CN102701222A - Method for producing white carbon black with coal gangue - Google Patents
Method for producing white carbon black with coal gangue Download PDFInfo
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- CN102701222A CN102701222A CN2012101587396A CN201210158739A CN102701222A CN 102701222 A CN102701222 A CN 102701222A CN 2012101587396 A CN2012101587396 A CN 2012101587396A CN 201210158739 A CN201210158739 A CN 201210158739A CN 102701222 A CN102701222 A CN 102701222A
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- coal gangue
- carbon black
- white carbon
- water
- filter residue
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Abstract
The invention relates to a method for producing white carbon black with coal gangue, and belongs to the technical field of coal chemical industry. The method for producing the white carbon black with the coal gangue comprises the following steps: decomposing kaolinite in the coal gangue into SiO2 and Al2O3 through high-temperature calcinations, adding an acid, and heating and soaking, wherein the Al2O3 and other metal ions form soluble salts; then, filtering, and performing alkali fusion on filter residues so as to convert quartz and SiO2 in the filter residues into soluble silicate; adding water into molten silicate, and fragmentating the silicate by water quenching; then, standing, filtering and concentrating the silicate to obtain water glass; adding an organic solvent and inflating CO2 gas; and aging, washing and filtering to obtain a colloidal, and drying and sintering the colloidal to obtain the white carbon black. In the method for producing the white carbon black with the coal gangue, the coal gangue is taken as a raw material to produce the white carbon black, so that the production cost is reduced and the problem in utilizing coal gangue wastes is solved; and wastewater generated in the production process can be neutralized mutually, so that the influence of discharge of wastewater containing SO42- on equipment and environment is reduced.
Description
Technical field
The present invention relates to a kind of coal gangue and produce the method for WHITE CARBON BLACK, belong to technical field of coal chemical industry.
Background technology
Coal gangue contains the silicon-dioxide more than 40%, produces a large amount of enrichments of silicon-dioxide in the remaining coal gangue tailings of polymeric aluminum through the salt s.t., and is better active.Silicon-dioxide is the main raw material of producing water glass; In the numerous collieries of China, pile up like a mountain as the coal gangue of coal mining by-product, not only land occupation, but also be prone to become the source that air-borne dust pollutes, be badly in need of innoxious use.At present, the method for preparing WHITE CARBON BLACK both at home and abroad has vapor phase process, the carbonization precipitator method, the precipitator method, reversed phase micelle microemulsion method, sol-gel method etc., and aforesaid method adopts the pure chemistry raw material synthetic more, and the production technique investment is high, and product cost is higher.The tradition coal gangue is earlier calcined coal gangue acidleach or alkali fusion to be obtained water glass for the feedstock production method for white carbon black, uses water glass and sulfuric acid (or hydrochloric acid) for raw material prepares WHITE CARBON BLACK again, though the simple output of its technology is high, contains SO in the mother liquor
4 2-(or Cl
-) be difficult for reclaiming, produce a large amount of waste water; And sulfuric acid or hydrochloric acid life-time service meeting etching apparatus and pipeline cause industrial loss.
Summary of the invention
The objective of the invention is shortcomings such as higher for the method cost that solves the traditional preparation process WHITE CARBON BLACK, that product pollution is serious, and solve the utilization of waste material problem of coal gangue, is the method for raw material production WHITE CARBON BLACK with the coal gangue and provide a kind of.
The present invention makes the kaolinite in the coal gangue resolve into unbodied SiO through high-temperature roasting in fluidizing furnace earlier
2And Al
2O
3, add the acid back and add heat soaking for some time, make Al wherein
2O
3Generate soluble salt with other metals ions, filter then,, make quartz and the SiO of amorphous state in the filter residue again with filter residue alkali fusion appropriate time at a certain temperature
2All be converted into soluble silicate; In fused silicate, add entry again, make silicate cracked through the shrend effect, impurity is left standstill, removes by filter in shrend after for some time, concentrates to obtain water glass; In water glass, add organic solvent and feed CO
2Gas reacts, and forms a large amount of silica gel, ageing, and washing is filtered, and the gained colloid is dried in baking oven, puts into the fluidizing furnace calcination after the drying and obtains WHITE CARBON BLACK.
