CN102424394A - Process for preparing water glass from silicon micropowder by using wet method - Google Patents
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- CN102424394A CN102424394A CN2011102685565A CN201110268556A CN102424394A CN 102424394 A CN102424394 A CN 102424394A CN 2011102685565 A CN2011102685565 A CN 2011102685565A CN 201110268556 A CN201110268556 A CN 201110268556A CN 102424394 A CN102424394 A CN 102424394A
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Abstract
The invention provides a process for preparing water glass from silicon micropowder by using the wet method, belonging to the technical field of production of water glass. The process comprises the following steps: analyzing the content of SiO2 in silicon micropowder; mixing silicon micropowder and liquid alkali according to a mol ratio of 0.9-1.8:1; delivering obtained mixed liquor into a liquid phase reaction vessel under agitation; allowing steam to enter into the reaction vessel to heat the mixed liquor; carrying out a dwell reaction at a temperature of 70 to 220 DEG C for 0.5 to 6 h so as to prepare mixed liquor of water glass; discharging the mixed liquor of water glass out from the reaction vessel; adjusting the temperature of the mixed liquor of water glass to 50 to 95 DEG C in a feed liquid buffer tank; carrying out plate and frame pressurized filtering to obtain a filtrate which is water glass with a modulus of 1.80 to 3.20. The invention has the following advantages: since the water glass is prepared by using dust in the ferrosilicon alloy industry as a raw material and employing the characteristic that the reaction between amorphous SiO2 in silicon micropowder and alkali liquid has high activity, high conversion efficiency is obtained, the process is simple, the problem of dust pollution in the ferrosilicon alloy industry is overcome, and good economic benefits and social benefits are achieved.
Description
Technical field
The invention belongs to the water glass production technical field.Be particularly related to a kind of method of utilizing the SILICA FUME wet method to prepare water glass.
Background technology
SILICA FUME is in ferro-silicon and the industrial silicon production process, the siliceous industrial dust that SiO that in ore-smelting furnace, produces and Si gas are formed by the rapid oxidation of air and condensation.SILICA FUME belongs to pellet (PM10), directly gets into lung after SILICA FUME is absorbed by the body, and is very harmful to the person.In recent years, along with the reinforcement of country to the environmental protection dynamics, the environmental protection dust removal installation is installed by dictate ferro-silicon and industrial silicon manufacturing enterprise, and the SILICA FUME output that ferro-silicon enterprise reclaims constantly increases.
SiO
2Content is used for concrete material between 88～92% SILICA FUME, has good anti-corrosion, insulativity, wear resistance, impervious anti-freezing property; SiO
2Content greater than 92% can be used as organic cpds such as refractory materials, rubber, resin packing material; And work as SiO
2Content is lower than 88% o'clock SILICA FUME does not almost have market.At present, the application of domestic SILICA FUME is very limited.Patent CN201010170951.5 discloses the application of a kind of active silica fume as rubber, engineering plastic additive WHITE CARBON BLACK; But because the influence of colourity and impurity, SILICA FUME has significant limitation in the use of rubber, engineering plastics.Patent CN200810115333.3 also discloses and has a kind ofly prepared the method for titanium white material with SILICA FUME, through with being prepared into the titanium dioxide composite material with nucleocapsid structure characteristic at its surperficial cladding titanium dioxide after SILICA FUME activation, removal of impurities, dispersion, the adjustment sheet surface charge; But this process method is complicated, the TiO of surface coating layer in the composite particles
2Structure be difficult to control.
SiO in the SILICA FUME
2Have typical non-crystalline state characteristic, content generally can reach 69.3% (wt)～93.5% (wt).Non-crystalline state SiO
2The more, SILICA FUME is active bigger, and response capacity is stronger in basic soln.Therefore, be ferro-silicon industrial dust higher value application and the effective ways that reduce the dust secondary pollution with the SILICA FUME for the feedstock production soluble glass of high modulus.
