CN1743271A - Diffusion combustion reactor for preparing nano titanium dioxide and its use - Google Patents
Diffusion combustion reactor for preparing nano titanium dioxide and its use Download PDFInfo
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- CN1743271A CN1743271A CN 200510027963 CN200510027963A CN1743271A CN 1743271 A CN1743271 A CN 1743271A CN 200510027963 CN200510027963 CN 200510027963 CN 200510027963 A CN200510027963 A CN 200510027963A CN 1743271 A CN1743271 A CN 1743271A
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Abstract
This invention discloses a diffusion combustion reactor for nano-titanium dioxide (TiO2) preparation and its application. This reactor enables the reactants material and combustion-supporting gas to uniformly mix and spray out in high speed from the central tube, then quickly mix with the flame center of the combustion gas at the second ring. Otherwise there is third ring to conduct protection function. Advantages: overcome the defects of un-uniform temperature field and concentration field, easy-to-scar etc., the nano-titanium dioxide (TiO2) is small in grain-size and high in catalytic activity.
Description
Technical Field
The invention relates to a method for preparing nano titanium dioxide (TiO)2) In particular to a reactor adopting diffusion combustion flame and an application method thereof in preparing vapor-phase nano titanium dioxide.
Background
Nano TiO prepared by gas phase method2The nanometer material is a high-tech inorganic fine chemical product, has the characteristics of high reaction activity, good visible light transmittance, strong ultraviolet absorption performance and the like besides the special properties of nanometer materials, and has wide application prospect in the fields of catalysis, magnetic materials, sensors, medicine, bioengineering and the like.
Gas phase method for preparing nano TiO2Generally from titanium tetrachloride (TiCl)4) Gas-phase combustion hydrolysis reaction, and the reaction formula is as follows:
or
Preparation of nano TiO by gas phase combustion2As the technology is complex and no industrialized report exists in China, reactors used in foreign research are summarized into two types, one type is a diffusion combustion reactor, and the other type is a premixed combustion flame reactor. The existing traditional diffusion combustion flame reactor (shown as attached figure 2) is characterized in that titanium tetrachloride, air and hydrogen are respectively introduced into different pipelines (commonly called nozzles) to be sprayed out for combustion, and the reactor has the advantages of simple structure, convenient manufacture and maintenance and safe combustion. However, the reactor has the defects of very uneven temperature field and concentration field, easy scabbing at the outlet of a nozzle and the like, so that the high-quality nano titanium dioxide product is difficult to prepare by adopting the traditional diffusion combustion flame reactor.
Disclosure of Invention
It is an object of the present invention to provide a novel diffusion combustion reactor, which overcomes the drawbacks of the conventional diffusion combustion flame reactors.
The second purpose of the invention is to provide an application method of the reactor, in particular to the preparation of nano TiO2The use of (1).
The idea of the invention is that:
cause the existing expanderThe reasons for the non-uniform temperature field and concentration field in the combustion reaction zone and the tendency of scabbing and clogging at the nozzle outlet in the dispersion combustion flame reactor are various, and through experiments, the inventors found that the reaction material (TiCl) other than the reaction material4And auxiliary combustion gas) and the nozzle and feed mode of the reactor. The structure of the existing traditional diffusion combustion flame reactor is generally double-sleeve, hydrogen is fed into a central pipe, and air and TiCl are fed into the central pipe and the two rings4The uneven temperature field is mainly caused by insufficient oxygen supply inside the flame and low temperature. The inhomogeneity of the concentration field is mainly due to the fact that the reaction mass is mixed outside the flame and H is not realized2And O2Due to rapid micro-mixing. In order to solve the problem, the inventor invents a coaxial multi-jet nozzle through a large amount of experiments, wherein a central pipe of the coaxial multi-jet nozzle is filled with reactant TiCl according to a certain proportion4And the mixed gas of the auxiliary combustion gas can ensure sufficient oxygen supply in the flame and can adjust the requirements of different temperatures; pure hydrogen is introduced into the two rings, and the burning flame and the reactant of the central pipe are quickly mixed at the center of the flame; and the protection air introduced by the three rings and the tangentially-entering air duct positioned at the upper part of the combustion chamber is fully mixed to ensure that H at each part inside the flame2、O2And the concentration field of reactants is uniform, the problem of insufficient oxygen supply does not exist, and the temperature field is naturally uniform. Because the central tube and the two rings generate larger momentum due to high gas velocity, TiO attached at the outlet of the central tube can be blown off2The particles can eliminate the phenomena of easy scabbing and blockage at the outlet of the nozzle.
