[go: up one dir, main page]

CN103272533B - Pitch sphere oxidative stabilization method - Google Patents

Pitch sphere oxidative stabilization method Download PDF

Info

Publication number
CN103272533B
CN103272533B CN201310227294.7A CN201310227294A CN103272533B CN 103272533 B CN103272533 B CN 103272533B CN 201310227294 A CN201310227294 A CN 201310227294A CN 103272533 B CN103272533 B CN 103272533B
Authority
CN
China
Prior art keywords
asphalt
temperature
balls
tunnel kiln
oxidized
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201310227294.7A
Other languages
Chinese (zh)
Other versions
CN103272533A (en
Inventor
李开喜
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shanxi Institute of Coal Chemistry of CAS
Original Assignee
Shanxi Institute of Coal Chemistry of CAS
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shanxi Institute of Coal Chemistry of CAS filed Critical Shanxi Institute of Coal Chemistry of CAS
Priority to CN201310227294.7A priority Critical patent/CN103272533B/en
Publication of CN103272533A publication Critical patent/CN103272533A/en
Application granted granted Critical
Publication of CN103272533B publication Critical patent/CN103272533B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Working-Up Tar And Pitch (AREA)

Abstract

一种沥青球氧化不熔化方法是在装有沥青球的旋转炉或固定床反应器中,按每公斤沥青球每小时需要200-800升空气通入空气;以20-50℃/h升温速率从室温升温到180-250℃,停留2-5h,获得初步氧化的沥青球;初步氧化的沥青球在隧道窑中进一步进行氧化处理,隧道窑分为5-10段,下一段的温度与上一段的温度相差20-40℃,起始温度为150-220℃,终止温度为290-350℃,沥青在隧道窑中的总停留时间为7-15h,获得氧化不熔化沥青球,其中通入的空气量按每小时每公斤沥青球300-1000升的空气量。本发明采用两种炉型进行氧化不熔化,避免了沥青氧化过程中的着火,保证了安全生产,产品的氧化均匀性的优点。A kind of asphalt pellets oxidation non-melting method is that in the rotary furnace or the fixed bed reactor that is equipped with pitch pellets, need 200-800 liters of air per hour per kilogram of pitch pellets to feed into the air; Raise the temperature from room temperature to 180-250°C and stay for 2-5 hours to obtain preliminary oxidized pitch balls; the preliminary oxidized pitch balls are further oxidized in the tunnel kiln. The tunnel kiln is divided into 5-10 sections, and the temperature of the next section is the same as that of the upper section. The temperature difference in one stage is 20-40°C, the initial temperature is 150-220°C, and the end temperature is 290-350°C. The total residence time of asphalt in the tunnel kiln is 7-15h to obtain oxidized and non-melting asphalt balls. The air volume is 300-1000 liters of air per kilogram of asphalt balls per hour. The present invention adopts two types of furnaces to oxidize without melting, avoids ignition in the process of asphalt oxidation, ensures safe production, and has the advantages of uniform oxidation of products.

Description

沥青球氧化不熔化方法Oxidation and non-melting method of asphalt balls

技术领域 technical field

本发明属于一种沥青球氧化不熔化方法。 The invention belongs to a method for oxidation and non-melting of asphalt balls.

背景技术 Background technique

沥青基球状活性炭属于高性能的活性炭,在众多领域均有应用。但其制备制备过程中的氧化不熔化是必不可少的。 Pitch-based spherical activated carbon is a high-performance activated carbon that is used in many fields. However, it is essential for oxidation and non-melting in the preparation process.

