CN1446621A - Tube type device respondent to water heat in high temperature and pressure - Google Patents
Tube type device respondent to water heat in high temperature and pressure Download PDFInfo
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- CN1446621A CN1446621A CN 03121941 CN03121941A CN1446621A CN 1446621 A CN1446621 A CN 1446621A CN 03121941 CN03121941 CN 03121941 CN 03121941 A CN03121941 A CN 03121941A CN 1446621 A CN1446621 A CN 1446621A
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Abstract
A high-temp and-perssure hydrothermal tubular reactor for preparing powder material is composed of a main body of tuber reactor with forced circulation, high-temp circulating pump, heater, gas-liquid separator and valves. Its advantages are large heat-transfer area, high heat exchanging efficiency, small size, simple structure, and less chemical corrosion.
Description
Technical field
The present invention relates to a kind of high-temperature high-voltage reaction device that is used for the powder body material hydrothermal preparation, belong to technical field of powdered material preparation.
Background technology
Along with modern society is growing to the demand of high-performance new function powder body material, promoted the powder body material Development of Preparation Technology.Advantage as the normal temperature synthetic method of one of powder body material technology of preparing is that component is easily controlled, equipment is simple, production cost is low; But the synthetic common pattern of powder is irregular, crystallinity is not good enough, easily reunite and the Separation of Solid and Liquid difficulty, and its application is restricted.If on the synthetic basis of normal temperature, carry out hydro-thermal reaction and surface modification treatment, can significantly improve the performance of normal temperature synthetic product, make its epigranular, the dispersed raising.Hydrothermal treatment consists is to be solvent with the synthetic slurries of normal temperature, (carries out chemical reaction under the 0.1Mpa～22Mpa) at uniform temperature (between the boiling point and supercritical temperature of water, promptly 100 ℃～373 ℃) and pressure.In high-temperature high-pressure water solution, the molecular motion aggravation causes reaction speed to improve, make the moisture chemical combination that is adsorbed on the crystal face, thereby destroy the liquid level that is adsorbed on the crystal face, reduce the resistance that adsorption layer is grown up to crystal, realize being difficult at normal temperatures and pressures the many control particle nucleation of carrying out and the reaction of the speed of growth, make it generate pattern, structure and all controllable powder granule of size.The reaction temperature of hydro-thermal method is in 100 ℃～120 ℃ basically at present, reaction pressure is 0.1～0.2Mpa, prepared powder body material still has very big defective on feature and function, its fundamental cause is: in corrosive medium, hydro-thermal reaction fails to obtain the reaction condition of HTHP.
Hydro-thermal method as the preparation powder body material in the prior art has been used to synthesizing superfine and different in nature powder, for example materials such as new ceramics, crystal, composite oxides.But when the hydro-thermal reaction of some materials is handled, owing to contain chlorion (Cl in the slurries
-), bromide ion (Br
-), hydroxide ion (OH
-) wait corrosion composition, the slurries rerum natura condition that adds HTHP is (with the rising of temperature, the corrosivity of most of corrosion compositions strengthens), and the time of hydro-thermal reaction is very long mostly, this exacting terms has proposed higher requirement to the structure and the material of reactor.
For the global design of high-temperature high-pressure anti-corrosive erosion hydrothermal reactor, mainly consider the sticking wall of powder granule in the viscosity of mode of heating, thermal conductivity factor, slurries and the slurries etc.Primary structure pattern as the liquid phase water thermal reactor, what use was maximum at present is tank reactor, the HTHP tank reactor has been subjected to the restriction of following several respects when the inside lining anti-corrosive nonmetallic materials: 1. the heat transfer coefficient of wall is lower, prolong heat time heating time greatly, increased the consumption of the energy; 2. when the sticking wall of powder granule in the slurries was big, the thermal conductivity factor of wall reduced more; 3. the sealing difficulty of kettle, security descends; 4. nonmetal anti-corrosion material is subjected to the restriction of creep temperature can not obtain temperature required requirement etc.Therefore for the hydrothermal reactor of high temperature, high anti-corrosive properties, the sticking wall of high particle, it is irrational being designed to the still formula.
