CN202290062U - Complete equipment for preparing mesocarbon microbeads and catalyst pretreatment device - Google Patents

Complete equipment for preparing mesocarbon microbeads and catalyst pretreatment device Download PDF

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Publication number
CN202290062U
CN202290062U CN2011201842282U CN201120184228U CN202290062U CN 202290062 U CN202290062 U CN 202290062U CN 2011201842282 U CN2011201842282 U CN 2011201842282U CN 201120184228 U CN201120184228 U CN 201120184228U CN 202290062 U CN202290062 U CN 202290062U
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catalyst
catalyst pretreatment
pretreatment unit
cylindrical shell
metal oxide
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CN2011201842282U
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杨红强
苗艳丽
李花
李福华
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BTR New Material Group Co Ltd
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TIANJIN BTR NEW ENERGY MATERIAL CO Ltd
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Abstract

The utility model aims at providing complete equipment for preparing mesocarbon microbeads; the complete equipment is characterized by comprising a catalyst pretreatment device, wherein the catalyst pretreatment device comprises a cylinder body 1 and a jacket 2; a feed bin 3 and a circulation smoke abatement pipe are arranged at the upper end of the cylinder body; a discharge port 9 is formed at the lower end of the cylinder body; and preferentially, the jacket is provided with a water inlet 14 and a water outlet 15. According to the complete equipment provided by the utility model, the catalyst can be subjected to pretreatment of heating and melting by the catalyst pretreatment device, so that the catalyst can be uniformly blended with a reaction raw material (e.g. bitumen), closed feeding and efficient catalyzing can be achieved, in addition, the defects that the catalyst is not uniformly blended with the raw material, local part is overheated, mixed liquor spouts from a slot and causes a fire due to the drastic catalytic reaction and the like are overcome, and the advantages of simplicity in operation, no dust, low preparation cost, prevention against environmental pollution and the like are achieved.

