CN101486460B - Production method for preparing high adsorption active carbon and white carbon black from rice hull - Google Patents
Production method for preparing high adsorption active carbon and white carbon black from rice hull Download PDFInfo
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- CN101486460B CN101486460B CN2008101723746A CN200810172374A CN101486460B CN 101486460 B CN101486460 B CN 101486460B CN 2008101723746 A CN2008101723746 A CN 2008101723746A CN 200810172374 A CN200810172374 A CN 200810172374A CN 101486460 B CN101486460 B CN 101486460B
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Abstract
The invention provides a method for preparing high-adsorption activated carbon and white carbon black by utilizing rice husks, which relates to the field of chemical raw material preparation. The current method for producing activated carbon and white carbon black has the problems of high energy consumption, serious environmental pollution, and the like. In order to overcome the disadvantages, the method adopts the rice husks as raw materials; gasified rice husks reacts with a sodium carbonate aqueous solution under the condition of heating and filter residues are obtained after solid-liquid separation; the filter residues are washed and immersed with ferric chloride or ferrous sulfate additive, and then activation, acid pickling, washing, drying, crushing and packaging are carried out, thus obtaining the finished product of activated carbon; the obtained filtrate is cooled down and decomposed, and then second-time solid-liquid separation, neutralization, filter wash, drying, crushing and packaging are carried out, thus obtaining the finished product of white carbon black. The raw material of the method is easy to be obtained, and the method has low production energy consumption, stable product quality and no environmental pollution.
Description
Technical field
The present invention relates to the industrial chemicals preparation field, relate in particular to the production method of a kind of high adsorption active carbon and white carbon black.
Background technology
Gac is a kind of sorbent material with high porosity, and specific surface area is generally in 600-1200 meters squared per gram.In industrial production, main timber, Exocarpium cocois (Cocos nucifera L), peat, brown coal, bituminous coal, hard coal, refinery coke and the synthetic polymer of adopting, prepare gac by Re Fa or chemical method, the traditional preparation process method exists production cost height, raw material seriously polluted, that produce high performance active carbon to be difficult for problems such as acquisition.White carbon black is the general name of white powder amorphous silicic acid and silicate product, main at present employing soda ash and quartz sand are made solid water glass in fusion more than 1300 ℃ in high temperature reaction stove, solid water glass makes liquid soluble glass in the logical steam dissolving of heating, and liquid soluble glass adds the strong acid reaction again and makes white carbon black.This production method exists energy consumption height, with serious pollution shortcoming.
Rice husk is an isolated rice hulls in the rice processing.For a long time, the rice husk use that generally only acts as a fuel, and the rice hull ash after the burning is not fully utilized especially, usually be considered as refuse by people, be piled up in roadside, the edge of the village, come down in torrents, environment is caused severe contamination in the river pond, utilize rice hull ash to prepare gac and white carbon black, have considerable economic and social benefit.