Water glass is a kind of purposes inorganic chemical product very widely.The working method of water glass is divided into two kinds of dry method and wet methods, and wherein dry method is with the frit reaction preparation in the stove of melting at 1400～1500 ℃ of silica sand and yellow soda ash or sodium sulfate.Be characterized in to prepare as required the water glass product of different moduluses, but power consumption is bigger.Wet method is to be 140～160 ℃ with sodium hydroxide solution and silica sand in temperature, and pressure is that reaction is produced under 0.37～0.63MPa condition.Though energy consumption is lower than dry method, crystal habit SiO in the silica sand
2Dissolution rate is low, alkaline consumption is high.
For making full use of resource, reducing production costs, many researchs just are being devoted to develop the new technology that different silicon sources produces water glass.Patent CN201010176401.4 discloses a kind of with rice hull ash and yellow soda ash mixing, the method for burning solid water glass under 900 ℃ temperature; Patent CN200910072958.0 also discloses and has a kind ofly utilized rice hull ash and alkali reaction after the power plant burning to generate sodium silicate solution or colloidal sol, and insolubles makes the method for activated carbon product through acidification; Patent CN200810132277.4 discloses a kind of with the active silica in the white liquor leaching industrial flyash, dissolves the method for the sodium silicate solution of preparation high-module through silicic acid and low modulus water glass; Patent CN200610017165.5 discloses and a kind of coal gangue has been generated alum liquor with the sulfuric acid reaction of concentration 40～60% in reaction kettle, and the silicon-dioxide filter residue reacts the method that makes liquid sodium silicate with liquid caustic soda.It is main raw material with the coal series kaolin rock that CN200410058137.9 also discloses a kind of, and through acidleach, sour molten slag alkali dissolves the method for producing Poly aluminum Chloride (PAC) and high-module liquid sodium silicate; Patent CN200910154795.0 discloses a kind of aluminium scrap ash and Na of utilizing
2CO
3The method for preparing crystal aluminum chloride and water glass through the high temperature solid-state thermolysis; Patent CN201010230406.0 discloses a kind of method of utilizing organosilicon or polysilicon industry preparing water glass from byproduct silicon tetrachloride; Patent CN200910102418.2 discloses a kind of method of utilizing the silica containing fluorine of phosphate fertilizer industrial by-product for the feedstock production water glass; Patent CN200580051917.3 also discloses a kind of method that is used for preparing from the kimberlite ore deposit that diamond mining produces as solid waste water glass.
Summary of the invention
The object of the present invention is to provide a kind of method of utilizing the SILICA FUME wet method to prepare water glass.Solved the large technology barrier of dissolving with higher value application of ferro-silicon industrial dust, for the higher value application of ferro-silicon or Pure Silicon Metal manufacture dust provides simple and effective new way.
In order to solve the problems of the technologies described above, concrete technological step is following:
1, analyzes SiO in the supplied materials SILICA FUME
2Content
SILICA FUME is that silicon is the flue dust that iron alloy (like Pure Silicon Metal, ferro-silicon, silicomanganese etc.) industrial furnace produces, through the silica soot that contains of cleaning apparatus collection.SiO wherein
2: the SILICA FUME of 69.3～93.5% (wt) can be used as raw material.Other chemical compositions have following scope: Al
2O
3: 0.35～0.38% (wt); Fe
2O
3: 0.40～4.80% (wt); CaO:0.17～1.20% (wt); MgO:0.4～5.19% (wt); C:0.46～0.52% (wt); K
2O:1.01～7.97% (wt); Na
2O:0.22～1.52% (wt); Loss on ignition: 2.18～4.61% (wt).
To meet SiO
2: 69.3～93.5% (wt), preferable range is that the SILICA FUME of 83～93.5% (wt) is made raw material, is that the alkali lye of 30-50% (wt) mixes mutually with SILICA FUME and naoh concentration, wherein SiO
2: the NaOH mol ratio is controlled to be 0.90～1.80: 1, and preferable range is 1.20～1.60: 1.
2, under whipped state, the step is gathered 1 mixed solution that makes with being pumped in the liquid phase reaction still of opening stirring, feed the water vapor direct heating in the reaction kettle.Reactor temperature is controlled at 70～220 ℃, and preferable range is 152～170 ℃, reacts to make the water glass mixed solution after 0.5～6 hour.
