydroxide solution;
Step F, gained water glass mixed solution I II in the step e is carried out heat with the 3rd strainer 6 consider, heat filters that temperature is 1100 ± 2 ℃ in the journey; Obtain 449.32Kg water glass product 7 after removing impurity;
Step G, gained filtrate water glass in the step F is sent into underpressure distillation device 8 carry out underpressure distillation, when the solution water content reaches nine crystal water, discharge the back and cool off, wash to check the weight after drying, drying and the pulverizing with water cooler 9, washing and spin-drying machine 10, moisture eliminator 11, pulverizer 12 and be packaged to be 1045.82Kg non-hydrate sodium metasilicate crystal product 13.
A kind ofly separate the method that filter cake prepares water glass coproduction non-hydrate sodium metasilicate, comprise being prepared as follows step with the alum mud acid:
Steps A, alum is starched pack into 1 li of first corrosion-resistant reactor of 1000Kg, add 1～3 times of water and fully stir, hydrolysis reaction obtains compounding substances I; Wherein calculate by pure 155.2Kg sulphur trioxide, 224.8Kg silicon-dioxide in the alum slurry;
Step B, gained compounding substances I in the steps A is filtered with first strainer 2;
Step C, send into 3 li of second corrosion-resistant reactors with hydrochloric acid at 1: 1.14 with the pure mass ratio of converting, under stirring slowly, carrying out deferred reaction, the compounding substances II of reaction generation aluminum chloride, calcium chloride and silicon-dioxide filtering the gained filter cake among the step B;
Step D, gained compounding substances II among the step C is filtered with second strainer 4; The deep processing separately of the aluminum chloride that obtains, calcium chloride;
Step e, send into 5 li of the 3rd corrosion-resistant reactors at 1: 1.51 with the pure mass ratio of converting with filtering gained silica filter cake and sodium hydroxide among the step D, the stirring that under the condition of pressurization of heating, blows slowly, reaction generates water glass mixed solution I II, wherein temperature is 2000 ℃, pressure is 1500KPa, and wherein sodium hydroxide is that concentration of volume percent is 40% sodium hydroxide solution;
Step F, gained water glass mixed solution I II in the step e is carried out heat with the 3rd strainer 6 consider, heat filters that temperature is 1100 ± 2 ℃ in the journey; Obtain 517.92Kg water glass product 7 after removing impurity;
Step G, gained filtrate water glass in the step F is sent into underpressure distillation device 8 carry out underpressure distillation, when the solution water content reaches nine crystal water, discharge the back and cool off, wash to check the weight after drying, drying and the pulverizing with water cooler 9, washing and spin-drying machine 10, moisture eliminator 11, pulverizer 12 and be packaged to be 1205.47Kg non-hydrate sodium metasilicate crystal product 13.
The foregoing description is preferred embodiment of the present invention, is not to be used for limiting the scope of the present invention, so all equivalences of being done with described feature of claim of the present invention and principle change or modify, all should be included within the claim scope of the present invention.
Claims (4)
1. separate the method that filter cake prepares water glass coproduction non-hydrate sodium metasilicate with the alum mud acid for one kind, it is characterized in that, comprise being prepared as follows step:
Steps A, with alum slurry first corrosion-resistant reactor (1) lining of packing into, add 1～3 times of water and fully stir, hydrolysis reaction obtains compounding substances I;
Step B, gained compounding substances I in the steps A is filtered with first strainer (2);
Step C, send into second corrosion-resistant reactor (3) lining with the pure mass ratio of converting 1: 0.74～1.14 with filtering gained filter cake and hydrochloric acid among the step B, carry out deferred reaction under stirring slowly, reaction generates the compounding substances II of aluminum chloride, calcium chloride and silicon-dioxide;
Step D, gained compounding substances II among the step C is filtered with second strainer (4); The deep processing separately of the aluminum chloride that obtains, calcium chloride;
Step e, send into the 3rd corrosion-resistant reactor (5) lining with the pure mass ratio of converting 1: 1.11～1.51 with filtering gained silica filter cake and sodium hydroxide among the step D, the stirring that blows slowly under the condition of pressurization of heating, reaction generate water glass mixed solution I II;
Step F, gained water glass mixed solution I II in the step e is carried out heat with the 3rd strainer (6) consider, heat filters that temperature is 1100 ± 2 ℃ in the journey; Obtain water glass product (7) after removing impurity;
Step G, gained filtrate water glass in the step F is sent into underpressure distillation device (8) carry out underpressure distillation, when the solution water content reaches nine crystal water, discharge the back and cool off, wash to check the weight after drying, drying and the pulverizing with water cooler (9), washing and spin-drying machine (10), moisture eliminator (11), pulverizer (12) and be packaged to be non-hydrate sodium metasilicate crystal product (13).
