CN102992332A - Method for preparing white carbon blacks by using waste silica bricks - Google Patents
Method for preparing white carbon blacks by using waste silica bricks Download PDFInfo
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- CN102992332A CN102992332A CN2012105505516A CN201210550551A CN102992332A CN 102992332 A CN102992332 A CN 102992332A CN 2012105505516 A CN2012105505516 A CN 2012105505516A CN 201210550551 A CN201210550551 A CN 201210550551A CN 102992332 A CN102992332 A CN 102992332A
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Abstract
The invention relates to a method for preparing white carbon blacks by using waste silica bricks, which is characterized by comprising the following steps: removing sundries in waste silica bricks, washing and then drying the waste silica bricks, and crushing the waste silica bricks into silica brick powder with a particle size of less than 0.1 mm; carrying out stirred reaction on the silica brick powder and a NaOH aqueous solution with a mass percentage of 5-10% in a rate of 1:20 in an airtight reaction kettle at a temperature of 90-150 DEG C for 4-10 hours, standing and then obtaining the obtained object so as to obtain a sodium silicate solution; adding the sodium silicate solution into a dilute hydrochloric acid, so that flocculated precipitates are gradually produced in the solution, and filtering the obtained product so as to obtain flocculated silicagel precipitates; repeatedly washing the flocculated silicagel precipitates by using deionized water at a temperature of 70-90 DEG C, and carrying out filtered aging treatment on the flocculated silicagel precipitates so as to obtain crude white carbon black products; and drying the crude white carbon black products at a temperature of 100-110 DEG C, and calcinating the crude white carbon black products in a fluidized bed furnace at a temperature of 500-600 DEG C for 1-3 hours, thereby obtaining white carbon black products. The method disclosed by the invention has the advantages that a step of high temperature roasting for crystal form transformation is omitted, so that the energy is saved, thereby both achieving an effect of changing waste material into things of value, and reducing the production cost; and the problem of environmental pollution is also solved.
Description
Technical field
The invention belongs to the fine chemical technology field, relate in particular to a kind of method of utilizing waste and old silica brick to prepare white carbon black.
Background technology
White carbon black is the general name of white powder amorphous silicic acid and silicate product.Mainly refer to precipitated silica, aerosil, superfine silicon dioxide gel and aerogel, also comprise Powdered synthetic aluminium silicate and Calucium Silicate powder etc.Traditional production method has two kinds: (1) vapor phase process, be mainly chemical vapour deposition (CAV) method, and claim again pyrolysis method, dry method or combustion method.Its raw material is generally silicon tetrachloride, oxygen (or air) and hydrogen, and reaction forms under the high temperature.(2) precipitator method are again the water glass acidization, are by water glass and acid-respons, through precipitation, filter, and washing, dry and calcining forms.New production process adopts preparing white carbon black by precipitation method mainly take nonmetalliferous ore and extension thereof as the silicon source.Raw material mainly contains wollastonite, opal, halloysite, peridotites, snake mosquito stone, kaolin, hard kaoline, coal gangue, flyash, tailings of high silicon iron etc.Its key problem in technology is that the silicon-dioxide of crystallization and silicate are transformed into amorphous silicon di-oxide.White carbon black is of many uses, and white carbon black is used in the colorful rubber goods and carries out reinforcement with alternative carbon black in rubber item, satisfies the needs of white or translucent product.The whole world surpasses white carbon black over half and is used for rubber materials now, especially in the tire production near 30%, a large amount of uses are also arranged in toothpaste and foodstuffs industry, account for more than 20% of whole world output of white carbon black, all the other 20% are used for agricultural chemicals, paper industry, other industrial circles such as fire product.
China has a large amount of industrial furnaces to carry out large repairs or the maintenance rebuild work such as reorganization and expansion every year, the waste and old fire-resistant silica brick that output is a large amount of, though recovery is arranged, cheap (the highlyest be no more than 200 yuan/tons, road is slightly far namely offset by freight charges.) still being used for fire-resistant silica brick production after the recovery, the normal operation amount is very little.Most waste and old silica bricks have been abandoned with the solid refuse form.This has just caused the waste of resource.SiO in the used silica brick
2Account for more than 94%, and mainly be tridymite, larger basic active is arranged, be conducive to produce water glass.