3, step 2 gained water glass mixed solution is discharged reaction kettle, get in the feed liquid surge tank.In the feed liquid surge tank, add water and regulate water glass mixeding liquid temperature to 50～95 ℃, through sheet frame pressure filtration, it is 1.80～3.20 water glass that gained filtrating is modulus.
The invention has the advantages that:
The SILICA FUME of collecting with ferro-silicon industry is a raw material, makes full use of non-crystalline state SiO in the SILICA FUME
2Prepare water glass with the active high characteristics of alkaline reaction, technical process is simple, workable, has solved the large technology barrier of dissolving with higher value application of ferro-silicon industrial dust.Be the recycling SILICA FUME, high-level efficiency, the high-quality water glass of low-cost preparation provide a new approach.
Embodiment
Embodiment 1:
1, take by weighing SILICA FUME 120kg and place in the dosing vessel, analyze SiO
2Content is 83.3% (wt).Adding naoh concentration is 50% (wt) alkali lye, with mixed solution SiO
2: the NaOH mol ratio was modulated into 1.30: 1.
2, the mixed solution that under whipped state, step 1 is made feeds the water vapor direct heating with being pumped in the liquid phase reaction still of opening stirring in the reaction kettle., the still internal pressure stops steam supply when reaching 0.6MPa; The still internal pressure keeps 0.6MPa, and temperature is controlled to be 158 ℃, and the pressurize reaction made the water glass mixed solution in 3 hours.
3, reaction kettle is depressurized to 0.3MPa, and step 2 gained water glass mixed solution is discharged reaction kettle through overbottom pressure, gets in the feed liquid surge tank.In the feed liquid surge tank, add water and regulate water glass mixeding liquid temperature to 90 ℃, through sheet frame pressure filtration, gained filtrating is water glass.Through the silicon molybdenum blue spectrophotometric analysis, SiO in the water glass
2Content is 9.30% (wt), and modulus is 2.50, SiO in the SILICA FUME
2Transformation efficiency be 78.3%.
Embodiment 2:
1, take by weighing SILICA FUME 160kg and place in the dosing vessel, analyze SiO
2Content is 78.2% (wt).Adding naoh concentration is 50% (wt) alkali lye, with mixed solution SiO
2: the NaOH mol ratio was modulated into 1.80: 1.
2, the mixed solution that under whipped state, step 1 is made feeds the water vapor direct heating with being pumped in the liquid phase reaction still of opening stirring in the reaction kettle.The control temperature in the kettle reaches 70 ℃, reacts to make the water glass mixed solution in 6 hours.
3, step 2 gained water glass mixed solution is discharged reaction kettle, get in the feed liquid surge tank.In the feed liquid surge tank, add water and regulate water glass mixeding liquid temperature to 50 ℃, through sheet frame pressure filtration, gained filtrating is water glass.Through the silicon molybdenum blue spectrophotometric analysis, SiO in the water glass
2Content is 8.60% (wt), and modulus is 3.2, SiO in the SILICA FUME
2Transformation efficiency be 67.4%.
Embodiment 3:
1, take by weighing SILICA FUME 160kg and place in the dosing vessel, analyze SiO
2Content is 92.2% (wt).Adding naoh concentration is 30% (wt) alkali lye, with mixed solution SiO
2: the NaOH mol ratio was modulated into 1.40: 1.
2, the mixed solution that under whipped state, step 1 is made feeds the water vapor direct heating with being pumped in the liquid phase reaction still of opening stirring in the reaction kettle., the still internal pressure stops steam supply when reaching 0.8MPa; The still internal pressure keeps 0.8MPa, and temperature is controlled to be 170 ℃, and the pressurize reaction made the water glass mixed solution in 3 hours.
