CN1803599A - Process and apparatus for preparing high-purity silicon dioxide by utilizing rice hull - Google Patents
Process and apparatus for preparing high-purity silicon dioxide by utilizing rice hull Download PDFInfo
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- CN1803599A CN1803599A CN 200510031636 CN200510031636A CN1803599A CN 1803599 A CN1803599 A CN 1803599A CN 200510031636 CN200510031636 CN 200510031636 CN 200510031636 A CN200510031636 A CN 200510031636A CN 1803599 A CN1803599 A CN 1803599A
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Abstract
The disclosed method to prepare high-pure silicon dioxide with rice hull comprises: sieving the rice hull to remove sand and dust, drying hull and distillating to char the hull at 400-500Deg, and recovering chemical compound and gas; acid washing the hull to remove the alkali metal impurity, and drying the hull to obtain the silicon nitride, silicon carbide and carbon-containing crystal whisker material; controlling temperature 500-600Deg to burn and obtain the amorphous silicon dioxide as material for silicon nitride and silicon carbide; or acid washing to remove the alkali metal impurity, cleaning with pure water directly to obtain hihg-pure ultrathin white carbon black product.
Description
Technical field
The present invention relates to a kind of biomass extracting method, refer in particular to a kind of method of from rice husk, extracting high-purity amorphous silica, relate to a kind of device that from rice husk, extracts high-purity amorphous silica simultaneously, be mainly used in rice husk and make in the Chemical Pretreatment technology of silicon-based ceramic material.
Background technology
Silicon-dioxide is rich in many natural resourcess, does not almost exist with high-purity amorphous form.The silicon-dioxide of being found in the inorganics of natural resources is typical crystal habit, and contains inorganic impurity, and the effect of the silicon-dioxide of this crystalloid shape is also little.On the contrary, contained silicon-dioxide is the amorphous structure form in the biomass, the effect of the silicon-dioxide of this amorphousness shape can be just big, particularly in hard-core technologies such as making special cermacis blade, all uses the precursor of the silicon-dioxide of high-purity amorphousness shape as silicon based ceramic.But contained silicon-dioxide all contains organic impuritys such as comprising various hydrocarbon polymers and micro-inorganic impurity in the existing biomass, so must carry out purification processes.As everyone knows, rice husk has quite high-load inorganics composition, and near the 20wt% of dried rice husk, wherein 94wt% is a silicon-dioxide, and all the other 6wt% comprise K
2O, CaO, MgO, MnO, Al
2O
3, P
2O
5, content successively decreases successively, and they are called impurity because of the performance that changes the silicon-dioxide that extracts from rice husk.Main butt organic compound is Mierocrystalline cellulose and hemicellulose 50wt%, and xylogen 26wt%, all the other 4wt% are other organism such as grease, protein etc.Organism and inorganics composition depend on following Several Factors: weather, soil and kind.Amorphous and the white silicon-dioxide that extracts from rice husk and rice bar has very high specific surface area, the component of rice bar (comprising leaf) is a silica 1 3.1, Mierocrystalline cellulose 37.4, hemicellulose 44.9 and xylogen 4.9, the weight ratio of rice bar and rice husk is near 3.6,300,000,000 tons of rice are produced in the whole world per year, show that the potential silicon-dioxide turnout from rice husk and rice bar reaches 4,000 ten thousand tons.People are inquiring into the silicon-dioxide that how to propose high-purity amorphousness shape from rice husk always now.Rice husk is the same with other biomass in fact, mainly is made up of Mierocrystalline cellulose, hemicellulose and three kinds of main extracts of forming branch and some solubility polarity or weak polar solvent of xylogen.Analyze from the biomass through pyrolysis reaction mechanism, three kinds of main constituents of biomass are usually supposed to carry out independently thermolysis, and hemicellulose is mainly 225～350 ℃ of decomposition, and Mierocrystalline cellulose is mainly 325～375 ℃ of decomposition, and xylogen is 250～500 ℃ of decomposition.Mierocrystalline cellulose and hemicellulose mainly produce volatile matter, and xylogen mainly resolves into charcoal.
