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WO2021212405A1 - Chlorination process-based titanium dioxide oxidation reactor - Google Patents

Chlorination process-based titanium dioxide oxidation reactor Download PDF

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Publication number
WO2021212405A1
WO2021212405A1 PCT/CN2020/086390 CN2020086390W WO2021212405A1 WO 2021212405 A1 WO2021212405 A1 WO 2021212405A1 CN 2020086390 W CN2020086390 W CN 2020086390W WO 2021212405 A1 WO2021212405 A1 WO 2021212405A1
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Prior art keywords
section
air inlet
reaction
titanium dioxide
oxidation reactor
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PCT/CN2020/086390
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French (fr)
Chinese (zh)
Inventor
孙洪涛
闫燕
解为清
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East China Engineering Science and Technology Co Ltd
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East China Engineering Science and Technology Co Ltd
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Priority to PCT/CN2020/086390 priority Critical patent/WO2021212405A1/en
Priority to CN202120556442.XU priority patent/CN214765498U/en
Priority to CN202110289503.5A priority patent/CN113041986B/en
Publication of WO2021212405A1 publication Critical patent/WO2021212405A1/en
Anticipated expiration legal-status Critical
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/24—Stationary reactors without moving elements inside
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006—Controlling or regulating processes
    • B01J19/0013—Controlling the temperature of the process
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053—Details of the reactor
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/04—Oxides; Hydroxides
    • C01G23/047—Titanium dioxide
    • C01G23/07—Producing by vapour phase processes, e.g. halide oxidation

