CN105253884A - Melting-free oxidation method for industrialized pitch ball activated carbon - Google Patents

Melting-free oxidation method for industrialized pitch ball activated carbon Download PDF

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Publication number
CN105253884A
CN105253884A CN201510768696.7A CN201510768696A CN105253884A CN 105253884 A CN105253884 A CN 105253884A CN 201510768696 A CN201510768696 A CN 201510768696A CN 105253884 A CN105253884 A CN 105253884A
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Prior art keywords
oxidation
gac
bitumen ball
reinforced frame
ball
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CN201510768696.7A
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CN105253884B (en
Inventor
郭军军
李开喜
金彦任
赵卯青
裴佩
王德周
安丽花
朱健娣
胡元宏
黄英
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Shanxi Xinhua Chemical Industry Co Ltd
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Shanxi Xinhua Chemical Industry Co Ltd
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Abstract

The invention relates to an oxidation method for activated carbon, in particular to a melting-free oxidation method for industrialized pitch ball activated carbon. The method includes the steps of firstly, placing pitch balls, wherein pitch ball activated carbon is placed in overlapped feed frames in an oxidation furnace in a layered mode, the interval between every two adjacent layers of feed frames is 1-3 cm, materials are kept fixed in the feed frames when melting-free oxidation is conducted, gas flows between the feed frames and makes contact and reacts with pitch ball activated carbon, and meanwhile the feed frames rotate in the furnace; secondly, conducting temperature rise and oxidation. By means of the method, the materials are prevented from being on fire when melting-free oxidation is conducted on the pitch ball activated carbon, oxidation is uniform, it is ensured that no cracking or melting is caused in the subsequent carbon activation high-temperature processing, and the method is verified through industrialized production.