Description

A kind of complexes and catalyst pretreatment unit for preparing MCMB
Technical field
The present invention relates to a kind of complexes and catalyst pretreatment unit for preparing MCMB.
Background technology
MCMB has outstanding advantages such as high-rate discharge ability, high security, and becomes present most important cathode material of lithium-ion power battery.
Existing MCMB preparation method comprises thermal polycondensation process, emulsion method, suspension method etc.Wherein, emulsion method is by (Kodama M, the Fujirua T such as Kodama of Japan; Esumi K et al.Carbon, 1988,26 (4): 595) develop; This method is dissolved in the condensed-nuclei aromatics compound in a certain amount of heat stable dielectric (like silicone oil) earlier, after heat treatment, the mesophasespherule that is emulsified into is passed through charing and graphitization processing again; Promptly get the MCMB material product, this method is had relatively high expectations to heat stable dielectric, and; In order to let MCMB in carbonization process, keep certain shape and structure; MCMB is many before charing need to carry out oxidation processes, so exist technological process complicacy, equipment various, defective such as be difficult to accomplish scale production.Suspension method (Lu Yonggen, Ling Licheng et al.Preparation of carbon microbeads from pitch and resin by suspention, novel charcoal material; 2001,16 (6): 1-5) earlier mesophase pitch is dissolved in the organic solvent, utilizes surfactant and water or other solvent composition suspension; Powerful at a certain temperature the stirring makes the mesophase pitch balling-up, and organic solvent is removed in heating then; Analyse, after the pre-oxidation, charing, promptly get through cooling, filter.Compare with emulsion process, suspension method has been used surfactant, can effectively prevent condensing and flocculation of mesophase ball; And through control temperature and mixing speed; With the particle diameter of control mesophasespherule, this method requires to use the solubility mesophase pitch, and process conditions control difficulty is big.Thermal polycondensation process (CN021 16840.7, CN101811694A etc.) discloses the adding appropriate catalyst; Under uniform temperature and pressure, carry out the thermal polycondensation reaction with pitch, processes such as reaction is washed after finishing, separation, charing, graphitization promptly get MCMB; Pass through in this method to add catalyst with fast reaction speed; Improve reaction yield, and reduce production costs, and become the main preparation methods of present MCMB.But; This method exists catalyst to add inconvenience; And add length consuming time, and problems such as, thermal polycondensation reaction hot-spot uneven with mixing of catalyst because of the reunion of catalyst and caking, raw material, and cause potential safety hazards such as catalytic reaction is too fierce, mixed liquor spray groove is on fire.Therefore, the security that how effectively to solve thermal polycondensation process becomes the technical problem that people press for solution.
Summary of the invention
The object of the present invention is to provide a kind of catalyst pretreatment unit, said catalyst pretreatment unit comprises cylindrical shell 1, chuck 2, and wherein, the cylindrical shell upper end is provided with and adds feed bin 3, circulation smoke elimination pipe 5, and the cylindrical shell lower end is provided with discharging opening 9; Preferred jacket is provided with water inlet 14, delivery port 15.
In the optimal technical scheme of the present invention, add feed bin 3 lower ends reinforced butterfly valve 4 is set.
In the optimal technical scheme of the present invention, eliminate smoke pipe 5 of circulation is connected with circulation smoke elimination pump 7, and circulation smoke elimination pump 7 is connected with smoke elimination groove 8.
In the optimal technical scheme of the present invention, be provided with agitating device in the cylindrical shell 1, preferred said agitating device is provided with shaft 12 and paddle 13.
In the optimal technical scheme of the present invention, agitating device is connected with reductor 11.
In the optimal technical scheme of the present invention, in the cylindrical shell 1 and/or chuck 2 be provided with Temperature Detector 6.
In the optimal technical scheme of the present invention, cylindrical shell 1 lower end discharging opening 9 is connected with discharge pipe, and discharge pipe is connected with metering device 10, and preferred metering device is a measuring pump.
In the optimal technical scheme of the present invention, said cylindrical shell 1 inboard is provided with erosion shield.
In the optimal technical scheme of the present invention; Said catalyst is selected from any or its combination of itrated compound of itrated compound, the aluminium of itrated compound, the cobalt of itrated compound, the nickel of metal oxide, the iron of metal oxide, the aluminium of metal oxide, the cobalt of metal oxide, the nickel of p-methyl benzenesulfonic acid, iron, is preferably any or its combination of alchlor, ferrocene, p-methyl benzenesulfonic acid.
The object of the present invention is to provide a kind of complexes that prepare MCMB; It is characterized in that; Said complexes comprise catalyst pretreatment unit of the present invention; Wherein, said catalyst pretreatment unit comprises cylindrical shell 1, chuck 2, and the cylindrical shell upper end is provided with and adds feed bin 3, circulation smoke elimination pipe 5; The cylindrical shell lower end is provided with discharging opening 9; Preferred jacket is provided with water inlet 14, delivery port 15.
In the optimal technical scheme of the present invention, said complete set of equipments also comprises thermal polycondensation agitated reactor and metering device (10).
In the optimal technical scheme of the present invention, said measuring pump 10 is connected with pipeline, agitated reactor successively, will dissolve catalyst and add agitated reactor after metering, and preferred metering device is a measuring pump, the kettle 16 outer heating jackets 19 that are provided with of preferred reaction still.
In the optimal technical scheme of the present invention, said agitated reactor upper end is provided with charge door 17, safety valve 18, circulation smoke elimination pipeline 5; Kettle 16 inside are provided with agitating device; Discharging opening 9 is established in the kettle lower end.
In the optimal technical scheme of the present invention, the discharging opening 9 of agitated reactor is connected with blowing jar 20.