Silica brick raw material and wedding agent comprise in " nanometer composite silicon brick and preparation methods " such as the Ye Fangbao of Zhengzhou University: silica granule and fine powder, useless silica brick particle, nano-calcium carbonate, nano-sized iron oxide, nano silicon, Fluorspar Powder, lime, lignosulfite.The present invention is take the conventional production process of present silica brick as the basis, and composite nano powder is cooperated, in the brickmaking technology of introducing silica brick, makes nano combined silica brick after efficient the dispersion with optimum proportion.The Wang Jie of Beijing Ruitai High-Temp Material Science and Technology Co., Ltd once waited in " a kind of advanced silica refractory and production technique thereof " and had provided a kind of siliceous refractory [material, proportioning is: 3.0~1.0mm natural silica 30~55%, the silica brick particle 0~15% 3.0~1.0mm gives up, 1.0~0.09mm natural silica 10-25%, the silica brick particle 0~15% 3.0~1.0mm gives up,<0.09mm natural silica+useless silica brick powder+calcined silica 10-25%, without aluminium high C3 S cement or calcium hydroxide powder 1-5%, SiO2 〉=98%, the silica micro mist 0~5% of meta particle diameter D50≤10 μ m, the silicon ash 1~5% of SiO2 〉=96%, high efficiency water reducing agent 0.05-1.0%, organic bond 0.03-1.0% mixes 1~2% fluorite outward, 0~6% calcium sulfate, 0~4% sal epsom or magnesium oxide are mineralizer.Its production technique is: the proportioning weighing, mix, after the moulding, drying, 1350-1460 ℃ of 10-36 hour burnt product.Provide a kind of coke oven that can be used in " refractory dry powder seal material for coke furnaces " such as the Gan Feifang of Baoshan Iron ﹠ Steel Co., Ltd with the component of refractory dry powder seal material.A kind of refractory dry powder seal material for coke furnace forms (% by weight) by following component: (1) silica, % by weight are 51~89%; (2) useless silica brick powder, % by weight is 5~25%; (3) feldspar, % by weight are 5~20%; (4) silicon powder, % by weight are 1~5%; Particle size is≤0.074mm.
" a kind of method for preparing white carbon black with iron tailings " of Xue Xiang Xin of Northeastern University etc. may further comprise the steps: (1) is with below the iron tailings ball milling 100-400 order, in 400 ℃-1000 ℃ lower calcining 3-5h activation; (2) iron tailings after usefulness activates and NaOH be SiO in molar ratio
2: NaOH=1: 2 mix, and add fully to stir behind a certain amount of water and produced sodium silicate solution in 2-8 hour 50 ℃-120 ℃ lower reactions; (3) above-mentioned sodium silicate solution fully being stirred evenly slow dropping HCl and carry out acidification, is to stop in 6~10 o'clock to the pH value, obtains flocks, namely obtains after filtering the thick product of white carbon black; (4) the white carbon black crude product is washed, checked Cl
-Content<1%, products obtained therefrom, oven dry, pulverizing get product; Advantage of the present invention: reduced environmental pollution, and solved the difficult problem of steel mill's mine tailing processing, technique is simple, and cost is low, and profit is high, and realizes easily suitability for industrialized production." a kind of method of producing white carbon black with coal gangue " of Han Zhao force provides the method that a kind of coal gangue is produced white carbon black, belongs to technical field of coal chemical industry.The present invention makes the kaolinite in the coal gangue resolve into SiO by high-temperature roasting
2And Al
2O
3, adding acid is rear and add heat soaking, makes Al wherein
2O
3Generate soluble salt with other metal ions, then filter, again with the filter residue alkali fusion, make quartz and SiO in the filter residue
2Be converted into soluble silicate; In the silicate of melting, add entry again, make silicate cracked by shrend, then leave standstill, filter, the concentrated water glass that obtains; Add again organic solvent and pass into CO
2Gas, through ageing, washing is filtered, and the oven dry of gained colloid and calcination obtain white carbon black.The present invention has reduced production cost take coal gangue as the raw material production white carbon black, and solves the utilization of waste material problem of coal gangue.
Waste and old silica brick will be through 1000-1400 ℃ calcination or roasting, stable α-SiO wherein in production and use procedure
2The crystal formation change has occured or has produced lattice defect in majority, makes it to have higher alkali reaction activity; SiO in the waste and old silica brick
2Content up to more than 94%, as the silicon raw material of producing white carbon black larger cost advantage is arranged.
Summary of the invention
The purpose of this invention is to provide and a kind ofly solve tradition to prepare the method cost of white carbon black higher, the large with serious pollution shortcoming that consumes energy solves simultaneously Industrial Stoves and safeguards that the waste and old silica brick that utilizes take waste and old silica brick as main raw material that utilizes problem of the waste and old silica brick that produces prepares the method for white carbon black.