Description

Oxidation for industrialization bitumen ball gac does not melt method
Technical field
The present invention relates to the method for oxidation of gac, be specially a kind of oxidation for industrialization bitumen ball gac and do not melt method.
Background technology
The full name of bitumen ball gac is asphalt-base spherical activated carbon, is the one of ball shape active carbon.Because of its have good sphericity, filling evenly, high, the good fluidity of physical strength, the series of advantages such as wear-resistant, corrosion-resistant and resistance is little when fixed bed uses, being widely used in various fields, is a kind of novel charcoal material of excellent property.But be oxidized in its preparation process that not melt operation essential.
At present, it take pitch as the technology that ball shape active carbon prepared by raw material that numerous patent has related to, as Chinese invention patent 201210317727 " the less energy-consumption preparation method of asphalt-base spherical activated carbon ", adopt the nitrogen containing oxygen to be oxidized bitumen ball not melt, Chinese invention patent 200410100531 " preparing the method for ball shape active carbon " is only mentioned and is adopted flow method to be oxidized bitumen ball and not melt process, Chinese invention patent 201310227294 " bitumen ball oxidation does not melt method " is mentioned use two kinds of stoves and is carried out being oxidized not melting, many Chinese patents are also had not melt as Chinese invention patent 97101617 " a kind of preparation method of spheric active carbon " and Chinese invention patent 201010143602 " a kind of preparation method of bitumen ball " all simply refer to oxidation, but do not melt process to how to be oxidized corresponding method is provided, and the relevant report be not applied in suitability for industrialized production.
Summary of the invention
The present invention mainly provides a kind of industrialization can be oxidized the method for not melting process to bitumen ball gac.Can guarantee that spheric active char combustion does not melt evenly, thoroughly, avoid the phenomenons such as material catches fire in oxidation, charcoal reactivation process, explosion, ensure to produce and normally carry out and keep the safety in production.
The present invention adopts following technical scheme to realize:
Oxidation for industrialization bitumen ball gac does not melt a method, comprises the steps:
(1), bitumen ball is placed:
The layering of bitumen ball gac is positioned in the reinforced frame of the superposition in oxidized still, every layer of reinforced frame interval 1-3cm, carry out being oxidized do not melt time, material keeps fixing in reinforced frame, gas flows between reinforced frame, contact with bitumen ball gac and react, reinforced frame rotates in stove simultaneously;
(2), heating and oxidation:
By per kilogram bitumen ball gac needs 3 ~ 10m per hour 3air passes in oxidized still;
A, beginning the temperature rise period, from room temperature to 80 ~ 160 DEG C in 1h, stop 1 ~ 5h, obtain the bitumen ball gac of preliminary oxidation;
The bitumen ball gac of b, preliminary oxidation is with 80 ~ 160 DEG C for initial temperature, and heat up with 4 ~ 10 DEG C/h temperature rise rate, final temperature is 300 ~ 330 DEG C, the residence time 2 ~ 5h, obtains the bitumen ball gac after oxidation.
Have the reinforced frame of superposition in oxidized still, every layer of reinforced frame keeps at a certain distance away, and material layering is seated in reinforced frame.Be in stationary state in the reinforced frame of material in oxidized still, such as, bitumen ball put into fixing groove, but rotate along with reinforced frame, carry out being oxidized do not melt time, material keeps fixing in reinforced frame, and gas flows between reinforced frame, contacts react with bitumen ball, reinforced frame rotates in stove simultaneously, ensure that material is evenly sent out in identical temperature, atmosphere surrounding to answer, compared with flow method, collision between material, friction can be avoided, cause material rough, even broken; Compared with traditional fixation method, material thermally equivalent, reaction can be ensured.Being oxidized the design of not melting stage employing percolation and adding swing, solve oxidation homogeneity question.
At present, the maximum loadings of oxidized still is 25 kilograms, passes into air by per kilogram bitumen ball needs 2 ~ 10 per hour cubic metres of air.In the beginning temperature rise period, with 80 ~ 160 DEG C/h temperature rise rate from room temperature to 80 ~ 160 DEG C, stop 1 ~ 5h, obtain the bitumen ball of preliminary oxidation.The bitumen ball of preliminary oxidation is with 80 ~ 160 DEG C for initial temperature, and heat up with 4 ~ 10 DEG C/h temperature rise rate, final temperature is 300 ~ 330 DEG C, total residence time 20 ~ 45h, obtains the bitumen ball after oxidation.Key point in method and protection point be to carry out being oxidized not in thaw process as processing parameters such as oxidizing temperature, temperature rise rate, oxidization times.Aforesaid method is mainly studied parameters such as oxidizing temperature, oxidization time, temperature rise rate, air inlets, guarantees that spheric active char combustion is even, thoroughly, does not affect the pyroprocessing such as follow-up charing, activation, meet industrialized production.
The inventive method makes bitumen ball gac material can not avoided to catch fire in thaw process being oxidized, and oxidation evenly, ensures not ftracture in follow-up charcoal activation pyroprocessing, thawing etc., and through the checking of suitability for industrialized production.
Embodiment
Below specific embodiments of the invention are described in detail.
embodiment 1
Oxidation for industrialization bitumen ball gac does not melt a method, comprises the steps:
(1), bitumen ball is placed:
The layering of bitumen ball gac is positioned in the reinforced frame of the superposition in oxidized still, every layer of reinforced frame interval 1-3cm, carry out being oxidized do not melt time, material keeps fixing in reinforced frame, gas flows between reinforced frame, contact with bitumen ball gac and react, reinforced frame rotates in stove simultaneously.
