A kind of oxyhydrogen flame stove for preparing rutile type nano titanic oxide
Technical field
The invention belongs to titanium dioxide production apparatus field, more particularly to a kind of rutile type nano titanic oxide for preparing
Oxyhydrogen flame stove.
Background technology
Titanium dioxide P25 is a kind of nano level 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 4g/cm3 density make
It has 50m2/g special surface.Titanium dioxide P25 belongs to mixed crystal type, and the weight ratio of anatase and rutile is about 71/
29, because two kinds of mixing up of structure increase the intracell defect concentrations of TiO2, the concentration of carrier is increased, makes electronics, hole
Quantity increase, makes it have solution components of the stronger capture on TiO2 surfaces(Water, oxygen, organic matter)Ability.Nanoscale
Titanium dioxide, there is the performances such as excellent ultraviolet radiation absorption, photo-catalyst, decomposing organic pollutant, available for nano paint, empty
Gas purifier, self-cleaning glass, ceramics etc..Nano titanium oxide 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, and 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 1950s mid-term, but nanometer Ti02 powder products are recent five years
The high-end product of listing, production technology is mainly by the De Gaosa companies of Germany, the Cabot Corporation in the U.S., moral mountain Cao of Ff sheets
Reach, the emerging production of light extraction, the monopolization of the large enterprise such as Osaka Ti industry company, the country still lacks this new and high technology.
The content of the invention
The present invention provides a kind of oxyhydrogen flame stove for preparing rutile type nano titanic oxide, to solve prior art production
Amount is low, it is more to waste big, production impurity, the uneconomical, technical problem such as not environmentally.
In order to solve above technical problem, the technical solution used in the present invention is:
A kind of oxyhydrogen flame stove for preparing rutile type nano titanic oxide, it is characterized in that using a kind of oxyhydrogen flame stove system
Standby rutile type nano titanic oxide, the oxyhydrogen flame stove is included outside body of heater, TiCl4 input pipes, hydrogen-containing fuel pipe, the body of heater
It is covered with water jacket, the body of heater and is provided with refractory masses, the top that bottom of furnace body is provided with reactant exit, body of heater is provided with combustion
Nozzle is burnt, burner noz(zle) is connected with mixed expanded bottom of the tube, and mixed expanded pipe top is respectively equipped with oxygen gas joint, indifferent gas
High pressure outer cover is arranged with outside body joint, mixed expanded pipe, TiCl4 input pipes are through high pressure outer cover with connecting in the middle part of mixed expanded pipe
Connect, hydrogen-containing fuel pipe is connected with high pressure outer cover, hollow fiber film assembly is provided between the mixed expanded pipe and high pressure outer cover;Institute
State hydrogen-containing fuel pipe to be connected with ammonia decomposer, ammonia decomposer is connected with ammonia head tank;The reactant exit is connected with transhipment pump,
Transhipment pump is connected with one-level spiral flocculator, and one-level spiral flocculator is connected with spherical reactor, spherical reactor and two grades of spiral shells
Flocculator connection is revolved, the end of deuterostrophies flocculator is connected through piping with cyclone separator, spherical reactor top and arteries and veins
Rush gas generator connection;
The preparation method comprises the following steps:A. liquefied ammonia is prepared, purity is 99% TiCl4, pure, drying oxygen,
Inert gas;Oxygen is allowed to be introduced directly into the mixed expanded pipe 21 of flame hydrolysis stove by oxygen gas joint, oxygen flow is 1-
2m3/ h, inert gas carrier is introduced directly into the mixed expanded pipe 21 of flame hydrolysis stove, inert gas flow by inert gas joint
For 1-2m3/h;Ammonia decomposer 7 passes through the mixture of hydrogen and nitrogen obtained by decomposing as hydrogen-containing fuel after blower
The high pressure outer cover that hydrogen-containing fuel pipe imports mixed expanded pipe is crossed, then hydrogen is penetrated into mixing by multiple hollow fiber film assemblies
In expansion tube, hydrogen-containing fuel flow is 0.5-1m3TiCl4 is introduced directly into flame by/h, TiCl4 input pipe through high pressure outer cover 3
The mixed expanded pipe of stove is hydrolyzed, TiCl4 flows are 3.3-4.1Kg/h;
B. each road gas enters burning at burner noz(zle), hydrolysis, the temperature control of body of heater internal furnace after expansion tube 21 collects
System is at 850-1000 DEG C;
C. the mixture that bottom of furnace body comes out imports the flocculation of one-level flocculator by transhipment pump, and the gas containing Ti02 particles is molten
After glue stops 3-8 seconds again in flocculator flocculation, into spherical reactor ageing reaction 1-2 minutes, temperature of reaction kettle control existed
200 DEG C, pulse gas generator 19 is loaded into nucleation gas to spherical reactor, and nucleation gas carrier is nitrogen, and nucleator is 18%
Potassium chloride, sodium aluminate mixed solution, wherein potassium chloride:Sodium aluminate=1:1.
