CN105860114B - A kind of preparation method of cellulose nano-fibrous solid electrolyte membrane - Google Patents

A kind of preparation method of cellulose nano-fibrous solid electrolyte membrane Download PDF

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CN105860114B
CN105860114B CN201610160523.1A CN201610160523A CN105860114B CN 105860114 B CN105860114 B CN 105860114B CN 201610160523 A CN201610160523 A CN 201610160523A CN 105860114 B CN105860114 B CN 105860114B
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cellulose
enzyme
nano
deionized water
dmoap
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CN105860114A (en
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王许云
王新
王西平
尚君顶
韩田琛
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Qingdao University of Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18—Manufacture of films or sheets
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C9/00—After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
    • D21C9/001—Modification of pulp properties
    • D21C9/002—Modification of pulp properties by chemical means; preparation of dewatered pulp, e.g. in sheet or bulk form, containing special additives
    • D21C9/005—Modification of pulp properties by chemical means; preparation of dewatered pulp, e.g. in sheet or bulk form, containing special additives organic compounds
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/005—Microorganisms or enzymes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M12/00—Hybrid cells; Manufacture thereof
    • H01M12/04—Hybrid cells; Manufacture thereof composed of a half-cell of the fuel-cell type and of a half-cell of the primary-cell type
    • H01M12/06—Hybrid cells; Manufacture thereof composed of a half-cell of the fuel-cell type and of a half-cell of the primary-cell type with one metallic and one gaseous electrode
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
    • C08J2301/02—Cellulose; Modified cellulose
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/16—Applications used for films
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/20—Applications use in electrical or conductive gadgets

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Medicinal Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Polymers & Plastics (AREA)
  • Health & Medical Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Microbiology (AREA)
  • Wood Science & Technology (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Cell Separators (AREA)
  • Primary Cells (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)

Abstract

The present invention relates to a kind of preparation methods of cellulose nano-fibrous solid electrolyte membrane.The paper pulp of disintegration is subjected to prerefining by grinding, refining is mixed with enzyme, carries out enzyme.Enzyme used in enzyme is mannase, the mixture of zytase or the two.Paper pulp after enzyme is cleaned with deionized water, and further grinding prepares cellulose porous nano-fibre.Disperse cellulose nano-fibrous in deionized water, obtains uniform cellulose fibre suspension.With N, N- dimethyl-N-[3- (trimethoxy silicon) propyl] chlorination octadecyl ammonium (DMOAP) is used as precursor.The mixture of cellulose fiber peacekeeping a certain concentration DMOAP methanol solution is stirred at room temperature, and mixture is centrifugated, and removes remaining DMOAP in solid phase with ethyl alcohol and deionized water repeated flushing.It by vacuum filter, dries at room temperature, then vacuum is crosslinked at a certain temperature, and functional fiber element film is made.Functional fiber element film obtained is impregnated in KOH solution, then is cleaned and is impregnated with deionized water, cellulose nano-fibrous solid electrolyte membrane is made.The method of the present invention can prepare that ultra-thin, oversoul is living, hydroxide (OH‑) conductivity is high, storage capacity is strong nano-cellulose dielectric film, it can be applied to preparation lightweight solid electrolyte and portable energy source storage equipment.

