CN1810640A - Process and apparatus for preparing dispersed composite nanometer TiO2/SiO2 particle - Google Patents
Process and apparatus for preparing dispersed composite nanometer TiO2/SiO2 particle Download PDFInfo
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- CN1810640A CN1810640A CN 200610024235 CN200610024235A CN1810640A CN 1810640 A CN1810640 A CN 1810640A CN 200610024235 CN200610024235 CN 200610024235 CN 200610024235 A CN200610024235 A CN 200610024235A CN 1810640 A CN1810640 A CN 1810640A
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 239000002245 particle Substances 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims abstract description 21
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims description 24
- 229910052681 coesite Inorganic materials 0.000 title claims description 23
- 229910052906 cristobalite Inorganic materials 0.000 title claims description 23
- 239000000377 silicon dioxide Substances 0.000 title claims description 23
- 229910052682 stishovite Inorganic materials 0.000 title claims description 23
- 229910052905 tridymite Inorganic materials 0.000 title claims description 23
- 239000002131 composite material Substances 0.000 title description 2
- 235000012239 silicon dioxide Nutrition 0.000 title 1
- 238000002485 combustion reaction Methods 0.000 claims abstract description 51
- 239000003570 air Substances 0.000 claims abstract description 23
- 239000001257 hydrogen Substances 0.000 claims abstract description 21
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 21
- 239000002114 nanocomposite Substances 0.000 claims abstract description 18
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000005049 silicon tetrachloride Substances 0.000 claims abstract description 11
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 8
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 6
- 239000007789 gas Substances 0.000 claims description 45
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- 150000002431 hydrogen Chemical class 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- 239000011246 composite particle Substances 0.000 abstract description 16
- 239000002159 nanocrystal Substances 0.000 abstract description 7
- 239000011159 matrix material Substances 0.000 abstract description 5
- 229910003849 O-Si Inorganic materials 0.000 abstract description 2
- 229910003872 O—Si Inorganic materials 0.000 abstract description 2
- 239000010936 titanium Substances 0.000 abstract description 2
- 229910010413 TiO 2 Inorganic materials 0.000 abstract 6
- 229910004298 SiO 2 Inorganic materials 0.000 abstract 5
- 229910021486 amorphous silicon dioxide Inorganic materials 0.000 abstract 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 230000007704 transition Effects 0.000 abstract 1
- 239000012071 phase Substances 0.000 description 21
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 5
- 239000006185 dispersion Substances 0.000 description 4
- 238000000635 electron micrograph Methods 0.000 description 4
- 239000007791 liquid phase Substances 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 238000003980 solgel method Methods 0.000 description 3
- 229910003910 SiCl4 Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000010924 continuous production Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 230000006911 nucleation Effects 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- -1 Hydrogen Chemical class 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000009841 combustion method Methods 0.000 description 1
- 238000005049 combustion synthesis Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
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Abstract
本发明公开了一种弥散相TiO2/SiO2纳米复合颗粒的制备方法。所述方法以四氯化钛、四氯化硅、氢气、空气为原料，按一定的体积比预混后加入燃烧反应器的中心环进行水解反应，反应温度为1200～2500℃，反应生成弥散相TiO2/SiO2复合颗粒的形态介于球形纳米TiO2和链状纳米SiO2颗粒之间，并随Ti∶Si摩尔比的不同而变化。在TiO2/SiO2复合颗粒中，TiO2以纳米晶的形式均匀分散在无定形的SiO2基体中，形成弥散结构。在复合颗粒中存在Ti－O－Si键，SiO2的存在可以抑制TiO2晶粒的生长和锐钛相向金红石相的转变。改变Si含量，可以控制复合颗粒中金红石相含量和复合颗粒粒度。
The invention discloses a preparation method of dispersed phase TiO 2 /SiO 2 nano composite particles. The method uses titanium tetrachloride, silicon tetrachloride, hydrogen, and air as raw materials, premixes them according to a certain volume ratio, and then adds them to the central ring of the combustion reactor for hydrolysis reaction. The morphology of phase TiO 2 /SiO 2 composite particles is between spherical nano-TiO 2 and chain-like nano-SiO 2 particles, and changes with the Ti:Si molar ratio. In TiO 2 /SiO 2 composite particles, TiO 2 is uniformly dispersed in the amorphous SiO 2 matrix in the form of nanocrystals, forming a dispersed structure. There are Ti-O-Si bonds in the composite particles, and the presence of SiO 2 can inhibit the growth of TiO 2 grains and the transition from anatase phase to rutile phase. By changing the Si content, the content of rutile phase in the composite particles and the size of the composite particles can be controlled.
