CN104916845A - Method for producing siloxane by modifying surface of carbon black - Google Patents
Method for producing siloxane by modifying surface of carbon black Download PDFInfo
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- CN104916845A CN104916845A CN201510375083.7A CN201510375083A CN104916845A CN 104916845 A CN104916845 A CN 104916845A CN 201510375083 A CN201510375083 A CN 201510375083A CN 104916845 A CN104916845 A CN 104916845A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a method for producing siloxane by modifying the surface of carbon black. A lithium ion battery conductive agent with good stability and conductivity is prepared. The method disclosed by the invention comprises the following steps: adding tetrahydrofuran and the carbon black into a reactor, wherein the mass ratio of the carbon black to tetrahydrofuran is 1 to 4.4; adding diethylamine and trimethylchlorosilane into the reactor, wherein the mass ratio of trimethylchlorosilane to diethylamine is 6 to 1; sealing the reactor; reacting for 20-24 hours under the stirring of a rotor of a magnetic stirrer: carrying out suction filtration and drying on a reaction product to obtain a siloxane product; and detecting the siloxane product by adopting an infrared spectrometer. According to the method disclosed by the invention, hydroxyls on the surface of the carbon black can react with trimethylchlorosilane to form siloxane; and the structure property of the carbon black is improved and the space steric hindrance of silicon atoms is also improved.
Description
Technical field
The present invention relates to the method with production of carbon black silicon ether, particularly a kind of carrying out carbon blacksurface modifies the method for producing silicon ether.
Background technology
In recent years, face the day by day exhausted of the non-renewable energy resources such as oil, research and development and the utilization of clean energy resource and regenerative resource have caused the extensive attention of various countries.Lithium ion battery is high owing to having operating voltage, quality is light, specific energy is large, self discharge is little, have extended cycle life, memory-less effect, the outstanding advantages such as non-environmental-pollution, becoming the ideal source of the electronic installation miniaturization ands such as video camera, mobile phone, notebook computer and portable surveying instrument, is also the first-selected power supply of future automobile high-energy power battery.In lithium battery preparation process, improving the electron conduction of electrode pad by adding conductive agent, reducing the internal resistance of cell, improving lithium ionic mobility.Therefore conductive agent is indispensable composition in lithium ion battery cathode, optimum conductive agent is selected to be ensure that battery has the key factor of superior performance.Wherein, carbon black is conventional lithium ion battery conductive agent, but carbon black in process of production, and surface often forms hydroxyl, carboxyl isoreactivity oxygen-containing functional group, and the existence of these functional groups affects the storage lithium function of carbon black.It is reported, Si-O-C material has higher reversible capacity and good cycle performance.The earliest C/Si-O-C amorphous materials is applied to lithium ion battery negative material be Canadian Dalhousie University Dahn professor.Professor Dahn thinks, C/Si-O-C amorphous materials both can keep the high power capacity of Si, the ductility of carbon can be utilized again to keep the integrality of silicon structure, thus prepare the Si/C negative material that reversible capacity is higher, do not have discharge and recharge hysteresis.Therefore silicon atom is introduced carbon blacksurface, form Si-O-C amorphous materials and become the important topic of carbon black in electrode material application.
Recently, article " finishing of carbon black and the impact on carbon black/silicon rubber heat conductivility thereof " on the Li Qiuying of East China University of Science etc. are published in " composite material " the 5th phase in 2012, report and with hydroxy silicon oil, carbon blacksurface is modified, import Liao Gui ether functional group on the surface of carbon black.Carbon black after silicone oil is modified, except improving the compatibility between rubber, also has good thermal conductivity.This method uses the unstable reagent that the reactivities such as thionyl chloride are strong, refines by methods such as toluene extractings to the carbon black after modification simultaneously.In addition, article " modified carbon black is on the impact of composite material dielectric property " one literary composition on the Zhang Enhe of University Of Nanhua etc. are published in " applied chemistry " the 1st phase in 2014, by silane coupler, carbon black is modified, also Liao Gui ether functional group is imported on the surface of carbon black, while improving carbon black compatibility, improve its surface dielectric constant.But above-mentioned two kinds of methods also exist certain limitation in the selection expanding the silicone functionalities that silicon is modified, and-OSi-key also exists again the problems such as the stability in air, the application of rear carbon black in actual electrode material is produced is modified in impact.According to the space stability ultimate load mechanism that Ortega-Vinuesa J proposes, make can not to continue each other between particle close by the have living space silicon atom of steric hindrance of lead-in zone on carbon black particle, thus the stability in the air of-OSi-key after modification while keeping its dispersion stabilization, can be improved again.Therefore, by the silicon modification reaction to carbon blacksurface carboxyl and hydroxyl, can improve and modify the practical application of rear carbon black as electrode material.
Summary of the invention
The invention provides a kind of carbon blacksurface is carried out and modify the method for producing silicon ether, prepare the lithium ion battery conductive agent of stability and the conductivity had.
Provided by the inventionly a kind ofly carbon blacksurface carried out modifying the method for producing silicon ether comprise the following steps:
A. under normal temperature, the rotor of magnetic stirring apparatus is inserted in reactor, and open magnetic stirring apparatus switch;
B. oxolane and carbon black are joined in reactor, carbon black be 1:4.4 with the mass ratio of oxolane;
C. add diethylamine and trim,ethylchlorosilane more in the reactor, the mass ratio of trim,ethylchlorosilane and diethylamine is 6:1, and reactor seals, and under the rotor of magnetic stirring apparatus stirs, react 20-24 hour, reaction equation is:
D. reaction product vacuum filtration is dry, obtain silicon ether product;
E. adopt infrared spectrometer to detect silicon ether product, silicon ether product is at wave number 2924 and 1110cm
-1characteristic peak correspond respectively to-CH
2-and the stretching vibration peak of Si-O-C, show in the modified carbon black successful grafting in surface silicon atom.
The present invention is compared with existing similar technique, its significantly beneficial effect be embodied in: under normal temperature condition of the present invention, adopt organic chemical reactions method, by carbon black and trim,ethylchlorosilane, surface chemical reaction is there is in tetrahydrofuran solvent, carbon blacksurface hydroxyl and trim,ethylchlorosilane are reacted and forms silicon ether, to also improve while carbon black structure on silicon atom sterically hindered improving.
Accompanying drawing explanation
Fig. 1 is that a kind of carrying out carbon blacksurface modifies the process chart producing silicon ether.
Fig. 2 is the infrared spectrum characterization figure of silicon ether.
Embodiment
Below in conjunction with accompanying drawing, for laboratory room small-sized production, the present invention is described in further detail.
As shown in Figure 1, a kind of step of carrying out modifying the method for producing silicon ether to carbon blacksurface is as follows:
A., under normal temperature, the rotor of magnetic stirring apparatus is inserted in conical flask, then conical flask is placed on magnetic stirring apparatus, and open whip switch;
B. weighing 66.5g oxolane joins in conical flask, joins in tetrahydrofuran solution by 15g carbon black (N330);
C. in conical flask, add 0.32g diethylamine again, 1.95g trim,ethylchlorosilane, then seals, and under the rotor of magnetic stirring apparatus stirs, react 20-24 hour, reaction equation is:
D. reaction product is dry through vacuum filtration, obtains silicon ether product;
E. adopt infrared spectrometer to detect silicon ether product, as shown in Figure 2, silicon ether product is at wave number 2924 and 1110cm
-1characteristic peak correspond respectively to-CH
2-and the stretching vibration peak of Si-O-C, show in the modified carbon black successful grafting in surface silicon atom.
