CN104725518B - A kind of method that ultrasonic-microwave prepares water hyacinth carboxymethyl cellulose - Google Patents
A kind of method that ultrasonic-microwave prepares water hyacinth carboxymethyl cellulose Download PDFInfo
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- CN104725518B CN104725518B CN201510103650.3A CN201510103650A CN104725518B CN 104725518 B CN104725518 B CN 104725518B CN 201510103650 A CN201510103650 A CN 201510103650A CN 104725518 B CN104725518 B CN 104725518B
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- water hyacinth
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Abstract
The present invention discloses a kind of method that ultrasonic-microwave prepares water hyacinth carboxymethyl cellulose.This method is to use 85% ethanol for solvent, and sodium hydroxide makees basifier, and monoxone is etherifying agent, and carboxymethyl cellulose is prepared under the conditions of ultrasonic-microwave.As a result show; ultrasonic-microwave method prepares water hyacinth carboxymethyl cellulose and shortens the reaction time; technological operation is simple; make reaction uniform and production cost can be reduced; carboxymethyl cellulose substitution value is made and viscosity is high; utilized for hyacinth resource utilization and provide new developing direction, to realize that the efficient utilizationization of environmental protection and renewable resource has established technical foundation.
Description
Technical field
The present invention relates to carboxymethyl cellulose preparation field technology, refer in particular to a kind of ultrasonic-microwave and prepare water hyacinth carboxylic first
The method of base cellulose.
Background technology
Cellulose is that reserves are most ancient on the earth, reserves most abundant renewable resource, be mainly derived from trees, cotton,
Fiber crops, cereal and some herbaceous plant, are produced by the photosynthesis of plant.It is most valuable that cellulose is generally considered the mankind
Renewable resource, it is with wide material sources, and with biological degradability, biocompatibility and the characteristics of easy derivatization, not only wide
It is general to be applied to weaving, papermaking and timber industry, and by as one of following main industrial chemicals.
Water hyacinth originates in South America, starts to introduce China in 1901.In China, water hyacinth extremely powerful breeding energy
Power and the adaptability body eutrophication to environment so that water hyacinth is bred in streamway madness, in the short time, captures river
Flowing flux, causes river course Severe blockage, influences water transportation, and even floods are triggered when serious.
The dry sample content of cellulose about 18.03% of water hyacinth, content of cellulose enriches.Cellulose is repeated by cellobiose
There are three active hydroxyls on the chain natural organic high-molecular that unit is formed by connecting with Isosorbide-5-Nitrae-β-glycosidic bond, each glucose unit ring
Base, by crystalline phase and noncrystalline staggered is formed；Oh group in wherein noncrystalline phase on most of glucose ring is in
Free state, easily chemically reacts；And substantial amounts of oh group in crystalline phase cellulose, the hydrogen bond of huge number is formd,
" network-like " structure that high-sequential is formd between cellulosic molecule is caused, this structure seriously hinders chemical reagent or biology
The effective contact and effect of enzyme and cellulose surface.
The content of the invention
In view of this, in view of the existing deficiencies of the prior art, its main purpose is to provide a kind of ultrasonic-microwave system to the present invention
The method of standby water hyacinth carboxymethyl cellulose, it can effectively be solved, and cellulose chemistry activity is not strong enough and greatly limitation cellulose should
The problem of using scope.
To achieve the above object, the present invention is using following technical scheme：
A kind of method that ultrasonic-microwave prepares water hyacinth carboxymethyl cellulose, includes following steps：
（1) the plain powder of water hyacinth fibre that 10~20 parts by weight cross 100 mesh sieves is weighed, 5%~10% appropriate alkali soluble is added
Liquid, mixes, 48h is soaked at room temperature；
（2) step（1）The plain suction filtration of the water hyacinth fibre of middle immersion, is washed three times, then suction filtration, then puts with clear water
Dried in 40~60 DEG C of baking oven；
（3) step is weighed（2）The obtained parts by weight of alkalization water hyacinth fibre element 5~10 are added to appropriate organic solvent
In, stir；
（4) appropriate sodium hydrate solid is weighed, 1g/ml NaOH solution is configured to；
（5) under conditions of stirring, by step（4）Obtained sodium hydroxide is added to step（3）Obtained water hyacinth is fine
Quaternization is carried out in dimension element；The ultrasonic min of quaternization 20~40 at 35 DEG C of water-bath；
（6) by step（5）The alkalinized celluloses suction filtration of gained, then adds appropriate 85% ethanol solution；
（7) etherifying reagent of 7~15 parts by weight is added to（6）In the material of gained, under 50~70 DEG C of ultrasonic-microwaves
React 20~40 min；
（8) sodium hydroxide for weighing 1~4.5 parts by weight is added to step（7）In the mixture of gained, at 50~70 DEG C
20~40 min are reacted under ultrasonic-microwave；
（9) by step（8）In material carry out suction filtration, add 85% ethanol washing；
（10) hydrochloric acid of the concentration for 0.1N is added dropwise to step（9）Middle material, to PH=7；Suction filtration, adds 85% alcohol, stirring
Wash 30 min；Same step is repeated once；
（11) by step（10）The carboxymethyl cellulose of gained is placed in 40~60 DEG C of baking ovens and dried.
