CN111434606A - Micro mixer and preparation method of hollow carbon spheres for lithium battery material - Google Patents

Micro mixer and preparation method of hollow carbon spheres for lithium battery material Download PDF

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Publication number
CN111434606A
CN111434606A CN201910034766.4A CN201910034766A CN111434606A CN 111434606 A CN111434606 A CN 111434606A CN 201910034766 A CN201910034766 A CN 201910034766A CN 111434606 A CN111434606 A CN 111434606A
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CN
China
Prior art keywords
spring type
type pipeline
fluid
rotating spring
micromixer according
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Pending
Application number
CN201910034766.4A
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Chinese (zh)
Inventor
李娟�
徐冬阳
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Chengdu Yinlong New Energy Co ltd
Yinlong New Energy Co Ltd
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Chengdu Yinlong New Energy Co ltd
Yinlong New Energy Co Ltd
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Application filed by Chengdu Yinlong New Energy Co ltd, Yinlong New Energy Co Ltd filed Critical Chengdu Yinlong New Energy Co ltd
Priority to CN201910034766.4A priority Critical patent/CN111434606A/en
Publication of CN111434606A publication Critical patent/CN111434606A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/05Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/40Static mixers
    • B01F25/42Static mixers in which the mixing is affected by moving the components jointly in changing directions, e.g. in tubes provided with baffles or obstructions
    • B01F25/43Mixing tubes, e.g. wherein the material is moved in a radial or partly reversed direction
    • B01F25/433Mixing tubes wherein the shape of the tube influences the mixing, e.g. mixing tubes with varying cross-section or provided with inwardly extending profiles
    • B01F25/4331Mixers with bended, curved, coiled, wounded mixing tubes or comprising elements for bending the flow
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/40Static mixers
    • B01F25/42Static mixers in which the mixing is affected by moving the components jointly in changing directions, e.g. in tubes provided with baffles or obstructions
    • B01F25/43Mixing tubes, e.g. wherein the material is moved in a radial or partly reversed direction
    • B01F25/433Mixing tubes wherein the shape of the tube influences the mixing, e.g. mixing tubes with varying cross-section or provided with inwardly extending profiles
    • B01F25/4334Mixers with a converging cross-section
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F33/00Other mixers; Mixing plants; Combinations of mixers
    • B01F33/30Micromixers

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Dispersion Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention relates to a micro mixer which comprises a rotary spring type pipeline, wherein two liquid injection pipes are arranged at the inlet of the rotary spring type pipeline, and a plurality of blocking structural members are arranged on the inner wall of the rotary spring type pipeline. A preparation method of hollow carbon spheres for a lithium battery material comprises the steps of dissolving silicon dioxide microspheres in a mixed solution to obtain a fluid A; mixing resorcinol and formaldehyde and dissolving in water to obtain a fluid B; respectively injecting the fluid A and the fluid B into the rotating spring type pipeline through two liquid injection pipes; an ultraviolet emission source is arranged at an outlet of the rotating spring type pipeline, and resorcinol and formaldehyde in the mixed liquid flowing through the outlet of the rotating spring type pipeline are promoted to be condensed by ultraviolet irradiation to form gel; sintering the gel to obtain a sintered sample; and cleaning the sintered sample, and removing silicon dioxide to obtain the hollow carbon spheres. The size of the micro mixer is shortened, the mixing time is reduced, and the mixing uniformity of the multiphase flow is improved.

