CN108002411B - A kind of method that the dissolution of defluorinate lepidolite multistage pressure tank mentions lithium - Google Patents
A kind of method that the dissolution of defluorinate lepidolite multistage pressure tank mentions lithium Download PDFInfo
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- CN108002411B CN108002411B CN201711319924.8A CN201711319924A CN108002411B CN 108002411 B CN108002411 B CN 108002411B CN 201711319924 A CN201711319924 A CN 201711319924A CN 108002411 B CN108002411 B CN 108002411B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/08—Carbonates; Bicarbonates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
- C01D5/06—Preparation of sulfates by double decomposition
- C01D5/10—Preparation of sulfates by double decomposition with sulfates of magnesium, calcium, strontium, or barium
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Abstract
The invention discloses a kind of defluorinate lepidolite multistage pressure tanks to dissolve out the method for mentioning lithium, by defluorinate lepidolite miberal powder, the sulfate and additive of alkali metal or alkaline-earth metal are sized mixing in proportion with water, slurry is transported in stepped heating pressurized tank with pump after preheater preheats and is warming up to reaction temperature and pressure step by step, it is transferred in heat preservation dissolution tank and carries out dissolution reaction, it is depressurized step by step by multi-step pressure reduction spontaneous evaporation cooling tank after the reaction was completed and cools down and recycle heat, and slurry is separated by solid-liquid separation and is washed, filtrate passes through concentration, removal of impurities, the crystallization of sodium carbonate sinker is added, lithium salts product is obtained by filtration, sinker Recycling Mother Solution to ingredient sizes mixing or recycles potassium sulfate after analysing sodium, rubidium sulfate and cesium sulfate.For the method for the present invention compared with the dissolution of other lepidolites proposes lithium technology, multistage pressure tank reactor can realize recycling for Process Energy, at low cost, energy consumption is small, have industrial applications prospect.
Description
Technical field
The invention belongs to ores to mention lithium technology field, and in particular to a kind of dissolution of defluorinate lepidolite multistage pressure tank mentions lithium
Method.
Background technique
Lithium has various excellent properties, and it is contour that lithium and lithium salts have been widely used in aluminium lithium alloy, lithium battery, nuclear fusion
New technical field.China's lepidolite is resourceful, is distributed mainly on the ground such as Jiangxi, and lepidolite extracted lithium technique mainly includes sulphur at present
Hydrochlorate method, limestone-based process, chlorinating roasting, sulfuric acid process and fluorine chemistry method, these methods are mentioned using lepidolite concentrate
Lithium reaction, there is high production cost, some problems such as energy consumption is high, the quantity of slag is big, so research defluorinate lepidolite extracted lithium technology pair
The development of world's new energy has a very important significance.
Lepidolite is a kind of fluorine-containing phyllosilicate containing lithium minerals, compact structure, and the fluorine in mineral can be to the extraction of lithium
Increase difficulty.The sulfate liquor high temperature and pressure multistage pressure of defluorinate lepidolite proposed by the present invention and alkali metal or alkaline-earth metal
The method dissolved out in power tank is produced into low, small investment；Ore pulp is high in multistage pressure tank and in multi-step pressure reduction spontaneous evaporation cooling tank
Effect utilizes secondary energy sources, and energy consumption is small, has industrial applications prospect.
Summary of the invention
It is an object of the invention to solve the technical issues of prior art cannot efficiently extract elemental lithium in lepidolite, mention
A kind of method that the dissolution of defluorinate lepidolite multistage pressure tank mentions lithium is gone out.Present device process is simple, more molten than traditional autoclave
Small investment needed for device, production cost are low out；In reaction process secondary steam efficiently utilize, energy consumption it is small.
To achieve the goals above, the present invention adopts the following technical scheme:
A kind of dissolution of defluorinate lepidolite multistage pressure tank propose the method for lithium the following steps are included:
(1) natural lepidolite is switched into after high-temperature roasting defluorinate defluorinate lepidolite, then is crushed and obtains defluorinate lepidolite ore
Defluorinate lepidolite miberal powder, the sulfate of alkali or alkaline earth metal, additive and water are stirred in mixing tank and are sized mixing by powder；
(2) slurry that step (1) prepares is delivered to the heating pressure for being delivered to plural serial stage after preheating in preheater with pump
It heats up in power tank, is added using the combination of primary steam, the secondary steam for depressurizing the extraction of spontaneous evaporation cooling tank or both step by step
Heat, afterbody heating pressurized tank reach the temperature of reaction using a high steam, dissolve out in tank and have reacted into heat preservation
Entirely；Reacted slurry enters in decompression spontaneous evaporation cooling tank the evaporation that cools down step by step again；After slurry cools to 50-70 DEG C, carry out
Solid-liquor separation obtains the leachate and leaching slag of sulfur acid lithium, sodium sulphate, potassium sulfate, rubidium sulfate and cesium sulfate；
(3) slurry plural serial stage heating pressurized tank temperature-rise period in steam condensate (SC) by temperature from high to low respectively by
Grade flows into corresponding primary steam condensate water pot and secondary steam condensate water pot, the primary steam condensate water pot of afterbody
Condensed water, which returns to boiler, to be continued to generate primary steam, and the condensed water of the secondary steam condensate water pot of afterbody is starched after being used as reaction
The washing water and configuration slurry for expecting solid-liquor separation use water；
(4) reaction of precipitating reagent sodium carbonate is added after removal of impurities concentration in the leachate that step (2) obtains, and filtering obtains carbonic acid
Lithium precipitating and main component are sodium sulphate and the sinker circulating mother liquor of other alkali metal sulfates, which returns
The ingredient in step (1), or sodium sulphate is precipitated by freezing or concentration, the solution after analysing sodium continues to recycle potassium sulfate, sulfuric acid
Rubidium and cesium sulfate；The sodium sulphate obtained is precipitated and carries out ingredient back to step (1) is middle.
Oxidation lithium content >=0.5wt% in natural lepidolite ore described in step (1) is crushed gained defluorinate lepidolite ore
Powder diameter D90≤180μm。
Defluorinate lepidolite miberal powder, alkali metal or the sulfate of alkaline-earth metal and the weight ratio of additive are in step (1)
1:0.1 ~ 1.5:0.01 ~ 1, the solid and liquid weight ratio of slurry are 1:4 ~ 25；The wherein sulfate of the alkali metal or alkaline-earth metal
Source include alkali metal and alkali earth metal sulfate contained by sinker circulating mother liquor in step (4).
The step (1) size mixing process additive be CaO, Ca (OH)2、NaOH、KOH、NaHCO3、Na2CO3、KHCO3With
K2CO3One or more of.
In step (2), it is 60-100 DEG C that slurry is preheating to temperature in preheater, and slurry flows in stepped heating pressurized tank
Dynamic speed is 0.05-0.5m/min；In heat preservation dissolution tank, reaction temperature is 130 ~ 260 DEG C, reaction time 30-150min, instead
Answering pressure is 1-5 MPa.
In step (2), the secondary steam that decompression spontaneous evaporation cooling tank is drawn heats slurry for corresponding heating pressurized tank,
The secondary steam that afterbody depressurizes spontaneous evaporation cooling tank introduces preheater and preheats slurry.
In step (2) in stepped heating pressurized tank heating method be by collet heating, be passed directly into high pressure steam heating,
One or several kinds of combinations of built-in steam pipe coil or steam multitube heating carry out high temperature and pressure dissolution reaction.
The heating of every grade of stepped heating pressurized tank is 10-25 DEG C in step (2), and the series for the pressurized tank that heats up is 6-10 grades,
Reach temperature required for reaction；The cooling for depressurizing every grade of spontaneous evaporation cooling tank is 10-25 DEG C, depressurizes the grade of spontaneous evaporation cooling tank
Number is 6-10 grades；Except afterbody heating pressurized tank is using primary steam heating, other use primary steam, correspond to decompression from steaming
The combination of secondary steam of cooling tank or both is sent out to heat, which depressurizes the temperature of the secondary steam of spontaneous evaporation cooling tank
It is consistent with temperature needed for the heating pressurized tank.
