CN101274763B - Method for preparing layered sodium disilicate by using waste white slime and alkali waste water - Google Patents
Method for preparing layered sodium disilicate by using waste white slime and alkali waste water Download PDFInfo
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- CN101274763B CN101274763B CN200710054156A CN200710054156A CN101274763B CN 101274763 B CN101274763 B CN 101274763B CN 200710054156 A CN200710054156 A CN 200710054156A CN 200710054156 A CN200710054156 A CN 200710054156A CN 101274763 B CN101274763 B CN 101274763B
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Abstract
The invention relates to a method for producing lamellar sodium disilicate by adopting waste silica slags and waste alkaline water as raw materials. The method of the invention comprises the procedures of the preparation of a sodium silicate solution, the impurity removal of solution, spraying and drying, high-temperature crystallization, crushing and packaging, and adopts the waste silica slags and the waste alkaline water produced in the production process of zirconium oxychloride as the raw materials. Zirconium slag can be recycled, which results in the reduction of the production cost; a great deal of impurities are removed during the procedure of the impurity removal of the solution and the obtained products have high purity, stable performance and good quality; meanwhile, the production technology is simple and is suitable for large-scale industrial production.
Description
Technical field
The invention belongs to chemical spent material reutilization technology field, being specifically related to a kind of is the working method of raw material production layered sodium disilicate with useless white residue and alkali waste water.
Background technology
200,000 tons of zirconium oxychlorides are produced in the whole nation per year, produce 170,000 tons of white residues, ten thousand tons of alkali waste water 350-400, and domestic treatment process mainly is at present:
1, alkali waste water: 30% is utilized, and produces Starso or papermaking, and 70% neutralizes afterwards with acid, and discharging is main.
2, white residue: impure more because of it, about 20% is utilized lower inclined to one side silicon of production added value or low-grade WHITE CARBON BLACK, and profit is lower.Mainly be the main processing means with the landfill at present, promptly contaminate environment is wasted resource again.
3, white residue and alkali waste water are produced metasilicate pentahydrate sodium with solution crystal process, and the zirconium slag is not fully utilized in this technological process, and complex process, and finished product purity is low, therefore do not form suitability for industrialized production.
Summary of the invention
The objective of the invention is to make full use of the zirconium slag in order to simplify technical process, improve finished product purity and invent a kind of be the method for raw material production layered sodium disilicate with the useless white residue and the alkali waste water that utilize the zirconium oxychloride production process to produce.
The objective of the invention is to realize like this: the present invention includes the following step:
A, usefulness are produced the Na that contains of zirconium oxychloride
2O6-10%, SiO
2The waste lye of 1%-3% with contain SiO
2The useless white residue of 15-25% is pressed certain weight ratio Na
2O:SiO
2=1:1 drops in the reaction kettle, airtight heating, and control reaction temperature is 100-150 ℃, the reaction times is 5-12 hour,
B, detection silicon sodium mol ratio: SiO
2: Na
2During O=0.95-1.05, adding concentration is that the modified cation of 0.005%-0.015% gathers the third ethernamine 0.5%-0.15%, wood charcoal powder 0.5%%-1.5% carries out physical reaction, with positive oxyhydroxide contamination precipitation polymerization absorption,
C, above reaction feed liquid is put into subsider, when temperature is reduced to 60-80 ℃, uses the plate type pressure filter press filtration, filter residue return the zirconates production system, filtrating is sodium silicate solution,
D, gained filtrating (water glass) among the C is added caustic soda carry out the mode transfer reaction with sodium silicate, concentrating and adjusting modulus is 1.9-2.1, and the control solid content is 45-60%,
F, with material among the E through 150-350 ℃ of spraying drying, indefiniteness powdery sodium disilicate,
G, F gained material is got layered sodium disilicate at 600-850 ℃ of calcined crystalline,
H, with G gained material pulverize again, sieve finished product.
