CN102849720A - A method for preparing mesocarbon microbeads by tubular continuous reaction - Google Patents
A method for preparing mesocarbon microbeads by tubular continuous reaction Download PDFInfo
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- CN102849720A CN102849720A CN2011101774877A CN201110177487A CN102849720A CN 102849720 A CN102849720 A CN 102849720A CN 2011101774877 A CN2011101774877 A CN 2011101774877A CN 201110177487 A CN201110177487 A CN 201110177487A CN 102849720 A CN102849720 A CN 102849720A
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- tube furnace
- mcmb
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
- Y02P20/129—Energy recovery, e.g. by cogeneration, H2recovery or pressure recovery turbines
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Abstract
The invention relates to a method for preparing mesocarbon microbeads by tubular continuous reaction. The method is continuous production process, and the disadvantages of the convenient single-kettle intermittent production for mesocarbon microbeads, such as low efficiency and low product stability, can be solved through the method; and the mode by substituting the reaction kettle with a tubular furnace for direct heating improves the conduction thermal efficiency of the product, and the waste heat is recovered to preheat the raw material asphalt, to increase the heat energy utilization rate and reduce the energy consumption. Its technical proposal adopts the tubular furnace heating mode, substitutes the reaction kettle with the tubular furnace tube, and controls the reaction extent through controlling the residence time of the materials in the tubular furnace and the temperature, to prepare qualified mesocarbon microbeads.
Description
Affiliated technical field:
The present invention relates to the preparation method that the lithium ion battery negative material MCMB is produced, particularly use tube furnace tubular type heating serialization to prepare the method for MCMB.
Background technology:
The preparation method of MCMB generally adopts single still batch production mode to produce, its inefficiency, and production capacity is little.In its preparation process heating material is adopted directly the reactor heating, material thermal conduction is slow, and heat energy can't effectively utilize, and thermo-efficiency is low, and energy consumption is high.
Summary of the invention:
The object of the invention provides the method that a kind of serialization prepares MCMB, by adopting the diamond heating mode, with tube furnace boiler tube surrogate response still, reach the control extent of reaction by control material index such as retention time, temperature in tube furnace, prepare qualified MCMB.Solved the purpose that efficient is low, product stability is poor of single still batch production by this method; Use simultaneously the direct-fired mode of tube furnace surrogate response still to improve the thermo-efficiency of product conduction, recovery waste heat is used for preheating material pitch, has increased the utilization ratio of heat energy, has reduced energy consumption.
Technical scheme of the present invention is: serialization prepares MCMB, adopts the tube furnace reaction to substitute single still reaction.Its process flow is followed successively by pitch to carry out interchanger preheating, pitch catalysis, pitch diamond heating, the cracking of pitch diamond heating and polymerize MCMB, the cooling of product interchanger, product thermal separation and go out MCMB.
Said interchanger is in the operation: interchanger is the cooling that same interchanger is used for pitch preheating and last material.
Said tube furnace is in the operation: tube furnace is heating installation, adopts coal gas, Sweet natural gas or oil fuel to be the heating material; Boiler tube is arranged the snakelike arranged in series mode that adopts.
Said product separation is in the operation: product solid-liquid mixed solution adopts press filtration filtering separation, centrifuging separation or sedimentation multi_layer extraction.
Adding the thermal control temperature in the operation in the said tube furnace is: reach 250-380 ℃ in tube furnace convective region asphalt temperature; 380-460 ℃ of tube furnace radiation zone asphalt temperature control.
Said interchanger heat-exchange temperature is in the operation: the preheating asphalt temperature reaches 180-300 ℃; The cooled product temperature reaches 300-200 ℃.
Said tube furnace radiation zone delay is in the operation: the residence time guarantees that by pitch velocity of flow in the pump adjustable pipe pitch is detained 5-12h at radiation zone.