Definitions

  • the invention relates to the technical field of titanium dioxide production, and more particularly to equipment for preparing titanium dioxide by gas phase oxidation of titanium tetrachloride in the preparation process of large and medium-sized chloride titanium dioxide.
  • Oxidation reactor is the core equipment in the production process of chlorination titanium dioxide, and it is a key factor that affects the normal operation of the entire chlorination titanium dioxide plant and whether it can produce high-quality products.
  • TiCl4 and O2 complete the reaction in a very short time under high temperature and pressure conditions, and generate micron-sized TiO2 particles.
  • it is necessary to solve (1) a reasonable reactor structure so that the particle size distribution of the product meets the requirements of pigment-grade TiO2; (2) a reasonable structure design of the heating section enables the O2 to be evened from 900°C in a short time Heat to about 1600°C.
  • the temperature in the heating section is very high, and the toluene combustion zone is as high as 3000°C.
  • a reasonable equipment structure should be selected to make the flow field reasonable and ensure the service life of the equipment.
  • High temperature TiCl4 is highly corrosive and high-speed air erosion at the exit of TiCl4 feeding ring. Appropriate corrosion-resistant and wear-resistant materials should be selected.
  • the particles are easy to stick to the wall, so reliable "anti-scar” and “scar removal” measures must be taken.
  • the heating section runs directly under the high temperature of the mixture of hot oxygen and toluene flame, the equipment lining life is quite short, and refractory materials need to be replaced regularly.
  • the structure of the equipment causes the flow and pressure of titanium tetrachloride in the mixing section to be insufficiently uniform, which affects the quality and operation effect of the oxidation base product.
  • the present invention optimizes the design of a more reasonable and effective oxidation reactor, which is suitable for the production of large and medium chlorination titanium dioxide, and has a single large capacity ( Achieve an annual output of 40,000 to 100,000 tons), good operation stability, long equipment life, high quality base materials and other advantages.
  • the chlorination process titanium dioxide oxidation reactor includes a heating section, a reaction section and a quenching section.
  • the heating section is composed of a left section, a middle section and a right section as a whole.
  • the left section and the middle section are fixed together by a first flange, the middle section and the right section Fixed together by the second flange, the left section, the middle section and the right section are coaxial and form a furnace body;
  • the left section of the left section is provided with a toluene gun interface, and the left section has a
  • To four hot oxygen inlet pipe ports the hot oxygen inlet pipe ports are distributed in an annular array on the left section centered on the circle center of the left section, and the angle between the hot oxygen inlet pipe ports and the axis line of the left section is 60 to 85 degrees;
  • the right end of the right section is connected to the reaction section.
  • the reaction section is composed of an air inlet chamber and a feeding ring.
  • the air inlet chamber is a volute ring structure.
  • the feeding ring is fixed on the inner wall of the air inlet chamber.
  • a pipe channel is formed on the feeding ring.
  • the high temperature resistant variable diameter ceramic tube is fixed on the inner wall of the tube channel, and the high temperature resistant variable diameter ceramic tube is a ceramic tube whose diameter gradually decreases from outside to inside;
  • the air inlet chamber is provided with a titanium tetrachloride air inlet, and the air inlet chamber is provided with an air inlet of the reaction section and an air outlet of the reaction section along the axial direction of the heating section.
  • the air inlet of the reaction section is connected with the right section, and the reaction section outlet
  • the gas port is connected to the left end of the quenching section.
  • the quenching section is a gas-liquid heat exchanger, and the base material from the reaction section enters the gas-liquid heat exchanger for heat exchange and cooling.
  • the bodies of the left section, the middle section and the right section are composed of a shell and a refractory heat-insulating material, the shell and the material are made of nickel-based alloy material, and the refractory and heat-insulating material is lined and fixed on the inner wall of the shell.
  • the feeding ring is a circular ring body, and the left and right ends of the feeding ring are respectively fixed on the inner wall of the air inlet chamber.
  • variable-diameter ceramic tube is inserted in the tube channel and clamped and fixed on the feeding ring.
  • the titanium gas chamber can effectively ensure the stable flow and pressure of titanium tetrachloride, make the hot oxygen and titanium tetrachloride fully mix and react, and improve the quality of the semi-finished base material produced by the reaction.
  • Figure 1 is a schematic diagram of the structure of the present invention
  • Figure 2 is a cross-sectional view from A to A in Figure 1;
  • Fig. 3 is a cross-sectional view of B-B in Fig. 1.
  • Heating section Heating section; 2. Reaction section; 3. Quenching section; 4. Hot oxygen pipe port; 5. First flange; 6. Second flange; 7. Toluene gun interface; 21. Inlet Air chamber; 22. Feeding ring; 23. Pipe passage; 24. Titanium tetrachloride air inlet.
  • the chlorination titanium dioxide oxidation reactor includes a heating section 1, a reaction section 2 and a quenching section 3.
  • the heating section 1 is composed of a left section 1a, a middle section 1b and a right section 1c as a whole ,
  • the left section 1a and the middle section 1b are fixed together by the first flange 5, the middle section 1b and the right section 1c are fixed together by the second flange 6, the left section 1a, the middle section 1b and the right section 1c are coaxial and
  • a furnace body is formed;
  • the left section 1a is provided with a toluene gun interface 7 in the middle of the left end, and the left section 1a is provided with a hot oxygen inlet pipe port 4 on the outer diameter surface of the left end.
  • the hot oxygen inlet pipe port 4 is centered on the left section 1a It is a central annular array distributed on the left section 1a, the hot oxygen inlet pipe port 4 and the axis line of the left section 1a form an angle of 60 to
  • the right end of the right section 1c is connected to the reaction section 2.
  • the reaction section 2 is composed of an air inlet chamber 21 and a feeding ring 22.
  • the air inlet chamber 21 is a volute ring structure, and the feeding ring 22 is fixed on the inner wall of the air inlet chamber 21 ,
  • a tube passage 23 is formed on the feeding ring 22, and a high-temperature-resistant variable-diameter ceramic tube is fixed on the inner wall of the tube channel 23.
  • the high-temperature-resistant variable-diameter ceramic tube is a ceramic tube whose diameter gradually decreases from outside to inside;
  • the air inlet chamber 21 is provided with a titanium tetrachloride air inlet 24, and the air inlet chamber 21 is provided with a reaction section air inlet 2a and a reaction section air outlet 2b along the axial direction of the heating section 1, and the reaction section air inlet 2a and the right
  • the section 1c is connected, and the reaction section gas outlet 2b is connected with the left end of the quenching section 3.
  • the quenching section 3 is a gas-liquid heat exchanger, and the base material from the reaction section 2 enters the gas-liquid heat exchanger for heat exchange and cooling.
  • the body of the left section 1a, the middle section 1b and the right section 1c is composed of a shell 11 and a refractory insulation material 12.
  • the shell 11 and the material are nickel-based alloy materials, and the refractory insulation material 12 is lined and fixed on the inner wall of the shell.
  • the feeding ring 22 is a circular ring body, and the left and right ends of the feeding ring 22 are respectively fixed on the inner wall of the air inlet chamber 21.
  • variable-diameter ceramic tube is inserted into the tube channel 23 and clamped and fixed on the feeding ring 22.
  • Example 1 The process flow of Example 1:
  • the preheated high-temperature hot oxygen (about 950°C) enters the heating section and flows forward in a spiral shape along the inner wall of the equipment through the hot oxygen pipe interface.
  • the high temperature flame (about 3000°C) further uniformly heats the surrounding hot oxygen in the central area of the heating section.
  • the heated and mixed hot oxygen (about 1600°C) enters the center of the mixing section along the axis of the equipment, and at the same time the preheated tetrachloride Titanium gas (about 450°C) enters the reaction section, is evenly distributed through the volute gas chamber, enters the center of the oxidation furnace along the radial direction through the titanium tetrachloride reducer channel, and mixes with hot oxygen, reacts quickly and quenches the section.
  • the material particles continue to grow here, and the cooling water is forced to circulate and exchange heat through the outer jacket of the reaction section to quickly cool the base material of the reaction section and control the particle size and particle size distribution within the required range.
  • Example 2 The process flow of Example 2:
  • the preheated high-temperature hot oxygen (about 950°C) enters the heating section, and flows spirally along the inner wall of the equipment through the hot oxygen pipe interface.
  • the top of the heating section is equipped with a toluene gun interface, which is burned by The high temperature flame (about 3000°C) further uniformly heats the surrounding hot oxygen in the central area of the heating section.
  • the heated and mixed hot oxygen (about 1600°C) enters the center of the mixing section along the axis of the equipment, and at the same time the preheated tetrachloride Titanium gas (about 450°C) enters the reaction section, is evenly distributed through the volute gas chamber, enters the center of the oxidation furnace along the radial direction through the titanium tetrachloride reducer channel, and mixes with hot oxygen, reacts quickly and quenches the section.
  • the material particles continue to grow here, and the cooling water is forced to circulate and exchange heat through the outer jacket of the reaction section to quickly cool the base material of the reaction section and control the particle size and particle size distribution within the required range.
  • the hot oxygen entering the heating section 1 can spirally flow forward along the inner wall of the heating section 1, so that the hot oxygen is evenly heated by the toluene burning flame in the central area of the heating section, and it can also prevent the equipment body from being directly burned by the flame. , Extend the service life of the equipment.
  • the volute inlet chamber 21 can ensure that the pressure and flow of the titanium tetrachloride entering the reaction section 2 are uniform and stable, so that the titanium tetrachloride radially enters the oxidation furnace and mixes with high-temperature oxygen quickly and evenly, in order to prevent the titanium tetrachloride from mixing
  • the pipe channel 23 is lined with a high-temperature resistant variable-diameter ceramic pipe.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
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Abstract

