CN110407209A - A kind of method that biomass prepares active carbon - Google Patents
A kind of method that biomass prepares active carbon Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 139
- 239000002028 Biomass Substances 0.000 title claims abstract description 74
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 26
- 238000000197 pyrolysis Methods 0.000 claims abstract description 74
- 230000004913 activation Effects 0.000 claims abstract description 70
- 239000007789 gas Substances 0.000 claims abstract description 31
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- 238000002485 combustion reaction Methods 0.000 claims abstract description 19
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 238000005406 washing Methods 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 6
- 239000003610 charcoal Substances 0.000 claims description 28
- 241000209094 Oryza Species 0.000 claims description 15
- 235000007164 Oryza sativa Nutrition 0.000 claims description 15
- 239000012190 activator Substances 0.000 claims description 15
- 239000010903 husk Substances 0.000 claims description 15
- 235000009566 rice Nutrition 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 8
- 239000001301 oxygen Substances 0.000 claims description 8
- 229910052760 oxygen Inorganic materials 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 5
- 229910000272 alkali metal oxide Inorganic materials 0.000 claims description 5
- 150000001340 alkali metals Chemical class 0.000 claims description 5
- 229910001860 alkaline earth metal hydroxide Inorganic materials 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 239000012065 filter cake Substances 0.000 claims description 5
- 239000000706 filtrate Substances 0.000 claims description 5
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical group O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 claims description 5
- 238000005470 impregnation Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 229910001414 potassium ion Inorganic materials 0.000 claims description 5
- 239000000047 product Substances 0.000 claims description 5
- 239000000376 reactant Substances 0.000 claims description 5
- 238000004064 recycling Methods 0.000 claims description 5
- 238000011144 upstream manufacturing Methods 0.000 claims description 5
- 125000000969 xylosyl group Chemical group C1([C@H](O)[C@@H](O)[C@H](O)CO1)* 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims 2
- 239000002296 pyrolytic carbon Substances 0.000 claims 2
- 238000007598 dipping method Methods 0.000 claims 1
- 238000007599 discharging Methods 0.000 claims 1
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 2
- 238000010924 continuous production Methods 0.000 abstract description 2
- 239000001257 hydrogen Substances 0.000 abstract description 2
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 2
- 238000001816 cooling Methods 0.000 abstract 1
- 230000002349 favourable effect Effects 0.000 abstract 1
- 238000004806 packaging method and process Methods 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 description 4
- 238000001914 filtration Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 125000003172 aldehyde group Chemical group 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 125000004185 ester group Chemical group 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 239000010902 straw Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
- C01B32/324—Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/336—Preparation characterised by gaseous activating agents
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/342—Preparation characterised by non-gaseous activating agents
- C01B32/348—Metallic compounds
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Materials Engineering (AREA)
- Carbon And Carbon Compounds (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
一种生物质制备活性炭的方法，属于生物质能源化工领域，包括：1)生物质热解生产热解气和热解炭；2)热解气引入中温蒸汽锅炉加热生产中温蒸汽，再引入高温蒸汽锅炉，同时引入中温蒸汽，燃烧加热高温蒸汽温度至850℃～950℃，引入回转活化炉；3)浸渍生物质炭从回转活化炉顶端加入，与高温蒸汽逆流行进，进入反应区，与从回转活化炉底端引入的高温蒸汽混合，活化反应生产活性炭，下行从回转活化炉尾端排出，经间接换热，降温，经水洗、干燥、包装；4)富氢气体上行加热浸渍生物质炭，引入燃烧炉燃烧生产高温蒸汽。本发明的方法生产活性炭能耗小、成本低，收率高，有利于连续化生产和规模放大。A method for preparing activated carbon from biomass belongs to the field of biomass energy chemical industry, and includes: 1) biomass pyrolysis to produce pyrolysis gas and pyrolysis carbon; 2) the pyrolysis gas is introduced into a medium-temperature steam boiler for heating to produce medium-temperature steam, and then high-temperature steam is introduced In the steam boiler, medium-temperature steam is introduced at the same time, and the temperature of the high-temperature steam is heated to 850 ° C ~ 950 ° C, and then introduced into the rotary activation furnace; 3) The impregnated biomass char is added from the top of the rotary activation furnace, and flows in countercurrent with the high-temperature steam, and enters the reaction zone. The high-temperature steam introduced at the bottom of the rotary activation furnace is mixed, activated and reacted to produce activated carbon, which is discharged downward from the end of the rotary activation furnace, and undergoes indirect heat exchange, cooling, washing, drying, and packaging; 4) The hydrogen-rich gas is heated upward to impregnate the biomass carbon. , the introduction of combustion furnace combustion to produce high-temperature steam. The method of the invention for producing activated carbon has low energy consumption, low cost and high yield, and is favorable for continuous production and scale enlargement.