With the immediate prior art of the present invention be that patent name is " rice hull ash coproduction water glass and a gac ", the patent of the patent No. 88105429.1 has announced in the file that a kind of rice hull ash of utilizing produces water glass and process of active carbon.Main summary of the invention is to be 2.5 kgfs/cm with rice hull ash at temperature more than 128 ℃, pressure
2With the caustic soda soln reaction, with the resultant filtering separation, the gained concentrating filter liquor makes water glass (Na under the condition
2OnSiO
2), the gained filter residue makes activated carbon product through boiling eccysis alkali, and this is invented by silicon dioxde reaction in caustic soda and the rice hull ash, (reaction formula 2NaOH+Sio2=Na
2SiO
3) generate water glass and extract silicon-dioxide, utilize water to flash to the volume change that occurs in the water vapour process simultaneously the carbon surface micropore is increased, make charcoal activatory purpose thereby reach.The high energy of gac specific surface area reaches 700 meters squared per gram, but this method has relatively high expectations to temperature of reaction, pressure, has the higher shortcoming of production energy consumption.Another patent name is " producing unformed white carbon black and gac novel method ", the patent No. 93103043.9.The main summary of the invention of this patent is that rice husk is made charring rice husk under 600-650 ℃, with degree Beaume be 8-11 sodium carbonate solution by weight percentage 1:37 drop in the retort, jar internal pressure 2-3Mpa, 120-130 ℃ of temperature, 2-3 hours reaction times, with reactant through boiling, solid-liquid separation, gained filtrate promptly gets white carbon black through low-temperature decomposition-separation-neutralization-diafiltration-drying-pulverizing, the gained filter residue promptly gets gac through pickling-washing-drying-activation-pulverizing, this method is utilized silicon dioxde reaction in yellow soda ash and the rice hull ash, and reaction formula is 2Na
2CO
3+ SiO
2+ H
2O=Na
2OSiO
2+ 2NaHCO
3From rice hull ash, extract silicon-dioxide, utilizing water to flash to the effect that the volume change that occurs in the water vapour process increases the carbon surface micropore activates, the activated carbon product performance of taking this method to produce is very low, inferior blue adsorptive power has only 10ml/0.1g, no caramel adsorptive power, procedure energy consumption height.
The creativity and innovation content
The purpose of this invention is to provide a kind ofly utilize that rice husk is energy-conservation as raw material, technological process, constant product quality, environmental pollution is low, absorption property is high gac and white carbon black production method.
The invention is characterized in
1. with rice husk gasification, the rice hull ash that obtains after the gasification under the condition of heating with the aqueous sodium carbonate reaction, after reaction finishes with reaction mass through solid-liquid separation, obtain filter residue and filtrate, reaction can be carried out under normal pressure.
With the gained filter residue through wash solid carbon, soaked 5 hours in the iron(ic) chloride 10% or the ferrous sulfate additive aqueous solution, activation then, pickling, washing, drying, pulverizing, packing are made the finished product gac, and gained filtrate is decomposed through lowering the temperature, solid-liquid separation, neutralization, diafiltration, drying, pulverizing, packing are made the white carbon black finished product once more.
The coal gas that produces of rice husk gasification as thermal source by pipe-line transportation to the gac manufacturing procedure, be supplied to washing, activation, pickling, drying process heating usefulness.
The present invention adopts rice husk to produce gac and white carbon black as raw materials for production, have the advantages that raw material sources extensively are easy to get, after in solid carbon, adding iron(ic) chloride or ferrous sulfate additive, additive and charcoal reaction produce relatively advanced hole, have improved the adsorptive power of gac and the quality of white carbon black product greatly.The coal gas that rice husk gasification simultaneously produces is used to the solid carbon manufacturing procedure, does not need to provide in addition thermal source, has energy-conservation effect.
Production method of the present invention in turn includes the following steps:
1. rice husk is purified the back and gasify in vapourizing furnace, the coal gas of generation supplies required thermal source usefulness in the production process, and gets rice hull ash, and is standby.
2. rice hull ash that 1. step is made and concentration be 8%-15% aqueous sodium carbonate by mass percentage 1:30-40 drop in the reactor, add and depress reaction, 130-160 ℃ of temperature of reaction, 2-3 hours reaction times.
The material that 3. will react good carries out the solid-liquid sharp separation under 100 ℃.
4. 3. step is separated the solid carbon that obtains with 90-100 ℃ of hot water wash to pH value to 8-9 after-filtration, filter residue is dipped in the aqueous solution of 10% iron(ic) chloride or ferrous sulfate, soaks and sloughs redundant solution with whizzer after 5 hours.
5. with step 4. the gained solid carbon place Reaktionsofen, furnace temperature is 800-1000 ℃, feeds water vapour, activates 2-4 hours.
6. 5. the gained solid carbon is come out of the stove that to put into concentration immediately be 15% with step---25% hydrochloric acid soln soaked 1 hour, and being washed to PH is 5-6, dry, be crushed to 120 orders above the finished product gac.