Description
Technical Field
The invention relates toAnd a disperse phase TiO2/SiO2A method for preparing nano composite particles.
Background
Nano TiO22The particles have high reaction activity, good visible light transmittance and good photocatalytic activity, and can be widely used as a catalyst or a catalyst carrier for photocatalytic reaction; TiO22-SiO2The nano composite photocatalyst can improve TiO2Surface active sites, increased surface area, increased surface hydroxyl content, improved dispersibility, SiO2Can also inhibit TiO2The phase transformation and the grain growth of the alloy, and the thermal stability of the alloy is enhanced. In order to meet the requirements of different fields of application, nanometer TiO is developed2-SiO2Various preparation technologies of the composite material, such as a Sol-Gel method (Sol-Gel), Chemical Vapor Deposition (CVD), gas phase combustion synthesis and the like. Compared with other methods for synthesizing nano materials, the method for synthesizing the nano composite particles by gas phase combustion has small particle size and high purity, is an important method for preparing nano particle materials, and is one of the preparation methods with the greatest industrial prospect.
Disperse phase TiO2/SiO2The nanocomposite particles are generally made from titanium tetrachloride (TiCl)4) Silicon tetrachloride (SiCl)4) Gas-phase combustion hydrolysis reaction, and the reaction formula is as follows:
at present, most of the commonly used preparation methods of the nano composite particles are liquid phase precipitation methods or sol-gel methods, and the gas phase combustion method for preparing the nano composite particles has no related patent report because of high technical difficulty.
The liquid phase process of preparing nanometer composite particle includes the hydrolysis reaction of the precursor dropped into water solutionFirst generation of intermediate Ti (OH)4Or Si (OH)4After filtration, the resultant was calcined at a high temperature to remove excess water and hydroxyl groups, thereby producing composite particles of an oxide. Since high-temperature calcination is required, the composite particles are easily sintered and are difficult to disperse. The liquid phase method has more steps and realizes a large gaugeThe continuous production of the die is difficult.
Disclosure of Invention
The technical problem to be solved by the invention is to provide disperse phase TiO2/SiO2The preparation method and the equipment of the nano composite particles overcome the defects of the existing liquid phase method and meet the requirements of large-scale continuous production of the nano composite particles.
The idea of the invention is that:
the temperature distribution of the reaction zone can be controlled by using a multi-jet oxyhydrogen flame combustion reactor through flow parameters, and precursor TiCl is controlled4And SiCl4The feeding concentration of the catalyst is controlled to be mixed at a molecular level in advance, the two are controlled to carry out homogeneous nucleation simultaneously, and the preparation of TiO can be controlled2/SiO2The inventor of the dispersed phase nano composite particle has conducted a great deal of experiments, and in the process flow, the invention adopts the method that a pre-mixed reactant (TiCl) is introduced into a central pipe of a multi-jet combustion reactor according to a certain proportion4、SiCl4Hydrogen, air); the combustion-supporting gas mixed by hydrogen and air is introduced into the two rings, and the combustion-supporting gas of the two rings can form stable flame, so that the stability of the whole combustion flame is maintained, and the temperature and the concentration distribution of the central jet flame can be adjusted within a larger range. The TiO can be controlled by adjusting the gas speed and the precursor concentration2、SiO2And simultaneously, homogeneous nucleation is carried out to form a dispersed phase nano composite structure.