The purpose of invention realizes by following technical proposals:
1, a kind of method of utilizing waste and old silica brick to prepare white carbon black of the present invention is characterized in that comprising the following steps:
A) waste and old silica brick is picked foreign material, dry after the water flushing, be crushed to<the silica brick powder of 0.1mm;
B) the NaOH aqueous solution of above-mentioned silica brick powder and mass percent 5-10% in 1: 20 ratio at 90-150 ℃ of constant temperature stirring reaction after 4-10 hour in airtight reactor, stop to stir and leave standstill, filtered while hot obtains water glass solution when temperature of charge is down to 90-95 ℃;
C) water glass solution obtained above is slowly joined carry out acidification in the dilute hydrochloric acid, make to produce gradually flocks in the solution, until the solution pH value till the 7-8, obtains cotton-shaped silica gel throw out more after filtration;
D) with the deionized water repetitive scrubbing of cotton-shaped silica gel throw out obtained above with 70-90 ℃, until the filtrate pH value is till the 6-8, ripening obtains the thick product of white carbon black after filtration;
E) the thick product of gained white carbon black changes in the fluidizing furnace at 500-600 ℃ of calcination 1-3 hour less than 10% through drying under 100-110 ℃ of condition to contained humidity, namely obtains white carbon black product.
Advantage of the present invention is: compare with traditional white carbon black production technique and new solid waste processing white carbon black production technique, the step of high-temperature roasting conversion crystal formation has been saved owing to use waste and old silica brick in the silica material source, has saved the energy, both turned waste into wealth, reduced again production cost; Also solve simultaneously problem of environmental pollution.
Adopt the white carbon black product of the inventive method preparation, meet the requirement of " HG/T3061-2009 chemical industry in China standard-rubber ingredients precipitated hydrated silica " fully, specific surface area 〉=150m
2/ g, weight loss on heating≤7%, burning decrement≤7%.
Embodiment
Further specify the specific embodiment of the present invention below in conjunction with embodiment.
Embodiment 1
Waste and old silica brick is picked foreign material, dry after the water flushing, be crushed to<the silica brick powder of 0.1mm; The NaOH aqueous solution 550g that gets 50g silica brick powder and mass percent 10% 120 ℃ in airtight reactor the constant temperature stirring reaction stop to stir and leave standstill cooling after 6 hours, filtered while hot obtains water glass solution when 95 ℃ of temperature of charge; The water glass solution placement is got in the uncovered tun, slowly add dilute hydrochloric acid, make to produce gradually flocks in the solution, until till the solution pH value to 8.Filtration obtains cotton-shaped silica gel throw out, at filter funnel with the cotton-shaped silica gel throw out of 70 ℃ deionized water repetitive scrubbing, until till the filtrate pH value to 7, obtain the thick product of white carbon black through ripening; The thick product of this white carbon black is dried to contained humidity 8% under 105 ℃ of conditions, changes in the fluidizing furnace 500 ℃ of calcinations 2 hours, namely obtains white carbon black product.
Embodiment 2
Waste and old silica brick is picked foreign material, dry after the water flushing, be crushed to<the silica brick powder of 0.1mm; The NaOH aqueous solution 650g that gets 50g silica brick powder and mass percent 8% constant temperature stirring reaction in 140 ℃ of airtight reactors stopped to stir and leaves standstill cooling after 4 hours, and filtered while hot obtains water glass solution when 90 ℃ of temperature of charge; The water glass solution placement is got in the uncovered tun, slowly add dilute hydrochloric acid, make to produce gradually flocks in the solution, until till the solution pH value to 8.Filtration obtains cotton-shaped silica gel throw out, at filter funnel with the cotton-shaped silica gel throw out of 75 ℃ deionized water repetitive scrubbing, until till the filtrate pH value to 7, obtain the thick product of white carbon black through ripening; The thick product of this white carbon black is dried to contained humidity 9% under 100 ℃ of conditions, changes in the fluidizing furnace 400 ℃ of calcinations 3 hours, namely obtains white carbon black product.
Embodiment 3
Waste and old silica brick is picked foreign material, dry after the water flushing, be crushed to<the silica brick powder of 0.1mm; The NaOH aqueous solution 1000g that gets 50g silica brick powder and mass percent 5% 120 ℃ in airtight reactor the constant temperature stirring reaction stop to stir and leave standstill cooling after 6 hours, filtered while hot obtains water glass solution when 95 ℃ of temperature of charge; The water glass solution placement is got in the uncovered tun, slowly add dilute hydrochloric acid, make to produce gradually flocks in the solution, until till the solution pH value to 8.Filtration obtains cotton-shaped silica gel throw out, at filter funnel with the cotton-shaped silica gel throw out of 70 ℃ deionized water repetitive scrubbing, until till the filtrate pH value to 7, obtain the thick product of white carbon black through ripening; The thick product of this white carbon black is dried to contained humidity 8% under 105 ℃ of conditions, changes in the fluidizing furnace 500 ℃ of calcinations 2 hours, namely obtains white carbon black product.
