CN105271319B - Method for preparing nanometer MgO - Google Patents
Method for preparing nanometer MgO Download PDFInfo
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- CN105271319B CN105271319B CN201510710486.2A CN201510710486A CN105271319B CN 105271319 B CN105271319 B CN 105271319B CN 201510710486 A CN201510710486 A CN 201510710486A CN 105271319 B CN105271319 B CN 105271319B
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Abstract
The invention provides a method for preparing nanometer MgO, and belongs to the technical field of material preparation. The method sequentially comprises the following steps: A, preparation of organic emulsion; B, preparation of a compound; C, roasting of the compound. According to the method for preparing the nanometer MgO provided by the invention, through the steps of the preparation of the organic emulsion, the preparation of the compound and the roasting of the compound, compared with a current preparation method, the method is simple to operate, the yield and grade of nanometer MgO products are improved, the pollution of waste residues and pollutants to environment due to directly calcining magnesite and dolomite, or using precipitants such as limestone is avoided, and the production cost is reduced.
Description
Technical field
The present invention relates to technical field of material, in particular to a kind of method preparing nanometer mgo.
Background technology
China has abundant magnesium resource, is also big producing country and the consumption big country of magnesium salt product.Not complete according to relevant information
Full statistics, the production scale of China's reheating magnesia and consumption figure are approximately 2,500,000 tons/year and 1,000,000 tons/year respectively, caustic-calcined magnesite
Production scale and consumption figure be approximately 1,000,000 tons/year and 600,000 tons/year respectively, the production scale of refractory grade magnesia and consumption figure
It is approximately 1,500,000 tons/year and 1,400,000 tons/year respectively.These common magnesia mostly come from calcined magnesite, and highly-purity magnesite lacks
Mouth is huge.Relevant information shows, about 100,000 tons/year of domestic high-purity mgo market demand, and about 1.0 ten thousand tons/year of yield；Lightweight
0.7 ~ 0.8 ten thousand yuan/ton of the price of mgo, up to 3.8 ten thousand yuan/ton of pharmaceutical grade mgo.Customs's data imported and exported by China's magnesium salt within 2013
Display, 84.6 ten thousand tons of the mgo export volume that magnesite calcining produces and beautiful yuan/ton of outlet average price 150, and about 0.4 ten thousand tons of import volume
With import price 1190 U.S. yuan/ton；573 tons of synthetic method mgo export volume and beautiful yuan/ton of outlet average price 3310, and import volume 7135
Ton and beautiful yuan/ton of import price 3900.This undoubtedly exposes magnesium salt industry long-term existence " first-class resource, second-class processing and third
The drawbacks of price ", it is to obtain economic worth to sacrifice mineral resources and ecological environment that magnesium oxide produces, and high-performance, height are additional
The high-purity magnesium oxide of value and super-refinement depends on import.
And prior art mainly passes through magnesite and dolomite calcination produces mgo, or reacted with lime cream using magnesium salt
Generate mg (oh)2, then process through high-temperature roasting and obtain mgo, but it does not only exist complex process, high cost, magnesium oxide product
Yield and grade all relatively low problems of ratio, but also a large amount of waste residues and pollutant can be produced.
Content of the invention
In order to solve the above problems, it is an object of the invention to provide a kind of method preparing nanometer mgo, to improve oxidation
The yield of magnesium products and grade, reduce the discharge of waste residue and pollutant, and with respect to existing preparation method, its operation letter
Single.
The technical solution adopted in the present invention is:
A kind of method preparing nanometer mgo, comprises the following steps:
A. organic emulsion preparation: by carbon number be 20 ~ 100 long-chain Organic substance and surfactant be added to distilled water
It is stirred emulsifying with the mixed solution of ethanol, prepare organic emulsion；
B. the preparation of complex: in the described organic emulsion that step a obtains, be simultaneously introduced sodium carbonate liquor and magnesium salt is molten
Liquid, and make the ph value of reaction system maintain 5.0 ~ 11.0, then react under agitation to complete, obtain suspended emulsion；Described
Suspended emulsion is through filtering, washing respectively obtains filtrate and filter cake, and described filter cake obtains after drying by basic magnesium carbonate/Organic substance group
The complex becoming；
C. the roasting of complex: the described complex that step b is obtained obtain after calcination process nano magnesia and
co2Gas.
The method of above-mentioned preparation nanometer mgo, it includes organic emulsion preparation process, the preparation process of complex and roasting step
Rapid so as to respect to existing preparation method, simple to operate, improve nanometer yield of mgo product and a grade, and avoid
Because of dinectly bruning magnesite and dolomite, or the precipitant such as limestone using and lead to the dirt to environment of waste residue and pollutant
Dye, reduces production cost.
Further, described long-chain Organic substance and the mass ratio of described surfactant are 100:5 ~ 30；Described mixed solution
In the volume ratio of described distilled water and described ethanol be 100:1 ~ 50.
Preferably, described long-chain Organic substance and the mass ratio of described surfactant are 100:20；In described mixed solution
The volume ratio of described distilled water and described ethanol be 100:25.
Further, described long-chain Organic substance is selected from paraffin, stearic acid, sodium stearate, magnesium stearate, paraffin crystallite and poly- second
Glycol；Described surfactant selects polyoxyethylene sorbitan monooleate dehydration, glycerol, cetyl trimethyl bromination
Ammonium, sodium lauryl sulphate, dodecylbenzene sodium sulfonate and Polyvinylpyrrolidone.
Further, step c includes vent gas treatment step: by the described co obtaining2Gas is passed through in naoh solution, through absorbing
It is prepared into the sodium carbonate liquor needed for step b afterwards, and return to step b is recycled.
In order to be this preparation method to more environment-friendly it is preferable that step c includes vent gas treatment step, by tail gas
Process step is by co produced by roasting2Gas is passed in naoh solution, makes co2Gas produces carbonic acid with naoh solution reaction
Sodium solution, thus avoid co2The discharge of gas；Meanwhile, sodium carbonate liquor can be to be used for the system of complex in return to step b
Standby, thus being conducive to the recycling of resource.
Further, the described sodium carbonate liquor in step b is equal with the volume of described magnesium salt solution, concentration ratio be 0.5 ~
2.5:1；The amount of substance concentration of described sodium carbonate liquor is 0.1 ~ 1.0 mol/l.
Preferably, the described sodium carbonate liquor in step b and the concentration ratio of described magnesium salt solution are 1:1；Described sodium carbonate
The amount of substance concentration of solution is 0.5 mol/l.
Further, the magnesium salt solution described in step b is mgcl2Solution；Step b includes filtrate process step: will be described
Filtrate carries out concentrating, obtain technical grade nacl after dried.
Step b is by selecting mgcl2As magnesium salt solution, the filtrate obtaining after such reacting liquid filtering is that nacl is molten to solution
Filtrate being carried out concentrating, is dried by filtrate process step simultaneously, thus obtaining technical grade nacl, therefore, not only avoid by liquid
Filtrate discharge and advantageously in environmental conservation, meanwhile, also prepared technical grade nacl, improve preparation nanometer mgo
The added value of method.
In above-mentioned preparation method, the emulsifying temperature of step a is 55 ~ 90 DEG C, and emulsification stirring speed is 2000 ~ 10000 r/
min；The sintering temperature of step c can be 600 ~ 1100 DEG C.And, in preparation process, can be by anti-in reactions steps
The adjustment of the parameter of condition is answered to control the shape of the crystal grain of nanometer mgo.
Further, the emulsifying temperature of step a is 25 ~ 90 DEG C, and emulsification stirring speed is 2000 ~ 10000 r/min；Step c
Sintering temperature be 600 ~ 750 DEG C, the grain shape of described nanometer mgo is flower-shaped.
Further, the emulsifying temperature of step a is 25 ~ 90 DEG C, and emulsification stirring speed is 2000 ~ 10000 r/min；Step c
Sintering temperature be 750 ~ 1100 DEG C, the grain shape of described nanometer mgo is hexagonal plate.
Further, the emulsifying temperature of step a is 25 ~ 90 DEG C, and emulsification stirring speed is 2000 ~ 10000 r/min；Step b
In described magnesium salt be magnesium sulfate；The sintering temperature of step c is the grain shape of 700 ~ 950 DEG C of described nanometers mgo is bar-shaped.
Under conditions of other conditions are constant, by changing the parameter of reaction condition, it is hereby achieved that diverse microcosmic knot
Nanometer mgo of configuration looks.
Further, the magnesium salt in the described magnesium salt solution in step b carries, by salt lake, the magnesium resource that potassium industrial by-product gives up in halogen
It is obtained.
Above-mentioned magnesium salt solution can use and carry, by lake, the prepared magnesium salt of magnesium resource that potassium industrial by-product gives up in halogen, therefore, make money
Source is fully used, it is to avoid the wasting of resources.
Beneficial effects of the present invention:
The method of preparation nanometer mgo provided by the present invention, by the preparation process of organic emulsion preparation process, complex
With the calcination stepses of complex so as to respect to existing preparation method, simple to operate, improve a nanometer yield for mgo product
And grade, and avoid because of dinectly bruning magnesite and dolomite, or the precipitant such as limestone using and lead to waste residue
And the pollution to environment for the pollutant, reduce production cost.
Brief description
Fig. 1 is the flow chart of the method for preparation nanometer mgo in embodiment.
Specific embodiment
Embodiment 1
Present embodiments provide a kind of method preparing nanometer mgo, it comprises the following steps:
A. paraffin and surfactant 100:5 ~ 30 in mass ratio are added in distilled water and the mixed solution of ethanol
Row stirring and emulsifying is reacted, and its reaction temperature is 25 ~ 90 DEG C, and its mixing speed is to mix speed for 500 ~ 10000 r/min, and emulsifying is anti-
Organic emulsion is prepared after answering 20 ~ 50min.
B., in the described organic emulsion that step a obtains, constant speed adds isopyknic sodium carbonate liquor and magnesium salt molten simultaneously
Liquid, the concentration of sodium carbonate liquor is 0.1 ~ 1.0 mol/l, and the concentration ratio of sodium carbonate liquor and magnesium salt solution is 0.5:1 ~ 2:1, makes
The ph value of reaction system maintains 5.0 ~ 11.0, then at 45 ~ 85 DEG C, reacts to complete under the stirring condition of 500 ~ 1000 r/min
Entirely, obtain suspended emulsion；Described suspended emulsion is through filtering, washing respectively obtains filtrate and filter cake, and described filter cake obtains after drying by alkali
The complex of formula magnesium carbonate/paraffin composition.
C. described complex step b being obtained in 600 ~ 1100 DEG C obtain after calcination process nano magnesia and
co2Gas.
The long-chain Organic substance that in the present embodiment, paraffin can also be 20 ~ 100 from other carbon numbers replaces, such as Hard Fat
Acid, sodium stearate, magnesium stearate, paraffin crystallite and Polyethylene Glycol etc..
Surfactant in the present embodiment selects polyoxyethylene sorbitan monooleate dehydration, glycerol, cetyl
Trimethylammonium bromide, sodium lauryl sulphate, dodecylbenzene sodium sulfonate and Polyvinylpyrrolidone etc..
Magnesium salt in the present embodiment is selected from magnesium chloride and magnesium sulfate etc..
A kind of preferred version as the present embodiment: above-mentioned steps c include vent gas treatment step: by the described co obtaining2
Gas is passed through in naoh solution, is prepared into the sodium carbonate liquor needed for step b after absorbing, and return to step b carries out reclaiming profit
With.
Preferably, the magnesium salt solution described in step b is mgcl solution, and step b includes filtrate process step: will be described
Filtrate carries out concentrating, obtain technical grade nacl after dried.
The magnesium salt solution described in step b that solution understands can also adopt other solution, and through filtrate process step
It is prepared into other sodium salt products.
In order to avoid the impact to subsequent reactions for fe, al, ca, b, li plasma in magnesium salt is it is preferable that above-mentioned magnesium salt is
The magnesium salt processing through remove impurity, therefore advantageously in the preparation of nanometer mgo.
As shown in figure 1, being the flow chart of the present embodiment preferred version, first long-chain Organic substance and surfactant are added
Carry out emulsion reaction in the mixed solution of distilled water and ethanol, prepare organic emulsion.
Then the magnesium salt processing through remove impurity and sodium carbonate liquor are added simultaneously in organic emulsion, reaction prepares alkali
Formula magnesium carbonate/paraffin suspended emulsion simultaneously carries out filtration treatment, and respectively obtain sodium salt solution and filter cake, and filter cake is repeatedly washed
Wash, to remove the salt of residual.Cleaning mixture merge with sodium salt solution after through concentration, be dried and be prepared into sodium salt product；Filter cake warp
Cross and prepare basic magnesium carbonate/Organic substance complex after being dried.
Finally above-mentioned magnesium carbonate/Organic substance complex is carried out roasting and prepares a nanometer mgo, and produces co2Gas.
Then the co that will produce2Gas is passed in sodium hydroxide solution and carries out absorption process, and is prepared into the sodium carbonate needed for step b
Solution and recycled in return to step b.
The long-chain Organic substance that paraffin in the present embodiment can also be 20 ~ 100 from other carbon numbers replaces, for example firmly
Fat acid, sodium stearate, magnesium stearate, paraffin crystallite and Polyethylene Glycol etc..
Surfactant in the present embodiment can from polyoxyethylene sorbitan monooleate dehydration, glycerol, 16
One of alkyl trimethyl ammonium bromide, sodium lauryl sulphate, dodecylbenzene sodium sulfonate and Polyvinylpyrrolidone etc.,
Can be from the compound being made up of two or more surfactants.
Magnesium salt in the present embodiment is selected from magnesium chloride and magnesium sulfate etc..
Embodiment 2
Present embodiments provide a kind of method preparing nanometer mgo, it comprises the following steps:
A. the compound of paraffin and surfactant polyethylene and Dodecyl trimethyl ammonium chloride composition is pressed quality
It is added in distilled water and the mixed solution of ethanol than 100:5 ~ 30 and is stirred emulsion reaction, its reaction temperature is 25 ~ 90 DEG C,
Its mixing speed is to mix speed for 500 ~ 10000 r/min, prepares organic emulsion after emulsion reaction 20 ~ 50min.
B., in the described organic emulsion that step a obtains, constant speed adds isopyknic sodium carbonate liquor and magnesium salt molten simultaneously
Liquid, the concentration of sodium carbonate liquor is 0.1 ~ 1.0 mol/l, and the concentration ratio of sodium carbonate liquor and magnesium salt solution is 0.5:1 ~ 2:1, makes
The ph value of reaction system maintains 5.0 ~ 11.0, then at 45 ~ 85 DEG C, reacts to complete under the stirring condition of 500 ~ 1000 r/min
Entirely, obtain suspended emulsion；Described suspended emulsion is through filtering, washing respectively obtains filtrate and filter cake, and described filter cake obtains after drying by alkali
The complex of formula magnesium carbonate/paraffin composition；Described filtrate is prepared into technical grade nacl after concentrating, being dried.
C. the described complex that step b obtains is obtained nano magnesia and co in 600 ~ 750 DEG C after calcination process2
Gas；Described co2Gas is passed through in naoh solution, is prepared into the sodium carbonate liquor needed for step b after absorbing, and return to step
B is recycled.
The grain shape of nanometer mgo manufactured in the present embodiment is flower-shaped, its petal thickness 10 ~ 50nm, and its particle diameter is 2 ~ 20 μ
m.
Embodiment 3
Present embodiments provide a kind of method preparing nanometer mgo, it comprises the following steps:
A. by the compound of paraffin surface activating agent Polyethylene Glycol and Dodecyl trimethyl ammonium chloride composition in mass ratio
100:5 ~ 30 are added in distilled water and the mixed solution of ethanol and are stirred emulsion reaction, and its reaction temperature is 25 ~ 90 DEG C, its
Mixing speed is to mix speed for 500 ~ 10000 r/min, prepares organic emulsion after emulsion reaction 20 ~ 50min；
B., in the described organic emulsion that step a obtains, constant speed adds isopyknic sodium carbonate liquor and magnesium salt molten simultaneously
Liquid, the concentration of sodium carbonate liquor is 0.1 ~ 1.0 mol/l, and the concentration ratio of sodium carbonate liquor and magnesium salt solution is 0.5:1 ~ 2:1, makes
The ph value of reaction system maintains 5.0 ~ 11.0, then at 45 ~ 85 DEG C, reacts to complete under the stirring condition of 500 ~ 1000 r/min
Entirely, obtain suspended emulsion；Described suspended emulsion is through filtering, washing respectively obtains filtrate and filter cake, and described filter cake obtains after drying by alkali
The complex of formula magnesium carbonate/paraffin composition；Described filtrate is prepared into technical grade nacl after concentrating, being dried.
C. described complex step b being obtained in 750 ~ 1100 DEG C obtain after calcination process nano magnesia and
co2Gas；Described co2Gas is passed through in naoh solution, is prepared into the sodium carbonate liquor needed for step b, and returns step after absorbing
Rapid b is recycled.
The grain shape of nanometer mgo manufactured in the present embodiment is hexagonal plate, its particle diameter: 20 ~ 100 nm.
Embodiment 4
Present embodiments provide a kind of method preparing nanometer mgo, it comprises the following steps:
A. the compound of paraffin and surfactant sodium dodecyl base benzene sulfonic acid sodium salt and Polyvinylpyrrolidone composition is pressed matter
Amount is added in distilled water and the mixed solution of ethanol than 100:5 ~ 30 and is stirred emulsion reaction, and its reaction temperature is 25 ~ 90
DEG C, its mixing speed is to mix speed for 500 ~ 10000 r/min, prepares organic emulsion after emulsion reaction 20 ~ 50min.
B., in the described organic emulsion that step a obtains, constant speed adds isopyknic sodium carbonate liquor and magnesium sulfate simultaneously
Solution, the concentration of sodium carbonate liquor is 0.1 ~ 1.0 mol/l, and the concentration ratio of sodium carbonate liquor and Adlerika is 0.5:1 ~ 2:
1, make the ph value of reaction system maintain 5.0 ~ 11.0, then at 45 ~ 85 DEG C, react under the stirring condition of 500 ~ 1000 r/min
To complete, obtain suspended emulsion；Described suspended emulsion is through filtering, washing respectively obtains filtrate and filter cake, and described filter cake obtains after drying
The complex being made up of basic magnesium carbonate/paraffin；Described filtrate is prepared into technical grade nacl after concentrating, being dried.
C. the described complex that step b obtains is obtained nano magnesia and co in 700 ~ 950 DEG C after calcination process2
Gas；Described co2Gas is passed through in naoh solution, is prepared into the sodium carbonate liquor needed for step b after absorbing, and return to step
B is recycled.
The grain shape of nanometer mgo manufactured in the present embodiment is bar-shaped shape, 1 ~ 100 μm of its particle diameter length, and it a diameter of 50
nm~10μm.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for the skill of this area
For art personnel, the present invention can have various modifications and variations.All within the spirit and principles in the present invention, made any repair
Change, equivalent, improvement etc., should be included within the scope of the present invention.
Claims (7)
1. a kind of method preparing nanometer mgo is it is characterised in that comprise the following steps:
A. organic emulsion preparation: by carbon number be 20～100 long-chain Organic substance and surfactant be added to distilled water and
It is stirred emulsifying in the mixed solution of ethanol, prepares organic emulsion, wherein, described carbon number is 20～100 length
Chain Organic substance is selected from paraffin, sodium stearate, magnesium stearate, paraffin crystallite and Polyethylene Glycol, and polyoxy selected by described surfactant
Ethylene Arlacel-80, glycerol, sodium lauryl sulphate, dodecylbenzene sodium sulfonate and Polyvinylpyrrolidone
In at least one；
B. the preparation of complex: in the described organic emulsion that step a obtains, it is simultaneously introduced sodium carbonate liquor and magnesium salt solution,
And make the ph value of reaction system maintain 5.0～11.0, then react under agitation to complete, obtain suspension；Described outstanding
Supernatant liquid is through filtering, washing respectively obtains filtrate and filter cake, and described filter cake obtains being made up of basic magnesium carbonate/Organic substance after drying
Complex, wherein, described magnesium salt be magnesium chloride or magnesium sulfate；
C. the roasting of complex: the described complex that step b is obtained obtains nanometer mgo and co after calcination process2Gas,
Wherein, when described magnesium salt is magnesium chloride and sintering temperature >=600 DEG C and 750 DEG C of ＜, the grain shape of described nanometer mgo is flower
Shape；When described magnesium salt is magnesium chloride and 750 DEG C of sintering temperature ＞ and≤1100 DEG C, the grain shape of described nanometer mgo is six
Gusset plate shape；When described magnesium salt, for magnesium sulfate and sintering temperature is 700～950 DEG C, and the grain shape of described nanometer mgo is bar-shaped.
2. the method for preparation nanometer mgo according to claim 1 is it is characterised in that described long-chain Organic substance and described table
The mass ratio of face activating agent is 100:5～30；Described distilled water in described mixed solution and the volume ratio of described ethanol are
100:1～50.
3. the method for preparation nanometer mgo according to claim 1 and 2 is it is characterised in that step c includes vent gas treatment step
Rapid: by the described co obtaining2Gas is passed through in naoh solution, is prepared into the sodium carbonate liquor needed for step b, and returns after absorbing
Return step b to be recycled.
4. the method for preparation nanometer mgo according to claim 3 is it is characterised in that described sodium carbonate liquor in step b
And substance withdrawl syndrome equal with the volume of described magnesium salt solution is than for 0.5～2.5:1；The amount of substance of described sodium carbonate liquor is dense
Spend for 0.1～1.0mol/l.
5. the method for preparation according to claim 1 and 2 is it is characterised in that the magnesium salt solution described in step b is chlorination
Magnesium solution；Step b includes filtrate process step: described filtrate is carried out concentrating, obtains technical grade nacl after dried.
6. the method for preparation nanometer mgo according to claim 1 and 2 is it is characterised in that the emulsifying temperature of step a is 25
～90 DEG C, emulsification stirring speed is 2000～10000r/min.
7. the method for preparation nanometer mgo according to claim 1 and 2 is it is characterised in that the described magnesium salt in step b is molten
Magnesium salt in liquid carries the magnesium resource in the useless halogen of potassium industrial by-product by salt lake and is obtained.
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| CN105883866B (en) * | 2016-05-20 | 2017-11-07 | 江苏师范大学 | A kind of synthetic method of the controllable basic magnesium carbonate nanometer rods of length and width |
| CN107337937A (en) * | 2017-06-09 | 2017-11-10 | 苏州市泽镁新材料科技有限公司 | A kind of preparation method for the surface-modified nano magnesium oxide material for being exclusively used in SMC thickenings |
| CN107433180B (en) * | 2017-08-23 | 2019-01-08 | 内江师范学院 | A kind of sandwich structure nano adsorber of carbon coating magnesia and preparation method thereof |
| CN108328629A (en) * | 2018-05-16 | 2018-07-27 | 湖南华佳纳米新材料科技有限公司 | A kind of method and system preparing nano magnesia |
| CN108706618A (en) * | 2018-08-28 | 2018-10-26 | 内江师范学院 | Utilize the method for micro-emulsion method for preparing nano aluminium oxide |
| CN109354048B (en) * | 2018-12-13 | 2021-07-27 | 沈阳理工大学 | Method for preparing magnesium hydroxide and magnesium carbonate series compound by ion catalysis of magnesite |
| WO2021097658A1 (en) * | 2019-11-19 | 2021-05-27 | 南京先进生物材料与过程装备研究院有限公司 | Polyethylene insulating material for high-voltage direct current cable |
| CN113413870B (en) * | 2021-05-17 | 2022-11-25 | 中国科学院青海盐湖研究所 | Magnesium oxide-metal sulfide-biomass charcoal composite material and preparation method and application thereof |
| CN115814752B (en) * | 2023-01-31 | 2024-04-05 | 成都理工大学 | Composite material of calcium carbonate and nano magnesium oxide and preparation and application methods thereof |
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| CN101353176B (en) * | 2007-07-26 | 2010-10-06 | 郑州大学 | Novel method for preparing nano-magnesia |
| KR101086192B1 (en) * | 2008-08-25 | 2011-11-25 | 부산대학교 산학협력단 | Nanoparticle magnesia and method for preparing the same |
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Inventor after: Zheng Xiaogang Inventor after: Liu Weihua Inventor after: Liu Yan Inventor after: Huang Zhongliang Inventor before: Zheng Xiaogang Inventor before: Huo Feng Inventor before: Liu Yong Inventor before: Wang Shuxian Inventor before: Song Yuchun Inventor before: Huang Min |
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Effective date of registration: 20180507 Address after: 425316 industrial parks in Daoxian County Industrial Park, Yongzhou, Hunan Patentee after: Hunan Hua Jia nano new Mstar Technology Ltd Address before: 641100 Dong Tung Road, Dongxing District, Neijiang, Sichuan Province, No. 705 Patentee before: Neijiang Normal University |