Description
技术领域technical field
本发明属于生物质能源化工领域，具体公开了一种生物质制备活性炭的方法。The invention belongs to the field of biomass energy chemical industry, and specifically discloses a method for preparing activated carbon from biomass.
背景技术Background technique
活性炭吸附性能优异，性质稳定，循环再生性好，被广泛应用于化学吸附脱色、环境治理等领域。但传统的活性炭制备原料多为不可再生资源，高质量的活性炭价格高，再生效率低，严重制约其大规模的工业应用。以农林废弃物为原料，不仅可降低成本，还可使农林废弃物得到资源化利用，同时还避免了无组织焚烧带来的环境污染问题。我国植物秸秆资源丰富，为制备活性炭提供了丰富的原料，但是水蒸气活化制备生物质基活性炭，最大的问题是生物质炭质轻、空隙多、容易燃烧，不能采用直接加热的办法制备活性炭，而采用间接加热水蒸气活化又存在能耗高、设备复杂、成本高的问题，无法与传统水蒸气活化法制备的活性炭竞争。Activated carbon has excellent adsorption performance, stable properties and good recyclability, and is widely used in chemical adsorption decolorization, environmental treatment and other fields. However, most of the traditional activated carbon preparation raw materials are non-renewable resources, high-quality activated carbon is expensive, and the regeneration efficiency is low, which seriously restricts its large-scale industrial application. Using agricultural and forestry wastes as raw materials not only reduces costs, but also enables agricultural and forestry wastes to be utilized as resources, and at the same time avoids environmental pollution problems caused by unorganized incineration. my country is rich in plant straw resources, which provide abundant raw materials for the preparation of activated carbon. However, the biggest problem in the preparation of biomass-based activated carbon by steam activation is that biomass carbon is light in weight, has many voids, and is easy to burn. Direct heating cannot be used to prepare activated carbon. However, the use of indirect heating steam activation has the problems of high energy consumption, complex equipment and high cost, and cannot compete with the activated carbon prepared by the traditional steam activation method.
如何解决生物质炭水蒸气活化的加热方法，如何提高收率，已经成为生物质基活性炭发展的障碍，因此现有技术中需要一种新的技术方案解决这些问题。How to solve the heating method of biomass carbon steam activation and how to improve the yield has become an obstacle to the development of biomass-based activated carbon, so a new technical solution is needed in the prior art to solve these problems.
发明内容SUMMARY OF THE INVENTION
本发明的目的是提供一种生物质制备活性炭的方法，采用该方法生产活性炭能耗小、成本低，有利于连续化生产和规模放大。The purpose of the present invention is to provide a method for preparing activated carbon from biomass, which has low energy consumption and low cost for producing activated carbon, and is beneficial to continuous production and scale enlargement.