In the optimal technical scheme of the present invention, the catalyst pretreatment unit is connected with the thermal polycondensation agitated reactor through pipeline, metering device.
In the optimal technical scheme of the present invention; Said catalyst is selected from any or its combination of itrated compound of itrated compound, the aluminium of itrated compound, the cobalt of itrated compound, the nickel of metal oxide, the iron of metal oxide, the aluminium of metal oxide, the cobalt of metal oxide, the nickel of p-methyl benzenesulfonic acid, iron, is preferably any or its combination of alchlor, ferrocene, p-methyl benzenesulfonic acid.
Complexes of the present invention carry out the heating and melting preliminary treatment through the catalyst pretreatment unit with catalyst; Being beneficial to it evenly mixes with reaction raw materials (like pitch); Realize airtight charging and efficient catalytic; And overcome catalyst and mix defectives such as the too violent mixed liquor spray groove that causes of inequality, hot-spot, catalytic reaction is on fire with raw material, and the accurate conveying through metering system, the production efficiency of phase carbon particle in the middle of significantly improving; Significantly reduce its production cost, have that simple to operate, no dust, preparation cost are low, advantage such as prevent the pollution of the environment.
Another object of the present invention is to provide the preparation method of MCMB, it is characterized in that, use catalyst pretreatment unit of the present invention that catalyst is carried out the heating and melting preliminary treatment.
In the optimal technical scheme of the present invention, described catalyst carries out the heating and melting pretreatment condition and does, pretreatment temperature is 50-100 ℃, and the mode of heating of chuck is the water-bath heating in the preferred catalyst pretreatment unit.
Another object of the present invention is to provide the application of catalyst pretreatment unit in the preparation MCMB.
Another object of the present invention is to provide the application of complexes of the present invention in the preparation MCMB.
Except as otherwise noted, percentage according to the invention is mass percent.
" thermal polycondensation agitated reactor " of the present invention claimed " agitated reactor " again.
Description of drawings
Fig. 1 the present invention prepares the structural representation of MCMB complexes,
1 is cylindrical shell among the figure, and 2 is chuck, and 3 for adding feed bin, and 4 are reinforced butterfly valve, and 5 are circulation smoke elimination pipe; 6 is detector, and 7 are circulation smoke elimination pump, and 8 are the smoke elimination groove, and 9 is discharging opening, and 10 is measuring pump; 11 is reductor, and 12 is shaft, and 13 is paddle, and 14 is water inlet, and 15 is delivery port; 16 is kettle, and 17 is charge door, and 18 is safety valve, and 19 is heating jacket, and 20 is the blowing jar.
The specific embodiment
Below will combine embodiment to specify the present invention, embodiments of the invention only are used to technical scheme of the present invention is described, and non-limiting essence of the present invention.
Embodiment 1The pretreating effect of catalyst alchlor
1) opens the reinforced butterfly valve of catalyst pretreatment unit, add the catalyst alchlor, add hot water from the chuck water inlet from adding feed bin; Open the chuck delivery port, keeping water bath heating temperature is 50-100 ℃, treat that the catalyst heating and melting mixes after; Through metering system pretreated alchlor is squeezed into agitated reactor; Make it evenly to mix, carry out the thermal polycondensation reaction, the preparation MCMB with pitch.
2) Comparative Examples: 80-100kg directly squeezes into agitated reactor with the catalyst alchlor, makes it to mix with pitch to carry out thermal polycondensation reaction, preparation MCMB.
Comparative study 1) and 2) preparation yield, the catalyst consumption cost aspects such as (ten thousand/ton finished products) of the MCMB of two kinds of methods, the result sees table 1.
Embodiment 2The pretreating effect of catalyst ferrocene
1) opens the reinforced butterfly valve of catalyst pretreatment unit, add the catalyst ferrocene, add hot water from the chuck water inlet from adding feed bin; Open the chuck delivery port, keeping water bath heating temperature is 50-100 ℃, treat that the catalyst heating and melting mixes after; Through metering system pretreated alchlor is squeezed into agitated reactor; Make it evenly to mix, carry out the thermal polycondensation reaction, the preparation MCMB with pitch.
2) Comparative Examples: 80-100kg directly squeezes into agitated reactor with the catalyst ferrocene, makes it to mix with pitch to carry out thermal polycondensation reaction, preparation MCMB.
Comparative study 1) and 2) preparation yield, the catalyst consumption cost aspects such as (ten thousand/ton finished products) of the MCMB of two kinds of methods, the result sees table 1.
Embodiment 3The pretreating effect of catalyst p-methyl benzenesulfonic acid
1) opens the reinforced butterfly valve of catalyst pretreatment unit, add the catalyst p-methyl benzenesulfonic acid, add hot water from the chuck water inlet from adding feed bin; Open the chuck delivery port, keeping water bath heating temperature is 50-100 ℃, treat that the catalyst heating and melting mixes after; Through metering system pretreated alchlor is squeezed into agitated reactor; Make it evenly to mix, carry out the thermal polycondensation reaction, the preparation MCMB with pitch.
2) Comparative Examples: 80-100kg directly squeezes into the thermal polycondensation agitated reactor with the catalyst p-methyl benzenesulfonic acid, makes it to mix with pitch to carry out thermal polycondensation reaction, preparation MCMB.
Comparative study 1) and 2) preparation yield, the catalyst consumption cost aspects such as (ten thousand/ton finished products) of the MCMB of two kinds of methods, the result sees table 1.
The pretreating effect research of table 1 catalyst
Figure BSA00000509813700041
Visible by table 1; Complexes of the present invention, particularly catalyst pretreatment unit have not only been eliminated because of catalyst mixes inequality, hot-spot, catalytic reaction with pitch and too acutely have been prone to cause mixed liquor spray groove phenomenon on fire; Handling rear catalyst evenly adds; Be beneficial to pitch and mix, realize that efficient catalytic prepares MCMB, and have that high efficiency, simple to operate, no dust, preparation cost are low, advantage such as prevent the pollution of the environment.