D. the mixture by ageing reaction enters two grades through flocculator, is flocculated again through flocculator by two grades, can be real
Existing more than 99.5% collection rate, is then separated in cyclone separator, and the product oxide obtained from cyclone separator is taking off
Collected after sour stove depickling through product hopper and obtain product.
The present invention is easy to get with raw material, and product very high purity, less, gained particle diameter distribution of reuniting are narrow, save the energy, carry
The features such as high-purity, increase efficiency.In preparation process, hydrogen-containing fuel gas, oxygenated fuel gas and control flame combustion feelings
The inert gas of condition is imported in burner noz(zle) hybrid chamber, in spray nozzle front end ignition after being well mixed.Handle carries gold simultaneously
The conspicuous unstrpped gas of category is uniformly blended in burning gases, occurs hydrolysis with combustion product vapor, and be aggregated into ten
Several nanometers of primary particle, primary particle is through flocculation, ageing, flocculating to grow up again can use cyclone separator to be collected, and obtains
To nano-powder.Present invention process can obtain purity be 99.9%, flat footpath particle diameter be 25-35 nanometers, average specific surface is 50
M2/g, be shaped as spherical, crystal formation be rutile-type nano TiO 2.
Brief description of the drawings
Fig. 1 is oxyhydrogen flame furnace structure schematic diagram of the present invention.
Embodiment
With reference to the accompanying drawings and detailed description, technical scheme is described in further detail.
With reference to shown in Fig. 1, oxyhydrogen flame stove includes body of heater 9, TiCl4 input pipes 15, hydrogen-containing fuel pipe 61, the body of heater 9
Outer be covered with water jacket, the body of heater is provided with refractory masses 9, and bottom of furnace body is provided with the top in reactant exit 93, body of heater
Provided with burner noz(zle) 5, the exit of burner noz(zle) 5 is provided with igniter 51.Burner noz(zle) 5 connects with the mixed expanded bottom of pipe 21
Connect, the mixed expanded top of pipe 21 is respectively equipped with outside oxygen gas joint 2, inert gas joint 1, mixed expanded pipe and is arranged with high pressure
Outer cover 3, TiCl4 input pipes 15 are connected through high pressure outer cover 3 with the mixed expanded middle part of pipe 21, hydrogen-containing fuel pipe 61 and high pressure outer cover
Connection, is provided with hollow fiber film assembly 16 between mixed expanded pipe and high pressure outer cover.There is hollow fiber film assembly separation to mix
The doughnut of gas function.Separation driving force is pressure difference, and operating pressure is 0.098-9.8MPa, using transmitance difference come real
Existing mixed gas separation, is gas or steam through thing.Preparation method be in using spinneret by thermoplastic resin melt-spun or will polymerization
Thing solution dry-jet wet-spinning, which is made after many microporous homogeneous films, coats ultra-thin organosilicon seperation film, and some solidification liquids can be also passed through in hollow bulb
To form anisotropic membrane structure.For the mixing qi leel such as hydrogen-nitrogen, oxygen-nitrogen, methane-helium, alcohol-water and ethane, methane and ethene
From.
Hydrogen-containing fuel pipe is connected with ammonia decomposer 7, and ammonia decomposer is connected with ammonia head tank 8.
Reactant exit 93 is connected with transhipment pump 92, and transhipment pump 92 is connected with one-level spiral flocculator 10, one-level spiral wadding
Condenser 10 is connected with spherical reactor 12, and spherical reactor 12 is connected with deuterostrophies flocculator 100, at the top of spherical reactor with
Pulse gas generator 19 is connected.The end of deuterostrophies flocculator 100 is connected through piping with cyclone separator.
Prepare liquefied ammonia, purity is 99% TiCl4, pure, dry oxygen, inert gas.Oxygen is allowed to pass through oxygen all the way
Gas connection 2 is introduced directly into the mixed expanded pipe 21 of flame hydrolysis stove, and oxygen flow is 1-2m3/h;
Inert gas carrier is introduced directly into the mixed expanded pipe 21 of flame hydrolysis stove by another road inert gas joint 1, lazy
Property gas flow be 1-2m3/h.Effect is to act on preventing burner noz(zle) mouthful from scabbing using the impacting with high pressure of air-flow.
Ammonia decomposer 7 is passed through after the mixture of hydrogen and nitrogen obtained by decomposing is pressurized through air blower 6 as hydrogen-containing fuel
The high pressure outer cover 3 that hydrogen-containing fuel pipe 61 imports mixed expanded pipe 21 is crossed, hydrogen-containing fuel flow is 0.5-1m3/h.Hydrogen-containing fuel stream
Amount again penetrates into hydrogen in mixed expanded pipe 21 by multiple hollow fiber film assemblies 16.
TiCl4 is introduced directly into the mixed expanded pipe 21, TiCl4 of flame hydrolysis stove by TiCl4 input pipes 15 through high pressure outer cover 3
Flow is 3.3-4.1Kg/h.
Each road gas enters burning at burner noz(zle), hydrolysis after expansion tube 21 collects.The temperature control of body of heater internal furnace
At 850-1000 DEG C.It is very fast that whole reaction occurs, and the whole course of reaction ratio almost instantaneously carried out will also in water
Rapidly, and under this hot conditions, the topmost product Ti0 of hydrolysis.The overwhelming majority all exists with rutile-type.
The mixture that the bottom of body of heater 9 comes out imports the flocculation of one-level flocculator by transhipment pump.Aerosol is in flocculation pipe
Flocculation, be usually unable to once to go grows up to several microns completely, therefore using spherical reactor ageing+two grades of flocculations of reaction
Mode solve, after the aerosol containing Ti02 particles stops 3-8 seconds again in flocculator flocculation, into spherical reactor
Ageing reaction 1-2 minutes, temperature of reaction kettle is controlled at 200 DEG C, is connected at the top of spherical reactor with pulse gas generator 19, arteries and veins
Rush gas generator 19 and nucleation gas is loaded into spherical reactor, nucleation gas carrier is nitrogen, and nucleator is 18% chlorination
Potassium, wherein sodium aluminate mixed solution, potassium chloride:Sodium aluminate=1:1, to promote Ti02 particle growths.
Mixture by ageing reaction enters two grades through flocculator, flocculates, can realize again through flocculator by two grades
More than 99.5% collection rate.Then separated in cyclone separator, the product oxide obtained from cyclone separator 81 is taking off
Collected after sour stove depickling through product hopper and obtain product.The sweep gas mixture come out from cyclone separator carries out condensation process, cold
Solidifying temperature is -23 DEG C, will be reclaimed after gas filtration.
With reference 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
Assay in following table.
Sequence number | Inspection project | Assay |
1 | Dry powder whiteness w | 90.3 |
2 | TiO2 contents % | 99.9 |
3 | 105 DEG C play thing % | 3.7 |
4 | Burn decrement(600℃)% | 1.0 |
5 | Water slurry pH value | 6.7 |
6 | Heat resistance DEG C | ﹤ 110 |
7 | Density(15℃) g/ml | 4.5 |