目前,众多专利涉及到了以沥青为原料制备球状活性炭的技术,如:中国发明专利201210317727“沥青基球形活性炭的低能耗制备方法”采用含有氧气的氮气对沥青球进行氧化不熔化、中国发明专利03178572“富含中孔的沥青基球状活性炭的制备方法”仅提到将沥青球用空气升温到250-300℃以得到不熔化沥青球、中国发明专利200410100531“制备球形活性碳的方法”仅提到采用流动法对沥青球进行氧化不熔化处理,还有不少中国专利如中国发明专利200610127621“一种制备重金属含量低的球形活性炭的方法”、中国发明专利200810035853“一种含氮沥青基球形活性炭的制备方法”、中国发明专利97101617“一种球状活性炭的制备方法”以及中国发明专利201010143602“一种沥青球的制备方法”均简单提到了氧化不熔化,却并未对如何进行氧化不熔化处理提供相应的方法。 At present, many patents involve the technology of preparing spherical activated carbon from asphalt, such as: Chinese invention patent 201210317727 "Preparation method of pitch-based spherical activated carbon with low energy consumption" uses nitrogen containing oxygen to oxidize asphalt balls without melting, Chinese invention patent 03178572 "Preparation method of pitch-based spherical activated carbon rich in mesopores" only mentions that the asphalt balls are heated to 250-300°C with air to obtain infusible pitch balls, Chinese invention patent 200410100531 "Method for preparing spherical activated carbon" only mentions The flow method is used to oxidize and infusible asphalt balls, and there are many Chinese patents such as Chinese invention patent 200610127621 "a method for preparing spherical activated carbon with low heavy metal content", Chinese invention patent 200810035853 "a nitrogen-containing pitch-based spherical activated carbon "Preparation Method of Spherical Activated Carbon", Chinese Invention Patent 97101617 "Preparation Method of Spherical Activated Carbon" and Chinese Invention Patent 201010143602 "Preparation Method of Pitch Balls" all briefly mentioned oxidation infusion, but did not discuss how to carry out oxidation infusion treatment Provide corresponding methods.

发明内容 Contents of the invention

本发明的目的是提供一种对沥青球进行氧化不熔化处理的方法。 The object of the present invention is to provide a method for oxidizing and infusible treatment of asphalt balls.

本发明的方法是按如下步骤实现的: Method of the present invention is realized according to the following steps:

(1)在装有沥青球的旋转炉或固定床反应器中,按每公斤沥青球每小时需要200-800升空气通入空气;以20-50℃/h升温速率从室温升温到180-250℃,停留2-5h,获得初步氧化的沥青球; (1) In a rotary furnace or a fixed bed reactor equipped with asphalt balls, 200-800 liters of air is required per kilogram of asphalt balls per hour to feed the air; the temperature is raised from room temperature to 180-180- 250°C, stay for 2-5 hours, and obtain the initially oxidized asphalt balls;

(2)初步氧化的沥青球在隧道窑中进一步进行氧化处理,隧道窑分为5-10段,下一段的温度与上一段的温度相差20-40℃,起始温度为150-220℃,终止温度为290-350℃,沥青在隧道窑中的总停留时间为7-15h,获得氧化不熔化沥青球,其中通入的空气量按每小时每公斤沥青球300-1000升的空气量。 (2) The initially oxidized asphalt balls are further oxidized in the tunnel kiln. The tunnel kiln is divided into 5-10 sections. The temperature difference between the next section and the previous section is 20-40°C, and the initial temperature is 150-220°C. The termination temperature is 290-350°C, and the total residence time of the asphalt in the tunnel kiln is 7-15 hours to obtain oxidized and non-melting asphalt balls, wherein the air volume introduced is 300-1000 liters of air per kilogram of asphalt balls per hour.

如上所述的沥青球的球径在0.1-1.5mm之间。 The ball diameter of the asphalt ball as mentioned above is between 0.1-1.5mm.

本发明的优点: Advantages of the present invention:

1 本专利既可处理直径较小如0.1mm的小球,又可处理直径高达1.5mm的沥青球; 1 This patent can not only process small balls with a diameter as small as 0.1mm, but also process asphalt balls with a diameter as high as 1.5mm;

2 采用两种炉型进行氧化不熔化,在提升产能的同时,避免了沥青氧化过程中的着火,这是沥青氧化过程中最大的安全生产问题;另外,隧道窑的使用还可大大提升产品的氧化均匀性; 2 Two types of furnaces are used for oxidation without melting. While increasing production capacity, it avoids ignition during asphalt oxidation, which is the biggest safety production problem in the process of asphalt oxidation; in addition, the use of tunnel kiln can also greatly improve product safety. Oxidation uniformity;

3由于预先在旋转炉或固定床中进行短时间、大容量的氧化不熔化处理,可扩大最终产品的产能; 3 Due to the short-time, large-capacity oxidation and non-melting treatment in the rotary furnace or fixed bed in advance, the production capacity of the final product can be expanded;

4通过预先在旋转炉或固定床中进行较高温度的氧化不熔化处理,这样可提升后续隧道窑中氧化的起始温度,从而加快氧化不熔化的速度,对提升产能也有一定益处。 4. By performing higher temperature oxidation and non-melting treatment in the rotary furnace or fixed bed in advance, this can increase the initial temperature of oxidation in the subsequent tunnel kiln, thereby speeding up the speed of oxidation and non-melting, and it is also beneficial to increase production capacity.