Claims (10)

1. a catalyst pretreatment unit is characterized in that, comprises cylindrical shell (1), chuck (2), and wherein, the cylindrical shell upper end is provided with and adds feed bin (3), circulation smoke elimination pipe (5), and the cylindrical shell lower end is provided with discharging opening (9), and preferred jacket is provided with water inlet (14), delivery port (15).
2. catalyst pretreatment unit according to claim 1, said feed bin (3) lower end that adds is provided with reinforced butterfly valve (4).
3. according to claim 2 or 3 described catalyst pretreatment units, said circulation smoke elimination pipe (5) is connected with circulation smoke elimination pump (7), smoke elimination groove (8) successively.
4. according to each described catalyst pretreatment unit of claim 1-3, said cylindrical shell is provided with agitating device in (1), and preferred said agitating device is provided with shaft (12) and paddle (13).
5. catalyst pretreatment unit according to claim 4, said agitating device is connected with reductor (11).
6. according to each described catalyst pretreatment unit of claim 1-5, be equipped with Temperature Detector (6) in the said cylindrical shell (1) and/or on the chuck (2).
7. according to each described catalyst pretreatment unit of claim 1-6, said cylindrical shell (1) inboard is provided with erosion shield.
8. according to each described catalyst pretreatment unit of claim 1-7; Said catalyst is selected from any or its combination of itrated compound of itrated compound, the aluminium of itrated compound, the cobalt of itrated compound, the nickel of metal oxide, the iron of metal oxide, the aluminium of metal oxide, the cobalt of metal oxide, the nickel of p-methyl benzenesulfonic acid, iron, is preferably any or its combination of alchlor, ferrocene, p-methyl benzenesulfonic acid.
9. complexes that prepare MCMB is characterized in that, said complexes comprise each described catalyst pretreatment unit of claim 1-9.
10. according to the complete set of equipments of claim 10, it is characterized in that said complete set of equipments also comprises thermal polycondensation agitated reactor and metering device (10).
CN2011201842282U 2011-05-27 2011-05-27 Complete equipment for preparing mesocarbon microbeads and catalyst pretreatment device Expired - Lifetime CN202290062U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102732281A (en) * 2012-07-16 2012-10-17 冀州信诚化工设备科技有限公司 Lake asphalt melting and stirring system

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102732281A (en) * 2012-07-16 2012-10-17 冀州信诚化工设备科技有限公司 Lake asphalt melting and stirring system

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