CN206500147U - A kind of reactor fast cooling device of Hydrothermal Synthesiss titanium dioxide nano material - Google Patents
A kind of reactor fast cooling device of Hydrothermal Synthesiss titanium dioxide nano material Download PDFInfo
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- CN206500147U CN206500147U CN201720191605.2U CN201720191605U CN206500147U CN 206500147 U CN206500147 U CN 206500147U CN 201720191605 U CN201720191605 U CN 201720191605U CN 206500147 U CN206500147 U CN 206500147U
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- conduction oil
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- reacting kettle
- cooling water
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Abstract
The utility model provides a kind of reactor fast cooling device of Hydrothermal Synthesiss titanium dioxide nano material, including the chuck set on reactor outer wall；Cooling water coil inside reactor and the compressed air line being connected with cooling water coil；Conduction oil basin with heat insulation function；And conduction oil feeding device；Chuck, conduction oil basin, conduction oil feeding device are in turn connected to form circulation loop.The device has that cooling is slow except solving the reactor of existing use electrical bar heating conduction oil, in addition to temperature fall time, while solution energy consumption is of a relatively high, the problems such as under low production efficiency.
Description
Technical field
The utility model belongs to titanium dioxide nano material production field, particularly Hydrothermal Synthesiss titanium dioxide nano material
Reactor fast cooling device.
Background technology
At present, the synthesis technique both at home and abroad on nano titanium oxide is varied, according to the physical aspect of reactant system
Preparation technology can be typically divided into three classes：Vapor phase method, liquid phase method and solid phase method.By contrast, liquid phase rule have equipment it is simple,
Operation is simple, product is controllable, industrialization low cost and other advantages, thus has obtained wider application.Common side in liquid phase method
Method includes Hydrolyze method, hydro-thermal method, micro emulsion method, sol-gel process, liquid phase deposition etc., the product crystal formation that wherein prepared by hydro-thermal method
Good, granularity is small, be uniformly difficult to reunite, and these unique advantages make it that hydro-thermal method increasingly causes extensive concern, become in recent years
The study hotspot of Material Field.
In the synthesis of titanium dioxide nano material, reaction temperature is to microcrystallization degree, particulate crystallite dimension, particle morphology
Deng influence it is very big.Preferably 160 DEG C or so of the reaction temperature typically used in current industry, the titanium dioxide prepared at this temperature
Titanium particulate crystal defect is less, and the higher particularly photocatalysis effect of crystallization degree is excellent.In Chemical Manufacture, once reaction temperature is super
150 DEG C are crossed, if using water vapour as heating medium, water vapor pressure is at least higher than 0.6MPa.Current country's chemical industry machine
When tool industry is using chuck heating (cooling), chuck design work pressure is generally below 0.6MPa, therefore in higher temperature, OK
Heat-conducting oil heating typically is selected in industry, in view of domestic severe Environmental Protection Situation, heating conduction oil typically uses electrical bar, user
Just, unlike producing the pollution such as sulfur dioxide, oxynitrides and dust using coal heating.
But there is the shortcomings of cooling is slow, temperature fall time is long in the reactor for heating conduction oil using electrical bar, especially to water
Thermal synthesis method is prepared for titanium dioxide fine particles, if place is likely to trigger side reaction, direct shadow in high temperature environments material for a long time
The titanium dioxide fine particles physicochemical property finally prepared is rung, or even influences whether the application effect of titanium dioxide fine particles.Therefore, solving
Reactor fast cooling problem is one of urgent need to solve the problem in industry.
Utility model content
To solve the above problems, the utility model provides a kind of fast prompt drop of Hydrothermal Synthesiss titanium dioxide nano material reactor
Warm device, the device is long in the presence of the slow, temperature fall time that cools except the reactor for solving existing use electrical bar heating conduction oil
The problems such as outside, while it is of a relatively high to solve energy consumption, the problems such as under low production efficiency.
The technical solution adopted in the utility model is as follows：
A kind of Hydrothermal Synthesiss titanium dioxide nano material reactor fast cooling device, including set on reactor outer wall
Chuck, reacting kettle jacketing top connection thermal oil vent road and conduction oil in-line, bottom connection conduction oil outlet line；
Cooling water coil inside reactor and the compressed air line being connected with cooling water coil；
Conduction oil basin with heat insulation function；
And conduction oil feeding device；
Reacting kettle jacketing, conduction oil basin and conduction oil feeding device are in turn connected to form circulation loop.
Specifically, conduction oil feeding device is Heat-transfer Oil Pump.