The primary steam of every grade of stepped heating pressurized tank heating and the condensed water of secondary steam respectively enter pair in step (3)
Answer the primary steam condensate water pot and secondary steam condensate water pot of pressure stage, and the condensate water pot with the heating pressurized tank of the superior and the subordinate
It is connected using drain valve, the condensed water of the primary steam condensate water pot of the heating pressurized tank of the first order returns to boiler and generates one again
Secondary steam, the condensed water in the secondary steam condensate water pot of the heating pressurized tank of the first order go ingredient or cleaning solution to consolidate isolate
The purposes such as material.
Compared with prior art, the present invention having following remarkable advantages:
1, slurry flow velocity in pressurized tank is lower, and equipment investment is few, and process is short, and heat makes full use of, heat loss is low；
2, multistage pressure tank dissolving-out method proposed by the present invention, decompression spontaneous evaporation temperature-fall period secondary steam can be sufficiently sharp
Stepped heating pressurized tank heating ore pulp is used, low energy consumption than traditional autoclave dissolving device, while depressurizing self-evaporation process can be with
Make to leach solution concentration, reduces the cost of subsequent concentration, process is simple, is easy to industrialize.
Detailed description of the invention
Fig. 1 is the process flow chart that defluorinate lepidolite multistage pressure tank of the present invention dissolution mentions lithium.
Specific embodiment
Below in conjunction with specific embodiment, the present invention will be further described, but the present invention is not limited only to these embodiments.
Embodiment 1
Lithium content will be aoxidized and be the natural lepidolite concentrate high-temperature roasting defluorinate of 3.6wt%, then be crushed to partial size D90=150 μ
M, obtained defluorinate lepidolite miberal powder, sodium sulphate, addition of C aO size mixing in mixing tank by weight 1:1:0.3 and water, slurry
Solid and liquid weight ratio is 1:8, and slurry is preheating to be transported in 6 grades of heating pressurized tanks after temperature is 80 DEG C with pump in preheater is passed through two
Secondary steam and primary steam are heated, and every grade of temperature heating is 25 DEG C, and the 6th grade is heated using primary steam, are finally heated up
To 240 DEG C, reaction time 45min is stopped in heat preservation dissolution tank, carries out high temperature and pressure dissolution reaction, pulp flow speed is
0.5m/min, reaction temperature are 240 DEG C, reaction pressure 3.4MPa, and decompression spontaneous evaporation cooling tank is 6 grades, and every grade of cooling is
25 DEG C, the secondary steam that spontaneous evaporation obtains removes the slurry of the heating pressurized tank under heating corresponding temperature, and stepped heating pressurized tank is every
The primary steam of grade heating and the condensed water of secondary steam respectively enter the primary steam condensate water pot of corresponding pressure grade with it is secondary
Steam condensate (SC) tank, and connect with the heating pressurized tank of the superior and the subordinate using drain valve, the primary steam of first order heating pressurized tank
The condensed water of condensate water pot returns to boiler and generates primary steam again, the first order heat up pressurized tank secondary steam condensate water pot in
Condensed water go ingredient or cleaning solution to consolidate separation of material.Last slurry is cooled to less than 65 DEG C, is then separated by solid-liquid separation, is obtained
To the filtrate of sulfur acid lithium, sodium sulphate, potassium sulfate, rubidium sulfate and cesium sulfate, the dissolution rate of lithium is up to 95% in defluorinate lepidolite；Filter
Sodium carbonate sinker is added in liquid, the mother liquor of lithium carbonate and sulfur acid sodium and other alkali metal sulfates, Recycling Mother Solution is obtained by filtration
It sizes mixing step to ingredient.