The objective of the invention is to realize through following technical scheme:
A kind of coal gangue of the present invention is the method for the white carbon black of feedstock production, comprises the following steps:
1) with coal gangue in 650～750 ℃ of roasting 1～2.5h; Under 60～100 ℃, join concentration then and be in 10%～98% the sulphuric acid soln and soak 2～5h; Coal gangue and sulphuric acid soln mass ratio 1: 5～8;
2) coal gangue after the 1st acidleach that obtains of step is filtered, filter residue is washed till pH value to 6～8 with 60 ℃～80 ℃ zero(ppm) water, filter residue is joined 20%～50% Na again
2CO
3In the solution, and temperature is heated to 300～400 ℃ of alkali fusion 1～2h, filter residue and Na
2CO
3The mass ratio of solution is 1: 1～2;
3) filter residue behind the 2nd alkali fusion that obtains of step is poured in the water, soaked 2～5h, filter then, evaporation concentration 43～48 degree Beaume of filtrating obtain water glass, and the mass ratio of filter residue and water is 1: 20～80;
4) in the 3rd water glass that obtains of step, add organic solvent, the speed with 100～500ml/min feeds CO in mixing solutions simultaneously
2Gas, stirring reaction 2～3h up to complete flocks occurring, leaves standstill 1～2h again under 60～80 ℃ of temperature condition; Wherein, organic solvent is a kind of of methyl alcohol, ethanol and acetone or the mixture more than two kinds, and the mass ratio of water glass and organic solvent is 1: 0.5～3;
5) distilled water wash to pH value to 6～8 of leaving standstill 60 ℃～80 ℃ of thing employings that the 4th step obtained; The gel that after the filtration ageing is obtained under not being higher than 200 ℃ condition in oven dry to the deposition moisture content less than 10%; High temperature sintering 1～3h under 400～600 ℃ condition can obtain the product WHITE CARBON BLACK at last.
When reclaiming waste liquid, can be with sulfuric acid waste and the step 2 in the step 1)) the alkali fusion waste liquid mix, make it carry out neutralization reaction, reclaim and obtain sodium sulfate, minimizing contains SO
4 2-The discharging of waste water.
Beneficial effect
The present invention for the raw material production WHITE CARBON BLACK has reduced production cost, and solves the utilization of waste material problem of coal gangue with the coal gangue.The waste water that the present invention produces in process of production can neutralize each other, reduces to contain SO
4 2-Discharge of wastewater to the influence of equipment and environment.
Embodiment
Below in conjunction with embodiment content of the present invention is described further.
Embodiment 1
Get the coal gangue of 50kg, in 750 ℃ of roasting 1h; Join 280kg concentration then and be in 40% the sulphuric acid soln and soak, soak 2h in 60 ℃.Filter, adopts 60 ℃ distilled water wash to pH value neutrality, it is 50% Na that the solid filter residue is joined 80kg concentration
2CO
3In the solution, will be heated to 400 ℃ of alkali fusion 2h; Pour in the 80L water fused filter residue into shrend leaching 2h, filter then, evaporation concentration 43 degree Beaume of filtrating obtain water glass; In water glass, add 50kg ethanol, the speed with 500ml/min feeds CO simultaneously
2Gas, stirring reaction 2h is up to complete flocks occurring; Under 80 ℃ of temperature condition, leave standstill 2h; Neutral with 60 ℃ distilled water washs to pH value, filter, ageing is obtained gel put into baking oven, under 100 ℃ condition, dry; When moisture content less than 10% the time in fluidizing furnace 600 ℃ of high temperature sintering 1h, can obtain the product WHITE CARBON BLACK.Reach the requirement of HG/T3061-1999 through each item index of test products.
Embodiment 2
Get the coal gangue of 80kg, in 700 ℃ of roasting 2.5h; Join 300kg concentration then and be in 40% the sulphuric acid soln and soak, soak 1h in 80 ℃.Filter, adopts 80 ℃ distilled water wash to pH value neutrality, it is 30% Na that the solid filter residue is joined 100kg concentration
2CO
3In the solution, will be heated to 450 ℃ of alkali fusion 1h; Pour in the 100L water fused filter residue into shrend leaching 2h, filter then, evaporation concentration 45 degree Beaume of filtrating obtain water glass; In water glass, add 80kg methyl alcohol, the speed with 300ml/min feeds CO simultaneously
2Gas, stirring reaction 1.5h is up to complete flocks occurring; Under 60 ℃ of temperature condition, leave standstill 3h; Washing is filtered, and ageing has been obtained gel put into baking oven, under 150 ℃ condition, dries; When moisture content less than 10% the time in fluidizing furnace 650 ℃ of high temperature sintering 2h, can obtain the product WHITE CARBON BLACK.Reach the requirement of HG/T3061-1999 through each item index of test products.