Claims (1)
1. carry out modifying a method of producing silicon ether to carbon blacksurface, it is characterized in that the method comprises the following steps:
A. under normal temperature, the rotor of magnetic stirring apparatus is inserted in reactor, and open magnetic stirring apparatus switch;
B. oxolane and carbon black are joined in reactor, carbon black be 1:4.4 with the mass ratio of oxolane;
C. add diethylamine and trim,ethylchlorosilane more in the reactor, the mass ratio of trim,ethylchlorosilane and diethylamine is 6:1, and reactor seals, and under the rotor of magnetic stirring apparatus stirs, react 20-24 hour, reaction equation is:
D. reaction product vacuum filtration is dry, obtain silicon ether product;
E. adopt infrared spectrometer to detect silicon ether product, silicon ether product is at wave number 2924 and 1110cm
-1characteristic peak correspond respectively to-CH
2-and the stretching vibration peak of Si-O-C, show in the modified carbon black successful grafting in surface silicon atom.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510375083.7A CN104916845A (en) | 2015-06-30 | 2015-06-30 | Method for producing siloxane by modifying surface of carbon black |
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| CN201510375083.7A CN104916845A (en) | 2015-06-30 | 2015-06-30 | Method for producing siloxane by modifying surface of carbon black |
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| CN104916845A true CN104916845A (en) | 2015-09-16 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108649225A (en) * | 2018-05-16 | 2018-10-12 | 辽宁科技大学 | The method that organic sulfur modification prepares lithium ion carbon negative pole material is carried out to carbon blacksurface |
| CN111525107A (en) * | 2020-04-20 | 2020-08-11 | 南昌大学 | Novel synthesis method of organic micromolecule coated silicon negative electrode material |
| CN112436146A (en) * | 2020-11-20 | 2021-03-02 | 安徽南都华拓新能源科技有限公司 | Lithium battery positive electrode material, preparation method and lithium battery |
| CN112467063A (en) * | 2020-11-10 | 2021-03-09 | 南昌大学 | Preparation method of silicon-based negative electrode plate of lithium ion battery |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1693375A (en) * | 2005-04-28 | 2005-11-09 | 浙江野马电池有限公司 | Surface-modified carbon black powder, preparation method thereof and application thereof in alkaline zinc-manganese battery |
| KR20080025434A (en) * | 2006-09-18 | 2008-03-21 | 주식회사 엘지화학 | Conductive agent for surface treatment for hydrophobic property and secondary battery containing the same |
-
2015
- 2015-06-30 CN CN201510375083.7A patent/CN104916845A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1693375A (en) * | 2005-04-28 | 2005-11-09 | 浙江野马电池有限公司 | Surface-modified carbon black powder, preparation method thereof and application thereof in alkaline zinc-manganese battery |
| KR20080025434A (en) * | 2006-09-18 | 2008-03-21 | 주식회사 엘지화학 | Conductive agent for surface treatment for hydrophobic property and secondary battery containing the same |
Non-Patent Citations (1)
| Title |
|---|
| 刘亚莉 等: "《聚合物改性炭黑的研究进展》", 《现代化工》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108649225A (en) * | 2018-05-16 | 2018-10-12 | 辽宁科技大学 | The method that organic sulfur modification prepares lithium ion carbon negative pole material is carried out to carbon blacksurface |
| CN108649225B (en) * | 2018-05-16 | 2021-01-05 | 辽宁科技大学 | Method for preparing lithium ion carbon negative electrode material by carrying out organic sulfur modification on carbon black surface |
| CN111525107A (en) * | 2020-04-20 | 2020-08-11 | 南昌大学 | Novel synthesis method of organic micromolecule coated silicon negative electrode material |
| CN111525107B (en) * | 2020-04-20 | 2022-06-14 | 南昌大学 | Novel synthesis method of organic micromolecule coated silicon negative electrode material |
| CN112467063A (en) * | 2020-11-10 | 2021-03-09 | 南昌大学 | Preparation method of silicon-based negative electrode plate of lithium ion battery |
| CN112436146A (en) * | 2020-11-20 | 2021-03-02 | 安徽南都华拓新能源科技有限公司 | Lithium battery positive electrode material, preparation method and lithium battery |
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Application publication date: 20150916 |