Description

A kind of preparation method of cellulose nano-fibrous solid electrolyte membrane
Technical field：
The present invention relates to a kind of preparation methods of cellulose nano-fibrous solid electrolyte membrane, belong to solid electrolyte membrane Preparation and application technical field.
Background technique：
Conventional batteries are due to than cumbersome, by serious in the application of the flexible portable electronic device of specific moulding Challenge.The following battery technology just develops towards thin, flexible with high-energy density direction.Lithium ion relative to completely enclosed system There is unique semi-closed system to make it with height using oxygen as reactant on its air electrode for battery, zinc-air battery The advantages that theoretical energy density and low production cost, safe operation, is expected to become promising in terms of flexible energy storage device Solution.However, most of zinc-air battery technology utilizes alkaline electrolyte so far, be not suitable for being integrated in just Take formula electronic equipment.To realize its flexible Application, being transitioned into the suitable solid electrolyte of shape from liquid electrolyte is urgently to solve Certainly the problem of.Solid electrolyte not only has the function of providing the liquid electrolyte of ionic conduction, but also can prevent electricity as partition Pond internal short-circuit designs and manufactures process so as to greatly simplified battery.
As most sufficient, renewable polymeric materials on the earth, native cellulose fibre is solving future source of energy and environment Vital effect is played in challenge.It is cellulose nano-fibrous have rich in hydroxyl, large specific surface area, high mechanical strength, The particular advantages such as light-weight store equipment and provide possibility for preparation lightweight solid electrolyte and portable energy source.Sufficiently benefit With cellulose nano-fibrous peculiar property, by being functionalized nanofiber surface, and make to send out in functionalized nano-fiber It is born from cross-linking reaction, further enhances the dimensional stability of film, and then develops ultra-thin, good mechanical property, with high-moisture-retention OH- Conductive fiber element nano fibrous membrane.It by improving cellulose nano-fibrous inherent physics and chemical property, answer it can It is used to prepare zinc-air battery lightweight solid electrolyte and portable energy source storage equipment.
Summary of the invention：
It is an object of the invention to overcome conventional liquid electrolytic cell heavy, in the application of portable electronic device by To the shortcomings that serious limitation, develop a kind of green, efficiently, be easy to amplify, can prepare that thin, oversoul is living, hydroxide (OH-) conduction The nano-cellulose dielectric film that rate is high, storage capacity is strong, solid electrolyte membrane and portable energy applied to zinc-air battery Source stores equipment solid electrolyte membrane.
In order to achieve the above-mentioned object of the invention, the preparation side of a kind of cellulose nano-fibrous solid electrolyte membrane of the invention Method operates in accordance with the following steps：
The paper pulp of disintegration is carried out under certain revolving speed prerefining using fiberizer, it is outstanding to obtain uniform slurry by the first step Supernatant liquid；
Second step mixes refining with enzyme, carries out enzyme.Enzyme used in enzyme be mannase, zytase or The mixture of the two.Paper pulp after enzyme is cleaned with deionized water, is subsequently poured into fiberizer, cellulose porous nano is prepared Fiber.
Third step is dispersed with stirring to obtain uniform cellulose fibre suspension in deionized water by cellulose nano-fibrous Liquid.It is 10% by the precursor methanol dilution for preparing functional fiber element nanofiber to concentration, cellulose fiber is then added It ties up in suspension.12h is stirred at room temperature in the mixture of cellulose fiber peacekeeping functionalization presoma, realizes the table of nano-cellulose Face functionalization.
4th step rinses 3~5 removings residual by mixture centrifuge centrifugal treating, and with ethyl alcohol and deionized water DMOAP.
5th step is dried at room temperature for 6~12 hours, then vacuum crosslinking at a certain temperature 20 by vacuum filter ~24 hours obtained functional fiber element films.
6th step, functional fiber element film obtained impregnates to 12 in certain density KOH solution~for 24 hours, then spend Ionized water cleaning and immersion, are made cellulose nano-fibrous solid electrolyte membrane.
Fiberizer described in the method for the present invention first step is PFI fiberizer, prerefining revolving speed be 10000~ 30000rpm。
Certain enzyme used in enzyme described in the method for the present invention second step is mannase, zytase or the two Mixture.
Fiberizer described in the method for the present invention second step is PFI fiberizer, prepares the revolving speed of cellulose porous nano-fibre Higher than 30000rpm.