The preparation method is characterized by comprising the following steps:
enabling mixed gas of titanium tetrachloride, silicon tetrachloride, hydrogen and air to enter a combustion reactor through a central pipe of a quadruple jet pipe arranged at the top of the combustion reactor;
simultaneously, air and hydrogen enter the combustion reactor through a double ring pipe of the quadruple jet pipe;
simultaneously, air enters the combustion reactor through a three-ring pipe of the quadruple jet pipe;
meanwhile, air enters the combustion reactor through a four-ring pipe of the quadruple jet pipe;
the mixture entering the combustion reactor is subjected to gas phase combustion hydrolysis reaction in the combustion reactor to generate the dispersed phase TiO2/SiO2And (3) separating the product of the nano composite particles by a collecting device, collecting the product, and absorbing tail gas by an absorbing device.
The reaction temperature in the combustion reactor is 1200-2500 ℃;
the standard volume ratio of the mixed gas of hydrogen, oxygen, titanium tetrachloride and silicon tetrachloride introduced into the central tube is as follows:
the total gas velocity of hydrogen, oxygen, titanium tetrachloride and silicon tetrachloride is 1: 0.4-3: 0.05-0.6: 0.02-0.9, and the temperature is 50-250 ℃;
the mixed gas introduced into the two loops is prepared from the following components in a standard volume ratio of hydrogen to air:
hydrogen and air are 1: 0.2-1, the total gas velocity is 50-150m/s, and the temperature is 20-100 ℃;
the air velocity of the air introduced into the three-ring pipe and the four-ring pipe (7) is 10-60m/s, and the temperature is 20-100 ℃;
the standard volume ratio of the mixed gas introduced into the central pipe, the mixed gas introduced into the second ring pipe, the mixed gas introduced into the third ring pipe and the mixed gas introduced into the fourth ring pipe is as follows:
the ratio of the mixed gas in the central pipe, the mixed gas in the two circular pipes, the mixed gas in the three circular pipes and the mixed gas in the four circular pipes is 1: 0.3-2: 2-10: 5-20.
The term "standard volume" means that the temperature of the gas is 25 ℃ and the pressure is 0.1 MPa.
TiO prepared by the method2/SiO2The shape of the nano composite particles is between that of spherical nano TiO2 and chain nano SiO2Between the particles and with TThe molar ratio of i to Si varies. In TiO2/SiO2In the composite particles, TiO2Uniformly dispersed in amorphous SiO in the form of nano crystal2In the matrix, a dispersion structure is formed. The presence of Ti-O-Si bonds, SiO, in the composite particles2Can inhibit TiO2Grain growth and transformation of the anatase phase to the rutile phase. By changing the Si content, the rutile phase content and the composite particle size in the composite particles can be controlled.
According to the technical scheme disclosed by the invention, the method has the advantages of simple equipment structure and convenience in operation, and the obtained disperse phase TiO is2/SiO2In the nano-composite particle, TiO2Uniformly dispersed in amorphous SiO in the form of nano crystal2In the matrix, a dispersion structure is formed, and industrial production is easy to realize.
Drawings
FIG. 1 is a schematic view of a combustion reactor configuration.
FIG. 2 is a schematic flow chart.
FIG. 3 is an electron micrograph of the product of example 1.
FIG. 4 is an electron micrograph of the product of example 2.
Detailed Description
With reference tofig. 1, the plant for carrying out the process of the invention comprises at least a combustion reactor 15 and a quadruple jet pipe 1 arranged at the top of the combustion reactor 15;
the quadruple jet pipe 1 comprises a central pipe 101, a double ring pipe 102, a triple ring pipe 103 and a four ring pipe 104 which are coaxial in sequence.