A chlorination process-based titanium dioxide oxidation reactor. A toluene gun connector (7) is provided in the middle of the left end of a left section (1a) of a heating zone (1); one to four hot oxygen intake pipe orifices (4) are provided on the outer diameter surface of the left end of the left section (1a); the hot oxygen intake pipe orifices (4) are distributed on the left section (1a) in an annular array with the circle center of the left section (1a) as the center; an included angle of 60 to 85 degrees is formed between each hot oxygen intake pipe orifice (4) and the axis line of the heating zone (1); an intake chamber (21) of a reaction zone (2) is provided with a titanium tetrachloride gas inlet (24), and the intake chamber (21) is provided with a reaction zone gas inlet (2a) and a reaction zone gas outlet (2b) in the axial direction of the heating zone (1); the reaction zone gas inlet (2a) is communicated with a right section (1c) of the heating zone (1); the reaction zone gas outlet (2b) is communicated with the left end of a quenching zone (3); the quenching zone (3) is a gas-liquid heat exchanger; and a base material discharged from the reaction zone (2) enters the gas-liquid heat exchanger for heat exchange and cooling.

Description

氯化法钛白氧化反应器Chloride titanium dioxide oxidation reactor 技术领域Technical field

本发明涉及钛白粉生产技术领域，更具地说涉及大中型氯化法钛白粉制备过程中的四氯化钛气相氧化制取二氧化钛的设备。The invention relates to the technical field of titanium dioxide production, and more particularly to equipment for preparing titanium dioxide by gas phase oxidation of titanium tetrachloride in the preparation process of large and medium-sized chloride titanium dioxide.