Wherein drop into the SiO in the reaction kettle in the steps A
2The SiO that promptly comprises 15%-25% in the useless white residue
2Also comprise the SiO that contains 1%-3% in the waste lye
2
The detection method of silicon sodium mole ratio is following:
Sodium oxide (Na
2O) mensuration
Because Na
2SiO
3Solution is alkalescence, is indicator so use first to pour orange, with hydrochloric acid standard solution titration Na
2SO
3+ 2HCl+H
2O → H
4SiO
4+ 2NaCl calculates the percentage composition of sodium oxide according to the ml number that consumes hydrochloric acid standard solution;
Required reagent: 0.1% first is poured the orange indicator aqueous solution, 0.1N salt standard acid solution
Analytical procedure: accurately take by weighing about sample 1 gram, place the 250ml Erlenmeyer flask, add the water that 100ml just boiled postcooling and make its dissolving, add 1 ~ 2 0.1% methyl orange indicator, become orange by yellow with 0.1N hydrochloric acid standard solution titration to solution.
Calculation formula:
In the formula: the equivalent concentration of N-hydrochloric acid standard solution consumes the ml number of hydrochloric acid standard solution, G-sample weight (gram), the mg equivalent of 0.03099-sodium oxide during V-titration.
The mensuration of silicon-dioxide
Measure SiO with silicon-dioxide rapid determination appearance
2Percentage composition
The calculating of silicon sodium (apperance)
The raw material waste residue liquid of producing as the present invention is provided by useless white residue and the alkali waste water that the zirconium oxychloride production process is produced; Reduced production cost on the one hand; Also solved simultaneously the technical barrier of useless white residue and alkali waste water reacted liquid sodium silicate; Solve the difficult problem that white residue foreign matter content height is difficult for being utilized, when having reached the waste residue and liquid utilization, avoided environmental pollution.
The present invention is a raw material with useless white residue and alkali waste water, and the zirconium slag can reuse, and has reduced production cost, and product purity height, stable performance, quality better, and production technique is easy to be suitable for large-scale industrial production.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
Shown in accompanying drawing, the present invention includes airtight heating, precipitation polymerization absorption press filtration, spraying drying, high temperature crystallization, pulverizing process, concrete process is following:
With the Na that contains that produces zirconium oxychloride
2O6-10%, SiO
2The waste lye of 1%-3% with contain SiO
2The useless white residue of 15-25% is pressed certain weight ratio Na
2O:SiO
2=1:1 drops in the reaction kettle, airtight heating, and control reaction temperature is 100-150 ℃, the reaction times is 5-12 hour, detects silicon sodium mol ratio: SiO
2: Na
2During O=0.95-1.05, adding concentration is that the modified cation of 0.005%-0.015% gathers the third ethernamine 0.5%-0.15%, wood charcoal powder 0.5%%-1.5% carries out physical reaction, with positive oxyhydroxide contamination precipitation polymerization absorption; Above reaction feed liquid is put into subsider, when temperature is reduced to 60-80 ℃, use the plate type pressure filter press filtration; Get filter residue and return the zirconates production system, filtrating is sodium silicate solution, and gained water glass filtrating adding caustic soda and sodium silicate are carried out the mode transfer reaction; Concentrating the adjustment modulus is 1.9-2.1; When the control solid content is 45-60%,, get indefiniteness powdery sodium disilicate through 150-350 ℃ of spraying drying; Indefiniteness powdery sodium disilicate is got layered sodium disilicate at 600-850 ℃ of calcined crystalline, with layered sodium disilicate pulverize again, sieve finished product.
Useless white residue and waste lye reaction can be heated under 120 ℃ of-130 ℃ of temperature and produced the water glass mixing solutions in 7-10 hour, detect silicon sodium mol ratio: SiO
2: Na
2The modified cation that adds concentration during O=0.98-1.03 and be 0.008%-0.012% gathers the third ethernamine 0.8%-1.2%, wood charcoal powder 0.8%%-1.2% carries out physical reaction positive oxyhydroxide contamination precipitation polymerization is adsorbed; Send in the subsider, temperature is reduced to 65 ℃-75 ℃, and oxide impurity is returned the zirconates production system with plate type pressure filter press filtration gained filter residue; Filtrating adds caustic soda and sodium silicate carries out the mode transfer reaction; Concentrating the adjustment modulus is 1.95-2.05, and the control solid content is 50-55%, through 200-300 ℃ of spraying drying; Get indefiniteness powdery sodium disilicate, indefiniteness powdery sodium disilicate gets layered sodium disilicate at 650 ℃ of-800 ℃ of calcined crystallines.
Useless white residue and waste lye reaction can also be heated under 125 ℃ of temperature and produced the water glass mixing solutions in 9 hours, detect silicon sodium mol ratio: SiO among the step B
2: Na
2Concentration is that 0.01 modified cation gathers third ethernamine 1%, wood charcoal powder 1% carries out physical reaction positive oxyhydroxide contamination precipitation polymerization is adsorbed during O=1; Send in the subsider, temperature is reduced to 70 ℃, and oxide impurity is returned the zirconates production system with plate type pressure filter press filtration gained filter residue; Filtrating adds caustic soda and sodium silicate carries out the mode transfer reaction; Concentrating the adjustment modulus is 2, and the control solid content is 55%, through 250 ℃ of spraying dryings; Get indefiniteness powdery sodium disilicate, indefiniteness powdery sodium disilicate gets layered sodium disilicate at 750 ℃ of calcined crystallines.
Embodiment 1
To contain Na
2O6-10%, SiO
2The waste lye of 1-3% with contain SiO
2The useless white residue of 15-25% is pressed certain weight ratio Na
2O:SiO
2=1:1 drops in the reaction kettle; Airtight heating reaction in 5 hours under 100 ℃ of high temperature; When making modulus and be 0.95 sodium silicate solution, add concentration and be that 0.005% modified cation gathers third ethernamine 0.5%, wood charcoal powder 0.5% carries out physical reaction positive oxyhydroxide contamination precipitation polymerization is adsorbed.Then above feed liquid is added in the subsider, temperature is reduced to 60 ℃ and is got filter residue with the plate type pressure filter press filtration and return the zirconates production system, and zirconia content 5% in the filter residue; Filtrating adds caustic soda and sodium silicate control solid content is 45%; Modulus is to squeeze into solution in 1.9 o'clock under 150 ℃ of hot blast direct heating, to process indefiniteness powdery sodium disilicate in the spray-drying tower; Adding continuously uniformly the inherent temperature of spray-drying tower to amorphous sodium disilicate powder again is to carry out high temperature crystallization in 600 ℃ the rotation crystal growing furnace; Amorphous sodium disilicate powdery through 30 minutes crystallization, makes layered sodium disilicate in stove.Then layered sodium disilicate is pulverized or is compacted into particulate state and be a layer silicon finished product, granulation layer silicon is processed in the layered sodium disilicate doping.
Embodiment 2
To contain Na
2O6-10%, SiO
2The waste lye of 1-3% with contain SiO
2The useless white residue of 15-25% is pressed certain weight ratio Na
2O:SiO
2=1:1 drops in the reaction kettle; Airtight heating reaction in 7 hours under 110 ℃ of high temperature; When making modulus and be 1.00 sodium silicate solution, add concentration and be that 0.08% modified cation gathers third ethernamine 0.8%, wood charcoal powder 0.8% carries out physical reaction positive oxyhydroxide contamination precipitation polymerization is adsorbed.Then above feed liquid is added in the subsider, temperature is reduced to 70 ℃ and is got filter residue with the plate type pressure filter press filtration and return the zirconates production system, and zirconia content 7% in the filter residue; Filtrating adds caustic soda and sodium silicate control solid content is 48%; Modulus is to squeeze into solution in 2.0 o'clock under 190 ℃ of hot blast direct heating, to process indefiniteness powdery sodium disilicate in the spray-drying tower; Joining temperature to amorphous sodium disilicate powder continuously uniformly again is to carry out high temperature crystallization in 650 ℃ the rotation crystal growing furnace; Amorphous sodium disilicate powdery through 30 minutes crystallization, makes layered sodium disilicate in stove.Then layered sodium disilicate is pulverized or is compacted into particulate state and be a layer silicon finished product, granulation layer silicon is processed in the layered sodium disilicate doping.
Embodiment 3
To contain Na
2O6-10%, SiO
2The waste lye of 1-3% with contain SiO
2The useless white residue of 15-25% is pressed certain weight ratio Na
2O:SiO
2=1:1 drops in the reaction kettle; Airtight heating reaction in 8 hours under 100 ℃ of high temperature; When making modulus and being 1.01 sodium silicate solutions, add concentration and be that 0.009% modified cation gathers third ethernamine 0.9%, wood charcoal powder 0.9% carries out physical reaction positive oxyhydroxide contamination precipitation polymerization is adsorbed.Then above feed liquid is added in the subsider, temperature is reduced to 80 ℃ and is got filter residue with the plate type pressure filter press filtration and return the zirconates production system, and zirconia content 8% in the filter residue; Filtrating adds caustic soda and sodium silicate control solid content is 50%; Modulus is to squeeze into solution in 2.03 o'clock under 230 ℃ of hot blast direct heating, to process indefiniteness powdery sodium disilicate in the spray-drying tower; Adding continuously uniformly temperature to amorphous sodium disilicate powder again is to carry out high temperature crystallization in 700 ℃ the rotation crystal growing furnace; Amorphous sodium disilicate powdery through 30 minutes crystallization, makes layered sodium disilicate in stove.Then layered sodium disilicate is pulverized or is compacted into particulate state and be a layer silicon finished product, granulation layer silicon is processed in the layered sodium disilicate doping.
Embodiment 4
To contain Na
2O6-10%, SiO
2The waste lye of 1-3% with contain SiO
2The useless white residue of 15-25% is pressed certain weight ratio Na
2O:SiO
2=1:1 drops in the reaction kettle; Airtight heating reaction in 9 hours under 130 ℃ of high temperature; When making modulus and be 1.02 sodium silicate solution, add concentration and be that 0.01% modified cation gathers third ethernamine 1%, wood charcoal powder 1% carries out physical reaction positive oxyhydroxide contamination precipitation polymerization is adsorbed.Then above feed liquid is added in the subsider, temperature is reduced to 70 ℃ and is got filter residue with the plate type pressure filter press filtration and return the zirconates production system, and zirconia content 10% in the filter residue; Filtrating adds caustic soda and sodium silicate control solid content is 54%; Modulus is to squeeze into solution in 1.97 o'clock under 270 ℃ of hot blast direct heating, to process indefiniteness powdery sodium disilicate in the spray-drying tower; Joining temperature to amorphous sodium disilicate powder continuously uniformly again is to carry out high temperature crystallization in 750 ℃ the rotation crystal growing furnace; Amorphous sodium disilicate powdery through 30 minutes crystallization, makes layered sodium disilicate in stove.Then layered sodium disilicate is pulverized or is compacted into particulate state and be a layer silicon finished product, granulation layer silicon is processed in the layered sodium disilicate doping.
Embodiment 5
To contain Na
2O6-10%, SiO
2The waste lye of 1-3% with contain SiO
2The useless white residue of 15-25% is pressed certain weight ratio Na
2O:SiO
2=1:1 drops in the reaction kettle; Airtight heating reaction in 10 hours under 140 ℃ of high temperature; When making modulus and be 1.03 sodium silicate solution, add concentration and be that 0.011% modified cation gathers third ethernamine 1.1%, wood charcoal powder 1.1% carries out physical reaction positive oxyhydroxide contamination precipitation polymerization is adsorbed.Then above feed liquid is added in the subsider, temperature is reduced to 70 ℃ and is got filter residue with the plate type pressure filter press filtration and return the zirconates production system, and zirconia content 10% in the filter residue; Filtrating adds caustic soda and sodium silicate control solid content is 58%; Modulus is to squeeze into solution in 2.05 o'clock under 310 ℃ of hot blast direct heating, to process indefiniteness powdery sodium disilicate in the spray-drying tower; Adding continuously uniformly temperature to amorphous sodium disilicate powder again is to carry out high temperature crystallization in 800 ℃ the rotation crystal growing furnace; Amorphous sodium disilicate powdery through 30 minutes crystallization, makes layered sodium disilicate in stove.Then layered sodium disilicate is pulverized or is compacted into particulate state and be a layer silicon finished product, granulation layer silicon is processed in the layered sodium disilicate doping.