Claims (2)
1. the method that coal gangue is the white carbon black of feedstock production is characterized in that comprising the following steps:
1) with coal gangue in 650～750 ℃ of roasting 1～2.5h; Under 60～100 ℃, join concentration then and be in 10%～98% the sulphuric acid soln and soak 2～5h; Coal gangue and sulphuric acid soln mass ratio 1: 5～8;
2) coal gangue after the 1st acidleach that obtains of step is filtered, filter residue is washed till pH value to 6～8 with 60 ℃～80 ℃ zero(ppm) water, filter residue is joined 20%～50% Na again
2CO
3In the solution, and temperature is heated to 300～400 ℃ of alkali fusion 1～2h, filter residue and Na
2CO
3The mass ratio of solution is 1: 1～2;
3) filter residue behind the 2nd alkali fusion that obtains of step is poured in the water, soaked 2～5h, filter then, evaporation concentration 43～48 degree Beaume of filtrating obtain water glass, and the mass ratio of filter residue and water is 1: 20～80;
4) in the 3rd water glass that obtains of step, add organic solvent, the speed with 100～500ml/min feeds CO in mixing solutions simultaneously
2Gas, stirring reaction 2～3h up to complete flocks occurring, leaves standstill 1～2h again under 60～80 ℃ of temperature condition; Wherein, organic solvent is a kind of of methyl alcohol, ethanol and acetone or the mixture more than two kinds, and the mass ratio of water glass and organic solvent is 1: 0.5～3;
5) distilled water wash to pH value to 6～8 of leaving standstill 60 ℃～80 ℃ of thing employings that the 4th step obtained; The gel that after the filtration ageing is obtained under not being higher than 200 ℃ condition in oven dry to the deposition moisture content less than 10%; High temperature sintering 1～3h under 400～600 ℃ condition can obtain the product WHITE CARBON BLACK at last.
2. a kind of coal gangue as claimed in claim 1 is the method for the white carbon black of feedstock production, it is characterized in that: with sulfuric acid waste and the step 2 in the step 1)) the alkali fusion waste liquid mix, obtain sodium sulfate.
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|---|---|---|---|
| CN2012101587396A CN102701222A (en) | 2012-05-22 | 2012-05-22 | Method for producing white carbon black with coal gangue |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101587396A CN102701222A (en) | 2012-05-22 | 2012-05-22 | Method for producing white carbon black with coal gangue |
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| CN102701222A true CN102701222A (en) | 2012-10-03 |
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| CN2012101587396A Pending CN102701222A (en) | 2012-05-22 | 2012-05-22 | Method for producing white carbon black with coal gangue |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104891504A (en) * | 2015-05-19 | 2015-09-09 | 河北工程大学 | A method of extracting white carbon black from coal cinder |
| CN106276935A (en) * | 2016-07-26 | 2017-01-04 | 岳阳明科催化技术有限公司 | Waterglass co-producing white carbon black cleanly production technique |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1128239A (en) * | 1995-06-14 | 1996-08-07 | 重庆大学 | Process for preparing active white carbon black from water glass |
| CN1903727A (en) * | 2005-07-26 | 2007-01-31 | 宁夏大学 | Method of coproducing aluminium oxide, white carbon black and low ash carbon by coal gangue ecological utilization |
| CN101112991A (en) * | 2006-07-24 | 2008-01-30 | 北京化工大学 | Method for preparing silicon dioxide with large pore volume and large aperture |
| CN102259872A (en) * | 2011-06-22 | 2011-11-30 | 武汉大学 | Method for preparing white carbon black by utilizing vanadium ore waste residue |
-
2012
- 2012-05-22 CN CN2012101587396A patent/CN102701222A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1128239A (en) * | 1995-06-14 | 1996-08-07 | 重庆大学 | Process for preparing active white carbon black from water glass |
| CN1903727A (en) * | 2005-07-26 | 2007-01-31 | 宁夏大学 | Method of coproducing aluminium oxide, white carbon black and low ash carbon by coal gangue ecological utilization |
| CN101112991A (en) * | 2006-07-24 | 2008-01-30 | 北京化工大学 | Method for preparing silicon dioxide with large pore volume and large aperture |
| CN102259872A (en) * | 2011-06-22 | 2011-11-30 | 武汉大学 | Method for preparing white carbon black by utilizing vanadium ore waste residue |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104891504A (en) * | 2015-05-19 | 2015-09-09 | 河北工程大学 | A method of extracting white carbon black from coal cinder |
| CN106276935A (en) * | 2016-07-26 | 2017-01-04 | 岳阳明科催化技术有限公司 | Waterglass co-producing white carbon black cleanly production technique |
| CN106276935B (en) * | 2016-07-26 | 2018-11-30 | 岳阳明科催化技术有限公司 | Waterglass co-producing white carbon black cleanly production technique |
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Application publication date: 20121003 |