具体实施方式 Detailed ways

实施例中沥青球氧化不熔化程度可按粘结率计算:将氧化不熔化沥青球在N2气氛中升温到800℃后停留1h,获得炭化沥青球;随机抽取30-50颗炭化后的沥青球,粘附在一起的颗粒总数占总颗粒数的百分比即为粘结率。 In the examples, the degree of oxidized infusibility of asphalt balls can be calculated according to the cohesive rate: heat the oxidized infusible asphalt balls to 800°C in N2 atmosphere and stay there for 1 hour to obtain carbonized asphalt balls; randomly select 30-50 carbonized asphalt balls For balls, the percentage of the total number of particles adhering together to the total number of particles is the cohesion rate.

实施例1 Example 1

在旋转炉内放入100公斤1.5mm的沥青球,通入800升/kg.h的空气,然后以20℃/h升温速率从室温升温到250℃,并停留2h;将该初步氧化的沥青球转入隧道窑内,该隧道窑的温度段分为8段,每段温差20℃,起始温度为150℃,终止温度为310℃,其中通入的空气量为1000升/kg.h。沥青在隧道窑中的总停留时间为15h,获得氧化不熔化沥青球。其粘结率为3.8%。 Put 100 kg of 1.5mm asphalt balls into the rotary furnace, pass in 800 liters/kg.h of air, then raise the temperature from room temperature to 250°C at a heating rate of 20°C/h, and stay for 2h; the initially oxidized asphalt The ball is transferred into the tunnel kiln. The temperature section of the tunnel kiln is divided into 8 sections, the temperature difference of each section is 20°C, the starting temperature is 150°C, and the ending temperature is 310°C. The air volume is 1000 liters/kg.h . The total residence time of asphalt in the tunnel kiln is 15h to obtain oxidized infusible asphalt balls. Its bonding rate is 3.8%.

实施例2 Example 2

在固定床内放入10公斤0.1mm沥青球,通入400升/kg.h的空气,然后以50℃/h升温速率从室温升温到200℃,并停留4h;将该初步氧化的沥青球转入隧道窑内,该隧道窑的温度段分为5段,每段温差30℃,起始温度为180℃,终止温度为330℃,其中通入的空气量为300升/kg.h。沥青在隧道窑中的总停留时间为7h,获得氧化不熔化沥青球。其粘结率为5.7%。 Put 10 kg of 0.1mm asphalt balls into the fixed bed, feed 400 liters/kg.h of air, then raise the temperature from room temperature to 200°C at a heating rate of 50°C/h, and stay for 4 hours; the initially oxidized asphalt balls Turning into the tunnel kiln, the temperature section of the tunnel kiln is divided into 5 sections, each section has a temperature difference of 30°C, the starting temperature is 180°C, and the ending temperature is 330°C, and the air volume is 300 liters/kg.h. The total residence time of asphalt in the tunnel kiln is 7h to obtain oxidized infusible asphalt balls. Its bonding rate is 5.7%.

实施例3 Example 3

在旋转炉内放入30公斤1.2mm沥青球,通入600升/kg.h的空气,然后以30℃/h升温速率从室温升温到230℃,并停留3h;将该初步氧化的沥青球转入隧道窑内,该隧道窑的温度段分为6段,每段温差25℃,起始温度为160℃,终止温度为310℃,其中通入的空气量为800升/kg.h。沥青在隧道窑中的总停留时间为13h,获得氧化不熔化沥青球。其粘结率为2.4%。 Put 30 kg of 1.2mm asphalt balls into the rotary furnace, feed 600 liters/kg.h of air, then raise the temperature from room temperature to 230°C at a heating rate of 30°C/h, and stay for 3h; the initially oxidized asphalt balls Turning into the tunnel kiln, the temperature section of the tunnel kiln is divided into 6 sections, each section has a temperature difference of 25°C, the starting temperature is 160°C, and the ending temperature is 310°C, and the air volume is 800 liters/kg.h. The total residence time of asphalt in the tunnel kiln is 13h to obtain oxidized infusible asphalt balls. Its bonding rate is 2.4%.

实施例4 Example 4

在固定床内放入4公斤1.0mm的沥青球,通入500升/kg.h的空气,然后以35℃/h升温速率从室温升温到180℃,并停留5h;将该初步氧化的沥青球转入隧道窑内,该隧道窑的温度段分为10段,每段温差30℃,起始温度为150℃,终止温度为350℃,其中通入的空气量为500升/kg.h。沥青在隧道窑中的总停留时间为12h,获得氧化不熔化沥青球。其粘结率为2.1%。 Put 4 kg of 1.0mm asphalt balls in the fixed bed, pass in 500 liters/kg.h of air, then raise the temperature from room temperature to 180°C at a heating rate of 35°C/h, and stay for 5h; the initially oxidized asphalt The ball is transferred into the tunnel kiln. The temperature section of the tunnel kiln is divided into 10 sections, the temperature difference of each section is 30°C, the starting temperature is 150°C, and the ending temperature is 350°C. The air volume is 500 liters/kg.h . The total residence time of asphalt in the tunnel kiln is 12h to obtain oxidized infusible asphalt balls. Its bonding ratio is 2.1%.