Embodiment 2
Lithium content will be aoxidized and be the natural lepidolite concentrate high-temperature roasting defluorinate of 1.5wt%, then be crushed to partial size D90=110 μ
M, obtained defluorinate lepidolite miberal powder, sodium sulphate, addition of C aO size mixing in mixing tank by weight 1:0.5:0.3 and water, slurry
Material solid and liquid weight ratio is 1:5, and slurry is preheating to be transported in 8 grades of heating pressurized tanks after temperature is 90 DEG C with pump in preheater to be passed through
Secondary steam and primary steam are heated, and every grade of temperature heating is 15 DEG C, and the 8th grade is heated using primary steam, are finally risen
Temperature stops reaction time 145min to 230 DEG C in heat insulation tank, carries out high temperature and pressure dissolution reaction, and pulp flow speed is
0.25m/min, reaction temperature are 230 DEG C, reaction pressure 2.8MPa, and decompression spontaneous evaporation cooling tank is 8 grades, and every grade of cooling is
15 DEG C, the secondary steam that spontaneous evaporation obtains removes the slurry of the heating pressurized tank under heating corresponding temperature, and stepped heating pressurized tank is every
The primary steam of grade heating and the condensed water of secondary steam respectively enter the primary steam condensate water pot of corresponding pressure grade with it is secondary
Steam condensate (SC) tank, and connect with the heating pressurized tank of the superior and the subordinate using drain valve, the primary steam of first order heating pressurized tank
The condensed water of condensate water pot returns to boiler and generates primary steam again, the first order heat up pressurized tank secondary steam condensate water pot in
Condensed water go ingredient or cleaning solution to consolidate separation of material.Last slurry is cooled to less than 65 DEG C, is then separated by solid-liquid separation, is obtained
To the filtrate of sulfur acid lithium, sodium sulphate, potassium sulfate, rubidium sulfate and cesium sulfate, the dissolution rate of lithium is up to 90.5% in defluorinate lepidolite；
Sodium carbonate sinker is added in filtrate, the mother liquor of lithium carbonate and sulfur acid sodium and other alkali metal sulfates is obtained by filtration, mother liquor follows
Ring to ingredient is sized mixing step.
Embodiment 3
Lithium content will be aoxidized and be the natural lepidolite concentrate high-temperature roasting defluorinate of 2.5wt%, then be crushed to partial size D90=50 μm,
Obtained defluorinate lepidolite miberal powder, sodium sulphate, additive NaOH sizes mixing in mixing tank by weight 1:1.2:0.1 and water, slurry
Material solid and liquid weight ratio is 1:6, and slurry is preheating to be transported in 6 grades of heating pressurized tanks after temperature is 80 DEG C with pump in preheater to be passed through
Secondary steam and primary steam are heated, and every grade of temperature heating is 20 DEG C, and the 6th grade is heated using primary steam, are finally risen
Temperature stops reaction time 145min in heat preservation dissolution tank to 220 DEG C, carries out high temperature and pressure dissolution reaction, pulp flow speed
For 0.15m/min, reaction temperature is 220 DEG C, reaction pressure 2.3MPa, and decompression spontaneous evaporation cooling tank is 6 grades, every grade of cooling
It is 20 DEG C, the secondary steam that spontaneous evaporation obtains removes the slurry of the heating pressurized tank under heating corresponding temperature, stepped heating pressurized tank
The condensed water of every grade of primary steam to heat up and secondary steam respectively enters the primary steam condensate water pot and two of corresponding pressure grade
Secondary steam condensate (SC) tank, and connect with the heating pressurized tank of the superior and the subordinate using drain valve, the primary steaming of first order heating pressurized tank
The condensed water of vapour condensate water pot returns to boiler and generates primary steam, the secondary steam condensate water pot of first order heating pressurized tank again
In condensed water go ingredient or cleaning solution to consolidate separation of material.Last slurry is cooled to less than 65 DEG C, is then separated by solid-liquid separation,
The filtrate of sulfur acid lithium, sodium sulphate, potassium sulfate, rubidium sulfate and cesium sulfate is obtained, the dissolution rate of lithium reaches in defluorinate lepidolite
91.5%；Sodium carbonate sinker is added in filtrate, the mother liquor of lithium carbonate and sulfur acid sodium and other alkali metal sulfates is obtained by filtration,
Recycling Mother Solution to ingredient is sized mixing step.
Embodiment 4
Lithium content will be aoxidized and be the natural lepidolite concentrate high-temperature roasting defluorinate of 2.5wt%, then be crushed to partial size D90=75 μm,
Obtained defluorinate lepidolite miberal powder, sodium sulphate, additive NaHCO3It sizes mixing in mixing tank by weight 1:0.6:0.13 and water,
Slurry solid and liquid weight ratio is 1:5, and slurry is preheating to be transported in 7 grades of heating pressurized tanks after temperature is 70 DEG C with pump in preheater to be led to
It crosses secondary steam and primary steam is heated, every grade of temperature heating is 20 DEG C, and the 7th grade is heated using primary steam, finally
235 DEG C are warming up to, is stopped the reaction time 85 minutes in heat insulation tank, high temperature and pressure dissolution reaction is carried out, pulp flow speed is
0.05m/min, reaction temperature are 235 DEG C, reaction pressure 2.9MPa, and decompression spontaneous evaporation cooling tank is 7 grades, and every grade of cooling is
20 DEG C, the secondary steam that spontaneous evaporation obtains removes the slurry of the heating pressurized tank under heating corresponding temperature, and stepped heating pressurized tank is every
The primary steam of grade heating and the condensed water of secondary steam respectively enter the primary steam condensate water pot of corresponding pressure grade with it is secondary
Steam condensate (SC) tank, and connect with the heating pressurized tank of the superior and the subordinate using drain valve, the primary steam of first order heating pressurized tank
The condensed water of condensate water pot returns to boiler and generates primary steam again, the first order heat up pressurized tank secondary steam condensate water pot in
Condensed water go ingredient or cleaning solution to consolidate separation of material.Last slurry is cooled to less than 55 DEG C, is then separated by solid-liquid separation, is obtained
To the filtrate of sulfur acid lithium, sodium sulphate, potassium sulfate, rubidium sulfate and cesium sulfate, the dissolution rate of lithium is up to 94% in defluorinate lepidolite；Filter
Sodium carbonate sinker is added in liquid, the mother liquor of lithium carbonate and sulfur acid sodium and other alkali metal sulfates, Recycling Mother Solution is obtained by filtration
It sizes mixing step to ingredient.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification, is all covered by the present invention.
Claims (3)
1. a kind of defluorinate lepidolite multistage pressure tank dissolves out the method for mentioning lithium, it is characterised in that: the following steps are included:
(1) broken natural lepidolite is fired after defluorinate and switchs to defluorinate lepidolite, then be crushed and obtain defluorinate lepidolite ore
Defluorinate lepidolite miberal powder, the sulfate of alkali or alkaline earth metal, additive and water are stirred in mixing tank and are sized mixing by powder；
(2) slurry that step (1) prepares is delivered to the heating pressurized tank for being delivered to plural serial stage after preheating in preheater with pump
In heat up step by step, the combination of the secondary steam or both drawn using primary steam, decompression spontaneous evaporation cooling tank is heated, most
Rear stage heating pressurized tank reaches the temperature of reaction using a high steam, dissolves out in tank into heat preservation and continues fully reacting；
Reacted slurry enters in decompression spontaneous evaporation cooling tank the evaporation that cools down step by step again；After slurry cools to 50-70 DEG C, it is solid to carry out liquid
Separation obtains the leachate and leaching slag of sulfur acid lithium, sodium sulphate, potassium sulfate, rubidium sulfate and cesium sulfate；
(3) steam condensate (SC) of the slurry in plural serial stage heating pressurized tank temperature-rise period is flowed step by step respectively from high to low by temperature
Enter in corresponding primary steam condensate water pot and secondary steam condensate water pot, the condensation of the primary steam condensate water pot of afterbody
Water, which returns to boiler, to be continued to generate primary steam, and the condensed water of the secondary steam condensate water pot of afterbody is as slurry liquid after reaction
Admittedly the washing water that separates and configuration slurry use water；
(4) after removal of impurities concentration the reaction of precipitating reagent sodium carbonate is added, it is heavy that filtering obtains lithium carbonate in the leachate that step (2) obtains