为实现上述目的，本发明采用如下的技术方案：一种生物质制备活性炭的方法，其特征在于，该方法包括如下步骤：To achieve the above object, the present invention adopts the following technical scheme: a method for preparing activated carbon from biomass, characterized in that the method comprises the following steps:
步骤一、生物质热解：Step 1. Biomass pyrolysis:
生物质粉碎至粒径30mm～100mm，经斗氏提升机加入热解塔，调整进入热解区的氧含量，使热解段温度保持在600℃～700℃，热解0.5h～1.0h，生物质分解为热解气和热解炭；The biomass is pulverized to a particle size of 30mm-100mm, and is added to the pyrolysis tower through a bucket elevator to adjust the oxygen content entering the pyrolysis zone, so that the temperature of the pyrolysis section is maintained at 600℃～700℃, and the pyrolysis is performed for 0.5h～1.0h. Biomass is decomposed into pyrolysis gas and pyrolysis carbon;
步骤二、热解气生产高温蒸汽：Step 2. Pyrolysis gas to produce high temperature steam:
将所述步骤一中得到的600℃～700℃的热解气引入中温蒸汽锅炉间接加热生产温度为150℃～180℃的中温蒸汽，再同时将热解气和中温蒸汽引入高温蒸汽锅炉，燃烧加热至850℃～950℃，生产高温蒸汽；The pyrolysis gas at 600°C to 700°C obtained in the step 1 is introduced into a medium temperature steam boiler for indirect heating to produce medium temperature steam with a temperature of 150°C to 180°C, and then the pyrolysis gas and the medium temperature steam are introduced into the high temperature steam boiler at the same time for combustion. Heating to 850℃～950℃ to produce high temperature steam;
步骤三、活化剂浸渍：Step three, activator impregnation:
按质量比为100：(1～3)将生物质炭与活化剂溶液喷淋混合均匀，再浸渍6h～12h，制备浸渍生物质炭；According to the mass ratio of 100: (1-3), the biomass charcoal and the activator solution are sprayed and mixed evenly, and then impregnated for 6h-12h to prepare the impregnated biomass charcoal;
步骤四、生物质炭活化：Step 4. Biochar activation:
将步骤二制备的高温蒸汽从带有倾角的回转活化炉炉底部加入，逆流上行，到达活化区；将步骤三制备的浸渍生物质炭从回转活化炉顶部加入，顺流下行，到达反应区，在温度为850℃～950℃的条件下，进行活化反应，产物气体经过上部反应物加入区，加热浸渍生物质炭，引入燃烧炉燃烧制备高温蒸汽；粗品活性炭从回转活化炉底部排出；The high-temperature steam prepared in step 2 is added from the bottom of the rotary activation furnace with an inclination angle, and the upstream is countercurrent to reach the activation zone; the impregnated biomass charcoal prepared in step 3 is added from the top of the rotary activation furnace, and flows downstream to reach the reaction zone, The activation reaction is carried out at a temperature of 850°C to 950°C. The product gas passes through the upper reactant addition zone, heats and impregnates the biomass carbon, and is introduced into the combustion furnace for combustion to prepare high-temperature steam; the crude activated carbon is discharged from the bottom of the rotary activation furnace;
步骤五、水洗干燥：Step 5. Wash and dry:
按照质量比为1:10将步骤四的粗品活性炭和去离子水加入到水洗釜中，第一次水洗、过滤，收集滤液返回步骤三循环利用，滤饼再水洗、过滤，至pH值为7，转移到干燥炉，在120℃干燥12h，活性炭出料、降温、包装。According to the mass ratio of 1:10, the crude activated carbon and deionized water of step 4 are added to the washing kettle, and the first time is washed and filtered, and the collected filtrate is returned to step 3 for recycling, and the filter cake is washed and filtered again to pH 7 , transferred to a drying oven, dried at 120 ℃ for 12h, activated carbon was discharged, cooled and packaged.
进一步，所述热解塔、中温蒸汽锅炉、高温蒸汽锅炉及回转活化炉首尾相连。Further, the pyrolysis tower, the medium temperature steam boiler, the high temperature steam boiler and the rotary activation furnace are connected end to end.
进一步，所述步骤四中从浸渍生物质炭加入到粗品活性炭从底部排出的时间为1h～2h。Further, in the step 4, the time from adding the impregnated biomass carbon to the crude activated carbon being discharged from the bottom is 1 h to 2 h.
进一步，所述步骤四中回转活化炉采用变频调节的方式回转，转速为10r/min～15r/min。Further, in the step 4, the rotary activation furnace is rotated by means of frequency conversion adjustment, and the rotating speed is 10r/min～15r/min.