实施例5 Example 5

在固定床内放入0.5公斤0.5mm的沥青球,通入200升/kg.h的空气,然后以40℃/h升温速率从室温升温到180℃,并停留3h;将该初步氧化的沥青球转入隧道窑内,该隧道窑的温度段分为7段,每段温差20℃,起始温度为150℃,终止温度为290℃,其中通入的空气量为500升/kg.h。沥青在隧道窑中的总停留时间为8h,获得氧化不熔化沥青球。其粘结率为1.2%。 Put 0.5kg of 0.5mm asphalt balls in the fixed bed, pass in 200 liters/kg.h of air, then raise the temperature from room temperature to 180°C at a heating rate of 40°C/h, and stay for 3h; the initially oxidized asphalt The ball is transferred into the tunnel kiln. The temperature section of the tunnel kiln is divided into 7 sections, the temperature difference of each section is 20°C, the starting temperature is 150°C, and the ending temperature is 290°C. The air volume is 500 liters/kg.h . The total residence time of asphalt in the tunnel kiln is 8h to obtain oxidized infusible asphalt balls. Its bonding rate is 1.2%.

实施例6 Example 6

在旋转炉内放入1000公斤0.3mm沥青球,通入300升/kg.h的空气,然后以45℃/h升温速率从室温升温到240℃,并停留2h;将该初步氧化的沥青球转入隧道窑内,该隧道窑的温度段分为5段,每段温差20℃,起始温度为220℃,终止温度为320℃,其中通入的空气量为500升/kg.h。沥青在隧道窑中的总停留时间为70h,获得氧化不熔化沥青球。其粘结率为0.8%。 Put 1000 kilograms of 0.3mm asphalt balls into the rotary furnace, pass in 300 liters/kg.h of air, then raise the temperature from room temperature to 240°C at a heating rate of 45°C/h, and stay for 2h; the initially oxidized asphalt balls Turning into the tunnel kiln, the temperature section of the tunnel kiln is divided into 5 sections, each section has a temperature difference of 20°C, the starting temperature is 220°C, and the ending temperature is 320°C, and the air volume is 500 liters/kg.h. The total residence time of asphalt in the tunnel kiln is 70h to obtain oxidized infusible asphalt balls. Its bonding rate is 0.8%.

Claims (2)

1.一种沥青球氧化不熔化方法,其特征在于包括如下步骤: 1. a kind of asphalt ball oxidation non-melting method is characterized in that comprising the steps: (1)在装有沥青球的旋转炉或固定床反应器中,按每公斤沥青球每小时需要200-800升空气通入空气;以20-50℃/h升温速率从室温升温到180-250℃,停留2-5h,获得初步氧化的沥青球; (1) In a rotary furnace or a fixed bed reactor equipped with asphalt balls, 200-800 liters of air is required per kilogram of asphalt balls per hour to feed the air; the temperature is raised from room temperature to 180-180- 250°C, stay for 2-5 hours, and obtain the initially oxidized asphalt balls; (2)初步氧化的沥青球在隧道窑中进一步进行氧化处理,隧道窑分为5-10段,下一段的温度与上一段的温度相差20-40℃,起始温度为150-220℃,终止温度为290-350℃,沥青在隧道窑中的总停留时间为7-15h,获得氧化不熔化沥青球,其中通入的空气量按每小时每公斤沥青球300-1000升的空气量。 (2) The initially oxidized asphalt balls are further oxidized in the tunnel kiln. The tunnel kiln is divided into 5-10 sections. The temperature difference between the next section and the previous section is 20-40°C, and the initial temperature is 150-220°C. The termination temperature is 290-350°C, and the total residence time of the asphalt in the tunnel kiln is 7-15 hours to obtain oxidized and non-melting asphalt balls, wherein the air volume introduced is 300-1000 liters of air per kilogram of asphalt balls per hour. 2.如权利要求1所述的一种沥青球氧化不熔化方法,其特征在于所述的沥青球的球径在0.1-1.5mm之间。 2. A kind of asphalt ball oxidation non-melting method as claimed in claim 1, is characterized in that the ball diameter of described pitch ball is between 0.1-1.5mm.
CN201310227294.7A 2013-06-08 2013-06-08 Pitch sphere oxidative stabilization method Active CN103272533B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201310227294.7A CN103272533B (en) 2013-06-08 2013-06-08 Pitch sphere oxidative stabilization method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201310227294.7A CN103272533B (en) 2013-06-08 2013-06-08 Pitch sphere oxidative stabilization method

