CN115725859A - Titanium sponge fluidization reaction system and method - Google Patents

Titanium sponge fluidization reaction system and method Download PDF

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Publication number
CN115725859A
CN115725859A CN202211456012.6A CN202211456012A CN115725859A CN 115725859 A CN115725859 A CN 115725859A CN 202211456012 A CN202211456012 A CN 202211456012A CN 115725859 A CN115725859 A CN 115725859A
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sieve plate
plate
titanium sponge
reaction system
feed inlet
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CN202211456012.6A
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CN115725859B (en
Inventor
赵志强
李学志
高俊
李树宏
苏立杰
裴玉贞
赵应应
许佳鹏
赵淘淘
王帅
张迎迎
史朝朝
李向阳
徐建伟
任宇芬
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Henan Longbai Intelligent Equipment Manufacturing Co ltd
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Henan Longbai Intelligent Equipment Manufacturing Co ltd
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
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Abstract

The invention relates to a titanium sponge fluidization reaction system which comprises a reaction furnace, wherein the reaction furnace is a fluidized bed reaction furnace, the top of the reaction furnace is provided with an exhaust port, the bottom of the reaction furnace is provided with an air inlet, an upper sieve plate and a lower sieve plate are arranged in the reaction furnace, the side wall of the fluidized bed is provided with an upper feed inlet and a lower feed inlet, the upper feed inlet is positioned above the upper sieve plate, and the lower feed inlet is positioned between the upper sieve plate and the lower sieve plate. The invention adopts a double-deck sieve plate fluidized bed, the upper space of the lower sieve plate is used as the main fluidized reaction area, and a layer of upper sieve plate is arranged above the upper space of the lower sieve plate.

Description

Titanium sponge fluidization reaction system and method
Technical Field
The invention relates to a titanium sponge fluidization reaction system and a method, and belongs to the technical field of titanium sponge production.
Background
Titanium tetrachloride is obtained after chlorination reaction of the high titanium slag, petroleum coke and chlorine, and titanium sponge can be obtained after reduction of the titanium tetrachloride. In the prior art, the preparation of titanium tetrachloride is generally carried out by boiling chlorination, which is carried out in a fluidized bed reactor. Because impurities such as calcium, magnesium and the like exist in the high titanium slag, liquid chloride is generated in the reaction furnace after chlorination reaction, is easy to be bonded with materials into a mass, blocks gas distribution holes of the sieve plate, and is inconvenient for slag discharge, most manufacturers adopt sieve plate-free fluidized beds at present. But the fluidized bed without the sieve plate has unstable fluidization state and great control difficulty due to uneven gas distribution. In addition, in the aspect of material granularity control, because the petroleum coke has low density and light weight relative to high titanium slag and is easy to float on the upper layer under the driving of air flow, the titanium slag and coke are not fully mixed, and the finer coke powder is easy to be taken away by the air flow, the granularity of the petroleum coke is generally controlled to be more than 1 mm. However, petroleum coke has a large particle size and a too small surface area, which limits the reaction rate.
Disclosure of Invention
Aiming at the problems, the invention provides a titanium sponge fluidization reaction system and a method, and the specific scheme is as follows:
the utility model provides a titanium sponge fluidization reaction system, includes the reacting furnace, and the reacting furnace is fluidized bed reacting furnace, and the reacting furnace top is equipped with the gas vent, and the bottom is equipped with the air inlet, is equipped with upper screen plate and lower screen plate in the reacting furnace, and the fluidized bed lateral wall is equipped with upper feed inlet and lower feed inlet, and upper feed inlet is located the upper screen plate top, and lower feed inlet is located between upper screen plate and the lower screen plate.
Furthermore, the upper sieve plate is provided with an overflow pipe, and the height of the overflow pipe is not more than 10cm.
Furthermore, the distance between the upper sieve plate and the lower sieve plate is not less than 1/2 of the height of the furnace body. The space between the upper and lower sieve plates is used as the main reaction area and the height of the space is equal to that of the upper and lower sieve plates
Further, the lower sieve plate comprises a fixed plate and a movable plate which are vertically superposed, the fixed plate is positioned on the upper layer, the movable plate is positioned on the lower layer, the plate surfaces of the fixed plate and the movable plate are both formed by V-shaped grooves, one side groove wall of each V-shaped groove is provided with a gas distribution hole, the gas distribution hole is positioned in the middle or upper part of the groove wall, the other side groove wall is provided with a slag discharge hole, and the height of the slag discharge hole is consistent with that of the groove wall; the movable plate is provided with a vibration mechanism.
Furthermore, the side wall of the reaction furnace is provided with an airtight chamber, the edge of the movable plate is provided with an ear plate, and the ear plate is positioned in the airtight chamber; the vibration mechanism is an electromagnetic vibrator, the electromagnetic vibrator is arranged in the airtight chamber, and an armature of the electromagnetic vibrator is fixed on the ear plate.
Furthermore, the air inlet is provided with a pressure sensor, and the pressure sensor is used for controlling the electromagnetic vibrator.
The titanium sponge fluidization reaction control method uses the titanium sponge fluidization reaction system, the material granularity of an upper feeding hole is 1-3 mm, and the material granularity of a lower feeding hole is 0.1-0.5 mm; the mass ratio of the titanium slag at the upper feed inlet to the coke is 1:0.3, the mass ratio of the titanium slag at the lower feed inlet to the coke is 1:3.
furthermore, the temperature between the upper sieve plate and the lower sieve plate is controlled to be 1000 to 1050 ℃, and the temperature above the upper sieve plate is controlled to be below 1000 ℃.
In the invention, a double-layer sieve plate fluidized bed is adopted, the upper space of a lower sieve plate is used as a main fluidized reaction area, a layer of upper sieve plate is arranged above the lower sieve plate, and in the aspect of material granularity control, the lower sieve plate adopts materials with finer granularity for feeding, so that the specific surface area of particles is increased, and the reaction speed is favorably improved. The upper sieve plate adopts materials with larger granularity for feeding, and an isolation layer is formed above the upper sieve plate, so that the fine coke particles below the upper sieve plate can be prevented from being taken away by airflow. In addition, in the improvement scheme, the lower sieve plate adopts the composite structure of fixed plate and movable plate, and when the admission pressure is unusual, through the vibration of vibration mechanism drive movable plate, arrange the sediment, can solve the problem that sieve gas distribution hole adhesion material takes place to block up.
Drawings
FIG. 1 is a schematic view of the structure of a reaction furnace according to the present invention;
fig. 2 is a schematic cross-sectional view of a lower screen deck of the present invention;
fig. 3 is a schematic structural view of the movable plate of the present invention.
Detailed Description
The following describes the embodiments of the present invention in detail with reference to specific examples.
Example 1
Referring to fig. 1 to 3, the fluidized reaction system for titanium sponge of the present embodiment includes a reaction furnace, which is a fluidized bed reaction furnace. The top of the reaction furnace is provided with an exhaust port which is used for connecting a cyclone separator and a condensing tower, and the cyclone separator is used for separating coke powder and other solid impurities in gas in the condensing tower and condensing gaseous titanium tetrachloride into liquid for recycling. The bottom of the reaction furnace is provided with an air inlet 1 which is used for introducing chlorine. In this scheme, be equipped with sieve 2 and lower sieve plate 3 in the reacting furnace, the fluidized bed lateral wall is equipped with upper feed inlet 4 and lower feed inlet 5, and upper feed inlet is located the sieve top, and lower feed inlet is located between sieve and the lower sieve plate.
In the prior art, a multi-layer sieve plate fluidized bed generally used for drying materials exists, a feed inlet of the multi-layer sieve plate fluidized bed is arranged on the uppermost layer, and the materials firstly enter the sieve plate on the uppermost layer and then sequentially enter the sieve plate on the lower layer along an overflow pipe. The difference of this scheme and prior art is that all set up the feed inlet below the upper screen plate, wherein the feed inlet is main feed inlet down, and most materials get into the reacting furnace along feed inlet down, and the last feed inlet is vice feed inlet, and a small part of material gets into the reacting furnace along last feed inlet. The mass ratio of the feeding quantity of the upper feeding hole to the feeding quantity of the lower feeding hole can be selected to be 1:6 to 10. The lower layer is used as a main reaction area, and the upper layer is only used for forming an isolation layer.
In this scheme, go up the sieve plate and be equipped with overflow pipe 6, the height of overflow pipe is not more than 10cm. The height referred to here is the height of the upper end of the overflow relative to the screening surface of the upper screen deck, which height is related to the thickness of the material on the upper screen deck during operation. The upper sieve plate is not used as a main reaction area and has the function of forming an isolation layer, and fine powder below the tissues is taken away by airflow, so that the material thickness of the upper sieve plate is not controlled too much. When the materials on the upper sieve plate are stacked and exceed the upper end of the overflow pipe, the materials fall into the lower part along the overflow pipe. The overflow pipe can set up a plurality ofly, and the equipartition is in last sieve.
In order to ensure that a larger reaction space is arranged between the upper sieve plate 2 and the lower sieve plate 3, the distance between the upper sieve plate and the lower sieve plate is not less than 1/2 of the height of the furnace body.
Aiming at the technical problem that the reaction furnace with the sieve plate is inconvenient for deslagging, in the scheme, the lower sieve plate comprises a fixed plate 7 and a movable plate 8 which are superposed up and down, the fixed plate is positioned on the upper layer, the movable plate is positioned on the lower layer, the plate surfaces of the fixed plate and the movable plate are both formed by V-shaped grooves, a gas distribution hole 9 is formed in the groove wall on one side of each V-shaped groove, the gas distribution hole is positioned in the middle or upper part of the groove wall, a deslagging hole 10 is formed in the groove wall on the other side of each V-shaped groove, and the height of the deslagging hole is consistent with the height of the groove wall; the movable plate is provided with a vibration mechanism 11. When the fixed plate and the movable plate are attached, the slag discharging hole with large aperture is shielded, when the vibrating mechanism works, the movable plate vibrates up and down, when the movable plate is separated from the fixed plate downwards, the slag discharging hole is exposed, and agglomerated solid slag deposited in the groove can roll down to the lower part of the lower sieve plate along the slag discharging hole and is discharged from a slag discharging valve at the bottom of the reaction furnace at regular intervals. The vibrating mechanism provides a rapping force for the movable plate at the same time, which is beneficial to the separation of solid slag adhered on the sieve plate.
In this embodiment, a specific connection structure of the movable plate is that an airtight chamber is provided on the sidewall of the reaction furnace, and the airtight chamber is isolated from the outside. The edge of the movable plate is provided with an ear plate 12 which is positioned in the airtight chamber; the vibration mechanism is an electromagnetic vibrator, the electromagnetic vibrator is arranged in the airtight chamber, and an armature of the electromagnetic vibrator is fixed on the ear plate. When the electromagnetic vibrator is electrified, the armature is driven to vibrate, and the movable plate is driven to vibrate.
In the scheme, a pressure sensor is arranged at the air inlet and used for controlling the electromagnetic vibrator. When the gas distribution holes on the lower sieve plate are blocked, the air inlet pressure is increased, and when the pressure signal acquired by the pressure sensor exceeds a threshold value, the electromagnetic vibrator is controlled to start.
The control method of the reaction system comprises the steps of controlling the granularity of materials at each feeding hole and the mass ratio of titanium slag to coke, wherein the granularity of the materials at the upper feeding hole is 1-3mm, and the granularity of the materials at the lower feeding hole is 0.1-0.5 mm; the material at the lower feed inlet has fine granularity and large surface area, and is beneficial to improving the reaction speed. The upper feeding hole has larger material granularity, avoids being taken away by the airflow, is favorable for forming a stable material layer on the upper sieve plate, and prevents the fine powder below from being taken away along with the airflow.
In addition, the mass ratio of the titanium slag at the upper feeding port to the coke is 1:0.3, the mass ratio of the titanium slag at the lower feed inlet to the coke is 1:3. the lower feeding adopts a higher coke proportion, which is beneficial to the complete reaction of the titanium slag. The titanium slag content in the material that the feed inlet got into is high, can not react completely at last sieve, and when the material pile of last sieve was more, fell into the below along the overflow pipe and continue the reaction.
The other beneficial point of the design is that the coke is light and is easy to float upwards under the drive of the airflow. In this scheme, the titanium sediment of going up the sieve falls behind along the overflow pipe, just in time mixes with the coke powder of come-up, avoids appearing the layering, is favorable to going on steadily of reaction.
In the scheme, the temperature between the upper sieve plate and the lower sieve plate is controlled to be 1000-1050 ℃, and the temperature above the upper sieve plate is controlled to be below 1000 ℃. The temperature is kept higher in the main reaction area, so that the reaction speed is improved, the temperature is controlled to be lower above the upper sieve plate, the temperature of tail gas can be reduced, and the condensation and recovery of the follow-up condensation tower on titanium tetrachloride are facilitated. The temperature control of each section in the reaction furnace can be realized by controlling the preheating temperature of materials at each feeding hole. For example, when the temperature above the upper sieve plate needs to be reduced, the preheating temperature of the materials conveyed to the upper feeding hole can be reduced.