Summary of the invention
The objective of the invention is at the needed high-temperature and high-pressure conditions of hydro-thermal reaction, and fully take into account the sticking wall of powder granule in corrosivity, viscosity and the slurries of slurries and thermal conductivity factor characteristics etc., a kind of sticking wall restriction of medium when not being subjected to heat exchange is provided, has the higher coefficient of heat transfer and corrosion resistant tubular type high-temperature high pressure water thermal reaction apparatus, to adapt to the preparation of high-performance new function powder body material.
The present invention is achieved through the following technical solutions: a kind of tubular type high-temperature high pressure water thermal reaction apparatus, it is characterized in that: this device adopts tubular type to circulate reactor, described tubular type circulates reactor mainly by the tubular reactor body of forced circulation, be arranged on the high temperature circulation pump on the tubular reactor body, be arranged in reactor body external heated device, the gas-liquid separator and the corresponding valve that are vertically mounted on the reactor body are formed.
Feature of the present invention also is: the outlet that circulates reactor in described tubular type connects an atmospheric flashing filling, and this atmospheric flashing is irritated mainly and is made up of housing and the cyclone separator that is arranged in the housing.
The inside that the tubular reactor body that another technical characterictic of the present invention is described forced circulation, gas-liquid separator and atmospheric flashing are irritated all is lined with resistant material.
The tubular reactor body of described forced circulation adopts U type pipe or ring pipe; Be arranged in reactor body external heated device and adopt heating of sleeve pipe medium or electrical heating.
The present invention compared with prior art, have the following advantages and the high-lighting effect: by adopting the forced circulation tubular reactor, help on the one hand mixing and heating, improve the heat transfer area of reactor, strengthen the heat exchange of internal flow medium, improve the exchange capability of heat of slurries, thereby can save heat energy and shorten heat time heating time, reduce the volume of equipment; Because tube fluid has very big perturbation, can effectively prevent the sticking wall of powder granule simultaneously, guarantee the safe and stable operation of reactor, chemical mediator is to the etching problem of equipment when efficiently solving the HTHP hydro-thermal reaction.This apparatus structure is simple, and is easy and simple to handle, easy to utilize.
Description of drawings
Fig. 1 is the structural representation of tubular type high-temperature high pressure water thermal reaction apparatus embodiment provided by the invention.
The specific embodiment
Further specify the concrete structure of the present invention and the course of work below in conjunction with accompanying drawing.
Concrete structure of the present invention as shown in Figure 1, this device mainly comprises the tubular reactor body 6 of forced circulation, be arranged on the high temperature circulation pump 20 on the tubular reactor body, be arranged in reactor body external heated device 5, be vertically mounted on gas-liquid separator 10 and many group valves on the reactor body 6.This device makes the slurries shuttling movement in reactor that contains powder granule by the promotion of high temperature circulation pump, helps mixing and heating, and tubular reactor body 6 can be designed to different patterns, as " U " type tubular type, annular tube type etc.
In feed pipe 1, charging valve 2 were sent into the pipe reaction pipe 6 of forced circulation, the reaction tube material can adopt common steel tube inside lining anti-corrosive material 7 by the slurry of normal temperature synthesis reaction vessel preparation; For different corrosion slurries,, can select different corrosion resisting liner materials for use according to the physical parameter of hydro-thermal reaction; For example adopt corrosion resistant metal material or nonmetallic materials.The metal resistant material generally can adopt the anti-corrosion Langaloy F of Hasiteluoyi (Hastelloy-F), monel metal (Monel), Hasiteluoyi is anti-corrosion Langaloy C (Hastelloy-C), titanium, titanium alloy, Hasiteluoyi is anti-corrosion Langaloy B (Hastelloy-B), zirconium, tantalum etc.; Anticorrosion nonmetallic materials generally comprise steel glass, pottery, enamel, polyethylene, polypropylene, polytetrafluoroethylene (PTFE) etc.