The thermal cracking processes of biomass is divided into three phases:
(1) carburation by evaporation at first after the water molecules of dehydration in the biomass material is heated;
(2) material decomposes under anoxia condition is separated out in the decomposition of volatile matter, along with temperature raises, and corresponding the separating out of various materials in the material.Though material reaches point of ignition, do not burn owing to anoxic, gas phase flame can not appear;
(3) charing along with the deep layer volatile matter to outer field diffusion, finally form biomass charcoal.
Therefore, the most reliable method of organic matter removal in the biomass promptly is thermo-cracking (comprising destructive distillation, charing and burning).
Alkali metal maximum possible in the rice husk is scattered in organic substrate such as the hydrocarbon polymer, or with xylogen or other organic compound a little less than combine.In dried rice husk, these alkali metal impurity elements do not mix with silicon-dioxide or combine.
Silicon-dioxide in the rice husk not with acid (except that HF) react with, and impurity element such as sodium, calcium, magnesium, potassium, manganese, iron etc. and sour react with, therefore, be in the technical process of the high-purity silicon dioxide of feedstock production by rice husk, the pickling cell process process that is absolutely necessary.
Silicon-dioxide in the rice husk at high temperature (as being higher than 650 ℃) can generate the silicate of molten state with the alkalimetal oxide react with, in higher reaction sintering temperature (as being higher than 1100 ℃), soft silica can become crystalline silicon dioxide, and loses the reactive behavior of further silicon carbide reaction-sintered, silicon nitride ceramic particles and whisker or silicon tetrachloride.
Can be found out by above-mentioned analysis, be feedstock production highly pure active charcoal, high-purity silicon dioxide and silicon-based ceramic material and silicoorganic compound with rice husk, and pickling and temperature control dry distillation charring and controlled temperature combustion technology are integrated to be the best-of-breed technology scheme.
With rice husk is feedstock production highly pure active charcoal, high-purity silicon dioxide and silicon-based ceramic material and silicoorganic compound, and existing many patent documentation notes are cut out.
Ramsey, Jr, et aL. USP 4, the technical process that rice husk prepares silicon carbide whisker has been described in 248,844 (February 3,1981), the SiC whisker be by sorting a large amount of be the material that raw material forms through two portions technology with the rice husk, at first carbonization under oxygen-free atmosphere incinerates another part rice husk in air atmosphere, with carbonization residue after the carbonization and unbodied silicon-dioxide SiO
2Heating obtains the SiC whisker in inert atmosphere.Do not mention the pickling of raw material and the control of carbonization temperature and temperature of combustion.
Shipley USP 6,406,678 (June 18,2002) technical process that rice husk prepares high purity ultra-fine silicon dioxide has been described, from containing the biological material of soft silica, especially rice husk, the technological process of producing high-purity soft silica is: at first adopt oxygenant to interrupt long-chain organic compound in the biomass, yet organic compound is removed in thermooxidizing, can adopt pulverizing before the oxidizer treatment technology, screening, the tensio-active agent washing, rinsing and being soaked in the water to quicken and to strengthen the infiltration of oxygenant, remaining silica pure water rinsing behind the thermal silicon dioxide oxidation removal volatile impunty, pickling obtains the silicon-dioxide of high pure and ultra-fine white at last to remove trace impurity.Though mention pickling, pickling is the preliminary processes of this method, and does not consider the control of temperature of combustion.
Ouyang's east Ji'nan University's Chinese patent (application number 200410026459.5) has been described a kind of rice husk incinerator, the nanostructure SiO of a kind of rice husk incinerator and output thereof
2Rice hull ash, this incinerator comprises an incinerating container, is distributed with many apertures on the container floor, is distributed with the heat exchange water pipe in the container, control incineration temperature in the rice husk below 600 ℃ by the distribution density of regulating the heat exchange water pipe, can guarantee that the rice hull ash of producing is nanostructure SiO
2Rice hull ash, and utilized the heat energy that burning process produced, also solved the restricted problem of rice husk stacking volume simultaneously.Though mention incineration temperature control, do not relate to pickling.