Description

Micro mixer and preparation method of hollow carbon spheres for lithium battery material
Technical Field
The invention relates to the field of lithium batteries, in particular to a micro mixer and a preparation method of hollow carbon spheres for a lithium battery material.
Background
The preparation process of the material in the lithium battery industry needs to uniformly mix all phase substances so as to obtain the nano material with uniform size, a micro mixer is usually used in the mixing process, at present, the commonly used micro mixer adopts a parallel lamination mixer to mix two-phase flow or multi-phase flow in the horizontal direction, the two-phase flow or the multi-phase flow is in parallel flow at the initial stage of mixing, and the multi-phase flow can only be subjected to micro mixing through molecular diffusion due to the fact that a micro channel structure does not have a special blocking structure, and the condition of uneven mixing exists.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a micro mixer and a preparation method of hollow carbon spheres for lithium battery materials, so as to overcome the defects in the prior art.
The technical scheme for solving the technical problems is as follows: a micro mixer comprises a rotary spring type pipeline, at least two liquid injection pipes communicated with an inlet of the rotary spring type pipeline are arranged at the inlet of the rotary spring type pipeline, and a plurality of blocking structural members are arranged on the inner wall of the rotary spring type pipeline.
The invention has the beneficial effects that: through the rotating spring type pipeline and the blocking structural parts additionally arranged in the pipeline, the turbulent flow condition of fluid in the pipeline can be further improved, the size of a micro mixer is shortened, the mixing time is shortened, and the mixing uniformity of multiphase flow is improved.
On the basis of the technical scheme, the invention can be further improved as follows.
Further, hinder the structure and include first hindrance board and second and hinder the board, first hindrance board and second hinder the board and stagger arrangement from top to bottom, and have the interval in the extending direction of swivel spring formula pipeline.
Further, the projection of the first hindering plate in the hindering structure part along the extending direction of the rotating spring type pipeline does not intersect with the projection of the second hindering plate along the extending direction of the rotating spring type pipeline.
Further, the interval between first hindrance board and the second in hindering the structure is 50um-500 um.
Further, the inner diameter of the rotating spring type pipeline is 50-500 μm.
Furthermore, the inlet structure of the liquid injection pipe is a longitudinal lamination type.
Adopt above-mentioned further beneficial effect to do: can effectively utilize the density difference of the molecular diffusion.
Furthermore, the rotating spring type pipeline and all the liquid injection pipes form a U-shaped, Y-shaped, T-shaped or mixed structure together.
Furthermore, the rotating spring type pipeline is made of transparent materials.
Further, the rotating spring type pipeline is made of glass.
Adopt above-mentioned further beneficial effect to do: facilitating observation of the mixing process.
A preparation method of hollow carbon spheres for a lithium battery material comprises the following steps:
s100, dissolving the silicon dioxide microspheres in the mixed solution to obtain a fluid A for later use;
s200, mixing resorcinol and formaldehyde and dissolving in water to obtain a fluid B for later use;
s300, injecting the fluid A and the fluid B into the rotating spring type pipeline through two liquid injection pipes at the same speed respectively;
s400, arranging an ultraviolet emission source at an outlet of the rotary spring type pipeline, and performing ultraviolet irradiation to promote condensation polymerization of resorcinol and formaldehyde in the mixed liquid flowing through the outlet of the rotary spring type pipeline to form gel;
s500, sintering the gel to obtain a sintered sample;
s600, cleaning the sintered sample, and removing silicon dioxide to obtain the hollow carbon sphere.
Adopt above-mentioned further beneficial effect to do: is beneficial to synthesizing hollow carbon spheres with uniform size.
Drawings
FIG. 1 is a schematic structural diagram of a micro mixer according to the present invention;
FIG. 2 is a schematic view of a partial structure of the coil spring type pipe of the present invention;
FIG. 3 is a cross-sectional view of FIG. 2;
FIG. 4 is a TEM image of hollow carbon spheres prepared according to the present invention;
FIG. 5 is an SEM image of hollow carbon spheres prepared according to the present invention;
FIG. 6 is a Raman image of hollow carbon spheres prepared according to the present invention.
Detailed Description
The principles and features of this invention are described below in conjunction with the following drawings, which are set forth by way of illustration only and are not intended to limit the scope of the invention.