背景技术Background technique

氧化反应器是氯化法钛白生产过程中的核心设备，是影响整个氯化法钛白装置能否正常运行、能否生产出高质量产品的关键因素。在工业化氯化法钛白生产过程中，TiCl4与O2在高温、压力条件下极短时间内完成反应，并生成微米级TiO2颗粒。在这一反应过程中，要解决(1)、合理的反应器结构使生成物粒度分布达到颜料级TiO2要求，(2)、加热段合理的结构设计使O2在短时间内从900℃被均匀加热到1600℃左右。(3)、加热段温度很高，甲苯燃烧区最高达3000℃，应选择合理的设备结构使流场合理，保证设备使用寿命。(4)、高温TiCl4强腐蚀性以及在TiCl4加料环出口高速气流冲蚀，应选择合适耐腐蚀、耐磨蚀材料。(5)、采取特殊设计的TiCl4加料环，确保径向TiCl4气体均亚稳流量加入，使得生成物粒度均匀，(6)、合理的冷却方式以保护TiCl4加料环，(7)、细微的TiO2颗粒极易粘壁，要有可靠的“防疤”、“除疤”措施。Oxidation reactor is the core equipment in the production process of chlorination titanium dioxide, and it is a key factor that affects the normal operation of the entire chlorination titanium dioxide plant and whether it can produce high-quality products. In the industrial chlorination process of titanium dioxide production, TiCl4 and O2 complete the reaction in a very short time under high temperature and pressure conditions, and generate micron-sized TiO2 particles. In this reaction process, it is necessary to solve (1) a reasonable reactor structure so that the particle size distribution of the product meets the requirements of pigment-grade TiO2; (2) a reasonable structure design of the heating section enables the O2 to be evened from 900°C in a short time Heat to about 1600°C. (3) The temperature in the heating section is very high, and the toluene combustion zone is as high as 3000℃. A reasonable equipment structure should be selected to make the flow field reasonable and ensure the service life of the equipment. (4). High temperature TiCl4 is highly corrosive and high-speed air erosion at the exit of TiCl4 feeding ring. Appropriate corrosion-resistant and wear-resistant materials should be selected. (5) Adopt a specially designed TiCl4 feeding ring to ensure that the radial TiCl4 gas is added at a metastable flow rate, so that the particle size of the product is uniform, (6), a reasonable cooling method to protect the TiCl4 feeding ring, (7), fine TiO2 The particles are easy to stick to the wall, so reliable "anti-scar" and "scar removal" measures must be taken.

在如此苛刻工艺条件，目前国内的氧化反应器还有很多不足之处：Under such harsh process conditions, the current domestic oxidation reactors still have many shortcomings:

1.加热段直接在热氧和甲苯火焰混合的高温下运行，设备内衬寿命相当较短，需要定期更换耐火材料。1. The heating section runs directly under the high temperature of the mixture of hot oxygen and toluene flame, the equipment lining life is quite short, and refractory materials need to be replaced regularly.

2.设备结构的原因导致混合段四氯化钛的加入流量和压力不够 均匀，影响氧化基料产品的质量和运行效果。2. The structure of the equipment causes the flow and pressure of titanium tetrachloride in the mixing section to be insufficiently uniform, which affects the quality and operation effect of the oxidation base product.

发明内容Summary of the invention

本发明针对上述问题及目前国内氯化法钛白装置在线氧化反应器的不足，优化设计一种更合理有效的氧化反应器，适用于大中型氯化法钛白生产，具有单台产能大(达到年产4－10万吨规模)、操作稳定性好、设备寿命长、基料产品质量高等优势。In view of the above-mentioned problems and the shortcomings of the on-line oxidation reactor of the current domestic chlorination titanium dioxide device, the present invention optimizes the design of a more reasonable and effective oxidation reactor, which is suitable for the production of large and medium chlorination titanium dioxide, and has a single large capacity ( Achieve an annual output of 40,000 to 100,000 tons), good operation stability, long equipment life, high quality base materials and other advantages.

本发明的技术解决措施如下：The technical solutions of the present invention are as follows:

氯化法钛白氧化反应器，包括加热段、反应段和急冷段，加热段整体由左段、中段和右段构成，左段和中段通过第一法兰盘固定在一起，中段和右段通过第二法兰盘固定在一起，左段、中段和右段同轴心线且形成一个炉体；左段的左端中部设置有甲苯枪接口，左段的左端的外径面上设置有一个至四个热氧进气管口，热氧进气管口以左段的圆心为中心环形阵列分布在左段上，热氧进气管口与左段的轴心线呈60至85度夹角；The chlorination process titanium dioxide oxidation reactor includes a heating section, a reaction section and a quenching section. The heating section is composed of a left section, a middle section and a right section as a whole. The left section and the middle section are fixed together by a first flange, the middle section and the right section Fixed together by the second flange, the left section, the middle section and the right section are coaxial and form a furnace body; the left section of the left section is provided with a toluene gun interface, and the left section has a To four hot oxygen inlet pipe ports, the hot oxygen inlet pipe ports are distributed in an annular array on the left section centered on the circle center of the left section, and the angle between the hot oxygen inlet pipe ports and the axis line of the left section is 60 to 85 degrees;