Jilin University's Chinese patents (application number 03133335.4) such as prince's sincere feeling have been described a kind of method for preparing high-purity nm silicon-dioxide from rice husk, it comprises the steps: that preparation concentration is the mineral acid treatment agent of 1～20wt% earlier, by 2～50: 1 weight ratio adds rice husk in treatment agent, boil 0.5～3h, through washing, drying, again rice husk was burnt 15～180 minutes down in 600～900 ℃ of environment, it is that 30～80nm, purity are 98～99% nano silicon that products of combustion obtains particle diameter after crushed, and used treatment agent is hydrochloric acid or sulfuric acid.The combustion heat of rice husk reclaims, the drying etc. that is used to handle rice husk with heat or other with heat as heating, bathing pool etc.It is first pickling, and afterfire can not be reclaimed chemical such as wooden vinegar, and sour consumption is very big.
The auspicious patent of Zhao Zhi (application) number (94111512.7) has been described with husk and has been produced the sooty method, remove shrivelled kernel, earth in the husk earlier, handling husk with inorganic acid solution then also stirs to remove metallic impurity or the bio-ligand in the husk, then wash hydrogen ion, metallic impurity or the bio-ligand on husk surface with treated water, last heating flame husk can obtain white carbon black.Though mention the raw material pickling, do not relate to controlled temperature combustion, can not reclaim chemical such as wooden vinegar, sour consumption is very big.
Poplar earlier and Research Institute of Highway, Ministry of Communications apply for (patent) number: 92100466.4 in the rice husk method of extraction of highly pure silica: rice husk or rice hull ash are placed in the sealed can, add concentrated nitric acid and concentration then respectively and be 30% hydrogen peroxide, tighten sealed tank cap, be incubated 3 hours down in 150 ℃; Naturally cool to room temperature, open sealed tank cap, be washed till neutrality, can obtain purity and be the silicon-dioxide more than 99.99% with deionized water.
Jair C.C.Freitas, Jean S.Moreira, Francisco G.Emmerich, Tito J.Bonagamba (Development ofSi/C/N/O ceramics from pyrolyzed and heat-treated rice hulls) introduces rice husk system silicon based ceramic technology, by the silicon compound (SiO that is scattered in the rich charcoal matrix
2, Si
2N
2O, Si
3N
4And SiC) makes silicon based ceramic by rice husk thermo-cracking and 1450～1700 ℃ of pyroreaction sintering treatment production.The product category difference, pyroreaction sintering atmosphere (N
2Or Ar) different with heating rate.The result proves and adopts rice husk to account for the feasibility that the silicon compound of dominating in the structure combines the potting ceramic material as the presoma of ceramic material with carbon containing matter.Do not mention the pickling of raw material and the control of carbonization temperature and temperature of combustion.
EGAMI KO JP 11-050060 (CARBONIZATION APPARATUS FOR RICE HULL 23.02.1999) has described a kind of charred rice husk device, burner and many heating tubes are arranged in the combustion chamber, certain space is arranged between the heating tube and pass the top board and the base plate of heating chamber.Rice husk adds by the funnel on combustion chamber and the burner top board, and the combustion chamber is heated to high temperature with burner.When heating tube during from indirect heating, the rice husk in the heating tube is heated and charing, and when the air throttle of heating tube bottom was opened, charring rice husk was fallen into material storing room.The unburned gas that produces in the heating tube is sent into heating chamber by flue tube, on the flue tube condenser must be housed, so that collect black liquor.Do not mention the pickling of raw material and the control of carbonization temperature.