The invention is realized by the following technical scheme:
the diffusion combustion reactor provided by the invention comprises a nozzle and a combustion chamber, wherein the nozzle is arranged at the upper part of the combustion chamber and is communicated with the combustion chamber at the outlet of each pipeline of the nozzle, a reaction section 15 of the combustion chamber comprises an ignition port 4, a temperature and pressure measuring port 5 and an expansion joint 9, and a discharge section 16 at the lower part of the combustion chamber is provided with a reactant outlet 11, and the diffusion combustion reactor is characterized in that the nozzle is formed by sequentially arranging a central pipe 1, a double ring pipe 2 and a three ring pipe 3 from inside to outside in a coaxial manner; the upper part of the reaction section 15 of the combustion chamber has a tangential inlet air duct 6.
The further improved scheme of the invention is as follows: the combustion chamber is provided with a circulating cooling water jacket 8, and a circulating cooling water inlet 7 and a circulating cooling water outlet 10 are respectively arranged at one side and the bottom of the combustion chamber.
The diameter ratio D1 to D2 of the nozzle of the diffusion combustion reactor and the reaction section of the combustion chamber is 1: 2-6.
In addition, the invention also provides application of the diffusion combustion reactor in preparing the nano TiO2, which comprises the following steps:
1. introducing mixed gas of titanium tetrachloride and auxiliary combustion gas which are mixed in advance into a central tube 1 of the diffusion combustion reactor, and spraying the mixed gas to a combustion chamber at a high speed through the central tube;
2. hydrogen is introduced into the two rings 2, is ignited by an ignition port 4 of the combustion reaction chamber, is sprayed out at high speed after being ignited, and is rapidly mixed with reaction materials of the central tube in the center of flame;
3. air is introduced into the three rings 3 and the tangential air inlet pipe 6, and TiO is formed after gas phase combustion2Powder, collected from the reaction product outlet 11;
wherein: the total gas velocity at the outlet of the central tube is 50-90 m/s; the gas velocity at the outlet of the two rings is 20-70m/s, and the gas velocity at the outlet of the three rings is 20-50 m/s; the air speed at the outlet of the tangential air inlet pipe is 10-40m/s, and the reaction temperature is 800-1600 ℃.
The central tube 1) assists the combustion gas to be selected from O2、N2One or more of air and argon;
in the presence of cooling water in the combustion reaction chamber, step 2 is to introduce hydrogen into the two rings 2, ignite the hydrogen through the ignition port 4 of the combustion reaction chamber, spray the hydrogen out after gas phase combustion hydrolysis reaction, and rapidly mix the hydrogen with the reaction material in the central tube at the center of flame, wherein the temperature of the cooling water is 80-100 ℃.
Advantageous effects
According to the technical scheme and the implementation method, the reaction materials and the auxiliary combustion gas are uniformly mixed and then are ejected from the central pipe at a high speed by changing the nozzle structure and the feeding mode of the traditional diffusion reactor, the reaction materials and the auxiliary combustion gas are quickly mixed in the flame center of the combustion gas with two rings, and the action of protective air entering through the three rings and the tangential air inlet pipe is added, so that the defects that the temperature field and the concentration field of the traditional diffusion combustion reactor are not uniform, a reaction nozzle is easy to scar and the like are better overcome, the primary particle size of the generated titanium dioxide is 10-40 nm, the generated titanium dioxide has high catalytic activity, and the nano titanium dioxide with small particle size and high catalytic activity is prepared.