右段的右端与反应段相通接，反应段由进气室和加料环构成，进气室为蜗壳式环状结构，加料环固定在进气室的内壁上，加料环上成型有管通道，管通道内壁上固定有耐高温变径陶瓷管，耐高温变径陶瓷管为由外向内直径渐次缩小的陶瓷管；The right end of the right section is connected to the reaction section. The reaction section is composed of an air inlet chamber and a feeding ring. The air inlet chamber is a volute ring structure. The feeding ring is fixed on the inner wall of the air inlet chamber. A pipe channel is formed on the feeding ring. , The high temperature resistant variable diameter ceramic tube is fixed on the inner wall of the tube channel, and the high temperature resistant variable diameter ceramic tube is a ceramic tube whose diameter gradually decreases from outside to inside;

进气室设置有四氯化钛进气口，同时进气室沿加热段的轴向设置有反应段进气口与反应段出气口，反应段进气口与右段相通接，反应段出气口与急冷段的左端相通接，急冷段为气液换热器，反应段出来的基料进入气液换热器中换热冷却。The air inlet chamber is provided with a titanium tetrachloride air inlet, and the air inlet chamber is provided with an air inlet of the reaction section and an air outlet of the reaction section along the axial direction of the heating section. The air inlet of the reaction section is connected with the right section, and the reaction section outlet The gas port is connected to the left end of the quenching section. The quenching section is a gas-liquid heat exchanger, and the base material from the reaction section enters the gas-liquid heat exchanger for heat exchange and cooling.

所述管通道为四至十二个。There are four to twelve tube channels.

所述左段、中段和右段的本体由外壳和耐火绝热材料构成，外壳和材料材质为镍基合金材料，耐火绝热材料内衬固定在外壳的内壁上。The bodies of the left section, the middle section and the right section are composed of a shell and a refractory heat-insulating material, the shell and the material are made of nickel-based alloy material, and the refractory and heat-insulating material is lined and fixed on the inner wall of the shell.

所述加料环为一圆环体，加料环的左右两端分别固定在进气室的内壁上。The feeding ring is a circular ring body, and the left and right ends of the feeding ring are respectively fixed on the inner wall of the air inlet chamber.

所述变径陶瓷管插套在管通道中且卡紧固定在加料环上。The variable-diameter ceramic tube is inserted in the tube channel and clamped and fixed on the feeding ring.

本发明的有益效果在于：The beneficial effects of the present invention are:

利用合理的热氧进气管口布局，使热氧进入加热段后沿其内壁轴向螺旋向前流动，避免设备内壁受火焰直接灼烧，延长设备的使用寿命；采用蜗壳形设计的四氯化钛气室可以有效保证四氯化钛流量压力稳定，使热氧和四氯化钛充分混合反应，提高反应生成的半成品基料质量。Use the reasonable layout of the hot oxygen inlet pipe to make the hot oxygen flow forward spirally along the inner wall axis after entering the heating section, avoiding the direct burning of the inner wall of the equipment by the flame, and prolonging the service life of the equipment; adopts the volute-shaped design of tetrachloride The titanium gas chamber can effectively ensure the stable flow and pressure of titanium tetrachloride, make the hot oxygen and titanium tetrachloride fully mix and react, and improve the quality of the semi-finished base material produced by the reaction.

附图说明Description of the drawings

图1为本发明的结构示意图；Figure 1 is a schematic diagram of the structure of the present invention;

图2为图1中A——A处剖视图；Figure 2 is a cross-sectional view from A to A in Figure 1;

图3为图1中B——B处剖视图。Fig. 3 is a cross-sectional view of B-B in Fig. 1.

图中：1、加热段；2、反应段；3、急冷段；4、热氧管口；5、第一法兰盘；6、第二法兰盘；7、甲苯枪接口；21、进气室；22、加料环；23、管通道；24、四氯化钛进气口。In the figure: 1. Heating section; 2. Reaction section; 3. Quenching section; 4. Hot oxygen pipe port; 5. First flange; 6. Second flange; 7. Toluene gun interface; 21. Inlet Air chamber; 22. Feeding ring; 23. Pipe passage; 24. Titanium tetrachloride air inlet.