Lead to specifically, reacting kettle jacketing is connected to conduction oil basin, conduction oil basin by reacting kettle jacketing outlet line
Cross Heat-transfer Oil Pump in-line to be connected with Heat-transfer Oil Pump, Heat-transfer Oil Pump adds pipeline by conduction oil and is connected to reacting kettle jacketing.
Specifically, cooling water coil connection cooling water inlet pipeline and coolant outlet pipeline, in coolant outlet pipeline
Top set goes out compressed air line；
It is preferred that, the cooling water coil is spiral shape.
It is preferred that, the cooling water coil is made up of stainless steel pipeline of the nominal diameter in the range of DN25 to DN40.
It is preferred that, the disk footpath of the cooling water coil is less than reactor internal diameter, simultaneously greater than agitating paddle maximum outside diameter, is stirring
Mix operating of the normal stirring state lower coil pipe of oar on agitating paddle and do not produce influence.
It is preferred that, the cooling water coil import, outlet are arranged on same two different flange ports of kettle cover, during operation
Preferably, coil pipe will not produce vibration to stability as independent entirety in the case of cooling water is passed through.
It is preferred that, the volume of conduction oil basin is more than four times of the chuck volume.And the conduction oil basin is carried
Heat-insulation layer.
It is preferred that, in the top cover of reactor, temperature measuring equipment is set.
Specifically, proximal response kettle end is set in reacting kettle jacketing outlet line between reacting kettle jacketing and conduction oil basin
There is reacting kettle jacketing conduction oil delivery valve, nearly conduction oil on the Heat-transfer Oil Pump in-line between conduction oil basin and Heat-transfer Oil Pump
Basin end is provided with conduction oil basin delivery valve, is set on the reacting kettle jacketing in-line between Heat-transfer Oil Pump and reacting kettle jacketing
It is equipped with Heat-transfer Oil Pump delivery valve and reacting kettle jacketing inlet valve；Reacting kettle jacketing passes through reacting kettle jacketing atmospheric valve coupled reaction kettle
Chuck blowdown piping；Conduction oil basin is additionally provided with conduction oil basin atmospheric valve.
The workflow of the reactor fast cooling device of this Hydrothermal Synthesiss titanic oxide material is as follows：
After material in reactor reaction terminates, electrically heated rod power supply is closed, coolant outlet pipeline, cooling water inlet is opened
Pipeline is passed through cooling water to reactor inner coil pipe；Reacting kettle jacketing conduction oil atmospheric valve is opened, reacting kettle jacketing delivery valve will be anti-
Kettle chuck conduction oil is answered to be put into by reacting kettle jacketing outlet line in conduction oil basin.When material in reactor is cooled to technique
After defined temperature, reactor material emptying valve is opened, material in reactor is released.Compressed air valve is opened, by coil pipe
Cooling water is extruded.
When next time feeds intake, feed intake and finish, open reacting kettle jacketing inlet valve, Heat-transfer Oil Pump delivery valve, conduction oil basin goes out
Fuel tap, closes reacting kettle jacketing delivery valve, opens Heat-transfer Oil Pump, conduction oil is squeezed into reacting kettle jacketing out of conduction oil basin
It is interior.The technological requirement for preparing titanium dioxide fine particles according to hydrothermal synthesis method is opened electrically heated rod power supply and operated.
It should be noted that：Reacting kettle jacketing thermal oil vent road, reacting kettle jacketing atmospheric valve is in normal operating condition
Under be constantly in opening.
A kind of Hydrothermal Synthesiss titanium dioxide nano material reactor fast cooling device that the utility model is provided, it is and existing
Method is compared, and its advantage is：
1st, after reaction terminates, high temperature heat conductive oil is released rapidly, and cooling water is passed through into cooling water coil, so, instead
Answer material in kettle to be cooled to the temperature of process stipulation rapidly, reduce side reaction, it is ensured that the matter of the titanium dioxide fine particles of preparation
Amount and subsequent applications effect；
2nd, conduction oil in reacting kettle jacketing is put into the basin with insulation, after material in reactor is released, by heat conduction
Oil is squeezed into reacting kettle jacketing again, and conduction oil temperature drop seldom, thus takes full advantage of heat, energy consumption is low, and energy is damaged
Lose few；
3rd, cooling water coil connection compressed air line, when reactor needs heating, with compressed air by coil pipe
Water is blown out, and further reduces heat energy loss.
4th, 2.5 hours, separate unit are at least reduced because reactor temperature fall time ratio carries out cooling with pump by heat exchanger
Production efficiency of equipment is improved.