NAGASAKI HIROMI JP 2001-335782 (CARBONIZATION APPARATUS 04.12.2001) has described a kind of charred rice husk device, the carbonizing apparatus of energy perfect combustion flue dust is made up of following technology: reactor is filled pending material, when lighting the pending material of reactor bottom, the airduct at blast pipe top is opened, the gas blower air blast, blast pipe rises to the reactor top off and on, deliver to the whole burner hearth charring rice husk of reactor thereby keep watch, black liquor collection box and flue dust roasting kiln are used to handle the flue dust that carbonization process produces.Carbonization still internal equipment the igniting thermal source, air trunking can move up and down at reaction chamber, this invention is the carbonizing apparatus of air blast in short-term in continuously carbonizing husk or timber bits process, and contains the black liquor of burnt oil and vinegar and the stack gas that thermal treatment contains burning gas in the collecting flue gas continuously in the device back.Do not mention the pickling of raw material and the control of carbonization temperature.
WADAICHIRO JP09-255964 (PROCESS AND APPARATUS FOR PRODUCING HIGHLYACTIVE RICE HULL ASH 30.09.1997) has described the production method of high reactivity rice hull ash, the top layer of the indoor rice husk heap of ignition combustion, lead cigarette and charring rice husk by from the top to bottom direction, the ash that goes out charing blasts at the rice husk bottom and to contain combustion exhaust and Air mixing combustion gas from bottom to top.Do not mention the pickling of raw material and the control of carbonization temperature.
VINOGRADOVVV; Etc.RU2163708 has described the device of rice husk production silicon-dioxide, and it comprises, and heating chamber, fire door, burn pot, top cover, axle, hybrid blade, stone roller roll, control lever.Axle is by electric motor driving, and rice husk is packed into from the feeder compartment, and fire box temperature is heated to 300～500 ℃, till rice husk burns and drains to black smoke.The incendiary rice husk contains ferric oxide and is no more than 0.05%, carbon black 5～7%.
U.S.Pat.No.3, Gravel has described a technology in 125,043: a rice husk upwards flows (about 500 ℃～800 ℃) in high temperature air, and the ash of generation is made up of soft silica, but still containing 2-10% impurity, impurities is too many concerning many application.
American documentation literature put down in writing the employing nanometer grade silica (vapor phase process production, granularity be 15～30nm) and carbon at high temperature sintering reaction generate silicon carbide whisker, the whisker production rate can reach 50% (general whisker production rate is up to 35%); China and United States Patent (USP) reported respectively with rice husk and can produce high purity ultra-fine silicon dioxide, and granularity is 30～80nm, and purity is more than 99.5%.
More than relevant patented technology and research have all illustrated a problem, by rice husk through suitable technology (mainly being thermo-cracking and pickling) but the gac of production high added value, silicon-dioxide and silicon-based ceramic material, but all system optimization research is not carried out in technical process in the existing technical literature, especially how to adopt the Green Chemistry pretreatment technology to lack research, and to contain acid treatment process mostly all be roasting after the first acid treatment, such acid treatment amount is very big, rice husk elder generation's pickling roasting again, the consumption of acid is very big, and strong acid is to organism such as Mierocrystalline cellulose, hemicellulose and the wooden corrosive nature that have, during roasting as adopting two sections burning (first anoxic charings, oxygen-enriched combusting again), chemical and energy recovery rate all seldom so pollution is also big, are unfavorable for industrial applications.
Summary of the invention
One of purpose of the present invention is the specification of quality according to the high pure and ultra-fine silicon-based ceramic material, and providing a kind of is the Chemical Pretreatment processing method of feedstock production high-purity silicon dioxide processing method with the rice husk.
What two of purpose of the present invention provided a kind of above-mentioned processing method is the Chemical Pretreatment device of feedstock production high-purity silicon dioxide processing method with the rice husk.
According to the technology implementation scheme that purpose of the present invention proposed be: the method that adopts conventional roasting and pickling to combine is extracted the silicon-dioxide in the rice husk, its characteristics are that technology of the present invention is earlier silt particle, dust to be removed in rice husk screening earlier, dry then rice husk, the temperature control dry distillation charring obtains charring rice husk and reclaims chemical and rice husk gas again, the control temperature of temperature control dry distillation charring is 400-500 ℃, does not change with the active condition that keeps silicon-dioxide in the rice husk.Again alkali metal impurity element in the charring rice husk is removed in the charring rice husk pickling, the used acid of pickling charring rice husk is hydrochloric acid or citric acid and acetate, the tap water pickling charring rice husk of handling with microfiltration membrane is to washings pH value=5.5-6.2, the membrane integrating technique that the acid-bearing wastewater that is produced during pickling adopts ion-exchange and embrane method to reclaim is handled, and the hot water that while temperature control dry distillation charring and controlled temperature combustion produced is used for pickling, washing thermal source.Charring rice husk after the dry again washing acid treatment can make silicon nitride, silicon-carbide particle and whisker and contain carbon feedstock; Exsiccant being washed charring rice husk after the acid treatment carries out controlled temperature combustion and just obtains soft silica as silicon nitride, silicon carbide whisker silicon-containing material again, the control temperature of controlled temperature combustion is 500-600 ℃, does not change with the active condition that keeps silicon-dioxide in the rice husk.Also can directly obtain high pure and ultra-fine white carbon black product in charred rice husk pickling removal charring rice husk behind the alkali metal impurity element with pure water washing controlled temperature combustion pickling charring rice husk.
Used process unit comprises drying installation, temperature control destructive distillation or carbonizing apparatus, pickler and controlled temperature combustion device in this technology, so its characteristics are a kind of device of thin bed temperature control method for destructive distillation at temperature control destructive distillation or carbonizing apparatus, and the controlled temperature combustion device is a kind of annular firing stove, and pickler is a kind of washing device of handling with microfiltration membrane.And reclaim the chemical that the rice husk dry distillation charring produces and the retrieving arrangement of rice husk gas in described temperature control destructive distillation or the carbonizing apparatus in addition; Described controlled temperature combustion device is inside and outside water cycle cooling controlled temperature combustion device.
Adopt the inventive method, rice husk is dry earlier, the temperature control dry distillation charring, pickling then, chemical and energy recovery have been guaranteed in the technical process to greatest extent, rice husk weight after the charing has only 40% of raw material rice husk, bulk density after the charring rice husk fragmentation is 1.3～2 times of raw material rice husk, when charring rice husk spent pickling acid amount and acid-bearing wastewater generation have only the raw material pickling 1/3～1/4, and rice husk produces porous organization through charing, the infiltration and the biomass combustion that help acid, charring rice husk burns time ratio raw material rice husk much shorter, burn the back carbon content and significantly reduce, improved the purity of product.
Accompanying drawing and explanation
Figure 1 shows that this invented technology flow process (dotted portion is Chemical Pretreatment technology of the present invention among the figure);
Figure 2 shows that temperature control retorting carbonization device principle schematic;
Figure 3 shows that an embodiment of temperature control retorting carbonization device heating tube layout;
Figure 4 shows that another embodiment of temperature control retorting carbonization device heating tube layout;
Figure 5 shows that temperature control pickling charring rice husk combustion unit principle schematic.
Among the figure: 1, rice husk; 2, combustion chamber; 3, combustion tail gas vapor pipe; 4, temperature thermocouple; 5, row heating tube; 6, burner noz(zle); 7, charring rice husk material storing room; 8, porous wall inner cylinder; 9, air door at the bottom of the heating tube; 10, destructive distillation flue gas exhaust pipe; 11, condenser; 12, black liquor collecting chamber; 13, condensation black liquor tapping valve; 14, rice husk bin stock radiant heat drying storehouse; 15, rice husk feeding pipe; 16, rice husk feeding pipe port strobe; 17, rice husk bin stock radiant heat drying storehouse upper cone body; 18, rice husk bin stock radiant heat drying storehouse bottom old name for the Arabian countries in the Middle East ground cone; 19, storage bunker discharge port part; 20, feed regulated valve; 21, safe pressure valve; 22, dry damp and hot (cigarette) gas is through vapor pipe; 31, roasting kiln body; 32, the conical porous cylindrical body in top; 33, the outer water jacket of rectangular cross-section cooling; 34, combustion chamber; 35, rectangular cross-section or circular cross section cooling inner water sleeve; 36, discharge gate; 37, gas inlet pipe; 38, smoke discharge tube; 39, water outlet; 40 temperature thermocouples; 41, admission port; 42, water-in; 43, water outlet 44, charring rice husk material bin stock radiant heat drying storehouse.