具体实施方式Detailed ways

实施例1：见图1至3所示，氯化法钛白氧化反应器，包括加热段1、反应段2和急冷段3，加热段1整体由左段1a、中段1b和右 段1c构成，左段1a和中段1b通过第一法兰盘5固定在一起，中段1b和右段1c通过第二法兰盘6固定在一起，左段1a、中段1b和右段1c同轴心线且形成一个炉体；左段1a的左端中部设置有甲苯枪接口7，左段1a的左端的外径面上设置有一个热氧进气管口4，热氧进气管口4以左段1a的圆心为中心环形阵列分布在左段1a上，热氧进气管口4与左段1a的轴心线呈60至85度夹角；Example 1: As shown in Figures 1 to 3, the chlorination titanium dioxide oxidation reactor includes a heating section 1, a reaction section 2 and a quenching section 3. The heating section 1 is composed of a left section 1a, a middle section 1b and a right section 1c as a whole , The left section 1a and the middle section 1b are fixed together by the first flange 5, the middle section 1b and the right section 1c are fixed together by the second flange 6, the left section 1a, the middle section 1b and the right section 1c are coaxial and A furnace body is formed; the left section 1a is provided with a toluene gun interface 7 in the middle of the left end, and the left section 1a is provided with a hot oxygen inlet pipe port 4 on the outer diameter surface of the left end. The hot oxygen inlet pipe port 4 is centered on the left section 1a It is a central annular array distributed on the left section 1a, the hot oxygen inlet pipe port 4 and the axis line of the left section 1a form an angle of 60 to 85 degrees;

右段1c的右端与反应段2相通接，反应段2由进气室21和加料环22构成，进气室21为蜗壳式环状结构，加料环22固定在进气室21的内壁上，加料环22上成型有管通道23，管通道23内壁上固定有耐高温变径陶瓷管，耐高温变径陶瓷管为由外向内直径渐次缩小的陶瓷管；The right end of the right section 1c is connected to the reaction section 2. The reaction section 2 is composed of an air inlet chamber 21 and a feeding ring 22. The air inlet chamber 21 is a volute ring structure, and the feeding ring 22 is fixed on the inner wall of the air inlet chamber 21 , A tube passage 23 is formed on the feeding ring 22, and a high-temperature-resistant variable-diameter ceramic tube is fixed on the inner wall of the tube channel 23. The high-temperature-resistant variable-diameter ceramic tube is a ceramic tube whose diameter gradually decreases from outside to inside;

进气室21设置有四氯化钛进气口24，同时进气室21沿加热段1的轴向设置有反应段进气口2a与反应段出气口2b，反应段进气口2a与右段1c相通接，反应段出气口2b与急冷段3的左端相通接，急冷段3为气液换热器，反应段2出来的基料进入气液换热器中换热冷却。The air inlet chamber 21 is provided with a titanium tetrachloride air inlet 24, and the air inlet chamber 21 is provided with a reaction section air inlet 2a and a reaction section air outlet 2b along the axial direction of the heating section 1, and the reaction section air inlet 2a and the right The section 1c is connected, and the reaction section gas outlet 2b is connected with the left end of the quenching section 3. The quenching section 3 is a gas-liquid heat exchanger, and the base material from the reaction section 2 enters the gas-liquid heat exchanger for heat exchange and cooling.

所述管通道23为八个。There are eight tube channels 23.

所述左段1a、中段1b和右段1c的本体由外壳11和耐火绝热材料12构成，外壳11和材料材质为镍基合金材料，耐火绝热材料12内衬固定在外壳的内壁上。The body of the left section 1a, the middle section 1b and the right section 1c is composed of a shell 11 and a refractory insulation material 12. The shell 11 and the material are nickel-based alloy materials, and the refractory insulation material 12 is lined and fixed on the inner wall of the shell.

所述加料环22为一圆环体，加料环22的左右两端分别固定在进气室21的内壁上。The feeding ring 22 is a circular ring body, and the left and right ends of the feeding ring 22 are respectively fixed on the inner wall of the air inlet chamber 21.

所述变径陶瓷管插套在管通道23中且卡紧固定在加料环22上。The variable-diameter ceramic tube is inserted into the tube channel 23 and clamped and fixed on the feeding ring 22.

实施例1的工艺流程：预热后的高温热氧(约950℃)进入加热段，经过热氧管接口沿设备内壁螺旋形向前流动，加热段顶端设有甲苯枪接口，通过甲苯燃烧的高温火焰(约3000℃)在加热段中央区域对四周的热氧进一步均匀加热升温，升温并混合后的热氧(约1600℃)沿设备轴向进入混合段中心，同时预热后的四氯化钛气体(约450℃)进入反应段，经蜗壳气室均匀分布后经四氯化钛变径管通道沿径向进入氧化炉中心与热氧混合，快速反应并急冷段，生成的基料颗粒在此不断长大，通过反应段外部夹套冷却水强制循环换热，快速冷却反应段的基料并控制颗粒粒径和粒径分布在要求范围。The process flow of Example 1: The preheated high-temperature hot oxygen (about 950°C) enters the heating section and flows forward in a spiral shape along the inner wall of the equipment through the hot oxygen pipe interface. The high temperature flame (about 3000℃) further uniformly heats the surrounding hot oxygen in the central area of the heating section. The heated and mixed hot oxygen (about 1600℃) enters the center of the mixing section along the axis of the equipment, and at the same time the preheated tetrachloride Titanium gas (about 450℃) enters the reaction section, is evenly distributed through the volute gas chamber, enters the center of the oxidation furnace along the radial direction through the titanium tetrachloride reducer channel, and mixes with hot oxygen, reacts quickly and quenches the section. The material particles continue to grow here, and the cooling water is forced to circulate and exchange heat through the outer jacket of the reaction section to quickly cool the base material of the reaction section and control the particle size and particle size distribution within the required range.