Close charging valve 2 and valve 22 after filling material, material circulates in reaction tube under the promotion of high temperature circulation pump 20, and heat provides by being arranged in reaction tube external heated device 5, and this heater can adopt sleeve pipe medium or electrical heating; When adopting the sleeve pipe heating, heat medium enters heating muff by import 4, flows out heating muff by outlet 8.Operating temperature in the pipe reaction pipe is by the temperature sensor measurement in the temperature-measuring casing 3, and regulates control by temperature regulating device.One vapour liquid separator 10 is installed at the top of reactor, its objective is in reactor, fill slurries after, in the increasing temperature and pressure process, the gas that does not have in the dilation of slurries and the reactor to have arranged is entered vapour liquid separator 10 through valve 9, so both helped guaranteeing the pressure stability in the reactor, and can prevent that again the high temperature circulation pump from cavitating.Vapor-liquid separation can take place in the slurries that enter simultaneously in the vapour liquid separator; In pressure is higher than reactor, during operating pressure, can keep pressure stability, make pressure be no more than rated operating pressure by the safety valve 11 on separator top.Outlet 12 on the vapour liquid separator is the pressure measxurement mouth, is used for measuring the pressure in the reactor.After hydro-thermal reaction finished, the pressure loading valve 13 on Open valve 22 and the reactor discharge nozzle 14, material entered atmospheric flashing jar 15 under differential pressure action.This flash tank is made of housing and the cyclone separator 16 that is arranged in the housing.Circulate the atmospheric flashing jar 15 that reactor is connected with tubular type and can play quick cooling effect.After hydro-thermal reaction finishes, slurries in the reactor enter flash tank, in the extremely short time, make the pressure of slurries reduce to normal pressure, also corresponding the reducing to below 100 ℃ of temperature of while slurries, part water evaporates in this process in the slurries, slurries are concentrated, alleviated sedimentation time and filter pressure subsequently.Built-in cyclone separator 16, its effect are to separate the powder granule of carrying secretly in the gas of flash distillation generation; Water vapour that flash distillation produces and the powder granule that carries thereof are after cyclone separator 16 separates, and outside the gas drain tank, particle precipitates drying along with slurries are discharged through material outlet valve 19.The inside and outside wall of cyclone separator 16, flash tank 15 all serves as a contrast anti-corrosion material; The atmospheric pressure environment of flash tank inside is controlled by the safety valve 18 on top, is the Pressure gauge installing port in the outlet 17 of flash drum overhead.
Embodiment 1:
When adopting above-mentioned tubular type high-temperature high pressure water thermal reaction apparatus to carry out high-purity fine fire retardant magnesium hydroxide hydro-thermal reaction (chloride ion-containing in the slurries), the inside lining anti-corrosive material is a polytetrafluoroethylene (PTFE), can prevent the corrosion of chlorion well.Temperature is controlled to be 200 ℃ in the pipe, the hydro-thermal time set is 4 hours, velocity in pipes is 4m/s, and the crystal property of gained magnesium hydroxide particle has had very big improvement before than hydro-thermal reaction as a result, has obtained that pattern rule, particle diameter are evenly distributed, the hexagonal plate magnesium hydroxide product of high degree of dispersion.
Embodiment 2
Adopt above-mentioned tubular type high-temperature high pressure water thermal reaction apparatus to carry out the hydro-thermal reaction of alkali magnesium sulfate crystal whisker, reactor tube liner nickel alloy can effectively prevent the corrosion of hydroxide ion.Temperature is controlled at 180～200 ℃ in the pipe, and the hydro-thermal time set is 6 hours, can obtain the high-quality alkali magnesium sulfate crystal whisker of needle-like pattern.
Claims (5)
1. tubular type high-temperature high pressure water thermal reaction apparatus, it is characterized in that: this device adopts tubular type to circulate reactor, described tubular type circulates reactor mainly by the tubular reactor body (6) of forced circulation, be arranged on the high temperature circulation pump (20) on the tubular reactor body, be arranged in reactor body external heated device (5), the gas-liquid separator (10) and the corresponding valve that are vertically mounted on the reactor body are formed.
2. according to the described tubular type high-temperature high pressure water of claim 1 thermal reaction apparatus, it is characterized in that: the outlet that circulates reactor in described tubular type connects an atmospheric flashing filling (15), and this flash distillation is irritated mainly and is made up of housing and the cyclone separator (16) that is arranged in the housing.
3. according to claim 1 or 2 described tubular type high-temperature high pressure water thermal reaction apparatus, it is characterized in that: the inside that described forced circulation tubular reactor body, gas-liquid separator and atmospheric flashing are irritated all is lined with resistant material.
4. according to the described tubular type high-temperature high pressure water thermal reaction apparatus of claim 3, it is characterized in that: described forced circulation tubular reactor body adopts U type pipe or ring pipe.