Brief description of the drawings
Fig. 1 is structural representation of the present utility model.
Wherein 1- reacting kettle jacketings；2- conduction oil basins, 3- Heat-transfer Oil Pumps, 4- cooling water coils；E1- electrically heated rods；P1-
Reacting kettle jacketing blowdown piping, P2- reacting kettle jacketing in-lines, P3- reacting kettle jacketing outlet line, P4- Heat-transfer Oil Pumps are entered
Oil pipe line, P5- compressed air lines；V1- reacting kettle jacketing conduction oil atmospheric valves, V2- reacting kettle jacketing inlet valves, V3- coolings
Water out valve, V4- cooling sea water inlet valves, V5- compressed air valves, V6- reacting kettle jacketing delivery valves, V7- discharging valve of reaction kettle,
V8- conduction oil basin atmospheric valves, V9- conduction oil basin delivery valves, V10- Heat-transfer Oil Pump delivery valves.
Fig. 2 is the structural representation of comparative example.
Wherein 1- reacting kettle jacketings；3- Heat-transfer Oil Pumps；5- coolers；E1- electrically heated rods；V6- reacting kettle jacketing delivery valves；
V10- Heat-transfer Oil Pump delivery valves.
Embodiment
The utility model is elaborated below in conjunction with the accompanying drawings：
As shown in Figure 1, a kind of reactor fast cooling device of Hydrothermal Synthesiss titanium dioxide nano material, including reaction
The chuck 1 set on kettle outer wall, the top coupled reaction kettle chuck blowdown piping P1 of reacting kettle jacketing 1 and reacting kettle jacketing oil inlet pipe
Road P2, bottom coupled reaction kettle chuck outlet line P3；Cooling water coil 4 inside reactor and connect with cooling water coil
The compressed air line P5 connect；Conduction oil basin 2 with heat insulation function；And Heat-transfer Oil Pump 3；Reacting kettle jacketing 1 is by anti-
Answer kettle chuck outlet line P3 to be connected to conduction oil basin 2, conduction oil basin 2 and pass through Heat-transfer Oil Pump in-line P4 and conduction oil
Pump 3 is connected, and Heat-transfer Oil Pump 3 is connected to reacting kettle jacketing 1 by reacting kettle jacketing in-line P2.Reacting kettle jacketing 1, conduction oil
Basin 2, the formation circulation loop of Heat-transfer Oil Pump 3.
Cooling water coil 4 connects cooling water inlet pipeline and coolant outlet pipeline, in coolant outlet pipeline top set
Go out compressed air line P5；
Cooling water coil 4 is processed in the shape of a spiral by stainless steel pipeline, and internal diameter is less than reactor internal diameter more than stirring
Oar maximum outside diameter；The disk footpath of the cooling water coil is less than reactor internal diameter, simultaneously greater than agitating paddle maximum outside diameter.
Cooling water coil import, outlet are arranged on same two different flange ports of kettle cover.
The volume of conduction oil basin 2 is more than four times of the volume of reacting kettle jacketing 1.And the band of conduction oil basin 2
There is heat-insulation layer.
In the top cover of reactor, temperature measuring equipment is set.
Proximal response kettle end is provided with reacting kettle jacketing outlet line P3 between reacting kettle jacketing 1 and conduction oil basin 2
Closely led on reacting kettle jacketing conduction oil delivery valve V6, the Heat-transfer Oil Pump in-line P4 between conduction oil basin 2 and Heat-transfer Oil Pump 3
The end of deep fat basin 2 is provided with conduction oil basin delivery valve V9, and the reacting kettle jacketing between Heat-transfer Oil Pump 3 and reacting kettle jacketing 1 enters
Heat-transfer Oil Pump delivery valve V10 and reacting kettle jacketing inlet valve V2 are provided with oily P2 pipelines；Reacting kettle jacketing 1 is pressed from both sides by reactor
Cover atmospheric valve V1 coupled reaction kettle chuck blowdown pipings P1；Conduction oil basin 2 is additionally provided with conduction oil basin atmospheric valve V8.
Reacting kettle jacketing blowdown piping P1, reacting kettle jacketing atmospheric valve V1 is constantly in unlatching shape in normal operation condition
State.