According to the preferred technical scheme of the invention, the height-diameter ratio of the combustion reactor 15 is 3-20, and the flow cross-sectional area ratio of the central pipe 101, the double-ring pipe 102, the three-ring pipe 103 and the four-ring pipe 104 is as follows:
＝1∶0.2～3∶1.5～10∶2～20。
Referring to fig. 1 and 2, the method of the present invention comprises the steps of:
the mixed gas of titanium tetrachloride, silicon tetrachloride, hydrogen and air enters the combustion reactor 15 through a central pipe 101 of a quadruple jet pipe 1 arranged at the top of the combustion reactor 15;
meanwhile, air and hydrogen enter the combustion reactor 15 through the double loop pipe 102 of the quadruple jet pipe 1;
meanwhile, air enters the combustion reactor 15 through the three-loop pipe 102 of the quadruple jet pipe 1;
meanwhile, air enters the combustion reactor 15 through the four-ring pipe 102 of the quadruple jet pipe 1;
the mixture entering the combustion reactor 15 undergoes a gas phase combustion hydrolysis reaction in the combustion reactor 15 to form said dispersed phase TiO2/SiO2And (3) separating the product of the nano composite particles by a collecting device 16, collecting the product, and enabling tail gas to enter an absorbing device 17 for absorption.
Example 1
Equipment parameters:
the height of the combustion reactor 15 is 0.3 m, and the diameter is 0.05 m;
the flow cross-sectional area of the center pipe 101 is 12mm2The cross-sectional flow area of the two pipes 102 is 22m2And the cross-sectional flow area of the three ring pipes 103 is 34mm2The cross-sectional flow area of the four-ring pipe 104 is 100mm2
Titanium tetrachloride (0.5L/h) with the temperature of 90 ℃, silicon tetrachloride (1.2L/h) and hydrogen (1.0 m)3/h)And air (3 m)3The mixed gas of the/h) is introduced into a central pipe 101 of the quadruple jet pipe and enters the combustion reactor 15;
the temperature is 50 ℃ (0.6 m)3H) and hydrogen (0.6 m)3H) from a loop into the combustion reactor 15;
air (6 m) with a temperature of 80 DEG C3H) from the three-loop pipe 103 into the combustion reactor 15;
air (10 m) with a temperature of 80 DEG C3H) from the four ring pipe 104 into the combustion reactor 15;
the reaction temperature in the combustion chamber was 2000 ℃.
The product is separated by a collecting device, and the tail gas is absorbed by an absorbing device. Reaction to form dispersed phase TiO2/SiO2The shape of the composite particle is between that of spherical nano TiO2And chain-like nano SiO2The particle size between the particles is 20-40 nm. In TiO2/SiO2In the composite particles, TiO2Uniformly dispersed in amorphous SiO in the form of nano crystal2In a matrix of TiO2The diameter of the nanocrystal is 1-2 nm, and a dispersion structure is formed. The electron micrograph thereof is shown in FIG. 3.
Example 2
Equipment parameters:
the height of the combustion reactor 15 is 2.5 meters, and the diameter is 0.4 meter;
the flow cross-sectional area of the center tube 101 is 220mm2The cross-sectional flow area of the two loops 102 is 130mm2The cross-sectional flow area of the three-ring pipe 103 is 260mm2The cross-sectional flow area of the four-ring pipe 104 is 600m2；
Titanium tetrachloride (30L/h), silicon tetrachloride (30L/h) and hydrogen (10 m) at the temperature of 220 DEG C3H) and air (35 m)3The mixed gas of the/h) is introduced into a central pipe 101 of the quadruple jet pipe and enters the combustion reactor 15;
air (5 m) with a temperature of 50 DEG C3H) and hydrogen (3 m)3H) from a loop into the combustion reactor 15;
air (40 m) with a temperature of 20 DEG C3H) from the three-loop pipe 103 into the combustion reactor 15;
air (60 m) with the temperature of 20 DEG C3H) from the four ring pipe 104 into the combustion reactor 15;
the reaction temperature in the combustion chamber was 1200 ℃.
The product is separated by a collecting device, and the tail gas is absorbed by an absorbing device.