Embodiment 6
To contain Na
2O6-10%, SiO
2The waste lye of 1-3% with contain SiO
2The useless white residue of 15-25% is pressed certain weight ratio Na
2O:SiO
2=1:1 drops in the reaction kettle; Airtight heating reaction in 12 hours under 100 ℃ of high temperature; When making modulus and be 1.05 sodium silicate solution, add concentration and be that 0.015% modified cation gathers third ethernamine 1.5%, wood charcoal powder 1.5% carries out physical reaction positive oxyhydroxide contamination precipitation polymerization is adsorbed.Then above feed liquid is added in the subsider, temperature is reduced to 80 ℃ and is got filter residue with the plate type pressure filter press filtration and return the zirconates production system, and zirconia content 9% in the filter residue; Filtrating adds caustic soda and sodium silicate control solid content is 60%; Modulus is to squeeze into solution in 2.1 o'clock under 350 ℃ of hot blast direct heating, to process indefiniteness powdery sodium disilicate in the spray-drying tower; Joining temperature to amorphous sodium disilicate powder continuously uniformly again is to carry out high temperature crystallization in 850 ℃ the rotation crystal growing furnace; Amorphous sodium disilicate powdery through 30 minutes crystallization, makes layered sodium disilicate in stove.Then layered sodium disilicate is pulverized or is compacted into particulate state and be a layer silicon finished product, granulation layer silicon is processed in the layered sodium disilicate doping.
Fig. 1 is a process flow sheet of the present invention
Claims (3)
1. the method that useless white residue and alkali waste water are produced layered sodium disilicate may further comprise the steps:
A, usefulness are produced the Na that contains of zirconium oxychloride
2O 6%-10%, SiO
2The waste lye of 1%-3% with contain SiO
2The useless white residue of 15%-25% is pressed Na
2O: SiO
2=1: 1 weight ratio drops in the reaction kettle, airtight heating, and control reaction temperature is 100-150 ℃, the reaction times is 5-12 hour,
B, detection silicon sodium mol ratio: SiO
2: Na
2During O=0.95-1.05, adding concentration is that the modified cation of 0.005%-0.015% gathers the third ethernamine 0.5%-1.5%, wood charcoal powder 0.5%-1.5% carries out physical reaction, with positive oxyhydroxide contamination precipitation polymerization absorption,
C, above reaction feed liquid is put into subsider, when temperature is reduced to 60 ℃-80 ℃, use the plate type pressure filter press filtration, the filter residue that must contain zirconium white 5-10% returns the zirconates production system, filtrate to be sodium silicate solution,
D, gained filtrating water glass among the C is added caustic soda and sodium silicate carries out the mode transfer reaction, concentrating the adjustment modulus is 1.9-2.1, and the control solid content is 45%-60%,
E, with material among the D through 150 ℃ of-350 ℃ of spraying dryings, amorphous powdery sodium disilicate,
F, E gained material is got layered sodium disilicate at 600 ℃ of-850 ℃ of calcined crystallines,
G, with F gained material pulverize again, sieve finished product.
2. produce the method for layered sodium disilicate according to the said useless white residue of claim 1 and alkali waste water; It is characterized in that temperature of reaction is 120 ℃-130 ℃ in the said steps A; Time is 7-10 hour; When silicon sodium mol ratio was 0.98-1.03 among the said step B, adding concentration was that the modified cation of 0.008%-0.012% gathers the third ethernamine 0.8%-1.2%, wood charcoal powder 0.8%-1.2% carries out physical reaction, and temperature is 65 ℃-75 ℃ among the said step C.