(2), heating and oxidation:
By per kilogram bitumen ball gac needs 3 ~ 10m per hour 3air passes in oxidized still;
A, beginning the temperature rise period, from room temperature to 120 DEG C in 1h, stop 2h, obtain the bitumen ball gac of preliminary oxidation;
The bitumen ball gac of b, preliminary oxidation is with 120 DEG C for initial temperature, and heat up with 6 DEG C/h temperature rise rate, final temperature is 320 DEG C, residence time 4h, obtains the bitumen ball gac after oxidation.
embodiment 2
Oxidation for industrialization bitumen ball gac does not melt a method, comprises the steps:
(1), bitumen ball is placed:
The layering of bitumen ball gac is positioned in the reinforced frame of the superposition in oxidized still, every layer of reinforced frame interval 1-3cm, carry out being oxidized do not melt time, material keeps fixing in reinforced frame, gas flows between reinforced frame, contact with bitumen ball gac and react, reinforced frame rotates in stove simultaneously.
(2), heating and oxidation:
By per kilogram bitumen ball gac needs 3 ~ 10m per hour 3air passes in oxidized still;
A, beginning the temperature rise period, from room temperature to 120 DEG C in 1h, stop 2.5h, obtain the bitumen ball gac of preliminary oxidation;
The bitumen ball gac of b, preliminary oxidation is with 120 DEG C for initial temperature, and heat up with 8 DEG C/h temperature rise rate, final temperature is 320 DEG C, residence time 3h, obtains the bitumen ball gac after oxidation.
embodiment 3
Oxidation for industrialization bitumen ball gac does not melt a method, comprises the steps:
(1), bitumen ball is placed:
The layering of bitumen ball gac is positioned in the reinforced frame of the superposition in oxidized still, every layer of reinforced frame interval 1-3cm, carry out being oxidized do not melt time, material keeps fixing in reinforced frame, gas flows between reinforced frame, contact with bitumen ball gac and react, reinforced frame rotates in stove simultaneously.
(2), heating and oxidation:
By per kilogram bitumen ball gac needs 3 ~ 10m per hour 3air passes in oxidized still;
A, beginning the temperature rise period, from room temperature to 80 DEG C in 1h, stop 5h, obtain the bitumen ball gac of preliminary oxidation;
The bitumen ball gac of b, preliminary oxidation is with 80 DEG C for initial temperature, and heat up with 5 DEG C/h temperature rise rate, final temperature is 300 DEG C, residence time 4.5h, obtains the bitumen ball gac after oxidation.
embodiment 4
Oxidation for industrialization bitumen ball gac does not melt a method, comprises the steps:
(1), bitumen ball is placed:
The layering of bitumen ball gac is positioned in the reinforced frame of the superposition in oxidized still, every layer of reinforced frame interval 1-3cm, carry out being oxidized do not melt time, material keeps fixing in reinforced frame, gas flows between reinforced frame, contact with bitumen ball gac and react, reinforced frame rotates in stove simultaneously.
(2), heating and oxidation:
By per kilogram bitumen ball gac needs 3 ~ 10m per hour 3air passes in oxidized still;
A, beginning the temperature rise period, from room temperature to 100 DEG C in 1h, stop 3h, obtain the bitumen ball gac of preliminary oxidation;
The bitumen ball gac of b, preliminary oxidation is with 100 DEG C for initial temperature, and heat up with 10 DEG C/h temperature rise rate, final temperature is 330 DEG C, residence time 2h, obtains the bitumen ball gac after oxidation.
embodiment 5
Oxidation for industrialization bitumen ball gac does not melt a method, comprises the steps:
(1), bitumen ball is placed:
The layering of bitumen ball gac is positioned in the reinforced frame of the superposition in oxidized still, every layer of reinforced frame interval 1-3cm, carry out being oxidized do not melt time, material keeps fixing in reinforced frame, gas flows between reinforced frame, contact with bitumen ball gac and react, reinforced frame rotates in stove simultaneously.
(2), heating and oxidation:
By per kilogram bitumen ball gac needs 3 ~ 10m per hour 3air passes in oxidized still;
A, beginning the temperature rise period, from room temperature to 160 DEG C in 1h, stop 5h, obtain the bitumen ball gac of preliminary oxidation;
The bitumen ball gac of b, preliminary oxidation is with 160 DEG C for initial temperature, and heat up with 4 DEG C/h temperature rise rate, final temperature is 310 DEG C, residence time 5h, obtains the bitumen ball gac after oxidation.
embodiment 6
Oxidation for industrialization bitumen ball gac does not melt a method, comprises the steps:
(1), bitumen ball is placed:
The layering of bitumen ball gac is positioned in the reinforced frame of the superposition in oxidized still, every layer of reinforced frame interval 1-3cm, carry out being oxidized do not melt time, material keeps fixing in reinforced frame, gas flows between reinforced frame, contact with bitumen ball gac and react, reinforced frame rotates in stove simultaneously.
(2), heating and oxidation:
By per kilogram bitumen ball gac needs 3 ~ 10m per hour 3air passes in oxidized still;
A, beginning the temperature rise period, from room temperature to 140 DEG C in 1h, stop 1h, obtain the bitumen ball gac of preliminary oxidation;
The bitumen ball gac of b, preliminary oxidation is with 140 DEG C for initial temperature, and heat up with 4 DEG C/h temperature rise rate, final temperature is 310 DEG C, residence time 2h, obtains the bitumen ball gac after oxidation.
It should be noted last that; above embodiment is only in order to illustrate technical scheme of the present invention and unrestricted; although be described in detail with reference to the embodiment of the present invention; those of ordinary skill in the art is to be understood that; technical scheme of the present invention is modified or equivalent replacement; do not depart from the spirit and scope of technical scheme of the present invention, it all should be contained in claims of the present invention.

Claims (2)

1. the oxidation for industrialization bitumen ball gac does not melt a method, it is characterized in that: comprise the steps:
(1), bitumen ball is placed:
The layering of bitumen ball gac is positioned in the reinforced frame of the superposition in oxidized still, every layer of reinforced frame interval 1-3cm, carry out being oxidized do not melt time, material keeps fixing in reinforced frame, gas flows between reinforced frame, contact with bitumen ball gac and react, reinforced frame rotates in stove simultaneously;
(2), heating and oxidation:
By per kilogram bitumen ball gac needs 3 ~ 10m per hour 3air passes in oxidized still;
A, beginning the temperature rise period, from room temperature to 80 ~ 160 DEG C in 1h, stop 1 ~ 5h, obtain the bitumen ball gac of preliminary oxidation;
The bitumen ball gac of b, preliminary oxidation is with 80 ~ 160 DEG C for initial temperature, and heat up with 4 ~ 10 DEG C/h temperature rise rate, final temperature is 300 ~ 330 DEG C, the residence time 2 ~ 5h, obtains the bitumen ball gac after oxidation.
2. the oxidation for industrialization bitumen ball gac according to claim 1 does not melt method, it is characterized in that: in step (2),
A, beginning the temperature rise period, from room temperature to 120 DEG C in 1h, stop 2 ~ 2.5h, obtain the bitumen ball gac of preliminary oxidation;
The bitumen ball gac of b, preliminary oxidation is with 120 DEG C for initial temperature, and heat up with 6 ~ 8 DEG C/h temperature rise rate, final temperature is 320 DEG C, the residence time 3 ~ 4h, obtains the bitumen ball gac after oxidation.
CN201510768696.7A 2015-11-12 2015-11-12 Do not melt method for the oxidation for industrializing bitumen ball activated carbon Active CN105253884B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106115687A (en) * 2016-06-28 2016-11-16 山西新华化工有限责任公司 Method is not melted in the oxidation of flow-type bitumen ball
CN107790118A (en) * 2017-11-08 2018-03-13 山西新华化工有限责任公司 For the technique of asphalt-base spherical activated carbon modification
CN112142487A (en) * 2020-09-22 2020-12-29 中国科学院山西煤炭化学研究所 Microwave-assisted asphalt oxidation non-melting method

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103272533A (en) * 2013-06-08 2013-09-04 中国科学院山西煤炭化学研究所 Pitch sphere oxidative stabilization method
CN104276569A (en) * 2014-10-21 2015-01-14 中国科学院山西煤炭化学研究所 Method for improving crushing strength of asphalt-based spherical activated carbon
CN104927890A (en) * 2015-06-09 2015-09-23 中国科学院山西煤炭化学研究所 Large-scale pitch sphere oxidation non-fusible preparation process and device

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103272533A (en) * 2013-06-08 2013-09-04 中国科学院山西煤炭化学研究所 Pitch sphere oxidative stabilization method
CN104276569A (en) * 2014-10-21 2015-01-14 中国科学院山西煤炭化学研究所 Method for improving crushing strength of asphalt-based spherical activated carbon
CN104927890A (en) * 2015-06-09 2015-09-23 中国科学院山西煤炭化学研究所 Large-scale pitch sphere oxidation non-fusible preparation process and device

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106115687A (en) * 2016-06-28 2016-11-16 山西新华化工有限责任公司 Method is not melted in the oxidation of flow-type bitumen ball
CN106115687B (en) * 2016-06-28 2017-11-28 山西新华化工有限责任公司 Method is not melted in the oxidation of flow-type bitumen ball
CN107790118A (en) * 2017-11-08 2018-03-13 山西新华化工有限责任公司 For the technique of asphalt-base spherical activated carbon modification
CN112142487A (en) * 2020-09-22 2020-12-29 中国科学院山西煤炭化学研究所 Microwave-assisted asphalt oxidation non-melting method
CN112142487B (en) * 2020-09-22 2021-09-10 中国科学院山西煤炭化学研究所 Microwave-assisted asphalt oxidation non-melting method

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