Claims (8)

1. The utility model provides a titanium sponge fluidization reaction system, includes the reacting furnace, and the reacting furnace is fluidized bed reacting furnace, and the reacting furnace top is equipped with the gas vent, and the bottom is equipped with air inlet, its characterized in that: an upper sieve plate and a lower sieve plate are arranged in the reaction furnace, an upper feed port and a lower feed port are arranged on the side wall of the fluidized bed, the upper feed port is positioned above the upper sieve plate, and the lower feed port is positioned between the upper sieve plate and the lower sieve plate.
2. The titanium sponge fluidization reaction system according to claim 1, characterized in that: the upper sieve plate is provided with an overflow pipe, and the height of the overflow pipe is not more than 10cm.
3. The titanium sponge fluidization reaction system according to claim 2, characterized in that: the distance between the upper sieve plate and the lower sieve plate is not less than 1/2 of the height of the furnace body.
4. The titanium sponge fluidization reaction system according to claim 1, characterized in that: the lower sieve plate comprises a fixed plate and a movable plate which are vertically superposed, the fixed plate is positioned on the upper layer, the movable plate is positioned on the lower layer, the plate surfaces of the fixed plate and the movable plate are both formed by V-shaped grooves, one side groove wall of each V-shaped groove is provided with a gas distribution hole, the gas distribution hole is positioned in the middle or upper part of the groove wall, the other side groove wall is provided with a slag discharge hole, and the height of the slag discharge hole is consistent with the height of the groove wall; the movable plate is provided with a vibration mechanism.
5. The titanium sponge fluidization reaction system according to claim 4, characterized in that: the side wall of the reaction furnace is provided with an airtight chamber, the edge of the movable plate is provided with an ear plate, and the ear plate is positioned in the airtight chamber; the vibration mechanism is an electromagnetic vibrator, the electromagnetic vibrator is arranged in the airtight chamber, and an armature of the electromagnetic vibrator is fixed on the ear plate.
6. The titanium sponge fluidization reaction system according to claim 5, characterized in that: the air inlet is provided with a pressure sensor which is used for controlling the electromagnetic vibrator.
7. A titanium sponge fluidization reaction control method is characterized in that: the titanium sponge fluidization reaction system as claimed in any one of claims 1~6, wherein the material granularity of the upper feed inlet is 1-3mm, and the material granularity of the lower feed inlet is 0.1-0.5 mm; the mass ratio of the titanium slag at the upper feed inlet to the coke is 1:0.3, the mass ratio of the titanium slag at the lower feed inlet to the coke is 1:3.
8. the method for controlling fluidization of titanium sponge according to claim 7, wherein: the temperature between the upper sieve plate and the lower sieve plate is controlled to be 1000 to 1050 ℃, and the temperature above the upper sieve plate is controlled to be below 1000 ℃.
CN202211456012.6A 2022-11-21 2022-11-21 Titanium sponge fluidization reaction system and method Active CN115725859B (en)

