Control method of intermediate phase carbon microball D50 and device for producing intermediate phase carbon microball

A technology of mesophase carbon microspheres and pretreatment devices, which is applied in the direction of carbon preparation/purification, etc., can solve the problems of inconvenient catalyst addition, intense catalytic reaction, and long addition time, so as to reduce production costs, overcome uneven mixing, The effect of improving productivity

Inactive Publication Date: 2012-08-15
天津市贝特瑞新能源材料有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method is inconvenient to add the catalyst, and it takes a long time to add, and due to problems such as agglomeration and agglomeration of the catalyst, uneven mixing of the raw material and the catalyst, and local overheating of the thermal polycondensation reaction, the catalytic reaction is too intense and the mixed liquid spray tank Fire and other safety hazards

Method used

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  • Control method of intermediate phase carbon microball D50 and device for producing intermediate phase carbon microball
  • Control method of intermediate phase carbon microball D50 and device for producing intermediate phase carbon microball
  • Control method of intermediate phase carbon microball D50 and device for producing intermediate phase carbon microball

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] Example 1 Preparation of mesocarbon microspheres

[0056] 12 batches of coal tar pitch from different sources or treatments were selected, and the primary quinoline insoluble matter was tested according to "GB 2293-1980 Coal Pitch Quinoline Insoluble Matter Determination Method".

[0057] Take 400 grams of coal tar pitch from each batch and add them to the reactor, add 5.6 grams of iron oxide, and react for 4 hours at 420°C and 0.6Mpa to prepare the mesophase pellet precursor, and then reduce the mesophase. The precursor body of the ball is carbonized and graphitized to obtain the required D 50 Of mesophase carbon microspheres. Using the laser method and the British Malvern-Mastersizer 2000 laser particle size analyzer to determine its D 50 . The results are shown in Table 1.

[0058] Table 112 Preparation conditions and results of mesophase carbon microspheres from coal pitch

[0059]

[0060] It can be seen from Table 1 that the particle size of mesocarbon microspheres can...

Embodiment 2

[0061] Example 2 Preparation of mesocarbon microspheres and comparative study on the pretreatment effect of catalyst aluminum trichloride

[0062] According to "GB 2293-1980 Coal Pitch Quinoline Insoluble Matter Determination Method", the content of primary quinoline insoluble matter in coal pitch was determined to be 3.7%.

[0063] Open the feeding butterfly valve of the catalyst pretreatment device, add aluminum trichloride from the catalyst feeding bin, add hot water from the water inlet, open the water outlet, and keep the heating temperature of the water bath at 50-100°C. After the catalyst is heated to melt and mix uniformly, pass the metering The system injects the treated aluminum trichloride into the reaction kettle, mixes it evenly with the pitch, and performs thermal polycondensation reaction to prepare mesophase carbon microspheres.

[0064] Similarly, 80-100 kg of the catalyst aluminum trichloride is directly injected into the reaction kettle, and mixed with the pitch f...

Embodiment 3

[0066] Example 3 Study on the preparation of mesocarbon microspheres and the pretreatment effect of the catalyst ferrocene

[0067] According to "GB 2293-1980 Coal Pitch Quinoline Insoluble Matter Determination Method", the content of primary quinoline insoluble matter in coal pitch was determined to be 3.7%.

[0068] Open the feeding butterfly valve of the catalyst pretreatment device, add 80-100kg of catalyst ferrocene from the catalyst feeding bin, add hot water from the water inlet, open the water outlet, keep the heating temperature of the water bath at 50-100°C, and wait until the catalyst is heated to melt and mix evenly , Through the metering system, the treated ferrocene is injected into the reaction kettle to mix it uniformly with the pitch and perform thermal polycondensation reaction to prepare mesocarbon microspheres.

[0069] Similarly, 80-100kg of the catalyst ferrocene is directly injected into the reaction kettle, and mixed with the pitch for thermal polycondensatio...

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Abstract

The invention relates to a method for regulating and controlling the particle size of an intermediate phase carbon microball efficiently. The method is characterized by comprising the following step of regulating the content of primary quinoline insolubles (QI) in raw materials so as to prepare the intermediate phase carbon microball of the required meso-position particle size (D50), wherein the raw materials are selected from any one or the combination of pitch and heavy-weight oil, and the preferably selected pitch is selected from any one or the combination of coal tar, medium-temperature coal tar pitch, secondary coal tar pitch, petroleum pitch, secondary oil heavy weight oil, anthracene oil and polyaromatic hydrocarbon. The invention also relates to complete equipment and a catalyst pretreatment device for preparing the intermediate phase carbon microball. According to the invention, the meso-position particle size of the prepared intermediate phase carbon microball through regulating the content of the primary quinoline insolubles in the raw materials, the D50 of the prepared intermediate phase carbon microball is concentrated, and the yield reduction caused by the subsequent screening can be prevented effectively, thus the yield is high, the production cost is low, and the performances of the intermediate phase carbon microball can be ensured and improved, and the defect of ignition of a mixed liquid spraying tank caused by nonuniform mixing of the catalyst and raw materials, partial overheating, over severe catalyst reaction is overcome, and the complete equipment and the catalyst pretreatment device for preparing the intermediate phase carbon microball have the advantages of simplicity in operation, no dust, low preparation cost, environment pollution prevention and the like.

Description

Technical field [0001] The invention relates to a method for adjusting or controlling the particle size of mesophase carbon microspheres and a device for producing mesophase carbon microspheres. Background technique [0002] The mesocarbon microspheres are a new type of energy storage material with a graphite structure. It has a unique layered structure and excellent lithium ion intercalation-deintercalation performance, good structural stability, compatibility with electrolyte, technical maturity, and high Excellent performance and outstanding advantages such as rate discharge performance and high safety have become the most important anode material for lithium-ion power batteries. The mesocarbon microspheres of different particle sizes have different uses and are directly related to the electrochemical performance of lithium-ion power batteries (including power battery rate, power, or power rate compatibility, etc.). [0003] Existing literature (Power Technology 23(5), 251(1999...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02C01B31/04C01B32/05
Inventor 杨红强苗艳丽李花李福华
Owner 天津市贝特瑞新能源材料有限责任公司
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