It is used as a kind of preferred scheme, the step（1）Described aqueous slkali is ammoniacal liquor.
As a kind of preferred scheme, the ultrasonic-microwave frequency is 40 kHz.
It is used as a kind of preferred scheme, the step（3）In organic solvent be 85% ethanol solution.
It is used as a kind of preferred scheme, the step（7）In etherifying reagent be monoxone.
The present invention has clear advantage and beneficial effect compared with prior art, specifically, by above-mentioned technical proposal
Understand：
The present invention uses Ultrasonic Irradiation, with water hyacinth fibre element for raw material, and carrying out chemistry to water hyacinth fibre element changes
Property, by etherification reaction, the hydrogen in glucose molecule chain on active hydroxyl groups is replaced by functional group and is obtained cellulose ether, break
In bad cellulosic molecule and intermolecular very strong hydrogen bond action, improve the dissolubility synthesis carboxymethyl cellulose of cellulose, so
The chemism of water hyacinth fibre element is added, the application of the performance of product, more conducively water hyacinth resource is improved, as a result
Show, ultrasound wave irradiation synthesis technique is simple, reaction speed fast, it is uniform, easily operated to react, and can reduce reaction cost, shortens
Reaction time, business efficiency is considerable, while also achieving the efficient utilization of renewable resource cellulose, synthesizes water hyacinth carboxymethyl
Cellulose is laid a good foundation not only by the water hyacinth utilization of resources for the technical method for solving water hyacinth environmental problem, is made
Standby water hyacinth carboxymethyl cellulose substitution value and viscosity are high, are adapted to industrialized production.
More clearly to illustrate the architectural feature and effect of the present invention, come below in conjunction with the accompanying drawings with specific embodiment to this hair
It is bright to be described in detail.
Brief description of the drawings
The infrared spectrogram of water hyacinth carboxymethyl cellulose prepared by Fig. 1 present invention；
The SEM figures of water hyacinth carboxymethyl cellulose prepared by Fig. 2 present invention.
Embodiment
The present invention discloses a kind of method that ultrasonic-microwave prepares water hyacinth carboxymethyl cellulose, includes following steps：
（1) the plain powder of water hyacinth fibre that 10~20 parts by weight cross 100 mesh sieves is weighed（That is water hyacinth fibre plain powder
Grain graininess is more than 100 mesh）, 5%~10% appropriate aqueous slkali is added, mixes, 48h, described aqueous slkali is soaked at room temperature
It is ammoniacal liquor；
（2) step（1）The plain suction filtration of the water hyacinth fibre of middle immersion, is washed three times, then suction filtration, then puts with clear water
Dried in 40~60 DEG C of baking oven；
（3) step is weighed（2）The obtained parts by weight of alkalization water hyacinth fibre element 5~10 are added to appropriate organic solvent
In, stir, the organic solvent is 85% ethanol solution；
（4) appropriate sodium hydrate solid is weighed, 1g/ml NaOH solution is configured to；
（5) under conditions of stirring, by step（4）Obtained sodium hydroxide is added to step（3）Obtained water hyacinth is fine
Quaternization is carried out in dimension element；The ultrasonic min of quaternization 20~40 at 35 DEG C of water-bath；
（6) by step（5）The alkalinized celluloses suction filtration of gained, then adds appropriate 85% ethanol solution；
（7) etherifying reagent of 7~15 parts by weight is added to（6）In the material of gained, the etherifying reagent is chloroethene
Acid, in reacting 20~40 min under 50~70 DEG C of ultrasonic-microwaves, the ultrasonic-microwave frequency is 40 kHz；
（8) sodium hydroxide for weighing 1~4.5 parts by weight is added to step（7）In the mixture of gained, at 50~70 DEG C
20~40 min are reacted under ultrasonic-microwave, the ultrasonic-microwave frequency is 40 kHz；
（9) by step（8）In material carry out suction filtration, add 85% ethanol washing；
（10) hydrochloric acid of the concentration for 0.1N is added dropwise to step（9）Middle material, to PH=7；Suction filtration, adds 85% alcohol, stirring
Wash 30 min；Same step is repeated once；
（11) by step（10）The carboxymethyl cellulose of gained is placed in 40~60 DEG C of baking ovens and dried.