Processing step more specifically: eu-bitumen (more than 120 ℃) pumps into the pitch pipeline by bitumenpump from the pitch storage tank tank, the flow velocity of pitch and flow by adjusting pump electric machine frequency or install return line adjustment additional.Pitch is by the interchanger material-heat-exchanging complete with reaction, and temperature reaches 180-300 ℃.The complete pitch of preheating continues to add catalyzer in proportion fully to be mixed with pitch.Mixed solution enters convective region, tube furnace top and further heats up, and asphalt temperature is controlled at 250-380 ℃.Enter afterwards the tube furnace radiation zone, the diamond heating mode can adopt the heating that acts as a fuel of coal gas, Sweet natural gas or fuel wet goods.The radiation zone temperature of charge keeps 380-460 ℃, temperature control precision ± 5 ℃; Keep constant pressure, at discharge port surge tank is set; Adjust flow rate of liquid by control pump, guarantee that material reaches 5-12h in the tube furnace radiation zone residence time, pitch generates MCMB through the Pintsch process polymerization during this period.By interchanger and the heat exchange of charging pitch, the product cooling reaches 300-200 ℃ behind the material process tube furnace.Material, is collected solid and is obtained MCMB solid MCMB and unreacted eu-bitumen solid-liquid separation by heat filtering afterwards.
Effect of the present invention: the present invention has realized product serialization production by use tube furnace alternative reaction still, improving productivity 30%, and Energy Intensity Reduction 22%, the consistence of product is controlled.
Embodiment:
The invention will be further described by the following examples.
In an embodiment, the material that uses the inventive method to produce comes the characterizing material performance by tester material granularity size.Its testing method is as follows:
Testing method: laser diffractometry
Testing apparatus: laser particle analyzer (Ma Erwen 2000 laser particle analyzers)
Test process: the solid MCMB of separating is put into dispersion agent (dehydrated alcohol) dissolving, pour in the laser particle analyzer sample pool, ultrasonic 1min, testing averages for three times is test value.
It below is specific embodiment.
Embodiment one:
The use toothed gear pump carries 250 ℃ of eu-bitumens to enter interchanger and output object carries out heat exchange, realizes the preheating of pitch, and asphalt temperature reaches about 280 ℃ after the heat exchange.Add subsequently the catalyzer for preparing in pipeline in the pitch, the add-on of catalyzer adds according to the certain proportion with pitch.Enter afterwards and fully mix rear inflow tubular type furnace roof section in the surge tank and continue heat temperature raising, flow into the tube furnace radiation zone after temperature reaches 420 ℃ and keep steady temperature.Tube furnace boiler tube length guarantees that under certain flow conditions, reactant reaches 6h in the flat-temperature zone residence time.The material that reacts complete enters the interchanger cooling from the tube furnace outflow and reaches 260 ℃, enters pressure filter and carries out heat filtering, and eu-bitumen reclaims, and solid is MCMB.
Embodiment two:
The use toothed gear pump carries 220 ℃ of eu-bitumens to enter interchanger and output object carries out heat exchange, realizes the preheating of pitch, and asphalt temperature reaches about 260 ℃ after the heat exchange.Add subsequently the catalyzer for preparing in pipeline in the pitch, the add-on of catalyzer adds according to the certain proportion with pitch.Enter afterwards and fully mix rear inflow tubular type furnace roof section in the surge tank and continue heat temperature raising, flow into the tube furnace radiation zone after temperature reaches 360 ℃ and continue to be warming up to 440 ℃, keep steady temperature.Tube furnace boiler tube length guarantees that under certain flow conditions, reactant reaches 8h in the flat-temperature zone residence time.The material that reacts complete enters the interchanger cooling from the tube furnace outflow and reaches 220 ℃, enters whizzer and takes off liquid, and eu-bitumen reclaims, and solid is MCMB.
In order to contrast the present invention and background technology, below the comparative example adopt background technology.
The comparative example:
260 ℃ raw materials are added in the reactor, add in proportion catalyzer simultaneously, keep stirring, be incubated 440 ℃.Reactor adopts electrically heated, keeps material to generate the MCMB solid at reactor internal reaction 8h.The centrifugal solid MCMB that obtains behind solid materials and the solvent cut.
The various embodiments described above data are as follows:
| Embodiment | Technique | Granularity (μ m) |
| Embodiment one | The tube furnace preparation | 16.8 |
| Embodiment two | The tube furnace preparation | 18.3 |
| The comparative example | Single still preparation | 18.2 |
By the Data Comparison of the present invention and background technology embodiment, can reach a conclusion:
The present invention adopts the tube furnace preparation to substitute the technique that single still prepares MCMB, makes production process become continous way by intermittent type, and guaranteeing under the constant condition of product performance: production efficiency has improved 30%, has saved the production time; Production energy consumption has reduced by 22%, has saved production cost.
Claims (7)
1. the pipe type continuously reaction prepares the MCMB method, it is characterized in that comprising following processing step: raw material liq pitch is squeezed into interchanger by pump and is heated to 180-300 ℃, then injecting catalyst before bitumen pipeline enters tube furnace further is heated to 250-380 ℃ by tube furnace top convection zone; Enter afterwards the tube furnace radiation zone and carry out the cracking polyreaction, guarantee radiation zone pitch residence time 5-12h, temperature 380-460 ℃; Separate after last material is cooled to 300-200 ℃ by interchanger and obtain MCMB.
2. described serialization prepares the MCMB method according to claim 1, it is characterized in that said interchanger is: interchanger is the cooling that same interchanger is used for pitch preheating and last material.
3. described serialization prepares the MCMB method according to claim 1, and it is characterized in that said tube furnace is: tube furnace is heating installation, adopts coal gas, Sweet natural gas or oil fuel to be the heating material; Boiler tube is arranged the snakelike arranged in series mode that adopts.
4. described serialization prepares the MCMB method according to claim 1, it is characterized in that said feed separation operation is: product solid-liquid mixed solution adopts press filtration filtering separation, centrifuging separation or sedimentation multi_layer extraction.
5. described serialization prepares the MCMB method according to claim 1, it is characterized in that adding in the said tube furnace thermal control temperature to be: reach 250-380 ℃ in tube furnace convective region asphalt temperature; 380-460 ℃ of tube furnace radiation zone asphalt temperature control.
6. described serialization prepares the MCMB method according to claim 1, and it is characterized in that said interchanger heat-exchange temperature is: the preheating asphalt temperature reaches 180-300 ℃; The cooled product temperature reaches 300-200 ℃.
7. described serialization prepares the MCMB method according to claim 1, and it is characterized in that said tube furnace radiation zone delay is: the residence time guarantees that by pitch velocity of flow in the pump adjustable pipe pitch is detained 5-12h at radiation zone.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011101774877A CN102849720A (en) | 2011-06-29 | 2011-06-29 | A method for preparing mesocarbon microbeads by tubular continuous reaction |
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| CN2011101774877A CN102849720A (en) | 2011-06-29 | 2011-06-29 | A method for preparing mesocarbon microbeads by tubular continuous reaction |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106430142A (en) * | 2016-05-11 | 2017-02-22 | 湖北鑫固久技术装备有限公司 | Carbon microspheres obtained through salt bath heating production |
| CN109850863A (en) * | 2019-01-16 | 2019-06-07 | 浙江大学 | A kind of mesoporous carbon nanospheres material of type gear shape, preparation method and application |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101985353A (en) * | 2009-12-10 | 2011-03-16 | 天津爱敏特电池材料有限公司 | Mesocarbon microbeads (MCMB) prepared by three-section tempering method |
-
2011
- 2011-06-29 CN CN2011101774877A patent/CN102849720A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101985353A (en) * | 2009-12-10 | 2011-03-16 | 天津爱敏特电池材料有限公司 | Mesocarbon microbeads (MCMB) prepared by three-section tempering method |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106430142A (en) * | 2016-05-11 | 2017-02-22 | 湖北鑫固久技术装备有限公司 | Carbon microspheres obtained through salt bath heating production |
| CN109850863A (en) * | 2019-01-16 | 2019-06-07 | 浙江大学 | A kind of mesoporous carbon nanospheres material of type gear shape, preparation method and application |
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Application publication date: 20130102 |