It forms sediment and main component is sodium sulphate and the sinker circulating mother liquor of other alkali metal sulfates, which returns to step
Suddenly ingredient in (1), or by freezing or concentration be precipitated sodium sulphate, analyse sodium after solution continue recycle potassium sulfate, rubidium sulfate with
Cesium sulfate；The sodium sulphate obtained is precipitated and carries out ingredient back to step (1) is middle；
Defluorinate lepidolite miberal powder, alkali metal or the sulfate of alkaline-earth metal and the weight ratio of additive are in the step (1)
1:0.1 ~ 1.5:0.01 ~ 1, the solid and liquid weight ratio of slurry are 1:4 ~ 25；The wherein sulfate of the alkali metal or alkaline-earth metal
Source include alkali metal and alkali earth metal sulfate contained by sinker circulating mother liquor in step (4)；
It is 60-100 DEG C that slurry is preheating to temperature in preheater in the step (2), and slurry flows in stepped heating pressurized tank
Dynamic speed is 0.05-0.5m/min；In heat preservation dissolution tank, reaction temperature is 130 ~ 260 DEG C, reaction time 30-150min, instead
Answering pressure is 1-5 MPa；
In the step (2), the secondary steam that decompression spontaneous evaporation cooling tank is drawn heats slurry for corresponding heating pressurized tank,
The secondary steam that afterbody depressurizes spontaneous evaporation cooling tank introduces preheater and preheats slurry；
In the step (2) in stepped heating pressurized tank heating method be by collet heating, be passed directly into high pressure steam heating,
One or several kinds of combinations of built-in steam pipe coil or steam multitube heating carry out high temperature and pressure dissolution reaction；
The heating of every grade of stepped heating pressurized tank is 10-25 DEG C in the step (2), and the series for the pressurized tank that heats up is 6-18 grades,
Reach temperature required for reaction；The cooling for depressurizing every grade of spontaneous evaporation cooling tank is 10-25 DEG C, depressurizes the grade of spontaneous evaporation cooling tank
Number is 6-18 grades；Except afterbody heating pressurized tank is using primary steam heating, other use primary steam, correspond to decompression from steaming
The combination of secondary steam of cooling tank or both is sent out to heat, which depressurizes the temperature of the secondary steam of spontaneous evaporation cooling tank
It is consistent with temperature needed for the heating pressurized tank；
The primary steam of every grade of stepped heating pressurized tank heating and the condensed water of secondary steam respectively enter pair in the step (3)
Answer the primary steam condensate water pot and secondary steam condensate water pot of pressure stage, and the condensate water pot with the heating pressurized tank of the superior and the subordinate
It is connected using drain valve, the condensed water of the primary steam condensate water pot of the heating pressurized tank of the first order returns to boiler and generates one again
Secondary steam, the condensed water in the secondary steam condensate water pot of the heating pressurized tank of the first order go ingredient or cleaning solution to consolidate isolate
Expect purposes.
2. a kind of defluorinate lepidolite multistage pressure tank according to claim 1 dissolves out the method for mentioning lithium, it is characterised in that: step
Suddenly oxidation lithium content >=0.5wt% in natural lepidolite ore described in (1) is crushed gained defluorinate lepidolite ore powder diameter D90≤
180μm。
3. a kind of defluorinate lepidolite road according to claim 1 multistage pressure tank dissolves out the method for mentioning lithium, it is characterised in that:
The step (1) size mixing process additive be CaO, Ca (OH)2、NaOH、KOH、NaHCO3、Na2CO3、KHCO3And K2CO3In
One or more.
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| CN110482576B (en) * | 2019-09-26 | 2022-05-06 | 福州大学 | Method for preparing lithium salt from lepidolite through hydrothermal method |
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| CN201586522U (en) * | 2009-12-11 | 2010-09-22 | 江西赣锋锂业股份有限公司 | Horizontal continuous pressure leaching kettle for defluorinated lepidolite |
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Effective date of registration: 20230802 Address after: 336699 North of Qingyi Road, Chengxi Industrial Park, Fenyi County, Xinyu City, Jiangxi Province Patentee after: Xinyu Guoxing Lithium Industry Co.,Ltd. Address before: No.2, Xueyuan Road, University Town, Shangjie Town, Minhou County, Fuzhou City, Fujian Province Patentee before: FUZHOU University |