Publications (2)

Publication Number Publication Date
CN103272533A CN103272533A (en) 2013-09-04
CN103272533B true CN103272533B (en) 2015-01-07

Family

ID=49055215

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201310227294.7A Active CN103272533B (en) 2013-06-08 2013-06-08 Pitch sphere oxidative stabilization method

Country Status (1)

Country Link
CN (1) CN103272533B (en)

Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104276569B (en) * 2014-10-21 2016-01-27 中国科学院山西煤炭化学研究所 A method for improving the crushing strength of pitch-based spherical activated carbon
CN104927890B (en) * 2015-06-09 2017-03-08 中国科学院山西煤炭化学研究所 Large-scale preparation process and device for oxidizing and infusible pitch pellets
CN105253884B (en) * 2015-11-12 2017-09-26 山西新华化工有限责任公司 Do not melt method for the oxidation for industrializing bitumen ball activated carbon
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
CN106350089B (en) * 2016-08-30 2021-10-26 中国科学院山西煤炭化学研究所 Process for preparing asphalt balls by continuous method
CN106318425B (en) * 2016-08-30 2019-01-11 中国科学院山西煤炭化学研究所 One kind micro mist containing naphthalene pitch prepares grade bitumen ball method
CN111017905A (en) * 2020-02-25 2020-04-17 山西中纳合创科技有限公司 Method for preparing oxidized infusible carbon material under pressure
CN111500304B (en) * 2020-04-17 2021-03-26 中国科学院山西煤炭化学研究所 Pretreatment method for asphalt ball oxidation non-melting

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH05193918A (en) * 1992-01-23 1993-08-03 Toho Gas Co Ltd Production of fine carbon particle
CN1048955C (en) * 1996-12-24 2000-02-02 中国科学院山西煤炭化学研究所 Method for producing activated carbon with high specific surface area from asphalt

Also Published As

Publication number Publication date
CN103272533A (en) 2013-09-04

Similar Documents

Publication Publication Date Title
CN103272533B (en) Pitch sphere oxidative stabilization method
CN104909365B (en) Bitumen ball aoxidizes nonfused promotion method
CN104118874B (en) A kind of preparation method of gac/graphene complex
CN104499097A (en) Method for preparing active carbon fibers by utilizing hydrogen peroxide intensified water vapor to activate
CN101721972B (en) A preparation method of spherical activated carbon with large adsorption capacity for CO2
CN103508437A (en) Preparation method of phenolic resin-based glass carbon microspheres
CN105734271A (en) Pellet containing chromium, vanadium and titanium and production method of pellet
CN103908143A (en) Activated carbon fiber curtain
CN105803141A (en) High-chrome vanadium-titanium magnetite blast furnace smelting charging material and blast furnace smelting method
CN105820859A (en) Preparation method of titanium dioxide nano-particle modified transformer oil
CN105217602A (en) The brilliant material preparation method of a kind of pitch base carbon
CN102795624B (en) Low energy consumption preparation method of pitch-based spherical activated carbon
CN105000562A (en) Preparation method of silicon carbide hollow sphere
CN104087746B (en) A kind of preparation method of magnesia titaniferous pellet
CN103320902B (en) A kind of bio-based activated carbon fibre filtering material and preparation method thereof
CN101219784A (en) Preparation method of polyacrylonitrile-based carbon nanospheres
CN106318425B (en) One kind micro mist containing naphthalene pitch prepares grade bitumen ball method
CN102515731A (en) Magnesium silicate ceramic fibre and preparation method therof
CN103387403A (en) Spinel/graphene composite powder for refractory material and preparation method thereof
CN106115687B (en) Method is not melted in the oxidation of flow-type bitumen ball
CN106222402B (en) A kind of production method of ilmenite concentrate pelletizing
KR101425375B1 (en) post-treatment method of carbon materials using dehydrocyclization and post-treated carbon materials using the same and polymer composite materials comprising thereof
CN105253884A (en) Melting-free oxidation method for industrialized pitch ball activated carbon
CN105198226A (en) Forsterite fiber and preparation method thereof
CN103695019A (en) Low energy one-step method for preparing asphalt balls

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant