CN107572580B - A kind of superfine tin indium oxide flour producing process - Google Patents
A kind of superfine tin indium oxide flour producing process Download PDFInfo
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Abstract
This patent discloses a kind of superfine tin indium oxide flour producing process, are related to oxide preparation field；Its oxidation unit used, including rack, chlorine storage tank, the reaction tube being fixed in rack and in reaction tube and can be moved towards along reaction tube sliding extruding axis；It squeezes to be fixed in the middle part of axis and cooperates spacing block with reaction tube, the top of reaction tube is equipped with two groups of gas-guide tubes that can be connected to the first reaction chamber and the second reaction chamber, when spacing block slides into reaction tube end, spacing block by gas-guide tube wherein one end port block, the connection for the check valve for being connected with check valve in the middle part of gas-guide tube, and being connected on two groups of gas-guide tubes is contrary；The lower part of reaction tube is set there are two the blow-off valve that can be connected to respectively with the first reaction chamber and the second reaction chamber, and chlorine storage tank is equipped with air inlet pipe, and air inlet pipe is connected to gas-guide tube, and air inlet pipe is connected with shut-off valve.Using the structure tin indium oxide, when indium powder and glass putty is discharged, the chlorine of discharge is less, reduces the waste of chlorine.
Description
Technical field
The present invention relates to oxide preparation fields, and in particular to a kind of superfine tin indium oxide flour producing process.
Background technique
Indium tin oxide is the mixture of a kind of indium oxide and tin-oxide, can be prepared with excellent photoelectric properties member
Part such as has good translucency, the reflectivity of infrared ray, the attractability of ultraviolet light and the decaying to microelectronics wave
The transparent membrane of property.
Currently, the method for preparing In-Sn oxide powder is more, existing frequently-used mainly hydrothermal synthesis indium tin oxide
The method of powder.And after hydrothermal synthesis method is using precipitating reagent precipitating, it needs to wash by deionized water, filters, is aged, does
Dry, calcining and etc., it is very complicated；Ionized water washing process will cause the loss of small part useful component, cause centainly to lose.For
The consumption for reducing raw material, improves production technology.Its specifically: eliminate the washers of conventional hydrothermal synthetic method
Skill reduces the loss of indium tin oxide colloidal sol material to simplify process flow, improves process economics the quality control of running water
It is flat.
The step of improved processing technology, is as follows:
(1) it aoxidizes: indium grain and tin grain is each led into excessive chlorine, sufficiently generate indium trichloride and four chlorinations after reaction
Tin；
(2) water-soluble: the indium trichloride of generation and tin tetrachloride being dissolved in water respectively, make four that mass concentration is 30%
Tin chloride solution, the indium trichloride solution that mass concentration is 69%；
(3) it precipitates: taking 300-350 parts of tin tetrachloride solution of mass concentration 30%, 69% indium trichloride of mass concentration is molten
150-200 parts of liquid, it is configured to indium trichloride and tin tetrachloride mixed aqueous solution, is added after being sufficiently stirred 50-60 minutes excessive
Ammonium hydroxide stirs 50-60 minutes；
(4) it filters: the colloidal precipitation of solution and generation after stirring is separated by filtration；
(5) dry: to choose and filter resulting colloidal precipitation, colloidal precipitation is placed in the environment that temperature is 80-100 DEG C and is done
Dry 60 minutes, then 330-350 DEG C of drying 40 minutes is raised the temperature to, finally raise the temperature to 60 points of 500-550 DEG C of drying
Zhong Hou, drying process need to stir always, take out remaining solid；
(6) it crushes: the solid of acquirement being crushed, obtained powder is indium tin oxide.
Currently, above oxidation step is usually reacted in oxidation cylinder, indium powder and glass putty are respectively in different oxidations
Oxidation reaction is carried out in cylinder.Since chlorine is toxic gas, and need in oxidation reaction to be passed through excessive chlorine, thus chlorine without
Method is reacted completely；So the remaining chlorine in cylinder will first be aoxidized by, which needing, extracts out when indium powder and glass putty is discharged, then could arrange
Indium powder or glass putty out.But since oxidation cylinder product is larger, and after extracting the chlorine in oxidation cylinder out, it still can not make to reach in oxidation cylinder
To absolute vacuum state, so still having more chlorine discharge after opening oxidation cylinder；And can also it increase to aoxidizing cylinder and being vacuumized
Add energy consumption.
Summary of the invention
The purpose of the present invention is to provide the superfine tin indium oxide flour producing process that can reduce chlorine discharge.
In order to achieve the above objectives, base case of the invention is as follows:
Superfine tin indium oxide flour producing process aoxidizes indium powder and glass putty using a kind of oxidation unit；Oxidation unit packet
Including rack, chlorine storage tank, the reaction tube being fixed in rack, the reciprocal axis for passing through out of reaction tube and being connect with housing slide,
And the reciprocating air cylinder that the reciprocal axis of driving moves back and forth；It is fixed with the spacing block contacted with reaction tube inner wall in the middle part of reciprocal axis,
It is respectively indium oxidation unit and tin oxidation unit at left and right sides of spacing block, indium oxidation unit and tin oxidation unit include reaction
The reaction chamber of chamber, pressurization part, inlet valve and blow-off valve, indium oxidation unit and tin oxidation unit is separated by spacing block, and reaction tube
Top be equipped with two groups can by two reaction chambers be connected to gas-guide tubes, when spacing block is located at left end or right end, spacing block general
The port of gas-guide tube wherein one end blocks, and is connected with the first check valve in the middle part of gas-guide tube, and be connected on two groups of gas-guide tubes
The connection of first check valve is contrary；Pressurization part includes air storing cavity in the reaction tube, pressurizing chamber and is set to pressurizing chamber
Interior piston, air storing cavity and pressurizing chamber by being only capable of be connected to the second one-way valve of air storing cavity air inlet, pressurizing chamber pass through be only capable of to
The third check valve of pressurizing chamber air inlet is connected to outside, and the piston is fixed on reciprocal axis；Blow-off valve be equipped with can with react
The air inlet and discharge gate of chamber connection, air storing cavity are connected to by pipeline with air inlet；Chlorine storage tank is equipped with air inlet pipe, air inlet pipe
It is connected to gas-guide tube, and is connected with shut-off valve in air inlet pipe；
Oxidation step includes:
(1) it feeds: closing blow-off valve, keep reciprocal axis mobile, when spacing block slides into left end, open indium oxidation unit
Inlet valve fills indium powder into the reaction chamber of indium oxidation unit；When spacing block slides into right end, open tin oxidation unit into
Expect valve, fills glass putty into the reaction chamber of tin oxidation unit；After indium powder or glass putty is added, that is, close inlet valve；
(2) aerating: opening the shut-off valve in air inlet pipe, after the pressure in reaction chamber reaches 1-1.5MPa, closes cut-off
Valve；
(3) it aoxidizes: moving left and right reciprocal axis back and forth, and aoxidize 30-40min；
(4) discharge: discharge: when spacing block slides into left end, the blow-off valve of indium oxidation unit is opened, indium powder is discharged, is closed
Close the blow-off valve of indium oxidation unit；Spacing block is slid into right end, opens the blow-off valve of tin oxidation unit, glass putty is discharged, is closed
Close the blow-off valve of tin oxidation unit.
The principle of this programme superfine tin indium oxide flour producing process is:
In step (1) fill process, when spacing block is moved to left end, just it is added into the reaction chamber of indium oxidation unit
Indium powder；When spacing block is moved to right end, glass putty is added in the reaction chamber of Cai Xiangxi oxidation unit.Indium oxidation unit and tin at this time
The space of the reaction chamber of oxidation unit is compressed into minimum, and is filled up reaction chamber by indium powder or glass putty；Then in step (4)
In discharging process, indium powder or glass putty occupy the most space of reaction chamber, and spacing block blocks the Single port of gas-guide tube at this time,
The amount for the chlorine that then reaction chamber of indium oxidation unit and tin oxidation unit is not communicated at this time, therefore is discharged together with indium powder or glass putty
It is less.
In step (2) fueling process, the shut-off valve in air inlet pipe is opened, high pressure chlorine is added into reaction tube, and anti-
After answering intracavitary pressure to reach 1-1.5MPa, shut-off valve is turned off, so as to make the chlorine in reaction chamber reach excessive state, with
Guarantee that indium powder, glass putty can sufficiently be reacted with chlorine.
During step (3) is reciprocal, reciprocating air cylinder will drive reciprocal axis to move back and forth in reaction tube；When spacing block to
When reaction tube left end is mobile, the space positioned at the reaction chamber of spacing block left end reduces, and be located at the reaction chamber of spacing block right end
Space increases, therefore the chlorine on the left of spacing block in reaction chamber will reaction chamber flows to the right by gas-guide tube.And work as spacing block
When being moved to left end, the ratio of the volume of the volume and reaction chamber of the indium powder in reaction chamber is maximum.When spacing block to the right
When reaction chamber is mobile, the space of left side reaction chamber is gradually increased, and the chlorine in the reaction chamber of right side passes through gas-guide tube side reaction to the left
Chamber flowing, to enhance the gas flowing in the reaction chamber of left side, then under the blowing of air-flow, indium powder gradually fluffs scattered.Back and forth
During axis moves back and forth, the ratio cyclically-varying of indium powder and glass putty and reaction chamber, to have vibration to indium powder and glass putty
The effect of swinging, while under air blast effect of the air-flow to powder can make powder in state of waving, thus in the process to indium powder and
Glass putty has stirring action.
After indium powder, glass putty and chlorine sufficiently react, when spacing block is moved to reaction tube left end, blow-off valve is opened, then is stored up
Air cavity is connected to reaction chamber, while discharge gate is connected to outside.During reciprocal axis moves back and forth, piston can also pressurize
Intracavitary reciprocating movement, when the space in piston compression pressurizing chamber, air enters air storing cavity by second one-way valve；Work as pressurizing chamber
When interior space increases, outside air will enter in pressurizing chamber by third check valve, so as to so that pressure in air storing cavity
It is gradually increased.Therefore after opening blow-off valve, the high pressure gas in air storing cavity enters in reaction chamber, to make indium powder or glass putty pine
It dissipates, and it is blown out from discharge gate.
The beneficial effect that this programme generates is:
(1) chlorine in reaction chamber during spacing block is moved back and forth relative to reaction tube, at left and right sides of spacing block
Gas will form the air-flow of alternately flowing by conduction pipe, so that indium powder and glass putty form certain stream under the action of air-flow
Dynamic state, to sufficiently be contacted with chlorine conducive to glass putty and indium powder.
(2) indium powder is being discharged and when glass putty, the space in reaction chamber is compressed to minimum, and at this time spacing block by air guide
The port of pipe blocks, therefore when indium powder and glass putty is discharged, the chlorine of discharge is less, is easily processed, and reduces the waste of chlorine.
In addition, when indium powder and glass putty is discharged, it is not necessary to extract the chlorine in reaction tube out, so as to improve efficiency.
Preferred embodiment one: advanced optimizing as to base case, and the feed step and discharge step carry out simultaneously,
After indium powder is discharged, i.e., indium powder is added into the reaction chamber of indium oxidation unit；After glass putty is discharged, i.e., the reaction chamber to tin oxidation unit
Interior addition glass putty.Due to indium tin oxidation reaction after, a certain amount of chlorine is also remained in reaction chamber；Therefore it feeds and arranges
Expect while carrying out, then a chlorine is only discharged in charging and discharge；And the reaction chamber that indium powder or glass putty occupy when due to discharge
Space it is larger, therefore can make discharge chlorine amount it is minimum.
Preferred embodiment two: advanced optimizing as to base case, and the frequency that the reciprocal axis moves back and forth is 20-30
Secondary/min is conducive to indium tin and comes into full contact with chlorine so that the flow velocity of the gas of reaction chamber is enough that indium powder or glass putty is driven to flow；
The frequency that reciprocal axis moves back and forth is excessive, then gas flow rate is too fast, easily make indium powder enter the reaction chamber for accommodating glass putty or glass putty into
Enter to accommodate the reaction chamber of indium powder.
Preferred embodiment three: advanced optimizing as to base case, is equipped with and is fixed on the rack below the reaction tube
Dissolving tank, the discharge gate of blow-off valve is connected with the drainage conduit protruded into dissolving tank.After indium powder and glass putty and chlorine reaction, under
One step is water-soluble.Therefore water is added in dissolving tank, and indium powder and glass putty is directly discharged into dissolving tank, then can be directly entered
Water-soluble step；In addition, a small amount of chlorine can be discharged, therefore by stretching drainage conduit due to while indium powder and glass putty is discharged
Enter dissolving tank, chlorine leach can be made in water.
Preferred embodiment four: advanced optimizing as to base case, is fixed in the rack and is located at reciprocal axis
The pressure switch at both ends, the blow-off valve are solenoid valve, and adjacent blow-off valve is electrically connected with pressure switch by conducting wire, and conducting wire
It is equipped with electric brake.In preferred embodiment four, when needing to be discharged indium powder and glass putty, it is closed electric brake, then when one end of reciprocal axis is squeezed
When pressure pressure switchs, pressure switch so that blow-off valve is opened, then can arrange indium powder or glass putty to blow-off valve input electrical signal
Out.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of oxidation unit in the embodiment of the present invention.
Specific embodiment
Below by specific embodiment, the present invention is described in further detail:
Appended drawing reference in Figure of description includes: reaction tube 10, diversion pipe 11, the first check valve 12, place-limited edge 13,
One reaction chamber 14, the second reaction chamber 15, blow-off valve 16, drainage conduit 17, reciprocal axis 20, spacing block 21, piston 22, air storing cavity 23,
Pressurizing chamber 24, second one-way valve 25, third check valve 26, dissolving tank 30, rack 40, pressure switch 41.
The superfine tin indium oxide flour producing process of the present embodiment aoxidizes indium powder and glass putty using oxidation unit.Such as figure
Shown in 1, oxidation unit includes rack 40, chlorine storage tank, reaction tube 10, reciprocal axis 20, dissolving tank 30 and reciprocating air cylinder.Reaction tube
10 are cylindric and are fixed in rack 40；Reciprocal axis 20 is passed through out of reaction tube 10, and reciprocal axis 20 is slidably connected at rack
On 40, reciprocating air cylinder is connect with reciprocal axis 20, so that reciprocating air cylinder can drive reciprocal axis 20 to transport along the axial reciprocating of reaction tube 10
It is dynamic.The middle part of reciprocal axis 20 is fixed with spacing block 21, is respectively indium oxidation unit and tin oxidation unit at left and right sides of spacing block 21,
Indium oxidation unit and tin oxidation unit include reaction chamber, pressurization part, inlet valve and blow-off valve 16, and indium oxidation unit and tin aoxidize
The reaction chamber of unit is respectively the first reaction chamber 14 and the second reaction chamber 15；First reaction chamber 14 and the second reaction chamber 15 are by separating
Block 21 separates.The top of reaction tube 10 is equipped with two groups of gas-guide tubes that can be connected to the first reaction chamber 14 with the second reaction chamber 15, often
Group gas-guide tube is equipped with four altogether, and two groups of gas-guide tubes are spaced setting one by one, and gas-guide tube is uniformly distributed along the upper half of reaction tube 10.
The inner wall at 10 both ends of reaction tube be equipped with place-limited edge 13, place-limited edge 13 can the both ends respectively with spacing block 21 offset, thus to point
Spacer block 21 is limited.When the place-limited edge 13 in left side and spacing block 21 offset, spacing block 21 seals the port of gas-guide tube left end
It is stifled；When the place-limited edge 13 on right side and spacing block 21 offset, spacing block 21 blocks the port of gas-guide tube right end.In gas-guide tube
Portion is connected with the first check valve 12, and the connection for being connected to the first check valve 12 on two groups of gas-guide tubes is contrary；Divide to work as
Spacer block 21 is in reaction tube 10 when one Slideslip of direction, and only one group of gas-guide tube connects the first reaction chamber 14 and the second reaction chamber 15
It is logical.In addition, the height of gas-guide tube is equal to the diameter of reaction tube 10, then in a stroke of reciprocal axis 20 operation, indium powder or tin
The limited height that powder rises in gas-guide tube, to can avoid indium powder and glass putty mixing.
Pressurization part includes air storing cavity 23, pressurizing chamber 24 in reaction tube 10, and the piston in pressurizing chamber 24
22；Air storing cavity 23 is with pressurizing chamber 24 by being only capable of being connected to the second one-way valve 25 of 23 air inlet of air storing cavity, and pressurizing chamber 24 is by only
It can be connected to the third check valve 26 of 24 air inlet of pressurizing chamber with outside, and piston 22 is fixed on reciprocal axis 20.On blow-off valve 16
Equipped with the air inlet and discharge gate that can be connected to reaction chamber, air storing cavity 23 is connected to by pipeline with air inlet；When blow-off valve 16 is beaten
It opens, feed inlet and discharge gate open simultaneously；And blow-off valve 16 is closed, feed inlet and discharge gate simultaneously close off.Dissolving tank 30 is fixed
In rack 40 and it is located at below reaction tube 10, the discharge gate of blow-off valve 16 is connected with the drainage conduit 17 protruded into dissolving tank 30.
So as to dissolve in water that indium powder or glass putty are directly discharged into dissolving tank 30, and chlorine is avoided to be discharged into air.
Chlorine storage tank is equipped with air inlet pipe, and air inlet pipe is connected to gas-guide tube, and air inlet pipe is connected with shut-off valve.In rack 40
Equipped with the pressure switch 41 for being located at reciprocal 20 left and right ends of axis, blow-off valve 16 uses solenoid valve, and adjacent blow-off valve 16
It is connect with pressure switch 41 by conducting wire, conducting wire is equipped with electric brake.When closure electric brake, pressure switch 41 and blow-off valve 16 form one
A closed circuit, i.e. pressure switch 41 are pressurized can be to 16 input electrical signal of blow-off valve, and opens blow-off valve 16.
Oxidation step includes:
(1) it feeds: closing blow-off valve 16, keep reciprocal axis 20 mobile, when spacing block 21 slides into left end, open indium oxidation
The inlet valve of unit fills indium powder into the first reaction chamber 14；When spacing block 21 slides into right end, tin oxidation unit is opened
Inlet valve fills glass putty into the second reaction chamber 15；After indium powder or glass putty is added, that is, close inlet valve.
(2) aerating: keep spacing block 21 mobile, the port of the unclosed gas-guide tube of spacing block 21, thus 14 He of the first reaction chamber
When second reaction chamber 15 is connected to, the shut-off valve in air inlet pipe is opened, after the pressure in reaction chamber reaches 1-1.5MPa, closes and cuts
Only valve.In the case where the first reaction chamber 14 is connected to the second reaction chamber 15, it is passed through chlorine into reaction tube 10, chlorine can be made
It enters in the gap between indium powder or glass putty, to guarantee that chlorine reaches excessive standard.
(3) it aoxidizes: moving left and right reciprocal axis 20 back and forth, and aoxidize 30-40min, the frequency that reciprocal axis 20 moves back and forth
For 25 times/min.
(4) discharge: when spacing block 21 slides into left end, by being closed corresponding electric brake, the row of indium oxidation unit is opened
Expect valve 16, indium powder is discharged, turns off the blow-off valve 16 of indium oxidation unit；Another electric brake is reclosed, spacing block 21 is slid into most
Right end opens the blow-off valve 16 of tin oxidation unit, and glass putty is discharged, turns off the blow-off valve 16 of tin oxidation unit.In addition, step
(1) charging and step (2) discharge carry out simultaneously, after indium powder is discharged, i.e., indium powder are added into the reaction chamber of indium oxidation unit；Discharge
After glass putty, i.e., glass putty is added into the reaction chamber of tin oxidation unit.
In step (1) fill process, when spacing block 21 is moved to left end, just add into the reaction chamber of indium oxidation unit
Enter indium powder；When spacing block 21 is moved to right end, glass putty is added in the reaction chamber of Cai Xiangxi oxidation unit.First reaction chamber at this time
14 and second the space of reaction chamber 15 be compressed into minimum, and reaction chamber is filled up by indium powder or glass putty；It is arranged in step (4)
During material, indium powder or glass putty occupy the most space of reaction chamber, and spacing block 21 blocks the Single port of gas-guide tube at this time,
Then the first reaction chamber 14 and the second reaction chamber 15 are not communicated at this time, thus the amount for the chlorine being discharged together with indium powder or glass putty compared with
It is few.In step (4) discharging process, by be closed electric brake, then reciprocal axis 20 extruding on the left of pressure switch 41 when, left side
Blow-off valve 16 is opened, and indium powder is discharged.When reciprocal axis 20 squeezes the pressure switch 41 on right side, the blow-off valve 16 on right side is opened, will
The discharge of indium powder.Drainage conduit 17 will dissolve in water that indium powder and glass putty are directly discharged into dissolving tank 30, and pass through drainage conduit 17
A small amount of chlorine of discharge is dissolved in water.
In step (2) fueling process, the shut-off valve in air inlet pipe is opened, high pressure chlorine is added into reaction tube 10, and
After pressure in reaction chamber reaches 1-1.5MPa, shut-off valve is turned off, so as to make the chlorine in reaction chamber reach excessive state,
It can sufficiently be reacted with chlorine with guaranteeing indium powder, glass putty.
During step (3) is reciprocal, reciprocating air cylinder will drive reciprocal axis 20 to move back and forth in reaction tube 10；Work as separation
When block 21 is mobile to 10 left end of reaction tube, the space of the first reaction chamber 14 reduces, and the space of the second reaction chamber 15 increases, therefore
Chlorine in first reaction chamber 14 will be flowed by gas-guide tube to the second reaction chamber 15.And work as the place-limited edge of spacing block 21 and left side
When 13 contact, the ratio of the volume of the volume and reaction chamber of the indium powder in reaction chamber is maximum.When the reaction of spacing block 21 to the right
When chamber is mobile, the space of left side reaction chamber is gradually increased, and the chlorine in the second reaction chamber 15 passes through gas-guide tube to the first reaction chamber
14 flowings, to enhance the gas flowing in the first reaction chamber 14, then under the blowing of air-flow, indium powder gradually fluffs scattered.It is past
During multiple axis 20 moves back and forth, the ratio cyclically-varying of indium powder and glass putty and reaction chamber, to have to indium powder and glass putty
There is oscillation action, while under air blast effect of the air-flow to powder, powder can be made in state of waving, therefore in the process to indium
Powder and glass putty have stirring action.
After indium powder, glass putty and chlorine sufficiently react, when spacing block 21 is moved to 10 left end of reaction tube, blow-off valve is opened
16, then air storing cavity 23 is connected to reaction chamber, while discharge gate is connected to outside.It is living during reciprocal axis 20 moves back and forth
Plug 22 can also move back and forth in pressurizing chamber 24, and when piston 22 compresses the space in pressurizing chamber 24, air is unidirectional by second
Valve 25 enters air storing cavity 23；When space when piston 22 is mobile in pressurizing chamber 24 increases, outside air will be unidirectional by third
Valve 26 enters in pressurizing chamber 24, so as to so that the pressure in air storing cavity 23 is gradually increased.Therefore after opening blow-off valve 16, gas storage
High pressure gas in chamber 23 enters in reaction chamber, to keep indium powder or glass putty loose, and it is blown out from discharge gate.
What has been described above is only an embodiment of the present invention, and the common sense such as well known specific structure and characteristic are not made herein in scheme
Excessive description.It, without departing from the structure of the invention, can be with it should be pointed out that for those skilled in the art
Several modifications and improvements are made, these also should be considered as protection scope of the present invention, these all will not influence what the present invention was implemented
Effect and patent practicability.The scope of protection required by this application should be based on the content of the claims, in specification
The records such as specific embodiment can be used for explaining the content of claim.