3. produce the method for layered sodium disilicate according to the said useless white residue of claim 1 and alkali waste water; It is characterized in that temperature of reaction is 125 ℃ in the said steps A; Time is 9 hours; Silicon sodium mol ratio is 1 o'clock among the said step B, adds concentration and be that 0.01% modified cation gathers third ethernamine 1%, wood charcoal powder 1% carries out physical reaction, and temperature is 70 ℃ among the said step C.
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|---|---|---|---|
| CN200710054156A CN101274763B (en) | 2007-03-28 | 2007-03-28 | Method for preparing layered sodium disilicate by using waste white slime and alkali waste water |
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Families Citing this family (7)
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| CN105905914B (en) * | 2016-04-18 | 2018-01-02 | 苏州吉人高新材料股份有限公司 | A kind of preparation method of EHM extra high modulus silicate |
| CN108163864A (en) * | 2018-01-04 | 2018-06-15 | 福建华夏蓝新材料科技有限公司 | A kind of method for comprehensively utilizing by-product sodium metasilicate in zirconium oxychloride production |
| CN110713193B (en) * | 2019-11-18 | 2021-05-04 | 中国科学院过程工程研究所 | Method for recycling zirconium resource from waste silicon slag discharged in zirconium oxychloride production |
| CN110937608B (en) * | 2019-12-30 | 2020-11-03 | 安徽龙泉硅材料有限公司 | Preparation method of high-quality sodium silicate for silicon dioxide |
| CN113880099B (en) * | 2021-10-29 | 2023-07-18 | 山东东岳有机硅材料股份有限公司 | Method for preparing sodium silicate by recycling organic silicon three wastes in green manner |
| CN115650255A (en) * | 2022-11-18 | 2023-01-31 | 浙江工业大学 | Method for simultaneously preparing sodium chloride and hydrophobic silica aerogel from silicon smelting byproducts |
| CN117142480A (en) * | 2023-11-01 | 2023-12-01 | 太原逸峰源科技有限公司 | Silicate mineral-based water glass production method |
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|---|---|---|---|---|
| CN1088547A (en) * | 1991-12-21 | 1994-06-29 | 赫彻斯特股份公司 | The crystalline sodium disilicate preparation method |
| US6740300B1 (en) * | 1998-08-14 | 2004-05-25 | Korea Research Institute Of Chemical Technology | Method for manufacturing crystalline layered sodium disilicate |
| CN1597513A (en) * | 2004-09-18 | 2005-03-23 | 山东胜通集团股份有限公司 | Production method of lamellar crystalline sodium disilicate |
| CN1837042A (en) * | 2006-04-11 | 2006-09-27 | 云南盐化股份有限公司 | Process for industrial production of laminated sodium disilicate crystal with low cost |
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2007
- 2007-03-28 CN CN200710054156A patent/CN101274763B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1088547A (en) * | 1991-12-21 | 1994-06-29 | 赫彻斯特股份公司 | The crystalline sodium disilicate preparation method |
| US6740300B1 (en) * | 1998-08-14 | 2004-05-25 | Korea Research Institute Of Chemical Technology | Method for manufacturing crystalline layered sodium disilicate |
| CN1597513A (en) * | 2004-09-18 | 2005-03-23 | 山东胜通集团股份有限公司 | Production method of lamellar crystalline sodium disilicate |
| CN1837042A (en) * | 2006-04-11 | 2006-09-27 | 云南盐化股份有限公司 | Process for industrial production of laminated sodium disilicate crystal with low cost |
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Application publication date: 20081001 Assignee: Henan Sinolink Chemical Co. Ltd. Assignor: Wan Fang Contract record no.: 2014410000034 Denomination of invention: Method for preparing layered sodium disilicate by using waste white slime and alkali waste water Granted publication date: 20120905 License type: Exclusive License Record date: 20140422 |
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