With specific embodiment, the present invention will be described below.
Embodiment 1
The plain powder of water hyacinth fibre that 10g crosses 100 mesh sieves is weighed in beaker, the ammonia spirits of 400ml 5%, stirring is added
Uniformly 48h is soaked at room temperature.By the water hyacinth fibre element washing suction filtration after processing, in triplicate, 50 DEG C of baking oven is placed in
Middle drying is stand-by.The element of the water hyacinth fibre after the above-mentioned alkalization of 5g is weighed in beaker, 120ml 85% ethanol solution, stirring is added
After uniform, 5ml 1g/ml NaOH solutions are slowly instilled.Beaker is sealed with preservative film, is placed in 40 kHz Ultrasound Instrument anti-
Answer 30 min.After above-mentioned reactant suction filtration, 11g monoxones and appropriate 85% ethanol are added, is placed in again with preservative film sealing
In 40 kHz Ultrasound Instrument, it is warming up to 70 DEG C and continues to react 30 min.1 ml 1g/ml NaOH solutions are then added dropwise in above-mentioned
It is further continued for reacting 30min after mixed liquor.Product suction filtration is taken out, 85% ethanol washing suction filtration is added.The salt that concentration is 0.1N is added dropwise
Acid is neutralized to pH=7 in above-mentioned substance；Use 85% ethanol, the min of agitator treating 30；After same step is repeated once, it will produce
Thing is placed in 50 DEG C of baking ovens and dried, and obtains water hyacinth carboxymethyl cellulose.
Embodiment 2
The plain powder of water hyacinth fibre that 11g crosses 100 mesh sieves is weighed in beaker, the ammonia spirits of 450ml 7%, stirring is added
Uniformly 48h is soaked at room temperature.By the water hyacinth fibre element washing suction filtration after processing, in triplicate, 40 DEG C of baking oven is placed in
Middle drying is stand-by.The element of the water hyacinth fibre after the above-mentioned alkalization of 6g is weighed in beaker, 130ml 85% ethanol solution, stirring is added
After uniform, 6ml 1g/ml NaOH solutions are slowly instilled.Beaker is sealed with preservative film, is placed in 40kHz Ultrasound Instrument anti-
Answer 30min.After above-mentioned reactant suction filtration, 12g monoxones and appropriate 85% ethanol are added, is placed in again with preservative film sealing
In 40kHz Ultrasound Instrument, it is warming up to 70 DEG C and continues to react 30 min.1.5 ml 1g/ml NaOH solutions are then added dropwise in above-mentioned
It is further continued for reacting 30 min after mixed liquor.Product suction filtration is taken out, 85% ethanol washing suction filtration is added.It is 0.1N's that concentration, which is added dropwise,
Hydrochloric acid is neutralized to pH=7 in above-mentioned substance；Use 85% ethanol, the min of agitator treating 30；, will after same step is repeated once
Product is placed in 55 DEG C of baking ovens and dried, and obtains water hyacinth carboxymethyl cellulose.
Embodiment 3
The plain powder of water hyacinth fibre that 13g crosses 100 mesh sieves is weighed in beaker, the ammonia spirits of 500ml 6%, stirring is added
Uniformly 48h is soaked at room temperature.By the water hyacinth fibre element washing suction filtration after processing, in triplicate, 60 DEG C of baking oven is placed in
Middle drying is stand-by.The element of the water hyacinth fibre after the above-mentioned alkalization of 7g is weighed in beaker, 140ml 85% ethanol solution, stirring is added
After uniform, 7ml 1g/ml NaOH solutions are slowly instilled.Beaker is sealed with preservative film, in the Ultrasound Instrument for being placed in 40 kHz
React 30 min.After above-mentioned reactant suction filtration, 14g monoxones and appropriate 85% ethanol are added, juxtaposition is sealed with preservative film again
In 40kHz Ultrasound Instrument, it is warming up to 70 DEG C and continues to react 30 min.2.5 ml 1g/ml NaOH solutions are then added dropwise in upper
State and be further continued for reacting 30 min after mixed liquor.Product suction filtration is taken out, 85% ethanol washing suction filtration is added.Dropwise addition concentration is 0.1N
Hydrochloric acid pH=7 are neutralized in above-mentioned substance；Use 85% ethanol, the min of agitator treating 30；After same step is repeated once,
Product is placed in 50 DEG C of baking ovens and dried, water hyacinth carboxymethyl cellulose is obtained.
Embodiment 4
The plain powder of water hyacinth fibre that 12g crosses 100 mesh sieves is weighed in beaker, the ammonia spirits of 450ml 8%, stirring is added
Uniformly 48h is soaked at room temperature.By the water hyacinth fibre element washing suction filtration after processing, in triplicate, 55 DEG C of baking oven is placed in
Middle drying is stand-by.The element of the water hyacinth fibre after the above-mentioned alkalization of 9g is weighed in beaker, 160ml 85% ethanol solution, stirring is added
After uniform, 9ml 1g/ml NaOH solutions are slowly instilled.Beaker is sealed with preservative film, in the Ultrasound Instrument for being placed in 40 kHz
React 30 min.After above-mentioned reactant suction filtration, 13g monoxones and appropriate 85% ethanol are added, juxtaposition is sealed with preservative film again
In 40kHz Ultrasound Instrument, it is warming up to 70 DEG C and continues to react 30 min.3.5 ml 1g/ml NaOH solutions are then added dropwise in upper
State and be further continued for reacting 30 min after mixed liquor.Product suction filtration is taken out, 85% ethanol washing suction filtration is added.Dropwise addition concentration is 0.1N
Hydrochloric acid pH=7 are neutralized in above-mentioned substance；Use 85% ethanol, the min of agitator treating 30；After same step is repeated once,
Product is placed in 45 DEG C of baking ovens and dried, water hyacinth carboxymethyl cellulose is obtained.
Embodiment 5
The plain powder of water hyacinth fibre that 15g crosses 100 mesh sieves is weighed in beaker, the ammonia spirits of 550ml 10% is added, stirs
Mix and uniformly soak 48h at room temperature.By the water hyacinth fibre element washing suction filtration after processing, in triplicate, 55 DEG C of baking is placed in
Dried in case stand-by.The element of the water hyacinth fibre after the above-mentioned alkalization of 8g is weighed in beaker, 150ml 85% ethanol solution is added, stirs
After mixing uniformly, 8ml 1g/ml NaOH solutions are slowly instilled.Beaker is sealed with preservative film, 40 kHz Ultrasound Instrument is placed in
30 min of middle reaction.After above-mentioned reactant suction filtration, 14g monoxones and appropriate 85% ethanol are added, again with preservative film sealing simultaneously
It is placed in 40kHz Ultrasound Instrument, is warming up to 70 DEG C and continues to react 30 min.Then be added dropwise 4.5 ml 1g/ml NaOH solutions in
It is further continued for reacting 30 min after above-mentioned mixed liquor.Product suction filtration is taken out, 85% ethanol washing suction filtration is added.Concentration, which is added dropwise, is
0.1N hydrochloric acid is neutralized to pH=7 in above-mentioned substance；Use 85% ethanol, the min of agitator treating 30；Same step is repeated once
Afterwards, product is placed in 60 DEG C of baking ovens and dried, obtain water hyacinth carboxymethyl cellulose.
Embodiment 6
The plain powder of water hyacinth fibre that 20g crosses 100 mesh sieves is weighed in beaker, the ammonia spirits of 380ml 5%, stirring is added
Uniformly 48h is soaked at room temperature.By the water hyacinth fibre element washing suction filtration after processing, in triplicate, 40 DEG C of baking oven is placed in
Middle drying is stand-by.The element of the water hyacinth fibre after the above-mentioned alkalization of 5g is weighed in beaker, 160ml 85% ethanol solution, stirring is added
After uniform, 9ml 1g/ml NaOH solutions are slowly instilled.Beaker is sealed with preservative film, in the Ultrasound Instrument for being placed in 40 kHz
React 20 min.After above-mentioned reactant suction filtration, 7g monoxones and appropriate 85% ethanol are added, juxtaposition is sealed with preservative film again
In 40kHz Ultrasound Instrument, it is warming up to 50 DEG C and continues to react 20 min.1 ml 1g/ml NaOH solutions are then added dropwise in above-mentioned
It is further continued for reacting 20 min after mixed liquor.Product suction filtration is taken out, 85% ethanol washing suction filtration is added.It is 0.1N's that concentration, which is added dropwise,
Hydrochloric acid is neutralized to pH=7 in above-mentioned substance；Use 85% ethanol, the min of agitator treating 30；, will after same step is repeated once
Product is placed in 40 DEG C of baking ovens and dried, and obtains water hyacinth carboxymethyl cellulose.
Embodiment 7
The plain powder of water hyacinth fibre that 18g crosses 100 mesh sieves is weighed in beaker, the ammonia spirits of 280ml 10% is added, stirs
Mix and uniformly soak 48h at room temperature.By the water hyacinth fibre element washing suction filtration after processing, in triplicate, 60 DEG C of baking is placed in
Dried in case stand-by.The element of the water hyacinth fibre after the above-mentioned alkalization of 10g is weighed in beaker, 180ml 85% ethanol solution is added,
After stirring, 10ml 1g/ml NaOH solutions are slowly instilled.Beaker is sealed with preservative film, 40 kHz ultrasound is placed in
40 min are reacted in instrument.After above-mentioned reactant suction filtration, 15g monoxones and appropriate 85% ethanol are added, is sealed again with preservative film
It is placed in 40kHz Ultrasound Instrument, is warming up to 70 DEG C and continues to react 40 min.4.5 ml 1g/ml NaOH solutions are then added dropwise
In be further continued for after above-mentioned mixed liquor react 40 min.Product suction filtration is taken out, 85% ethanol washing suction filtration is added.Concentration, which is added dropwise, is
0.1N hydrochloric acid is neutralized to pH=7 in above-mentioned substance；Use 85% ethanol, the min of agitator treating 30；Same step is repeated once
Afterwards, product is placed in 60 DEG C of baking ovens and dried, obtain water hyacinth carboxymethyl cellulose.
Embodiment 8
The plain powder of water hyacinth fibre that 16g crosses 100 mesh sieves is weighed in beaker, the ammonia spirits of 430ml 7.5% is added, stirs
Mix and uniformly soak 48h at room temperature.By the water hyacinth fibre element washing suction filtration after processing, in triplicate, 50 DEG C of baking is placed in
Dried in case stand-by.The element of the water hyacinth fibre after the above-mentioned alkalization of 7.5g is weighed in beaker, 190ml 85% ethanol solution is added,
After stirring, 12ml 1g/ml NaOH solutions are slowly instilled.Beaker is sealed with preservative film, 40 kHz ultrasound is placed in
30 min are reacted in instrument.After above-mentioned reactant suction filtration, 11g monoxones and appropriate 85% ethanol are added, is sealed again with preservative film
It is placed in 40kHz Ultrasound Instrument, is warming up to 60 DEG C and continues to react 30 min.3.5 ml 1g/ml NaOH solutions are then added dropwise
In be further continued for after above-mentioned mixed liquor react 30 min.Product suction filtration is taken out, 85% ethanol washing suction filtration is added.Concentration, which is added dropwise, is
0.1N hydrochloric acid is neutralized to pH=7 in above-mentioned substance；Use 85% ethanol, the min of agitator treating 30；Same step is repeated once
Afterwards, product is placed in 50 DEG C of baking ovens and dried, obtain water hyacinth carboxymethyl cellulose.
Infrared spectrum analysis is carried out to water hyacinth carboxymethyl cellulose obtained above, as shown in figure 1,3446.0cm-1It is
The stretching vibration of hydroxyl-OH on glucose unit ring, 1630.0cm-1And 1418.3cm-1 It is stretching for-C on carboxyl=O- respectively
The symmetric vibration peak of contracting vibration peak and-C-OH, 1102.9cm-1It is the outer-C-O-C- of ring stretching vibration peak, thus can determine that
Water hyacinth carboxymethyl cellulose is made.
Use SEM（SEM）Microcosmic imaging is carried out to water hyacinth carboxymethyl cellulose obtained above, obtained
Obtained SEM figures are as shown in Fig. 2 as shown in Figure 2, obtained its surface roughness of water hyacinth carboxymethyl cellulose increases, instead
Expanded surface area is answered, reactivity is improved.
The technical principle of the present invention is described above in association with specific embodiment.These descriptions are intended merely to explain the present invention's
Principle, and limiting the scope of the invention can not be construed in any way.Based on explanation herein, the technology of this area
Personnel, which would not require any inventive effort, can associate other embodiments of the present invention, and these modes are fallen within
Within protection scope of the present invention.
Claims (3)
1. a kind of method that ultrasonic-microwave prepares water hyacinth carboxymethyl cellulose, it is characterised in that：Include following steps：
（1) the plain powder of water hyacinth fibre that 10~20 parts by weight cross 100 mesh sieves is weighed, 5%~10% appropriate aqueous slkali is added,
Mix, 48h is soaked at room temperature；Described aqueous slkali is ammoniacal liquor；
（2) step（1）The plain suction filtration of the water hyacinth fibre of middle immersion, is washed three times, then suction filtration, is subsequently placed in 40 with clear water
Dried in~60 DEG C of baking oven；
（3) step is weighed（2）The obtained parts by weight of alkalization water hyacinth fibre element 5~10 are added in appropriate organic solvent, are stirred
Mix uniform；
（4) appropriate sodium hydrate solid is weighed, 1g/ml NaOH solution is configured to；
（5) under conditions of stirring, by step（4）Obtained sodium hydroxide is added to step（3）Obtained water hyacinth fibre element
Middle carry out quaternization；The ultrasonic min of quaternization 20~40 at 35 DEG C of water-bath；
（6) by step（5）The alkalinized celluloses suction filtration of gained, then adds appropriate 85% ethanol solution；
（7) etherifying reagent of 7~15 parts by weight is added to（6）In the material of gained, in reaction under 50~70 DEG C of ultrasonic-microwaves
20~40 min；The ultrasonic-microwave frequency is 40 kHz；
（8) sodium hydroxide for weighing 1~4.5 parts by weight is added to step（7）In the mixture of gained, in 50~70 DEG C of ultrasounds
20~40 min are reacted under microwave；The ultrasonic-microwave frequency is 40 kHz；
（9) by step（8）In material carry out suction filtration, add 85% ethanol washing；
（10) hydrochloric acid of the concentration for 0.1N is added dropwise to step（9）Middle material, to pH=7；Suction filtration, adds 85% alcohol, agitator treating
30 min；Same step is repeated once；
（11) by step（10）The carboxymethyl cellulose of gained is placed in 40~60 DEG C of baking ovens and dried.
2. the method that a kind of ultrasonic-microwave according to claim 1 prepares water hyacinth carboxymethyl cellulose, it is characterised in that：
The step（3）In organic solvent be 85% ethanol solution.
3. the method that a kind of ultrasonic-microwave according to claim 1 prepares water hyacinth carboxymethyl cellulose, it is characterised in that：
The step（7）In etherifying reagent be monoxone.
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Inventor after: Tan Zhi Inventor after: Zhan Zhiwei Inventor after: Peng Jinping Inventor after: Li Meimin Inventor after: Lu Yingfang Inventor after: Liu Xiaochao Inventor after: Deng Yiqiu Inventor after: Chen Qiuqiang Inventor after: Li Xiaowei Inventor before: Tan Zhi Inventor before: Peng Jinping Inventor before: Li Meimin Inventor before: Zhan Zhiwei Inventor before: Lu Yingfang Inventor before: Liu Xiaochao Inventor before: Deng Yiqiu Inventor before: Chen Qiuqiang Inventor before: Li Xiaowei |
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Free format text: CORRECT: INVENTOR; FROM: TAN ZHI PENG JINPING LI MEIMIN ZHAN ZHIWEI LU YINGFANG LIU XIAOCHAO DENG YIQIU CHEN QIUQIANG LI XIAOWEI TO: TAN ZHI ZHAN ZHIWEI PENG JINPING LI MEIMIN LU YINGFANG LIU XIAOCHAO DENG YIQIU CHEN QIUQIANG LI XIAOWEI |
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Granted publication date: 20171103 Termination date: 20210310 |