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Citations (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1651337A (en) * 2004-02-05 2005-08-10 中国科学院过程工程研究所 Reactor, its device for making titanium tetrachloride using rich state material chlorination and its method
CN2923014Y (en) * 2006-07-17 2007-07-18 贵阳铝镁设计研究院 Boiling chlorination furnace with sieving plate
CN101254445A (en) * 2007-12-17 2008-09-03 沈阳东方钛业有限公司 Fluidized bed reactor
CN201785203U (en) * 2010-09-01 2011-04-06 贵州航天乌江机电设备有限责任公司 Tower tray type chlorination reaction container with detachable bottom
CN102021038A (en) * 2009-09-14 2011-04-20 新奥科技发展有限公司 Multilayer fluidized bed gasification furnace for preparing methane-rich gas by coal gasification
CN201912927U (en) * 2010-11-16 2011-08-03 攀钢集团钢铁钒钛股份有限公司 Low-temperature boiling chlorination furnace
CN103979603A (en) * 2014-05-26 2014-08-13 攀钢集团攀枝花钢铁研究院有限公司 Low-temperature boiling chlorination system
CN203877931U (en) * 2013-08-30 2014-10-15 漯河兴茂钛业股份有限公司 Boiling chlorination furnace with sieve plate
CN104107671A (en) * 2013-04-18 2014-10-22 上海碧科清洁能源技术有限公司 Fluidized bed reactor and method for carrying out methanol to olefin reaction by using the fluidized bed reactor
CN104613734A (en) * 2015-02-17 2015-05-13 无锡昊瑜节能环保设备有限公司 Vibrated fluidized bed
CN112588211A (en) * 2021-01-18 2021-04-02 重庆大学 Titanium dioxide carbonization boiling chlorination simulation reactor and simulation method
CN112973584A (en) * 2021-02-07 2021-06-18 中国科学院过程工程研究所 Fluidized bed reaction device and application thereof

Patent Citations (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1651337A (en) * 2004-02-05 2005-08-10 中国科学院过程工程研究所 Reactor, its device for making titanium tetrachloride using rich state material chlorination and its method
CN2923014Y (en) * 2006-07-17 2007-07-18 贵阳铝镁设计研究院 Boiling chlorination furnace with sieving plate
CN101254445A (en) * 2007-12-17 2008-09-03 沈阳东方钛业有限公司 Fluidized bed reactor
CN102021038A (en) * 2009-09-14 2011-04-20 新奥科技发展有限公司 Multilayer fluidized bed gasification furnace for preparing methane-rich gas by coal gasification
CN201785203U (en) * 2010-09-01 2011-04-06 贵州航天乌江机电设备有限责任公司 Tower tray type chlorination reaction container with detachable bottom
CN201912927U (en) * 2010-11-16 2011-08-03 攀钢集团钢铁钒钛股份有限公司 Low-temperature boiling chlorination furnace
CN104107671A (en) * 2013-04-18 2014-10-22 上海碧科清洁能源技术有限公司 Fluidized bed reactor and method for carrying out methanol to olefin reaction by using the fluidized bed reactor
CN203877931U (en) * 2013-08-30 2014-10-15 漯河兴茂钛业股份有限公司 Boiling chlorination furnace with sieve plate
CN103979603A (en) * 2014-05-26 2014-08-13 攀钢集团攀枝花钢铁研究院有限公司 Low-temperature boiling chlorination system
CN104613734A (en) * 2015-02-17 2015-05-13 无锡昊瑜节能环保设备有限公司 Vibrated fluidized bed
CN112588211A (en) * 2021-01-18 2021-04-02 重庆大学 Titanium dioxide carbonization boiling chlorination simulation reactor and simulation method
CN112973584A (en) * 2021-02-07 2021-06-18 中国科学院过程工程研究所 Fluidized bed reaction device and application thereof

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