Drawings
FIG. 1 is a schematic view of a conventional diffusion combustion reactor
Wherein: 11. a reaction product outlet, 12, a titanium tetrachloride inlet, 13, a fuel inlet, 14 and an oxidant inlet;
FIG. 2 is a schematic view of a diffusion combustion reactor
Wherein: 1. a central tube; 2. a second ring pipe; 3. a third ring pipe; 4. an ignition port; 5. temperature and pressure measuring ports 6, a tangential air inlet pipe 9, an expansion joint 11, a reaction product outlet 15, a combustion chamber reaction section 16, a combustion chamber discharge section D2 and the diameter of the combustion chamber reaction section;
FIG. 3 is a schematic diagram of a further improved diffusion combustion reactor
Wherein: 1. a central tube; 2. a second ring pipe; 3. a third ring pipe; 4. an ignition port; 5. the device comprises a temperature and pressure measuring port 6, a tangential air inlet pipe 7, a circulating cooling water inlet 8, a circulating cooling water jacket 9, an expansion joint 10, a circulating cooling water outlet 11, a reaction product outlet 15, a combustion chamber reaction section 16, a combustion chamber discharge section D2 and the diameter of the combustion chamber reaction section;
FIG. 4 is a sectional view of the nozzle taken along the line A-A
Wherein: 1. a central tube; 2. a second ring pipe; 3. a third ring pipe; d1, nozzle diameter;
Detailed Description
The invention is further illustrated by the following examples in conjunction with the accompanying drawings, which are not intended to limit the scope of the invention:
examples
The combustion diffusion reactor of the invention is used for preparing nano TiO 2:
the liquid titanium tetrachloride is first electrically heated to vaporize, and the vapor and the air after being dried, purified and preheated are mixed via T-joint and fed into mixer with O2And N2The mixed gas is dried and purified and is also introduced into the mixer. The mixed gas is mixed according to a certain proportion (considering that the first mixing is not uniform, two mixers are connected in series), the mixed gas is introduced into a central pipe 1 of the reactor to be sprayed out at a high speed, and the total gas velocity at the outlet of the central pipe is 62m/s (oxygen, nitrogen and silicon tetrachloride steam are in a chemical theoretical ratio). And purified and excessive hydrogen is introduced into the reactor dicyclic ring 2 and is ignited to spray out at high speed, the total gas speed at the outlet of the dicyclic ring is 45m/s, and the reaction materials in the central pipe 1 are quickly mixed in the center of the flame. Purified air is respectively introduced into a three-ring 3 and a tangential air inlet pipe 6 of the reactor to carry out sharp quenching on a reaction system, the air speed of a three-ring air outlet is 29m/s, the air speed of a tangential conduit outlet for protecting air is 14m/s, and the reaction temperature is 1000 ℃. Forming TiO after gas phase combustion2Blowing the powder out along with high-speed airflow; then flocculating and cooling through a flocculator made of a plurality of sections of pipelines, finally deacidifying in a collecting deacidification tower, and packaging in a packaging machine through a bunker.
The whole reactor, the outlet pipe of the reactor, the pipe of the flocculator and the outlet pipe of the flocculator are all cooled by a jacket or a water tank at constant temperature. The thermostatic water bath has a separate circulating system and is controlled at about 100 ℃. When the thermostatic waterbath is started, steam is needed to preheat, once the reaction starts, the reaction heat can maintain the water temperature to be surplus, the surplus heat can be removed by a condenser if necessary to prevent water from evaporating, and the cooling wateris deionized water.
The obtained gas-phase nano titanium dioxide product: TiO22Purity 99.8%, BET specific surface area 56m2(ii)/g; the heating loss (free moisture removed at 105 ℃) is less than 2%; the ignition loss (structural water removed at 1000 ℃) is less than 2 percent, the primary particle size is 15nm, and the particle size is not less than that of a commercial product P25 determined by catalytic activity.
Claims (6)
1. A combustion diffusion reactor comprises a nozzle and a combustion chamber, wherein the nozzle is arranged at the upper part of the combustion chamber and communicated with the combustion chamber at the outlet of each pipeline of the nozzle, a reaction section (15) of the combustion chamber comprises an ignition port (4), a temperature and pressure measuring port (5), an expansion joint (9), and a discharge section (16) at the lower part of the combustion chamber is provided with a reactant outlet (11), and the combustion diffusion reactor is characterized in that the nozzle is formed by sequentially arranging a central pipe (1), a double ring pipe (2) and a three ring pipe (3) from inside to outside in a coaxial manner; the upper part of the reaction section (15) of the combustion chamber is provided with an air conduit (6) which enters tangentially.