2. separate the method that filter cake prepares water glass coproduction non-hydrate sodium metasilicate according to claim 1 is described with the alum mud acid, it is characterized in that, the temperature in the described step e in the 3rd corrosion-resistant reactor (5) is 1500 ℃～2000 ℃, and pressure is 1000KPa～1500KPa.
3. separate the method that filter cake prepares water glass coproduction non-hydrate sodium metasilicate according to claim 1 is described with the alum mud acid, it is characterized in that, employed hydrochloric acid is that concentration of volume percent is 30%～60% hydrochloric acid soln among the described step C.
4. separate the method that filter cake prepares water glass coproduction non-hydrate sodium metasilicate according to claim 1 is described with the alum mud acid, it is characterized in that, employed sodium hydroxide is that concentration of volume percent is 30%～40% sodium hydroxide solution in the described step e.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001039710A (en) * | 1999-07-23 | 2001-02-13 | Nippon Paper Industries Co Ltd | Production of aluminum-based chemical and silica-based chemical from coal ash |
| RU2285665C1 (en) * | 2005-01-11 | 2006-10-20 | Открытое акционерное общество "Асбестовский магниевый завод" (ОАО "АМЗ") | Method of production of the liquid glass |
| CN101234763A (en) * | 2008-02-18 | 2008-08-06 | 周华明 | Method for preparing sodium silicate and sodium metasilicate from white residue |
| CN101296865A (en) * | 2005-11-10 | 2008-10-29 | 科学与工业研究委员会 | Process for the preparation of sodium silicate from kimberlite tailing |
| CN101428837A (en) * | 2008-11-19 | 2009-05-13 | 王声如 | Method for joint production of potash alum or ammonium alum and polyaluminium chloride |
| CN101863505A (en) * | 2010-02-11 | 2010-10-20 | 汪晋强 | Method for preparing calcium chloride to coproduce water glass by utilizing yellow phosphorus slag |
-
2010
- 2010-12-21 CN CN 201010598180 patent/CN102249254A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001039710A (en) * | 1999-07-23 | 2001-02-13 | Nippon Paper Industries Co Ltd | Production of aluminum-based chemical and silica-based chemical from coal ash |
| RU2285665C1 (en) * | 2005-01-11 | 2006-10-20 | Открытое акционерное общество "Асбестовский магниевый завод" (ОАО "АМЗ") | Method of production of the liquid glass |
| CN101296865A (en) * | 2005-11-10 | 2008-10-29 | 科学与工业研究委员会 | Process for the preparation of sodium silicate from kimberlite tailing |
| CN101234763A (en) * | 2008-02-18 | 2008-08-06 | 周华明 | Method for preparing sodium silicate and sodium metasilicate from white residue |
| CN101428837A (en) * | 2008-11-19 | 2009-05-13 | 王声如 | Method for joint production of potash alum or ammonium alum and polyaluminium chloride |
| CN101863505A (en) * | 2010-02-11 | 2010-10-20 | 汪晋强 | Method for preparing calcium chloride to coproduce water glass by utilizing yellow phosphorus slag |
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Application publication date: 20111123 |