5. according to the described tubular type high-temperature high pressure water thermal reaction apparatus of claim 1, it is characterized in that: the heater (5) that is arranged in the tubular reactor body exterior adopts heating of sleeve pipe medium or electrical heating.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031219411A CN1185046C (en) | 2003-04-18 | 2003-04-18 | Tube type device respondent to water heat in high temperature and pressure |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031219411A CN1185046C (en) | 2003-04-18 | 2003-04-18 | Tube type device respondent to water heat in high temperature and pressure |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1446621A true CN1446621A (en) | 2003-10-08 |
| CN1185046C CN1185046C (en) | 2005-01-19 |
Family
ID=28050550
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB031219411A Expired - Fee Related CN1185046C (en) | 2003-04-18 | 2003-04-18 | Tube type device respondent to water heat in high temperature and pressure |
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|---|---|
| CN (1) | CN1185046C (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102120162A (en) * | 2011-01-06 | 2011-07-13 | 上海交通大学 | Combined type reactor for high-temperature high-voltage hydro-thermal treatment and treating method thereof |
| WO2013117000A1 (en) * | 2012-02-09 | 2013-08-15 | 同济大学 | System and method for hydrothermal reaction |
| CN103933924A (en) * | 2013-12-16 | 2014-07-23 | 江苏梅兰化工有限公司 | Multitube large power cracking reactor |
| CN105130175A (en) * | 2015-09-08 | 2015-12-09 | 安徽凤阳淮河玻璃有限公司 | Continuously operable chemically-toughened glass ultrasonic hydrothermal kettle |
| CN106732310A (en) * | 2017-01-22 | 2017-05-31 | 清华大学 | Method, the system of a kind of hydro-thermal reaction device and its treatment powder body material |
| CN107175052A (en) * | 2017-05-24 | 2017-09-19 | 中国科学院上海高等研究院 | Gas-liquid tubular reactor, gas liquid reaction system and its application with fractal structure |
| CN114107695A (en) * | 2021-10-26 | 2022-03-01 | 江西理工大学 | Method and device for synchronously and deeply removing heavy metal impurities in zinc hydrometallurgy solution |
-
2003
- 2003-04-18 CN CNB031219411A patent/CN1185046C/en not_active Expired - Fee Related
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102120162A (en) * | 2011-01-06 | 2011-07-13 | 上海交通大学 | Combined type reactor for high-temperature high-voltage hydro-thermal treatment and treating method thereof |
| CN102120162B (en) * | 2011-01-06 | 2013-01-09 | 上海交通大学 | Combined type reactor for high-temperature high-voltage hydro-thermal treatment and treating method thereof |
| WO2013117000A1 (en) * | 2012-02-09 | 2013-08-15 | 同济大学 | System and method for hydrothermal reaction |
| US9662623B2 (en) | 2012-02-09 | 2017-05-30 | Tongji University | System and method for hydrothermal reaction |
| CN103933924A (en) * | 2013-12-16 | 2014-07-23 | 江苏梅兰化工有限公司 | Multitube large power cracking reactor |
| CN105130175A (en) * | 2015-09-08 | 2015-12-09 | 安徽凤阳淮河玻璃有限公司 | Continuously operable chemically-toughened glass ultrasonic hydrothermal kettle |
| CN106732310A (en) * | 2017-01-22 | 2017-05-31 | 清华大学 | Method, the system of a kind of hydro-thermal reaction device and its treatment powder body material |
| CN106732310B (en) * | 2017-01-22 | 2019-01-15 | 清华大学 | A kind of hydro-thermal reaction device and its method, the system for handling powder body material |
| CN107175052A (en) * | 2017-05-24 | 2017-09-19 | 中国科学院上海高等研究院 | Gas-liquid tubular reactor, gas liquid reaction system and its application with fractal structure |
| CN107175052B (en) * | 2017-05-24 | 2019-11-19 | 中国科学院上海高等研究院 | Gas-liquid tubular reactor, gas liquid reaction system and its application with fractal structure |
| CN114107695A (en) * | 2021-10-26 | 2022-03-01 | 江西理工大学 | Method and device for synchronously and deeply removing heavy metal impurities in zinc hydrometallurgy solution |
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| Publication number | Publication date |
|---|---|
| CN1185046C (en) | 2005-01-19 |
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