As shown in figures 1, 2 and 3, the micromixer comprises a rotating spring type pipeline 1, at least two liquid injection pipes 2 communicated with the inlet of the rotating spring type pipeline 1 are arranged at the inlet of the rotating spring type pipeline 1, in the invention, only two fluids are required to be injected when the micromixer is used for preparing the hollow carbon spheres in the later period, therefore, the number of the liquid injection pipes 2 can be only two, and the number of the liquid injection pipes 2 can be three, four, five, six and the like under different conditions, and in addition, a plurality of obstruction structural members 110 are arranged on the inner wall of the rotating spring type pipeline 1. The coil spring type pipe 1 is made of transparent material, such as glass.
The two liquid injection pipes 2 are connected with the rotating spring type pipeline 1 to form a U shape, certainly a Y shape or a T shape, the inner diameters of the rotating spring type pipeline 1 and the liquid injection pipes 2 are 50-500 μm, and specifically can be 50um, 80um, 100um, 150um, 170um, 210um, 260um or 300 um.
The blocking structure 110 comprises a first blocking plate 111 and a second blocking plate 112, the first blocking plate 111 and the second blocking plate 112 are arranged in a staggered manner up and down, and are spaced in the extending direction of the rotary spring type pipeline 1, and the projection of the first blocking plate 111 in the extending direction of the rotary spring type pipeline 1 in the blocking structure 110 does not intersect with the projection of the second blocking plate 112 in the extending direction of the rotary spring type pipeline 1, as shown in fig. 3; the interval between the first hindering plate 111 and the second hindering plate 112 in the same hindering structure 110 is 50um-500um, specifically can be 50um, 80um, 100um, 150um, 170um, 210um, 260um or 300 um.
The inlet structure of the liquid injection pipe 2 is a longitudinal lamination type.
The micro mixer pipeline can also be arranged in a slotted structure in the flat plate.
As shown in fig. 4, 5 and 6, a method for preparing hollow carbon spheres for a lithium battery material using the micromixer includes the steps of:
s100, dissolving the silicon dioxide microspheres in the mixed solution to obtain a fluid A for later use;
s200, mixing resorcinol and formaldehyde and dissolving in water to obtain a fluid B for later use;
s300, injecting the fluid A and the fluid B into the rotary spring type pipeline 1 through the two liquid injection pipes 2 at the same speed respectively;
s400, arranging an ultraviolet emission source at an outlet of the rotary spring type pipeline 1, and performing ultraviolet irradiation to promote condensation polymerization of resorcinol and formaldehyde in the mixed liquid flowing through the outlet of the rotary spring type pipeline 1 to form gel;
s500, sintering the gel to obtain a sintered sample;
s600, cleaning the sintered sample, and removing silicon dioxide to obtain the hollow carbon sphere.
Application example:
a method for preparing hollow carbon spheres for a lithium battery material by using the micromixer comprises the following steps:
s100, dissolving 1.2g of silica microspheres prepared by a template method in 30ml of mixed solution to obtain a fluid A for later use;
s200, mixing resorcinol and formaldehyde according to a molar ratio of 1:2, and dissolving the mixture obtained after mixing in water to form a water sample with a solute content of 10% to obtain a fluid B for later use;
s300, respectively injecting the fluid A and the fluid B into the rotary spring type pipeline 1 through two liquid injection pipes 2 by using a syringe pump at the same speed, wherein the inner diameters of the two liquid injection pipes 2 and the rotary spring type pipeline 1 are 100 mu m, the injection speed is 0.1-10mm/S, actually 0.1mm/S, 0.8mm/S, 1mm/S, 2.6mm/S, 3.5mm/S, 5.8mm/S, 7.5mm/S, 9mm/S or 10mm/S, and good mixing is achieved through the rotary spring type pipeline 1 according to the characteristics of the fluid A and the fluid B and the inner diameters of the liquid injection pipes 2 and the rotary spring type pipeline 1, wherein the injection speed is preferably 1 mm/S;
s400, arranging an ultraviolet emission source at an outlet of the rotary spring type pipeline 1, and performing ultraviolet irradiation to promote condensation polymerization of resorcinol and formaldehyde in the mixed liquid flowing through the outlet of the rotary spring type pipeline 1 to form gel;
s500, sintering the gel at 1500 ℃ to obtain a sintered sample;
s600, cleaning the sintered sample by using hydrofluoric acid, and removing silicon dioxide to obtain the hollow carbon sphere.
Micro-mixing and coupling with a gel method can prepare solid carbon spheres;
in the gel method, the gel can be organic matters such as resorcinol and formaldehyde which can be subjected to dehydration or alcohol loss condensation polymerization so as to synthesize carbon sources such as phenolic resin and epoxy resin.
Solid carbon spheres can be prepared by coupling micro-mixing with a hydrothermal method;
in the hydrothermal method, the carbon source can be petroleum asphalt, coal asphalt, sucrose, glucose, starch, cellulose, sodium citrate, phenolic resin, epoxy resin and other organic carbon sources.
Micro-mixing and template method coupling can prepare hollow carbon spheres;
the template can be an organic template such as Polystyrene (PS), polymethyl methacrylate (PMMA) and the like, or an inorganic template such as SiO2, MnO and the like.
Micro-mixing may be coupled with vapor deposition.
Can be used for the carbon coating process of the anode nano material;
the nano material comprises lithium iron phosphate, metal oxide, metal sulfide and other lithium battery anode materials.
Fluid: can be gas, liquid or gas-liquid-solid two-phase mixture.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.