7. 3. step is separated the filtrate that obtains and enter in the cooling pan, reduced in 60 minutes below 50 ℃, the cooling rate that slows down was then progressively reduced to solution temperature about 15 ℃ in three hours, separated out silicon-dioxide this moment.The mixture of silica solid and sodium carbonate solution composition is carried out solid-liquid separation, isolated sodium carbonate solution Returning reactor again re-uses, silicon-dioxide after the separation neutralizes by weight 1:1 with the hydrochloric acid of concentration 15%, in whizzer,, be crushed to the above finished product white carbon black that gets of 325 orders with deionized water wash, drying.
The present invention has following beneficial effect:
1. the gac Ya Liji adsorptive value that makes significantly improves, and reaches 16ml/0.1g, and α caramel percent of decolourization 110%, white carbon black meet national HG/T3061-1999 standard fully.
2. the present invention adopts the agricultural wastes rice husk to substitute raw materials such as timber, has both turned waste into wealth, and saved valuable timber again, and raw material is easy to get conveniently.
3. the coal gas that produces with the rice husk gasification among the present invention is used for the gac operation as thermal source, and both recycle heat energy reduced production energy consumption, had reduced environmental pollution again.
Description of drawings
Fig. 1 utilizes rice husk to prepare the production method schema of high adsorption active carbon and white carbon black
Embodiment
With embodiment the present invention is further explained below.
Embodiment 1:
1. gasify in vapourizing furnace after getting 1000 kilograms of purifications of rice husk, the coal gas of generation obtains 450 kilograms of rice hull ash for required thermal source usefulness in the production process, and is standby.
2. be that 8% aqueous sodium carbonate drops in the reactor for 18000 kilograms with above-mentioned rice hull ash and concentration, reactor pressure is 3Mpa, 130 ℃ of temperature, 3 hours reaction times.
3. the material that will react good carries out the solid-liquid sharp separation under 100 ℃.
4. step 3 is separated the solid carbon obtain with 90-100 ℃ of hot water wash to pH value to 8-9 after-filtration, filter residue is dipped in 10% the ferric chloride in aqueous solution, soaks and sloughs redundant solution with whizzer after 5 hours.
5. step 4 gained solid carbon is placed Reaktionsofen, furnace temperature is 1000 ℃, feeds water vapour, activates 2 hours.
6. step 5 gained solid carbon being come out of the stove and putting into concentration immediately is that 25% hydrochloric acid soln soaked 1 hour, and being washed to PH is 5-6, dry, be crushed to 120 orders above 70 kilograms of finished product gacs.
7. step 3 is separated the filtrate that obtains and enter in the cooling pan, reduced in 60 minutes below 50 ℃, the cooling rate that slows down was then progressively reduced to solution temperature about 15 ℃ in three hours, separated out silicon-dioxide.The mixture of silica solid and sodium carbonate solution composition is carried out solid-liquid separation, isolated sodium carbonate solution Returning reactor again re-uses, the 250 kilograms of neutralizations of hydrochloric acid of concentration 15% of silicon-dioxide after the separation, in whizzer with deionized water wash, drying, pulverize 175 kilograms of finished product white carbon blacks.
Embodiment 2:
1. gasify in vapourizing furnace after getting 1000 kilograms of purifications of rice husk, the coal gas of generation obtains 450 kilograms of rice hull ash for required thermal source usefulness in the production process, and is standby.
2. be that 12% aqueous sodium carbonate drops in the reactor for 13500 kilograms with above-mentioned rice hull ash and concentration, reactor pressure is 5Mpa, 160 ℃ of temperature, 2 hours reaction times.
3. the material that will react good carries out the solid-liquid sharp separation under 100 ℃.