Claims (5)
1. a kind of superfine tin indium oxide flour producing process, which is characterized in that carried out using a kind of oxidation unit to indium powder and glass putty
Oxidation；Oxidation unit includes rack, chlorine storage tank, the reaction tube being fixed in rack, passes through out of reaction tube and slide with rack
The reciprocal axis of dynamic connection, and the reciprocating air cylinder that the reciprocal axis of driving moves back and forth；Be fixed in the middle part of reciprocal axis in reaction tube
The spacing block of wall contact, the spacing block left and right sides are respectively indium oxidation unit and tin oxidation unit, and indium oxidation unit and tin aoxidize
Unit includes reaction chamber, pressurization part, inlet valve and blow-off valve, and the reaction chamber of indium oxidation unit and tin oxidation unit is by spacing block
It separates, and the top of reaction tube is equipped with two groups of gas-guide tubes that can be connected to two reaction chambers, spacing block is located at left end or most right
When end, spacing block blocks the port of gas-guide tube wherein one end, is connected with the first check valve in the middle part of gas-guide tube, and be connected to two
The connection of the first check valve on group gas-guide tube is contrary；Pressurization part include air storing cavity in the reaction tube, pressurizing chamber with
And the piston in pressurizing chamber, air storing cavity and pressurizing chamber are pressurizeed by being only capable of being connected to the second one-way valve of air storing cavity air inlet
Chamber, which passes through, to be only capable of being connected to the third check valve of pressurizing chamber air inlet with outside, and the piston is fixed on reciprocal axis；On blow-off valve
Equipped with the air inlet and discharge gate that can be connected to reaction chamber, air storing cavity is connected to by pipeline with air inlet；Chlorine storage tank is equipped with
Air inlet pipe, air inlet pipe are connected to gas-guide tube, and shut-off valve is connected in air inlet pipe；
Oxidation step includes:
Charging: closing blow-off valve, keeps reciprocal axis mobile, when spacing block slides into left end, opens the inlet valve of indium oxidation unit,
Indium powder is filled into the reaction chamber of indium oxidation unit；When spacing block slides into right end, the inlet valve of tin oxidation unit is opened, to
Glass putty is filled in the reaction chamber of tin oxidation unit；After indium powder or glass putty is added, that is, close inlet valve；
Aerating: opening the shut-off valve in air inlet pipe, after the pressure in reaction chamber reaches 1-1.5MPa, closes shut-off valve；
Oxidation: it moves left and right reciprocal axis back and forth, and aoxidizes 30-40min；
Discharge: when spacing block slides into left end, the blow-off valve of indium oxidation unit is opened, indium powder is discharged, closes indium oxidation unit
Blow-off valve；Spacing block is slid into right end, opens the blow-off valve of tin oxidation unit, glass putty is discharged, closes tin oxidation unit
Blow-off valve.
2. superfine tin indium oxide flour producing process according to claim 1, which is characterized in that the feed step and discharge
Step carries out simultaneously, after indium powder is discharged, i.e., indium powder is added into the reaction chamber of indium oxidation unit；After glass putty is discharged, i.e., to tin oxygen
Change and glass putty is added in the reaction chamber of unit.
3. superfine tin indium oxide flour producing process according to claim 1, which is characterized in that the reciprocal axis moves back and forth
Frequency be 20-30 times/min.
4. superfine tin indium oxide flour producing process according to claim 1, which is characterized in that be equipped with below the reaction tube
The dissolving tank being fixed on the rack, the discharge gate of blow-off valve are connected with the drainage conduit protruded into dissolving tank.
5. superfine tin indium oxide flour producing process according to claim 1, which is characterized in that be fixed in the rack point
Not Wei Yu reciprocal axis both ends pressure switch, the blow-off valve is solenoid valve, and adjacent blow-off valve and pressure switch pass through conducting wire
Electrical connection, and conducting wire is equipped with electric brake.
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| JP3019551B2 (en) * | 1991-10-15 | 2000-03-13 | 三菱マテリアル株式会社 | Ultrafine low-resistance tin-doped indium oxide powder and its manufacturing method |
| JP3814841B2 (en) * | 1995-07-06 | 2006-08-30 | 住友化学株式会社 | Method for producing metal oxide powder |
| CN101367543B (en) * | 2008-09-17 | 2011-02-02 | 广东光华科技股份有限公司 | Preparation method for high purity stannous oxide |
| JP5514570B2 (en) * | 2010-02-08 | 2014-06-04 | Ｄｏｗａエレクトロニクス株式会社 | Method for producing tin-doped indium oxide powder and tin-doped indium oxide powder |
| CN105692691A (en) * | 2016-02-24 | 2016-06-22 | 云南锡业股份有限公司 | Preparation method of indium tin oxide |
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