Functionalization presoma described in the method for the present invention third step is N, N- dimethyl-N-[3- (trimethoxy silicon) propyl] chlorine Change octadecyl ammonium (DMOAP).
Functionalization presoma DMOAP and duplicate Portugal in cellulose fibre in suspension described in the method for the present invention third step The molar ratio of grape sugar unit is 100：1~300:1.
Cross-linking reaction temperature described in the 5th step of the method for the present invention is 40~70 DEG C.
The concentration of KOH solution described in the 6th step of the method for the present invention is 1.0~2.0molL-1。
Specific embodiment：
The method of the present invention is further elaborated combined with specific embodiments below.
Embodiment 1,
The paper pulp of disintegration is carried out under 10000rpm revolving speed prerefining using fiberizer, obtains uniform slurry by the first step Pulp suspension；
Second step mixes refining with mannase, carries out enzyme.Paper pulp after enzyme is cleaned with deionized water, It is subsequently poured into fiberizer, prepares cellulose porous nano-fibre.
Third step is dispersed with stirring to obtain uniform cellulose fibre suspension in deionized water by cellulose nano-fibrous Liquid.It is 10% by the precursor methanol dilution for preparing functional fiber element nanofiber to concentration, cellulose fiber is then added It ties up in suspension.The molar ratio for driving duplicate glucose unit in body DMOAP and cellulose fibre is 100：1.Cellulose fibre 12h is stirred at room temperature with the mixture of functionalization presoma, realizes the surface-functionalized of nano-cellulose.
4th step, by mixture centrifuge centrifugal treating, and it is remaining with ethyl alcohol and deionized water 5 removings of flushing DMOAP。
5th step is dried at room temperature for 12 hours, then vacuum crosslinking is made for 20 hours at 55 DEG C by vacuum filter Functional fiber element film.
6th step, by functional fiber element film obtained in 1.0molL-1KOH solution in impregnate 12h, then spend from Sub- water cleaning and immersion, are made cellulose nano-fibrous solid electrolyte membrane.
Embodiment 2,
The paper pulp of disintegration is carried out under 10000rpm revolving speed prerefining using fiberizer, obtains uniform slurry by the first step Pulp suspension；
Second step mixes refining with zytase, carries out enzyme.Paper pulp after enzyme is cleaned with deionized water, so After pour into fiberizer, prepare cellulose porous nano-fibre.
Third step is dispersed with stirring to obtain uniform cellulose fibre suspension in deionized water by cellulose nano-fibrous Liquid.It is 10% by the precursor methanol dilution for preparing functional fiber element nanofiber to concentration, cellulose fiber is then added It ties up in suspension.The molar ratio for driving duplicate glucose unit in body DMOAP and cellulose fibre is 200：1.Cellulose fibre 12h is stirred at room temperature with the mixture of functionalization presoma, realizes the surface-functionalized of nano-cellulose.
4th step, by mixture centrifuge centrifugal treating, and it is remaining with ethyl alcohol and deionized water 5 removings of flushing DMOAP。
5th step is dried at room temperature for 6 hours, then vacuum is crosslinked 24 hours at certain 60 DEG C by vacuum filter Functional fiber element film is made.
6th step, by functional fiber element film obtained in 1.0molL-1KOH solution in impregnate 12h, then spend from Sub- water cleaning and immersion, are made cellulose nano-fibrous solid electrolyte membrane.
Embodiment 3,
The paper pulp of disintegration is carried out under 10000rpm revolving speed prerefining using fiberizer, obtains uniform slurry by the first step Pulp suspension；
Refining and mass fraction are 1 by second step:1 mannase and zytase mixing, carries out enzyme.By enzyme Paper pulp after change is cleaned with deionized water, is subsequently poured into fiberizer, and cellulose porous nano-fibre is prepared.
Third step is dispersed with stirring to obtain uniform cellulose fibre suspension in deionized water by cellulose nano-fibrous Liquid.It is 10% by the precursor methanol dilution for preparing functional fiber element nanofiber to concentration, cellulose fiber is then added It ties up in suspension.The molar ratio for driving duplicate glucose unit in body DMOAP and cellulose fibre is 300：1.Cellulose fibre 12h is stirred at room temperature with the mixture of functionalization presoma, realizes the surface-functionalized of nano-cellulose.
4th step, by mixture centrifuge centrifugal treating, and it is remaining with ethyl alcohol and deionized water 5 removings of flushing DMOAP。
5th step is dried at room temperature for 6 hours, then vacuum crosslinking is made for 20 hours at 70 DEG C by vacuum filter Functional fiber element film.
6th step, by functional fiber element film obtained in 1.0molL-1KOH solution in impregnate 12h, then spend from Sub- water cleaning and immersion, are made cellulose nano-fibrous solid electrolyte membrane.
Cellulose nano-fibrous solid electrolyte film properties prepared by 1 embodiment of table