4. step 3 is separated the solid carbon obtain with 90-100 ℃ of hot water wash to pH value to 8-9 after-filtration, filter residue is dipped in 10% the ferrous sulfate aqueous solution, soaks and sloughs redundant solution with whizzer after 5 hours.
5. step 4 gained solid carbon is placed Reaktionsofen, furnace temperature is 800 ℃, feeds water vapour, activates 4 hours.
6. step 5 gained solid carbon being come out of the stove and putting into concentration immediately is that 25% hydrochloric acid soln soaked 1 hour, and being washed to PH is 5-6, dry, be crushed to 120 orders above 65 kilograms of finished product gacs.
7. step 3 is separated the filtrate that obtains and enter in the cooling pan, reduced in 60 minutes below 50 ℃, the cooling rate that slows down was then progressively reduced to solution temperature about 15 ℃ in three hours, separated out silicon-dioxide.The mixture of silica solid and sodium carbonate solution composition is carried out solid-liquid separation, isolated sodium carbonate solution Returning reactor again re-uses, the 250 kilograms of neutralizations of hydrochloric acid of concentration 15% of silicon-dioxide after the separation, in whizzer with deionized water wash, drying, pulverize 162.5 kilograms of finished product white carbon blacks.
The white carbon black performance that table 1 is produced for embodiment
| Project | Numerical value/character | Project | Numerical value/character |
| Form | White powder | Weight loss on heating % | 4 |
| Dioxide-containing silica % | 94 | PH value | 6—7 |
| The DBP oil-absorption(number) | 2.4 | Burning decrement | 3.2 |
| Specific surface area | 210 | Total iron content mg/kg | 20 |
The gac that table 2 is produced for embodiment
| Project | Numerical value | Project | Numerical value |
| Caramel decolorizing ability % | 110 | Calcium-magnesium content % | 0.12 |
| Inferior blue decolorizing ability ml/0.1g | 18 | Oxide compound % | 0.14 |
| PH value | 5.6 | Acid-soluble material % | 0.16 |
| Ignition residue | 3.0 | Iron level | 0.02 |
Claims (1)
1. production method of utilizing rice husk to prepare high-adsorption active carbon and white carbon black, may further comprise the steps: rice husk is gasified, the rice hull ash that obtains after the gasification is reacted with aqueous sodium carbonate under the pressurized conditions of heating, aqueous sodium carbonate concentration is 8%-15% during reaction, rice hull ash and aqueous sodium carbonate are pressed mass ratio 1: 30-40 reaction, reactor pressure 3-5Mpa, temperature 130-160 ℃, reaction times 2-3 hour; Through solid-liquid separation, the gained filter residue is to soak 5 hours, activation, pickling, washing, drying, pulverizing, packing in 10% iron(ic) chloride or the ferrous sulfate additive to make active carbon finished products through washing, in concentration, gained filtrate through cooling decompose, solid-liquid separation, neutralization, diafiltration, drying, pulverizing, packing are made the white carbon black finished product once more; The coal gas that rice husk gasification produces as thermal source by pipe-line transportation to the solid carbon manufacturing procedure, be supplied to washing, activation, pickling, drying process heating usefulness.
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| CN101486460B true CN101486460B (en) | 2011-07-27 |
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| CN102167319B (en) * | 2011-05-13 | 2013-03-13 | 江苏大学 | Method for preparing activated charcoal from vinegar residues |
| CN108640243A (en) * | 2018-05-16 | 2018-10-12 | 中国科学院新疆理化技术研究所 | A kind of method of synthesizing inorganic macromolecule coagulant poly-silicic acid iron sulfate |
| CN108927115A (en) * | 2018-07-17 | 2018-12-04 | 中国人民解放军海军航空大学青岛校区 | A kind of highly hygroscopic type desiccant of military mold-proof oxidation-resistant and preparation method thereof |
| CN113880088A (en) * | 2021-11-10 | 2022-01-04 | 广西民族大学 | Preparation method of papermaking sludge-based biochar |
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