Material in reactor reaction is finished, now 161 DEG C of material in reactor temperature, and 185 DEG C of heat conduction oil temperature closes electricity
Heating rod E1 power supplys, open cooling sea water outlet valve V3, cooling sea water inlet valve V4, cooling water coil 4 is passed through cooling into reactor
Water；Reacting kettle jacketing conduction oil atmospheric valve V1, reacting kettle jacketing delivery valve V6 are opened, reacting kettle jacketing conduction oil is passed through into reaction
Kettle chuck outlet line P3 is put into conduction oil basin 2.It is passed through 1 hour material in reactor temperature of cooling water and is down to 36 DEG C, leads
Hot oil temperature is down to 37 DEG C, opens discharging valve of reaction kettle V7, material in reactor is released.Compressed air valve V5 is opened, will be cold
But the hydraulic pressure in water coil goes out.
When next time feeds intake, feed intake and finish, open reacting kettle jacketing inlet valve V2, Heat-transfer Oil Pump delivery valve V10, heat conduction oil measure
Tank delivery valve V9, closes reacting kettle jacketing delivery valve V6, opens Heat-transfer Oil Pump 3, conduction oil is squeezed into instead out of conduction oil basin 2
Answer in kettle chuck 1.The technological requirement for preparing titanium dioxide fine particles according to hydrothermal synthesis method is opened electrically heated rod E1 power supplys and grasped
Make.
Material in reactor is post-processed according to the process of process stipulation, obtained final titanium dioxide fine particles are entered
Row analysis.One is observation X ray diffracting spectrum, and obtained titanium dioxide fine particles diffraction maximum is sharpened, the intensity enhancing at peak, crystal grain hair
Educate completely；Two be observation surface sweeping Electronic Speculum collection of illustrative plates, and obtained titanium dioxide fine particles size distribution is uniform, and crystallization degree is more complete, shape
Looks rule.
Comparative example：
As shown in Figure 2 the reactor with chuck, reactor folder are included for representative electric-heating heat-conductive oil heat sink
Set 1, Heat-transfer Oil Pump 3, cooler 5 are sequentially connected, and electrical bar E1 is installed in chuck, and cooler 5 connects cooling water outlet and inlet valve,
Reacting kettle jacketing 1 sets reacting kettle jacketing delivery valve V6.Using such reactor, finished in material in reactor reaction, this
When 160 DEG C of material in reactor temperature, 186 DEG C of heat conduction oil temperature opens cooler cooling water outlet and inlet valve, opens reactor
Chuck delivery valve V6, opens Heat-transfer Oil Pump delivery valve V10, starts conduction oil in Heat-transfer Oil Pump 3, chuck and starts the cycle over cooling, pump
Circulation 3.5 hours, material in reactor temperature is down to 35 DEG C, and heat conduction oil temperature is down to 36 DEG C, and material in reactor is released.
Material in reactor is post-processed according to the process of process stipulation, obtained final titanium dioxide fine particles are entered
Row analysis.One is observation X ray diffracting spectrum, and obtained titanium dioxide fine particles diffraction maximum peak width is wider, and peak intensity is also weaker；Two are
Surface sweeping Electronic Speculum collection of illustrative plates is observed, obtained titanium dioxide fine particles size distribution is uneven, and particle is larger, in irregular shape.
The interpretation of result of the final product titanium dioxide fine particles formation obtained using device in embodiment and comparative example is as follows：
The growth of titanium dioxide actually belongs to " dissolution-crystallization " process, and hydrothermal temperature affects the dissolving of titanium dioxide, also contributed to
The formation of titanium dioxide crystal, hydrothermal temperature decides the degree of supersaturation of activation energy of crystallization, the concentration of solute and solution；Hydro-thermal temperature
Degree is moderate, and crystal growth is fast, crystal grain is big, crystal development is complete.After reaction reaches to a certain degree, reaction mass temperature fall time
Length will have a direct impact to product.Temperature fall time is long, there is agglomeration, and particle diameter distribution is uneven, and part particle diameter is smaller,
Spherical in shape, obtained titanium dioxide fine particles have more irregular particle shape crystal；Temperature fall time is short, and the crystallite of aggregation is molten
The big titanium dioxide nanoparticle of synthesis, degree of supersaturation in the solution is also less and less, and crystalline rate is also gradually decreased, finally
System reaches " dissolution-crystallization poised state ", and temperature fall time is shorter, and grain diameter is more homogeneous.
Although above-mentioned the embodiment of the present invention is described with reference to accompanying drawing, not the utility model is protected
The limitation of scope is protected, one of ordinary skill in the art should be understood that on the basis of technical scheme, people in the art
Member need not pay the various modifications that creative work can make or deform still within protection domain of the present utility model.