Reaction to form dispersed phase TiO2/SiO2The shape of the composite particle is between that of spherical nano TiO2And chain-like nano SiO2The particle size between the particles is 30-50 nm. In TiO2/SiO2In the composite particles, TiO2Uniformly dispersed in amorphous SiO in the form of nano crystal2In a matrix of TiO2The diameter of the nanocrystal is 5-10 nm, and a dispersion structure is formed. The electron micrograph thereof is shown in FIG. 4.
Claims (6)
1. Disperse phase TiO2/SiO2The preparation method of the nano composite particles is characterized by comprising the following steps:
mixed gas of titanium tetrachloride, silicon tetrachloride, hydrogen and air enters a combustion reactor (15) through a central pipe (101) of a quadruple jet pipe (1) arranged at the top of the combustion reactor (15);
simultaneously, air and hydrogen enter the combustion reactor (15) through a double ring pipe (102) of the quadruple jet pipe (1);
meanwhile, air enters the combustion reactor (15) through a three-ring pipe (103) of the quadruple jet pipe (1);
meanwhile, air enters the combustion reactor (15) through a four-ring pipe (104) of the quadruple jet pipe (1);
the mixture entering the combustion reactor is subjected to gas phase combustion hydrolysis reaction in the combustion reactor to generate the dispersed phase TiO2/SiO2Separating the product of the nano composite particles by a collecting device, collecting the product, and absorbing the tail gas by an absorbing device, wherein the reaction temperature in the combustion reactor is 1200-2500 ℃.
2. The method of claim 1, wherein the standard volume ratio of the mixed gas of hydrogen, oxygen, titanium tetrachloride and silicon tetrachloride introduced into the central tube is as follows:
the total gas velocity of hydrogen, oxygen, titanium tetrachloride and silicon tetrachloride is 1: 0.4-3: 0.05-0.6: 0.02-0.9, the total gas velocity is 60-170m/s, and the temperature is 50-250 ℃.
3. The method according to claim 2, wherein the mixed gas introduced into the two loops is, based on the standard volume ratio of hydrogen to air:
the ratio of hydrogen to air is 1: 0.2-1, the total gas velocity is 50-150m/s, and the temperature is 20-100 ℃.
4. A method according to claim 3, characterized in that the air is introduced into the three-and four-loop (7) at a velocity of 10-60m/s and a temperature of 20-100 ℃.
5. The method according to claim 4, wherein the standard volume ratio of the mixed gas introduced into the central tube, the mixed gas introduced into the two loops, the mixed gas introduced into the three loops and the mixed gas introduced into the four loops is:
the ratio of the mixed gas in the central pipe, the mixed gas in the two circular pipes, the mixed gas in the three circular pipes and the mixed gas in the four circular pipes is 1: 0.3-2: 2-10: 5-20.
6. Device for implementing the method according to any one of claims 1 to 5, characterized in that it comprises at least: the device comprises a combustion reactor (15) and a quadruple jet pipe (1) arranged at the top of the combustion reactor (15);
the quadruple jet pipe (1) comprises a central pipe (101), a double-ring pipe (102), a three-ring pipe (103) and a four-ring pipe (104) which are coaxial in sequence, the height-diameter ratio of the combustion reactor (15) is 3-20, and the flow cross-sectional area ratio of the central pipe (101), the double-ring pipe (102), the three-ring pipe (103) and the four-ring pipe (104) is as follows:
the central pipe (101), the two-ring pipe (102), the three-ring pipe (103) and the four-ring pipe (104) are 1: 0.2-3: 5-10: 5-20.
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| CN105668622A (en) * | 2015-07-30 | 2016-06-15 | 四川大学 | Film coating method for titanium dioxide through vapor atomic deposition |
| CN107628640A (en) * | 2017-08-14 | 2018-01-26 | 中国恩菲工程技术有限公司 | Nano titanium oxide and preparation method thereof |
| CN109867788A (en) * | 2019-03-18 | 2019-06-11 | 台州学院 | A kind of preparation method of organosilicon-composite titania material |
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