实施例2，加热段1左端的外径面上设置有四个热氧进气管口4，所述管通道9为十二个，其余同实施例1。In the second embodiment, four hot oxygen inlet pipe ports 4 are provided on the outer diameter surface of the left end of the heating section 1, and the number of the pipe channels 9 is twelve, and the rest are the same as in the first embodiment.

实施例2的工艺流程：预热后的高温热氧(约950℃)进入加热段，经过热氧管接口沿设备内壁螺旋形向前流动，加热段顶端设有甲苯枪接口，通过甲苯燃烧的高温火焰(约3000℃)在加热段中央区域对四周的热氧进一步均匀加热升温，升温并混合后的热氧(约1600℃)沿设备轴向进入混合段中心，同时预热后的四氯化钛气体(约450℃)进入反应段，经蜗壳气室均匀分布后经四氯化钛变径管通道沿径向进入氧化炉中心与热氧混合，快速反应并急冷段，生成的基料颗粒在此不断长大，通过反应段外部夹套冷却水强制循环换热，快速冷却反应段的基料并控制颗粒粒径和粒径分布在要求范围。The process flow of Example 2: The preheated high-temperature hot oxygen (about 950°C) enters the heating section, and flows spirally along the inner wall of the equipment through the hot oxygen pipe interface. The top of the heating section is equipped with a toluene gun interface, which is burned by The high temperature flame (about 3000℃) further uniformly heats the surrounding hot oxygen in the central area of the heating section. The heated and mixed hot oxygen (about 1600℃) enters the center of the mixing section along the axis of the equipment, and at the same time the preheated tetrachloride Titanium gas (about 450℃) enters the reaction section, is evenly distributed through the volute gas chamber, enters the center of the oxidation furnace along the radial direction through the titanium tetrachloride reducer channel, and mixes with hot oxygen, reacts quickly and quenches the section. The material particles continue to grow here, and the cooling water is forced to circulate and exchange heat through the outer jacket of the reaction section to quickly cool the base material of the reaction section and control the particle size and particle size distribution within the required range.

工作原理：进入加热段1的热氧能够沿加热段1内壁螺旋向前快速流动，使热氧在被加热段中央区域的甲苯燃烧火焰均匀加热的同时， 也可避免设备本体受火焰直接灼烧，延长设备的使用寿命。Working principle: The hot oxygen entering the heating section 1 can spirally flow forward along the inner wall of the heating section 1, so that the hot oxygen is evenly heated by the toluene burning flame in the central area of the heating section, and it can also prevent the equipment body from being directly burned by the flame. , Extend the service life of the equipment.

蜗壳式进气室21可以保证进入反应段2中的四氯化钛压力和流量均匀稳定，使四氯化钛径向进入氧化炉与高温氧气垂直快速均匀混合，为防止四氯化钛对加料环22的冲刷和腐蚀，管通道23内衬耐高温变径陶瓷管。The volute inlet chamber 21 can ensure that the pressure and flow of the titanium tetrachloride entering the reaction section 2 are uniform and stable, so that the titanium tetrachloride radially enters the oxidation furnace and mixes with high-temperature oxygen quickly and evenly, in order to prevent the titanium tetrachloride from mixing For the scouring and corrosion of the feeding ring 22, the pipe channel 23 is lined with a high-temperature resistant variable-diameter ceramic pipe.