3, reaction kettle is depressurized to 0.15MPa, and step 2 gained water glass mixed solution is discharged reaction kettle through overbottom pressure, gets in the feed liquid surge tank.In the feed liquid surge tank, add water and regulate water glass mixeding liquid temperature to 80 ℃, through sheet frame pressure filtration, gained filtrating is water glass.Through the silicon molybdenum blue spectrophotometric analysis, SiO in the water glass
2Content is 12.80% (wt), and modulus is 2.7, SiO in the SILICA FUME
2Transformation efficiency be 84.6%.
Embodiment 4:
1, take by weighing SILICA FUME 120kg and place in the dosing vessel, analyze SiO
2Content is 83.3% (wt).Adding naoh concentration is 40% (wt) alkali lye, with mixed solution SiO
2: the NaOH mol ratio was modulated into 1.60: 1.
2, the mixed solution that under whipped state, step 1 is made feeds the water vapor direct heating with being pumped in the liquid phase reaction still of opening stirring in the reaction kettle., the still internal pressure stops steam supply when reaching 0.6MPa; The still internal pressure keeps 0.6MPa, and temperature is controlled to be 158 ℃, and the pressurize reaction made the water glass mixed solution in 0.5 hour.
3, reaction kettle is depressurized to 0.20MPa, and step 2 gained water glass mixed solution is discharged reaction kettle through overbottom pressure, gets in the feed liquid surge tank.In the feed liquid surge tank, add water and regulate water glass mixeding liquid temperature to 80 ℃, through sheet frame pressure filtration, gained filtrating is water glass.Through the silicon molybdenum blue spectrophotometric analysis, SiO in the water glass
2Content is 11.60% (wt), and modulus is 3.1, SiO in the SILICA FUME
2Transformation efficiency be 80.4%.
Embodiment 5:
1, take by weighing SILICA FUME 120kg and place in the dosing vessel, analyze SiO
2Content is 92.2% (wt).Adding naoh concentration is 40% (wt) alkali lye, with mixed solution SiO
2: the NaOH mol ratio was modulated into 0.95: 1.Mixed solution feeds water vapor direct heating to 90 ℃.
2, the mixed solution that under whipped state, step 1 is made feeds the water vapor direct heating with being pumped in the liquid phase reaction still of opening stirring in the reaction kettle., the still internal pressure stops steam supply when reaching 0.8MPa.The still internal pressure keeps 0.8MPa, and temperature is controlled to be 170 ℃, and the pressurize reaction made the water glass mixed solution in 1 hour.
3, reaction kettle is depressurized to 0.25MPa, and step 2 gained water glass mixed solution is discharged reaction kettle through overbottom pressure, gets in the feed liquid surge tank.In the feed liquid surge tank, add water and regulate water glass mixeding liquid temperature to 50 ℃, through sheet frame pressure filtration, gained filtrating is water glass.Through the silicon molybdenum blue spectrophotometric analysis, SiO in the water glass
2Content is 5.60% (wt), and modulus is 1.82, SiO in the SILICA FUME
2Transformation efficiency be 90.9%.
Embodiment 6:
1, take by weighing SILICA FUME 120kg and place in the dosing vessel, analyze SiO
2Content is 92.2% (wt).Adding naoh concentration is 40% (wt) alkali lye, with mixed solution SiO
2: the NaOH mol ratio was modulated into 1.30: 1.Mixed solution feeds water vapor direct heating to 70 ℃.
2, the mixed solution that under whipped state, step 1 is made feeds the water vapor direct heating with being pumped in the liquid phase reaction still of opening stirring in the reaction kettle., the still internal pressure stops steam supply when reaching 2.4Mpa; The still internal pressure keeps 2.5MPa, and temperature is controlled to be 220 ℃, and the pressurize reaction made the water glass mixed solution in 3 hours.
3, reaction kettle is depressurized to 0.3MPa, and step 2 gained water glass mixed solution is discharged reaction kettle through overbottom pressure, gets in the feed liquid surge tank.In the feed liquid surge tank, add water and regulate water glass mixeding liquid temperature to 90 ℃, through sheet frame pressure filtration, gained filtrating is water glass.Through the silicon molybdenum blue spectrophotometric analysis, SiO in the water glass
2Content is 12.20% (wt), and modulus is 2.50, SiO in the SILICA FUME
2Transformation efficiency be 94.3%.