Embodiment
The invention will be further described below in conjunction with accompanying drawing, and accompanying drawing 1 is a technological principle synoptic diagram of the present invention.From accompanying drawing as can be seen, the present invention is chemical technology method and the device thereof that a kind of rice husk extracts silicon-dioxide, its operational path is: the method that adopts conventional roasting and pickling to combine is extracted the silicon-dioxide in the rice husk, its characteristics are that technology of the present invention is earlier silt particle, dust to be removed in rice husk screening earlier, dry then rice husk, the temperature control dry distillation charring obtains charring rice husk and reclaims chemical and rice husk gas again, the control temperature of temperature control dry distillation charring is 400-500 ℃, does not change with the active condition that keeps silicon-dioxide in the rice husk.Again alkali metal impurity element in the charring rice husk is removed in the charring rice husk pickling, the used acid of pickling charring rice husk is hydrochloric acid or citric acid and acetate, the tap water pickling charring rice husk of handling with microfiltration membrane is to washings pH value=5.5-6.2, the membrane integrating technique that the acid-bearing wastewater that is produced during pickling adopts ion-exchange and embrane method to reclaim is handled, and the hot water that while temperature control dry distillation charring and controlled temperature combustion produced is used for pickling, washing thermal source.Charring rice husk after the dry again washing acid treatment can make silicon nitride, silicon-carbide particle and whisker and contain carbon feedstock; Exsiccant being washed charring rice husk after the acid treatment carries out controlled temperature combustion and just obtains soft silica as silicon nitride, silicon carbide whisker silicon-containing material again, the control temperature of controlled temperature combustion is 500-600 ℃, does not change with the active condition that keeps silicon-dioxide in the rice husk.Also can in charred rice husk pickling removal charring rice husk behind the alkali metal impurity element, directly obtain high pure and ultra-fine white carbon black product with the pickling charring rice husk behind the pure water washing controlled temperature combustion.
Embodiment one
A kind of rice husk that utilizes is produced the high-purity silicon dioxide processing method, and its processing step is:
1, silt particle, dust are removed in rice husk screening earlier;
2, the rice husk after will sieving places the drying oven inner drying;
3, more dried rice husk is sent into and carried out the temperature control dry distillation charring in the temperature control retorting carbonization device and obtain charring rice husk, and recovery chemical and rice husk gas, it is 400 ℃ that the rice husk of temperature control dry distillation charring places control temperature, do not change with the active condition that keeps silicon-dioxide in the rice husk, the hot water that while temperature control dry distillation charring is produced is used for pickling, washing thermal source;
4, again charring rice husk is placed removal charring rice husk alkali metal impurity element in the pickler, the used acid of pickling charring rice husk is 5% hydrochloric acid, the tap water pickling charring rice husk of handling with microfiltration membrane is to washings pH value=5.5, and the acid-bearing wastewater that is produced during pickling adopts the membrane integrating technique of ion-exchange and embrane method recovery to handle;
5, the charring rice husk after the dry again washing acid treatment can make silicon nitride, silicon-carbide particle and whisker and contains carbon feedstock;
6, exsiccant being washed charring rice husk after the acid treatment carries out controlled temperature combustion and just obtains soft silica as silicon nitride, silicon carbide whisker silicon-containing material again, the control temperature of controlled temperature combustion is 500 ℃, does not change with the active condition that keeps silicon-dioxide in the rice husk.
Embodiment two
A kind of rice husk that utilizes is produced the high-purity silicon dioxide processing method, its processing step is the same with embodiment one, just to place control temperature be 450 ℃ to the rice husk of temperature control dry distillation charring, and the control temperature of controlled temperature combustion is 550 ℃, and the used acid of pickling charring rice husk is 15% citric acid.
Embodiment three
A kind of rice husk that utilizes is produced the high-purity silicon dioxide processing method, it is 490 ℃ that its processing step places control temperature with the embodiment one the same just rice husk of temperature control dry distillation charring, the control temperature of controlled temperature combustion is 600 ℃, the used acid of pickling charring rice husk is 15% acetate, and after the step 5 of implementing embodiment one, carry out controlled temperature combustion again, obtain high pure and ultra-fine white carbon black product with the pure water washing.
Its device of implementing technology of the present invention comprises rice husk screening, drying, temperature control dry distillation charring, charring rice husk pickling and washing, controlled temperature combustion, flue gas condensing, embrane method system water and ion-exchange+unit operations such as embrane method spent acid recovery, and wherein temperature control retorting carbonization device+charring rice husk pickling and pickling charring rice husk calciner are the key technical problems that the present invention solves.Accompanying drawing 2-5 has provided and has implemented the temperature control retorting carbonization device of technology of the present invention and an embodiment of controlled temperature combustion device.Temperature control retorting carbonization device of the present invention as can be seen is thin bed temperature control destructive distillation device from accompanying drawing, comprise that cloth multiple row heating tube 5 is made coking chamber in the combustion chamber 2, temperature thermocouple 4, heating tube steel or pottery are made, heating tube is a concentric cylinder, the annular space of inside and outside circle cylinder is a coking chamber, inner cylinder 8 is porous walls, air door 9 is adjustable at the bottom of the heating tube, burner noz(zle) 6 is the assisted gas nozzle, divide four jiaos of symmetrical distributions, the flue gas that destructive distillation produces is through vapor pipe 10 and the condenser 11 that is installed on the vapor pipe 10, black liquor collecting chamber 12 enters combustion chamber 2, the condensation black liquor is collected by tapping valve 13 discharging regularly, rice husk enters the top of charing heating tube 5 through bin stock radiant heat drying storehouse 14, establish safe pressure valve 21 on the bin stock radiant heat drying storehouse 14, and dry damp and hot (cigarette) gas that produces enters condenser 11 through vapor pipe 22, top, combustion chamber cloth water-cooled tube is carried out temperature of combustion control.Heating tube 5 can adopt two kinds of distribution modes, and the five equilibrium that can be square is arranged, also can be intersecting parallels and arrange that the distribution principle is that the thermal field of each heat pipe is similar.
And charring rice husk controlled temperature combustion device is the annular firing stove, comprise roasting kiln body 31, the conical porous cylindrical body 32 in top, the outer water jacket 33 of rectangular cross-section cooling, combustion chamber 34, rectangular cross-section or circular cross section cooling inner water sleeve 35, discharge gate 36, gas inlet pipe 37, smoke discharge tube 38, cool off outer water jacket 33 admission ports 41 and water outlet 39, temperature thermocouple 40, cooling inner water sleeve 35 water-ins 42 and water outlet 43, the charring rice husk material enters the top of combustion chamber 34 through bin stock radiant heat drying storehouse 44, establish safe pressure valve 21 dry damp-heats of discharging on the bin stock radiant heat drying storehouse 44 and enter chimney through smoke discharge tube 22.Inside and outside water cooling tube adopts the spirane structure form of circle or rectangular cross-section, is that the Dien whirlpool secondary stream in the crooked pipeline can the reinforcing mass transfer effect.
Claims (9)
1, a kind of rice husk that utilizes is produced the high-purity silicon dioxide processing method, the method that adopts conventional roasting and pickling to combine is extracted the silicon-dioxide in the rice husk, it is characterized in that described processing method is that rice husk is carried out earlier carrying out acid treatment again behind the temperature control dry distillation charring, earlier the exsiccant rice husk is adopted the charing of thin bed temperature control dry distillation to remove the rice husk organic substance and obtain charring rice husk, and then remove alkali metal impurity element in the charring rice husk with pickling, the acid-treated charring rice husk of dry again washing makes silicon nitride, silicon-carbide particle and whisker contain carbon feedstock, wash the silicon-dioxide that acid-treated charring rice husk is produced high-purity amorphousness shape by the controlled temperature combustion exsiccant again.
2, a kind of a kind of processing method of utilizing rice husk to produce high-purity silicon dioxide as claimed in claim 1, it is characterized in that described processing method is rice husk and removes in the charring rice husk behind the alkali metal impurity element in the charing pickling, directly, obtain high pure and ultra-fine white carbon black product with the pickling charring rice husk behind the pure water washing controlled temperature combustion.
3, a kind of a kind of processing method of utilizing rice husk to produce high-purity silicon dioxide as claimed in claim 1 or 2, the control temperature that it is characterized in that described temperature control dry distillation charring is 400 ℃-500 ℃, does not change with the active condition that keeps silicon-dioxide in the rice husk.
4, a kind of a kind of processing method of utilizing rice husk to produce high-purity silicon dioxide as claimed in claim 1 or 2, it is characterized in that the used acid of described pickling charring rice husk is hydrochloric acid or citric acid and acetate, during pickling be with clear water with the charring rice husk rinsing to washings pH value=5.5-6.2.
5, a kind of a kind of processing method of utilizing rice husk to produce high-purity silicon dioxide as claimed in claim 1, the control temperature that it is characterized in that described controlled temperature combustion is 500 ℃-600 ℃, does not change with the active condition that keeps silicon-dioxide in the rice husk.
6, a kind of a kind of processing method of utilizing rice husk to produce high-purity silicon dioxide as claimed in claim 1 or 2, the membrane integrating technique that the acid-bearing wastewater that is produced when it is characterized in that pickling adopts ion-exchange and embrane method to reclaim is handled, and the hot water that while temperature control dry distillation charring and controlled temperature combustion produced is used for pickling, washing thermal source.
7, a kind of a kind of device that utilizes rice husk to produce the processing method of high-purity silicon dioxide as claimed in claim 1, comprise drying installation, temperature control destructive distillation or carbonizing apparatus, pickler and controlled temperature combustion device, it is characterized in that temperature control destructive distillation or carbonizing apparatus are a kind of devices of thin bed temperature control method for destructive distillation, and the controlled temperature combustion device is a kind of annular firing stove, and pickler is a kind of washing device of handling with microfiltration membrane.
8, a kind of a kind of device that utilizes rice husk to produce the processing method of high-purity silicon dioxide as claimed in claim 7 is characterized in that reclaiming in addition in described temperature control destructive distillation or the carbonizing apparatus chemical of rice husk dry distillation charring generation and the retrieving arrangement of rice husk gas.
9, a kind of a kind of device that utilizes rice husk to produce the processing method of high-purity silicon dioxide as claimed in claim 7 is characterized in that described controlled temperature combustion device is inside and outside water cycle cooling controlled temperature combustion device.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510031636 CN1803599A (en) | 2005-05-31 | 2005-05-31 | Process and apparatus for preparing high-purity silicon dioxide by utilizing rice hull |
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| CN 200510031636 CN1803599A (en) | 2005-05-31 | 2005-05-31 | Process and apparatus for preparing high-purity silicon dioxide by utilizing rice hull |
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| CN101838946A (en) * | 2010-05-07 | 2010-09-22 | 李平 | Method for comprehensively treating silicon tetrachloride and papermaking pulping black liquor |
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| CN101503193B (en) * | 2008-10-17 | 2011-09-07 | 株洲兴隆化工实业有限公司 | White carbon black drying system using fire coal circulating fluid bed hot-air furnace |
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