Claims (5)

氯化法钛白氧化反应器，包括加热段(1)、反应段(2)和急冷段(3)，其特征在于：加热段(1)整体由左段(1a)、中段(1b)和右段(1c)构成，左段(1a)和中段(1b)通过第一法兰盘(5)固定在一起，中段(1b)和右段(1c)通过第二法兰盘(6)固定在一起，左段(1a)、中段(1b)和右段(1c)同轴心线且形成一个炉体；左段(1a)的左端中部设置有甲苯枪接口(7)，左段(1a)的左端的外径面上设置有一个至四个热氧进气管口(4)，热氧进气管口(4)以左段(1a)的圆心为中心环形阵列分布在左段(1a)上，热氧进气管口(4)与左段(1a)的轴心线呈60至85度夹角；The chlorination method titanium dioxide oxidation reactor includes a heating section (1), a reaction section (2) and a quenching section (3). It is characterized in that the heating section (1) is composed of the left section (1a), the middle section (1b) and The right section (1c) is composed, the left section (1a) and the middle section (1b) are fixed together by the first flange (5), and the middle section (1b) and the right section (1c) are fixed by the second flange (6) Together, the left section (1a), the middle section (1b) and the right section (1c) are coaxial and form a furnace body; the left section (1a) is provided with a toluene gun interface (7), and the left section (1a) ) Is provided with one to four hot oxygen inlet pipe ports (4) on the outer diameter surface of the left end, and the hot oxygen inlet pipe ports (4) are distributed in an annular array on the left section (1a) with the center of the left section (1a) as the center. Above, the included angle between the hot oxygen inlet pipe port (4) and the axis of the left section (1a) is 60 to 85 degrees; 右段(1c)的右端与反应段(2)相通接，反应段(2)由进气室(21)和加料环(22)构成，进气室(21)为蜗壳式环状结构，加料环(22)固定在进气室(21)的内壁上，加料环(22)上成型有管通道(23)，管通道(23)内壁上固定有耐高温变径陶瓷管，耐高温变径陶瓷管为由外向内直径渐次缩小的陶瓷管；The right end of the right section (1c) is connected to the reaction section (2). The reaction section (2) is composed of an air inlet chamber (21) and a feeding ring (22). The air inlet chamber (21) has a volute ring structure. The feeding ring (22) is fixed on the inner wall of the air inlet chamber (21), a pipe channel (23) is formed on the feeding ring (22), and the inner wall of the pipe channel (23) is fixed with a high temperature resistant variable diameter ceramic tube, which is resistant to high temperature change. Diameter ceramic tube is a ceramic tube whose diameter gradually decreases from outside to inside; 进气室(21)设置有四氯化钛进气口(24)，同时进气室(21)沿加热段(1)的轴向设置有反应段进气口(2a)与反应段出气口(2b)，反应段进气口(2a)与右段(1c)相通接，反应段出气口(2b)与急冷段(3)的左端相通接，急冷段(3)为气液换热器，反应段(2)出来的基料进入气液换热器中换热冷却。The air inlet chamber (21) is provided with a titanium tetrachloride air inlet (24), and the air inlet chamber (21) is provided with a reaction section air inlet (2a) and a reaction section air outlet along the axial direction of the heating section (1) (2b), the gas inlet (2a) of the reaction section is connected with the right section (1c), the gas outlet (2b) of the reaction section is connected with the left end of the quench section (3), and the quench section (3) is a gas-liquid heat exchanger , The base material from the reaction section (2) enters the gas-liquid heat exchanger for heat exchange and cooling. 根据权利要求1所述的氯化法钛白氧化反应器，其特征在于：管通道(23)为四至十二个。The chlorination method titanium dioxide oxidation reactor according to claim 1, characterized in that there are four to twelve tube channels (23). 根据权利要求1所述的氯化法钛白氧化反应器，其特征在于： 左段(1a)、中段(1b)和右段(1c)的本体由外壳(11)和耐火绝热材料(12)构成，外壳(11)和材料材质为镍基合金材料，耐火绝热材料(12)内衬固定在外壳的内壁上。The chlorination method titanium dioxide oxidation reactor according to claim 1, characterized in that: the body of the left section (1a), the middle section (1b) and the right section (1c) consists of a shell (11) and a refractory insulation material (12) Composition, the shell (11) and the material are nickel-based alloy materials, and the fire-resistant and heat-insulating material (12) is lined and fixed on the inner wall of the shell. 根据权利要求1所述的氯化法钛白氧化反应器，其特征在于：加料环(22)为一圆环体，加料环(22)的左右两端分别固定在进气室(21)的内壁上。The chlorination method titanium dioxide oxidation reactor according to claim 1, characterized in that: the feeding ring (22) is a circular ring body, and the left and right ends of the feeding ring (22) are respectively fixed in the inlet chamber (21). On the inner wall. 根据权利要求1所述的氯化法钛白氧化反应器，其特征在于：变径陶瓷管插套在管通道(23)中且卡紧固定在加料环(22)上。The chlorination method titanium dioxide oxidation reactor according to claim 1, characterized in that: the variable-diameter ceramic tube is inserted in the tube channel (23) and clamped and fixed on the feeding ring (22).
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