Claims (5)
1. a method of utilizing the SILICA FUME wet method to prepare water glass is characterized in that, process step is:
(1) analyzes SiO in the SILICA FUME raw material
2Content, will meet SiO
2: the SILICA FUME of 69.3～93.5wt% is made raw material, is that the alkali lye of 30-50wt% mixes mutually with SILICA FUME and naoh concentration, wherein SiO
2: the NaOH mol ratio is controlled to be 0.90～1.80: 1;
(2) under whipped state, gathered mixed solution that (1) make the step with being pumped in the liquid phase reaction still of opening stirring, feed the water vapor direct heating in the reaction kettle, make the water glass mixed solution after 0.5～6 hour in pressurize reaction under 70～220 ℃ of conditions of temperature;
(3) step (2) gained water glass mixed solution is discharged reaction kettle, get in the feed liquid surge tank, in the feed liquid surge tank, add water and regulate water glass mixeding liquid temperature to 50～95 ℃, through sheet frame pressure filtration, it is 1.80～3.20 water glass that gained filtrating promptly gets modulus.
2. method according to claim 1 is characterized in that, said SILICA FUME is that silicon is the flue dust that the ferroalloy industry electric furnace produces, through the silica soot that contains of cleaning apparatus collection.
3. method according to claim 2 is characterized in that SiO
2Content is 83～93.5wt%.
4. method according to claim 1 is characterized in that, SiO in step (1) SILICA FUME and the alkali lye premix
2: the NaOH mol ratio is 1.20～1.60: 1.
5. method according to claim 1 is characterized in that, the reactor temperature span of control is 152～170 ℃ in the step (2).
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| CN103910362A (en) * | 2014-04-29 | 2014-07-09 | 深圳市国大长兴科技有限公司 | Method for preparing silicate aqueous solution by utilizing silicon-containing tailing powder |
| CN103950911A (en) * | 2014-05-06 | 2014-07-30 | 云南磷化集团有限公司 | Method of preparing feed grade calcium hydrophosphate and co-producing water glass by using acid residues and yellow phosphorus slags |
| CN103964451A (en) * | 2014-04-29 | 2014-08-06 | 深圳市国大长兴科技有限公司 | Method for preparing silicate aqueous solution by using polished quartz stone waste powder |
| CN105948679A (en) * | 2016-04-29 | 2016-09-21 | 景德镇陶瓷大学 | Unburned water-permeable brick with solid wastes as base materials and preparation method thereof |
| CN106829984A (en) * | 2017-04-21 | 2017-06-13 | 江西省欧陶科技有限公司 | A kind of wet process technique of waterglass |
| CN107362910A (en) * | 2017-08-30 | 2017-11-21 | 云南磷化集团有限公司 | A kind of method that direct flotation phosphorus mine tailing prepares phosphate rock floating regulator |
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| CN112547314A (en) * | 2020-11-18 | 2021-03-26 | 云南磷化集团有限公司 | Full-quantity resource production method of siliceous and silicate refractory collophanite |
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| CN114180590A (en) * | 2022-01-29 | 2022-03-15 | 昆明道尔森科技有限公司 | Preparation method of silicate aqueous solution |
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| CN103910362A (en) * | 2014-04-29 | 2014-07-09 | 深圳市国大长兴科技有限公司 | Method for preparing silicate aqueous solution by utilizing silicon-containing tailing powder |
| CN103964451A (en) * | 2014-04-29 | 2014-08-06 | 深圳市国大长兴科技有限公司 | Method for preparing silicate aqueous solution by using polished quartz stone waste powder |
| CN103910362B (en) * | 2014-04-29 | 2016-01-13 | 深圳市国大长兴科技有限公司 | Utilize the method preparing aqueous silicate solution containing silicon tailings breeze |
| CN103964451B (en) * | 2014-04-29 | 2016-04-06 | 深圳市国大长兴科技有限公司 | The quartzite polishing powder that gives up is utilized to prepare the method for aqueous silicate solution |
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