Claims (1)
1. a method of utilizing waste and old silica brick to prepare white carbon black is characterized in that comprising the following steps:
A) waste and old silica brick is picked foreign material, dry after the water flushing, be crushed to<the silica brick powder of 0.1mm;
B) the NaOH aqueous solution of above-mentioned silica brick powder and mass percent 5-10% is in 1: 20 ratio constant temperature stirring reaction after 4-10 hour in 90-150 ℃ of airtight reactor, stop to stir and leave standstill, filtered while hot obtains water glass solution when temperature of charge is down to 90-95 ℃;
C) water glass solution obtained above is slowly joined carry out acidification in the dilute hydrochloric acid, make to produce gradually flocks in the solution, until the solution pH value till the 7-8, obtains cotton-shaped silica gel throw out more after filtration;
D) with the deionized water repetitive scrubbing of cotton-shaped silica gel throw out obtained above with 70-90 ℃, until the filtrate pH value is till the 6-8, ripening obtains the thick product of white carbon black after filtration;
E) the thick product of gained white carbon black changes in the fluidizing furnace at 500-600 ℃ of calcination 1-3 hour less than 10% through drying under 100-110 ℃ of condition to contained humidity, namely obtains white carbon black product.
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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106672981A (en) * | 2016-12-19 | 2017-05-17 | 河钢股份有限公司承德分公司 | Method and application of resource utilization of waste refractory brick |
CN108002397A (en) * | 2017-12-29 | 2018-05-08 | 云南磷化集团有限公司 | A kind of method that industrial waterglass prepares white carbon |
CN108929072A (en) * | 2018-07-18 | 2018-12-04 | 浙江工业大学 | A method of iron oxide and nano combined heat-insulating heat-preserving material are prepared from iron tailings |
CN109053230A (en) * | 2018-10-18 | 2018-12-21 | 铁岭吉宏峰五和农业科技有限公司 | It is a kind of water solubility silicic acid preparation method and its application in crops |
CN109133072A (en) * | 2018-08-28 | 2019-01-04 | 浙江工业大学 | A method of hydrophobic silica aerogel is prepared using iron tailings as raw material is supper-fast |
CN110255569A (en) * | 2019-07-01 | 2019-09-20 | 杨鈜博 | A method of directly production prepares white carbon black from quartz mineral powder |
CN114590813A (en) * | 2022-03-15 | 2022-06-07 | 北京化工大学 | Method and device for preparing nano silicon dioxide by high-valued utilization of silica gel solid waste |
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 |
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Cited By (11)
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CN106672981A (en) * | 2016-12-19 | 2017-05-17 | 河钢股份有限公司承德分公司 | Method and application of resource utilization of waste refractory brick |
CN108002397A (en) * | 2017-12-29 | 2018-05-08 | 云南磷化集团有限公司 | A kind of method that industrial waterglass prepares white carbon |
CN108929072A (en) * | 2018-07-18 | 2018-12-04 | 浙江工业大学 | A method of iron oxide and nano combined heat-insulating heat-preserving material are prepared from iron tailings |
CN108929072B (en) * | 2018-07-18 | 2020-10-23 | 浙江工业大学 | Method for preparing ferric oxide and nano composite heat insulation material from iron tailings |
CN109133072A (en) * | 2018-08-28 | 2019-01-04 | 浙江工业大学 | A method of hydrophobic silica aerogel is prepared using iron tailings as raw material is supper-fast |
CN109133072B (en) * | 2018-08-28 | 2020-08-11 | 浙江工业大学 | Method for preparing hydrophobic silica aerogel by using iron tailings as raw materials at ultra-fast speed |
CN109053230A (en) * | 2018-10-18 | 2018-12-21 | 铁岭吉宏峰五和农业科技有限公司 | It is a kind of water solubility silicic acid preparation method and its application in crops |
CN110255569A (en) * | 2019-07-01 | 2019-09-20 | 杨鈜博 | A method of directly production prepares white carbon black from quartz mineral powder |
CN114590813A (en) * | 2022-03-15 | 2022-06-07 | 北京化工大学 | Method and device for preparing nano silicon dioxide by high-valued utilization of silica gel solid waste |
CN114590813B (en) * | 2022-03-15 | 2023-09-22 | 北京化工大学 | Method and device for preparing nano silicon dioxide by utilizing silica gel solid waste in high-valued 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 |
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Application publication date: 20130327 |