Claims (2)

1. a kind of preparation method of cellulose nano-fibrous solid electrolyte membrane, it is characterised in that operate in accordance with the following steps：The The paper pulp of disintegration is carried out at 10000~30000rpm prerefining using PFI fiberizer, it is outstanding to obtain uniform slurry by one step Supernatant liquid；Second step mixes refining with enzyme, carries out enzyme, and enzyme used in enzyme is mannase, zytase or the two Mixture, the paper pulp after enzyme is cleaned with deionized water, be subsequently poured into PFI mill in, be higher than 30000rpm revolving speed system Standby cellulose porous nano-fibre；Third step is dispersed with stirring to obtain uniform fibre in deionized water by cellulose nano-fibrous Cellulose fiber suspension, with N, N- dimethyl-N-[3- (trimethoxy silicon) propyl] chlorination octadecyl ammonium (DMOAP) is as preparation DMOAP precursor methanol dilution to concentration is 10%, fiber is then added by the precursor of functional fiber element nanofiber In cellulosic fiber suspension, 12h is stirred at room temperature in the mixture of cellulose fiber peacekeeping DMOAP；Mixture is centrifuged by the 4th step Machine centrifugal treating, and rinsed 3~5 times with ethyl alcohol and deionized water and remove remaining DMOAP；5th step, by vacuum filter, It dries at room temperature 6~12 hours, then vacuum is crosslinked 20~24 hours obtained functional fiber element films at 40~70 DEG C；6th Step, by functional fiber element film obtained in 1.0~2.0molL-1Impregnate 12 in KOH solution~for 24 hours, then it is clear with deionized water It washes and impregnates, cellulose nano-fibrous solid electrolyte membrane is made.
2. a kind of preparation method of cellulose nano-fibrous solid electrolyte membrane according to claim 1, it is characterised in that The molar ratio of DMOAP and duplicate glucose unit in cellulose is 100 in suspension：1~300:1.
CN201610160523.1A 2016-03-21 2016-03-21 A kind of preparation method of cellulose nano-fibrous solid electrolyte membrane Expired - Fee Related CN105860114B (en)

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CN107808980A (en) * 2017-09-22 2018-03-16 哈尔滨理工大学 A kind of preparation method of the papery lithium ion battery solid electrolyte of high conductivity
CN109411243A (en) * 2018-11-07 2019-03-01 东华理工大学 A kind of flexible solid electrolyte and preparation method thereof

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1331848A (en) * 1998-12-22 2002-01-16 株式会社华仁电池 Microporous solid electrolytes and methods for preparing them
CN1341283A (en) * 1999-02-26 2002-03-20 瑞威殴公司 Solid gel membrane
CN103367712A (en) * 2013-07-26 2013-10-23 合肥国轩高科动力能源股份公司 Preparation method of lithium ion battery coating pole piece
CN104332319A (en) * 2014-10-31 2015-02-04 上海交通大学 Method for manufacturing dye-sensitized solar cell through full screen printing
CN104530452A (en) * 2014-12-10 2015-04-22 南通瑞达电子材料有限公司 Electrolyte membrane applied at high voltage and preparation method of electrolyte membrane
CN104600357A (en) * 2014-12-08 2015-05-06 上海大学 Polymer composite material solid electrolyte and preparation method thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1331848A (en) * 1998-12-22 2002-01-16 株式会社华仁电池 Microporous solid electrolytes and methods for preparing them
CN1341283A (en) * 1999-02-26 2002-03-20 瑞威殴公司 Solid gel membrane
CN103367712A (en) * 2013-07-26 2013-10-23 合肥国轩高科动力能源股份公司 Preparation method of lithium ion battery coating pole piece
CN104332319A (en) * 2014-10-31 2015-02-04 上海交通大学 Method for manufacturing dye-sensitized solar cell through full screen printing
CN104600357A (en) * 2014-12-08 2015-05-06 上海大学 Polymer composite material solid electrolyte and preparation method thereof
CN104530452A (en) * 2014-12-10 2015-04-22 南通瑞达电子材料有限公司 Electrolyte membrane applied at high voltage and preparation method of electrolyte membrane

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