Claims (10)

1. The micro mixer is characterized by comprising a rotating spring type pipeline (1), wherein at least two liquid injection pipes (2) communicated with an inlet of the rotating spring type pipeline (1) are arranged at the inlet of the rotating spring type pipeline (1), and a plurality of blocking structural members (110) are arranged on the inner wall of the rotating spring type pipeline (1).
2. A micromixer according to claim 1, characterized in that said blocking structure (110) comprises a first (111) and a second (112) blocking plate, said first (111) and second (112) blocking plates being staggered one above the other and spaced in the direction of extension of said rotating spring duct (1).
3. A micromixer according to claim 2, characterized in that the projection of the first blocking plate (111) in the blocking structure (110) in the direction of extension of the coil spring duct (1) does not intersect the projection of the second blocking plate (112) in the direction of extension of the coil spring duct (1).
4. A micromixer according to claim 3, characterized in that the distance between the first barrier plate (111) and the second barrier plate (112) in the barrier structure (110) is 50-500 um.
5. Micromixer according to claim 4, characterized in that the internal diameter of the rotating spring-loaded conduit (1) is 50-500 μm.
6. A micromixer according to claim 1, characterized in that the inlet structure of the injection pipe (2) is of the longitudinal lamination type.
7. The micromixer according to claim 1, characterized in that said coil spring type pipe (1) and all said injection pipes (2) together form a U-shaped, Y-shaped, T-shaped or a hybrid structure thereof.
8. Micromixer according to any of claims 1 to 7, characterized in that the rotating spring-type duct (1) is made of transparent material.
9. Micromixer according to claim 8, characterized in that the rotating spring-type pipe (1) is made of glass.
10. A method for preparing hollow carbon spheres for lithium battery materials, characterized in that a micromixer according to any one of claims 1 to 9 is used, the method comprising the following steps:
s100, dissolving the silicon dioxide microspheres in the mixed solution to obtain a fluid A for later use;
s200, mixing resorcinol and formaldehyde and dissolving in water to obtain a fluid B for later use;
s300, injecting the fluid A and the fluid B into the rotary spring type pipeline (1) through two liquid injection pipes (2) at the same speed respectively;
s400, arranging an ultraviolet emission source at an outlet of the rotary spring type pipeline (1), and irradiating by ultraviolet light to promote condensation polymerization of resorcinol and formaldehyde in the mixed liquid flowing through the outlet of the rotary spring type pipeline (1) to form gel;
s500, sintering the gel to obtain a sintered sample;
s600, cleaning the sintered sample, and removing silicon dioxide to obtain the hollow carbon sphere.
CN201910034766.4A 2019-01-15 2019-01-15 Micro mixer and preparation method of hollow carbon spheres for lithium battery material Pending CN111434606A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113499744A (en) * 2021-07-07 2021-10-15 山东泰和水处理科技股份有限公司 Micro-channel reactor manufactured based on 3D printer technology

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CN104828803A (en) * 2015-03-23 2015-08-12 山东省科学院能源研究所 A preparing method of a monodisperse phenolic resin carbon microbead
CN105776180A (en) * 2016-04-21 2016-07-20 南京理工大学 Preparation method for porous carbon nanospheres
CN106006600A (en) * 2016-05-12 2016-10-12 南京工业大学 Preparation method of nitrogen-doped carbon spheres with different morphologies

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Publication number Priority date Publication date Assignee Title
CN102974255A (en) * 2012-10-31 2013-03-20 中国科学院过程工程研究所 Passive spiral micro-structural mixing unit and application thereof
US20140120031A1 (en) * 2012-10-31 2014-05-01 Nanjing Jiuzhang Chemical Technology Co., Ltd Passive spiral micromixer and its applications
CN104828803A (en) * 2015-03-23 2015-08-12 山东省科学院能源研究所 A preparing method of a monodisperse phenolic resin carbon microbead
CN105776180A (en) * 2016-04-21 2016-07-20 南京理工大学 Preparation method for porous carbon nanospheres
CN106006600A (en) * 2016-05-12 2016-10-12 南京工业大学 Preparation method of nitrogen-doped carbon spheres with different morphologies

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113499744A (en) * 2021-07-07 2021-10-15 山东泰和水处理科技股份有限公司 Micro-channel reactor manufactured based on 3D printer technology

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Application publication date: 20200721