2. The combustion diffusion reactor according to claim 1, characterized in that the combustion chamber is provided with a cooling water circulating jacket (8) and is provided with a cooling water circulating inlet (7) and a cooling water circulating outlet (10) at the side and bottom of the combustion chamber, respectively.
3. The combustion diffusion reactor as claimed in claim 1 or 2, characterized in that the ratio of the diameters of the nozzle and the combustor reaction section (15) of the diffusion combustion reactor is D1: D2: 1: 2-6.
4. The use of the combustion diffusion reactor according to claim 1 or 2 for the preparation of nano-TiO 2, characterized in that it comprises the following steps:
1) introducing titanium tetrachloride and auxiliary combustion gas which are mixed in advance into a central tube (1) of the diffusion combustion reactor, and spraying the titanium tetrachloride and the auxiliary combustion gas to a combustion chamber at a high speed through the central tube (1);
2) hydrogen is introduced into the two rings (2), ignited by the ignition port (4) of the combustion reaction chamber, and sprayed out at high speed after being ignited, and the reaction materials in the central tube (1) are quickly mixed in the center of flame;
3) air is introduced into the three rings (3) and the tangential air inlet pipe (6) and forms TiO after gas phase combustion2Powder, collected by the reaction product outlet (11);
wherein: the total gas velocity at the outlet of the central tube (1) is 50-90 m/s; the gas velocity at the outlet of the two rings (2) is 20-70m/s, and the gas velocity at the outlet of the three rings (3) is 20-50 m/s; the air speed at the outlet of the tangential air inlet pipe (6) is 10-40m/s, and the reaction temperature is 800-1600 ℃.
5. The method of using a combustion diffusion reactor as claimed in claim 4, wherein the cooling water is at a temperature of 80-100 ℃ in the presence of the cooling water in the combustion chamber.
6. The method of application of the combustion diffusion reactor as claimed in claim 4, characterized in that the auxiliary combustion gas of the central tube (1) is selected from O2、N2One or more of air and argon.
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| CN 200510027963 CN1743271A (en) | 2005-07-21 | 2005-07-21 | Diffusion combustion reactor for preparing nano titanium dioxide and its use |
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| CN 200510027963 CN1743271A (en) | 2005-07-21 | 2005-07-21 | Diffusion combustion reactor for preparing nano titanium dioxide and its use |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1884083B (en) * | 2006-07-12 | 2011-02-09 | 华东理工大学 | Process for preparing nano alumina hollow sphere structure |
| CN102371132A (en) * | 2010-08-11 | 2012-03-14 | 中外炉工业株式会社 | Injection device and powder manufacturing device |
| CN107804870A (en) * | 2017-11-14 | 2018-03-16 | 黄林海 | A kind of production method of titanium dioxide |
| CN111285377A (en) * | 2018-12-07 | 2020-06-16 | 新特能源股份有限公司 | System and method for producing fumed silica |
| CN112610953A (en) * | 2020-12-17 | 2021-04-06 | 华中科技大学 | System for synthesizing nano-particles by flame |
| CN113041986A (en) * | 2020-04-23 | 2021-06-29 | 东华工程科技股份有限公司 | Titanium dioxide oxidation reactor by chlorination process |
-
2005
- 2005-07-21 CN CN 200510027963 patent/CN1743271A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1884083B (en) * | 2006-07-12 | 2011-02-09 | 华东理工大学 | Process for preparing nano alumina hollow sphere structure |
| CN102371132A (en) * | 2010-08-11 | 2012-03-14 | 中外炉工业株式会社 | Injection device and powder manufacturing device |
| CN107804870A (en) * | 2017-11-14 | 2018-03-16 | 黄林海 | A kind of production method of titanium dioxide |
| CN111285377A (en) * | 2018-12-07 | 2020-06-16 | 新特能源股份有限公司 | System and method for producing fumed silica |
| CN113041986A (en) * | 2020-04-23 | 2021-06-29 | 东华工程科技股份有限公司 | Titanium dioxide oxidation reactor by chlorination process |
| CN112610953A (en) * | 2020-12-17 | 2021-04-06 | 华中科技大学 | System for synthesizing nano-particles by flame |
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