Claims (10)
1. a kind of reactor fast cooling device of Hydrothermal Synthesiss titanium dioxide nano material, it is characterised in that including reactor
The chuck set on outer wall；
Cooling water coil inside reactor and the compressed air line being connected with cooling water coil；
Conduction oil basin with heat insulation function；
And conduction oil feeding device；
Chuck, conduction oil basin, conduction oil feeding device are in turn connected to form circulation loop.
2. reactor fast cooling device according to claim 1, it is characterised in that the reacting kettle jacketing top connection
Thermal oil vent road and conduction oil in-line, bottom connection conduction oil outlet line.
3. reactor fast cooling device according to claim 1, it is characterised in that the cooling water coil connection cooling
Water inlet pipeline and coolant outlet pipeline, in coolant outlet pipeline, top set goes out compressed air line.
4. reactor fast cooling device according to claim 1, it is characterised in that the cooling water coil is spiral
Shape.
5. reactor fast cooling device according to claim 1, it is characterised in that the cooling water coil is straight by nominal
Stainless steel pipeline of the footpath in the range of DN25 to DN40 is made.
6. reactor fast cooling device according to claim 1, it is characterised in that the disk footpath of the cooling water coil is small
In reactor internal diameter, simultaneously greater than agitating paddle maximum outside diameter.
7. reactor fast cooling device according to claim 1, it is characterised in that the cooling water coil import, go out
Mouth is arranged on same two different flange ports of kettle cover.
8. reactor fast cooling device according to claim 1, it is characterised in that the volume of conduction oil basin is described
More than four times of chuck volume, and the conduction oil basin carries heat-insulation layer.
9. reactor fast cooling device according to claim 1, it is characterised in that thermometric is set in the top cover of reactor
Device.
10. reactor fast cooling device according to claim 1, it is characterised in that the reacting kettle jacketing and heat conduction
Proximal response kettle end is provided with reacting kettle jacketing conduction oil delivery valve, conduction oil in reacting kettle jacketing outlet line between oil measure tank
Nearly conduction oil basin end is provided with conduction oil basin delivery valve on Heat-transfer Oil Pump in-line between basin and Heat-transfer Oil Pump, leads
Heat-transfer Oil Pump delivery valve and reacting kettle jacketing are provided with reacting kettle jacketing in-line between hot oil pump and reacting kettle jacketing
Inlet valve；Reacting kettle jacketing passes through reacting kettle jacketing atmospheric valve coupled reaction kettle chuck blowdown piping；Conduction oil basin is also set up
There is conduction oil basin atmospheric valve.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201720191605.2U CN206500147U (en) | 2017-03-01 | 2017-03-01 | A kind of reactor fast cooling device of Hydrothermal Synthesiss titanium dioxide nano material |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201720191605.2U CN206500147U (en) | 2017-03-01 | 2017-03-01 | A kind of reactor fast cooling device of Hydrothermal Synthesiss titanium dioxide nano material |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108149322A (en) * | 2018-01-30 | 2018-06-12 | 中国科学院福建物质结构研究所 | A kind of the synthesis tank arrangement and synthetic method of high deuterium DKDP crystal raw materials |
| CN111111575A (en) * | 2019-12-27 | 2020-05-08 | 北京英惠尔生物技术有限公司 | Method for improving efficiency of Vc ester reaction kettle and simple cold water supply system thereof |
| CN116212783A (en) * | 2022-12-29 | 2023-06-06 | 仁化县奥达胶合板有限公司 | Apparatus for producing of adhesive for composite plywood |
-
2017
- 2017-03-01 CN CN201720191605.2U patent/CN206500147U/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108149322A (en) * | 2018-01-30 | 2018-06-12 | 中国科学院福建物质结构研究所 | A kind of the synthesis tank arrangement and synthetic method of high deuterium DKDP crystal raw materials |
| CN108149322B (en) * | 2018-01-30 | 2023-09-08 | 中国科学院福建物质结构研究所 | Synthetic tank device and synthetic method of high deuterium DKDP crystal raw material |
| CN111111575A (en) * | 2019-12-27 | 2020-05-08 | 北京英惠尔生物技术有限公司 | Method for improving efficiency of Vc ester reaction kettle and simple cold water supply system thereof |
| CN116212783A (en) * | 2022-12-29 | 2023-06-06 | 仁化县奥达胶合板有限公司 | Apparatus for producing of adhesive for composite plywood |
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| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20170919 Termination date: 20180301 |
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| CF01 | Termination of patent right due to non-payment of annual fee |