CN107265500B - A kind of device of oxyhydrogen flame Hydrolyze method preparation high purity nanometer titania - Google Patents

A kind of device of oxyhydrogen flame Hydrolyze method preparation high purity nanometer titania Download PDF

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CN107265500B
CN107265500B CN201710277071.XA CN201710277071A CN107265500B CN 107265500 B CN107265500 B CN 107265500B CN 201710277071 A CN201710277071 A CN 201710277071A CN 107265500 B CN107265500 B CN 107265500B
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connect
pipe
furnace body
high pressure
mixed expanded
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CN107265500A (en
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吴兵生
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Xiantao Zhongxing Electronic Material Co ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00Compounds of titanium
    • C01G23/04Oxides; Hydroxides
    • C01G23/047Titanium dioxide
    • C01G23/053Producing by wet processes, e.g. hydrolysing titanium salts
    • C01G23/0536Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing chloride-containing salts
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/30Particle morphology extending in three dimensions
    • C01P2004/32Spheres
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/64Nanometer sized, i.e. from 1-100 nanometer
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/12Surface area
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity

Abstract

A kind of device of oxyhydrogen flame Hydrolyze method preparation high purity nanometer titania, including furnace body, TiCl4 input pipe, hydrogen-containing fuel pipe, water jacket is covered with outside the furnace body, refractory material layer is equipped in the furnace body, bottom of furnace body is equipped with reactant exit, the intracorporal top of furnace is equipped with burner noz(zle), burner noz(zle) is connect with mixed expanded bottom of the tube, mixed expanded pipe top is respectively equipped with oxygen gas connector, inert gas connector, high pressure outer cover is arranged with outside mixed expanded pipe, TiCl4 input pipe passes through to be connect in the middle part of high pressure outer cover and mixed expanded pipe, hydrogen-containing fuel pipe is connect with high pressure outer cover.

Description

A kind of device of oxyhydrogen flame Hydrolyze method preparation high purity nanometer titania
Technical field
The invention belongs to titanium dioxide production apparatus fields more particularly to a kind of oxyhydrogen flame Hydrolyze method preparation high-purity to receive The device of rice titanium dioxide.
Background technique
Titanium dioxide P25 is a kind of nanoscale white powder, and the hydroxyl group on surface makes it have hydrophily, and should Product does not have any pigment feature.The average grain diameter of basic granules is about 21nm, and the size of particle and the density of 4g/cm3 make Its special surface with 50m2/g.Titanium dioxide P25 belongs to mixed crystal type, and the weight ratio of anatase and rutile is about 71/ 29, since two kinds of mixing up of structure increase the intracell defect concentration of TiO2, the concentration of carrier is increased, electronics, hole are made Quantity increases, and makes it have the ability of solution components (water, oxygen, organic matter) of the stronger capture on the surface TiO2.Nanoscale Titanium dioxide has the performances such as excellent ultraviolet radiation absorption, photo-catalyst, decomposing organic pollutant, can be used for nano paint, empty Gas purifier, self-cleaning glass, ceramics etc..Nano-titanium dioxide antibacterial and mouldproof, exhaust gas purification, deodorization, water process, it is antifouling, The fields such as weather-proof anti-aging, automobile finish have a wide range of applications, it is in environment, information, material, the energy, medical treatment and health etc. Field has broad application prospects.
The titanium dioxide industry of China originates in mid-term the 1950s, but nanometer Ti02 powder product is recent five years The high-end product of listing, production technology is mainly by the De Gaosa company of Germany, the Cabot Corporation in the U.S., moral mountain Cao of Ff sheet It reaches, go out the monopolization of the large enterprises such as the emerging production of light, Osaka Ti industry company, the country still lacks this new and high technology.
Summary of the invention
The present invention provides a kind of device of oxyhydrogen flame Hydrolyze method preparation high purity nanometer titania, existing to solve Technical production is low, waste is big, the impurity of production is more, the uneconomical, technical problems such as not environmentally.
In order to solve the above technical problem, the technical solution used in the present invention is: prepared by a kind of oxyhydrogen flame Hydrolyze method The device of high purity nanometer titania, including furnace body, TiCl4 input pipe, hydrogen-containing fuel pipe, it is characterized in that the furnace body outer cover Equipped with water jacket, refractory material layer is equipped in the furnace body, bottom of furnace body is equipped with reactant exit, and the intracorporal top of furnace is equipped with burning Nozzle, burner noz(zle) are connect with mixed expanded bottom of the tube, and mixed expanded pipe top is respectively equipped with oxygen gas connector, inert gas Connector, mixed expanded pipe are arranged with high pressure outer cover outside, and TiCl4 input pipe passes through to be connect in the middle part of high pressure outer cover and mixed expanded pipe, Hydrogen-containing fuel pipe is connect with high pressure outer cover, and hollow fiber film assembly is equipped between the mixed expanded pipe and high pressure outer cover.
Preferably, the burner noz(zle) exit is equipped with igniter.
Preferably, the hydrogen-containing fuel pipe is connect with ammonia decomposer, ammonia decomposer is connect with ammonia head tank.
Preferably, the reactant exit is connect with transfer pump, transfer pump is connect with level-one spiral flocculator, level-one spiral shell Rotation flocculator is connect with spherical reaction kettle, and spherical reaction kettle is connect with deuterostrophies flocculator, the end of deuterostrophies flocculator It connect through piping with cyclone separator, is connect at the top of spherical reaction kettle with pulse gas transmitter.
The present invention is easy to get with raw material, product very high purity, reunion is less, gained particle diameter distribution is narrow, it is energy saving, mention High-purity increases the features such as efficiency.When the device works, hydrogen-containing fuel gas, oxygenated fuel gas and control flame combustion The inert gas of situation imports in burner noz(zle) mixing chamber, after mixing in spray nozzle front end ignition.Simultaneously unstripped gas Body is uniformly blended in burning gases, with combustion product vapor occur hydrolysis, and be aggregated into more than ten nanometer just Grade particle, primary particle through flocculation, ageing, again flocculate grow up i.e. can be used cyclone separator be collected, obtain nano-powder.This Invented technology can obtain that purity is 99.9%, flat diameter partial size is 25-35 nanometers, average specific surface in 50 m2/g, shape is ball Shape, the nano TiO 2 that crystal form is rutile-type or anatase titanium dioxide.
Detailed description of the invention
Fig. 1 is schematic structural view of the invention.
Specific embodiment
With reference to the accompanying drawings and detailed description, the technical solutions of the present invention will be further described.
As shown in connection with fig. 1, the oxyhydrogen flame Hydrolyze method prepare rutile type nano titanic oxide device include furnace body 9, TiCl4 input pipe 15, hydrogen-containing fuel pipe 61, the furnace body 9 are covered with water jacket outside, are equipped with refractory material layer 9, furnace in the furnace body Body bottom is equipped with reactant exit 93, and the intracorporal top of furnace is equipped with burner noz(zle) 5, and 5 exit of burner noz(zle) is equipped with igniting Device 51.Burner noz(zle) 5 is connect with mixed expanded 21 bottom of pipe, and mixed expanded 21 top of pipe is respectively equipped with oxygen gas connector 2, lazy Property gas connection 1, be arranged with high pressure outer cover 3 outside mixed expanded pipe, TiCl4 input pipe 15 pass through high pressure outer cover 3 with it is mixed expanded It is connected in the middle part of pipe 21, hydrogen-containing fuel pipe 61 is connect with high pressure outer cover, and doughnut is equipped between mixed expanded pipe and high pressure outer cover Membrane module 16.Hollow fiber film assembly has the doughnut of separation mixed gas function.Separation driving force is pressure difference, operation pressure Power is 0.098-9.8MPa, realizes that mixed gas is separated using transmitance difference, is gas or steam through object.Preparation method is to adopt Be made after more microporous homogeneous films with middle spinneret by thermoplastic resin melt-spun or by polymer solution dry-jet wet-spinning coat it is ultra-thin organic Silicon seperation film can also be passed through certain solidification liquids in hollow portion to form anisotropic membrane structure.For hydrogen-nitrogen, oxygen-nitrogen, methane- The mixed gas separations such as helium, alcohol-water and ethane, methane and ethylene.
Hydrogen-containing fuel pipe is connect with ammonia decomposer 7, and ammonia decomposer is connect with ammonia head tank 8.
Reactant exit 93 is connect with transfer pump 92, and transfer pump 92 is connect with level-one spiral flocculator 10, level-one spiral wadding Condenser 10 connect with spherical reaction kettle 12, and spherical reaction kettle 12 is connect with deuterostrophies flocculator 100, spherical reaction kettle top and Pulse gas generator 19 connects.The end of deuterostrophies flocculator 100 is connect through piping with cyclone separator.
Prepare liquefied ammonia, the TiCl4 that purity is 99%, pure, dry oxygen, inert gas.Oxygen is allowed to pass through oxygen gas Connector 2 is introduced directly into the mixed expanded pipe 21 of flame hydrolysis furnace, and inert gas carrier is directly led by another way inert gas connector 1 Enter the mixed expanded pipe 21 of flame hydrolysis furnace, effect is to prevent burner noz(zle) mouth from scabbing using the impacting with high pressure effect of air-flow.Ammonia The mixture of hydrogen and nitrogen obtained by decomposing is passed through hydrogen-containing fuel as hydrogen-containing fuel after the pressurization of air blower 6 by decomposer 7 Pipe 61 imports the high pressure outer cover 3 of mixed expanded pipe 21, using multiple hollow fiber film assemblies 16 by hydrogen penetrate into mixing it is swollen In tube expansion 21.
TiCl4 input pipe 15 passes through high pressure outer cover 3 and TiCl4 is introduced directly into the mixed expanded pipe 21 of flame hydrolysis furnace, each road Gas enters burning at burner noz(zle), hydrolysis after expansion tube 21 collects.Entire reaction occurs very fast, almost instantaneously into Capable entire reaction process is also rapider than in water, and under this hot conditions, the most important product Ti02 of hydrolysis.It is big absolutely Part is all existing for rutile-type.
The mixture that 9 bottom of furnace body comes out imports the flocculation of level-one flocculator by transfer pump.Aerosol is in flocculation pipe Flocculation is usually unable to being grown up completely to several microns for primary row, therefore using spherical reaction kettle ageing reaction+second level flocculation Mode solve, after the aerosol containing Ti02 particle stops 3-8 seconds again in flocculator flocculation, into spherical reaction kettle Ageing reaction 1-2 minutes, spherical reaction kettle top are connect with pulse gas generator 19, and pulse gas generator 19 is anti-to spherical shape It answers and is loaded into nucleation gas in kettle, nucleation gas carrier is nitrogen, potassium chloride, sodium aluminate mixed solution of the nucleating agent for 18%, wherein Potassium chloride: sodium aluminate=1:1.To promote Ti02 particle growth.
Mixture by ageing reaction enters second level through flocculator, flocculates, is able to achieve again through flocculator by second level 99.5% or more collection rate.Then it is separated in cyclone separator, the product oxide obtained from cyclone separator 81 is de- It collects to obtain product through product hopper after sour furnace depickling.The sweep gas mixture come out from cyclone separator carries out condensation process, cold Solidifying temperature is -23 DEG C, will be recycled after gas filtration.
Referring in 5.1.1, GB/T2511.4-85, GB/T3185-92 in GB/T 5211.20-1999, GB1706-9 5.7, GB/T 1717-86, GB/T 1716-79(89), GB/T 1713-89 Ti02 produced by the invention is detected, obtain Inspection result in following table.

Claims (4)

1. a kind of device of oxyhydrogen flame Hydrolyze method preparation high purity nanometer titania, including furnace body, TiCl4Input pipe contains Hydrogen fuel pipe is equipped with refractory material layer it is characterized in that being covered with water jacket outside the furnace body in the furnace body, bottom of furnace body is equipped with anti- Object is answered to export, the intracorporal top of furnace is equipped with burner noz(zle), and burner noz(zle) is connect with mixed expanded bottom of the tube, mixed expanded pipe top It is respectively equipped with oxygen gas connector, inert gas connector, high pressure outer cover, TiCl are arranged with outside mixed expanded pipe4Input pipe passes through It is connect in the middle part of high pressure outer cover and mixed expanded pipe, hydrogen-containing fuel pipe is connect with high pressure outer cover, outside the mixed expanded pipe and high pressure Hollow fiber film assembly is equipped between cover.
2. the device of oxyhydrogen flame Hydrolyze method preparation high purity nanometer titania according to claim 1, it is characterized in that The burner noz(zle) exit is equipped with igniter.
3. the device of oxyhydrogen flame Hydrolyze method preparation high purity nanometer titania according to claim 1, it is characterized in that The hydrogen-containing fuel pipe is connect with ammonia decomposer (7), and ammonia decomposer is connect with ammonia head tank.
4. the device of oxyhydrogen flame Hydrolyze method preparation high purity nanometer titania according to claim 1, it is characterized in that The reactant exit is connect with transfer pump, and transfer pump is connect with level-one spiral flocculator, and level-one spiral flocculator and spherical shape are anti- Kettle is answered to connect, spherical reaction kettle is connect with deuterostrophies flocculator, and the end of deuterostrophies flocculator is through piping and whirlwind point It connects from device, is connect at the top of spherical reaction kettle with pulse gas generator.
CN201710277071.XA 2016-08-31 2017-04-25 A kind of device of oxyhydrogen flame Hydrolyze method preparation high purity nanometer titania Active CN107265500B (en)

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CN109319836A (en) * 2018-10-16 2019-02-12 东北大学秦皇岛分校 TiO under a kind of electric field controls2The pyrolytic synthesis method of nano particle
CN113198390A (en) * 2021-05-28 2021-08-03 哈尔滨学院 High-efficient processingequipment of nanometer titanium dioxide

Citations (4)

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Publication number Priority date Publication date Assignee Title
CN1391078A (en) * 2001-06-11 2003-01-15 中国科学院化工冶金研究所 Oxidizing furnace able to remove scar by spraying titanium oxide particles and chlorination process and its method for removing scar
CN1721328A (en) * 2005-05-31 2006-01-18 昆明理工大学 Method and apparatus for preparing fumed nano oxide
CN1736879A (en) * 2005-07-21 2006-02-22 华东理工大学 Preparation method of gas phase nano titanium dioxide with average grain size
WO2006135272A1 (en) * 2005-06-14 2006-12-21 Mikhail Alexeevich Gorovoi Installation for synthesis of titanium dioxide and plasma chemical reactor

Patent Citations (4)

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Publication number Priority date Publication date Assignee Title
CN1391078A (en) * 2001-06-11 2003-01-15 中国科学院化工冶金研究所 Oxidizing furnace able to remove scar by spraying titanium oxide particles and chlorination process and its method for removing scar
CN1721328A (en) * 2005-05-31 2006-01-18 昆明理工大学 Method and apparatus for preparing fumed nano oxide
WO2006135272A1 (en) * 2005-06-14 2006-12-21 Mikhail Alexeevich Gorovoi Installation for synthesis of titanium dioxide and plasma chemical reactor
CN1736879A (en) * 2005-07-21 2006-02-22 华东理工大学 Preparation method of gas phase nano titanium dioxide with average grain size

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Title
氢氧火焰水解法制备纳米TiO2技术研究;冉青荣;《中国优秀硕士学位论文全文数据库 工程科技I辑》;20051215(第8期);第47页最后一段-第49页倒数第二段,第54页倒数第二段,第55页第3段,第56页最后一段,第57页第2段,第59页最后一段,第60页表4-1,第66页最后一段,图4-2,图4-5,图4-6

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