进一步，所述步骤四中回转活化炉升降角度10°～30°。Further, in the step 4, the lifting angle of the rotary activation furnace is 10°˜30°.
进一步，所述步骤四中用于活化的生物质炭是稻壳热解炭、酸处理除氧化物的净化稻壳热解炭或稻壳热解炭脱硅后炭粉。Further, the biomass carbon used for activation in the step 4 is rice husk pyrolysis carbon, acid-treated deoxidized purified rice husk pyrolysis carbon or rice husk pyrolysis carbon desiliconized carbon powder.
进一步，所述步骤四中用于活化的生物质炭是糠醛渣经水洗、干燥、炭化处理后的炭粉，或木糖渣经水洗、干燥、炭化处理后的炭粉。Further, the biomass carbon used for activation in the step 4 is the carbon powder after the furfural residue is washed, dried and carbonized, or the carbon powder after the xylose residue is washed, dried and carbonized.
进一步，所述步骤三中的活化剂是含有钾离子的碱金属和碱土金属氢氧化物的混合物。Further, the activator in the third step is a mixture of alkali metal and alkaline earth metal hydroxides containing potassium ions.
通过上述设计方案，本发明可以带来如下有益效果：Through the above-mentioned design scheme, the present invention can bring the following beneficial effects:
1、采用热解气燃烧加热水蒸气制备高温蒸汽，与净化炭进行水蒸气活化反应，加入K+催化形成含氧官能团(醇羟基、酚羟基-OH，醛基/酯基C＝O，羧基-COOH)，增加活性炭活性。1. Use pyrolysis gas to burn and heat water vapor to prepare high-temperature steam, conduct water vapor activation reaction with purified carbon, and add K+ to catalyze the formation of oxygen-containing functional groups (alcoholic hydroxyl group, phenolic hydroxyl group-OH, aldehyde group/ester group C=O, carboxyl group- COOH), increasing the activity of activated carbon.
2、水蒸气活化生物质炭制备活性炭，最大的问题是生物质炭容易燃烧，不能采用直接加热的办法，而采用间接加热活化又存在能耗高、设备复杂、成本高的问题，无法与传统水蒸气活化法制备的活性炭竞争。采用热解气燃烧加热水蒸气制备高温蒸汽，与净化炭进行水蒸气活化反应，提高活性，增加产率。2. The biggest problem in the preparation of activated carbon by steam activation of biomass charcoal is that biomass charcoal is easy to burn, so direct heating cannot be used, and indirect heating activation has the problems of high energy consumption, complex equipment and high cost, which cannot be compared with traditional heating methods. Competitive activated carbon prepared by steam activation method. The pyrolysis gas is used to burn and heat water vapor to prepare high-temperature steam, and the water vapor activation reaction is carried out with the purified carbon to improve the activity and increase the yield.
3、活化产生的氢气和CO可以用于燃烧加热蒸汽制备高温蒸汽，不用外加能源。3. The hydrogen and CO generated by the activation can be used for burning and heating steam to prepare high-temperature steam without additional energy.
4、本发明将热解炉、中温蒸汽锅炉、高温蒸汽炉、水蒸气活化炉首尾相连，衔接紧密，避免能量损失，更主要优势是容易规模放大和连续给料。4. The present invention connects the pyrolysis furnace, the medium temperature steam boiler, the high temperature steam furnace and the steam activation furnace end to end, and the connection is tight, so as to avoid energy loss, and the main advantage is easy scale enlargement and continuous feeding.
5、在燃烧加热蒸汽过程中，缺氧燃烧控制反应温度，燃烧尾气中不含氧，保证后续工序中在不含氧状态下进行，操作安全。5. In the process of burning and heating steam, oxygen-deficient combustion controls the reaction temperature, and the combustion exhaust gas does not contain oxygen, ensuring that the subsequent process is carried out in an oxygen-free state and the operation is safe.
具体实施方式Detailed ways
为了更清楚地说明本发明，下面结合优选实施例对本发明做进一步的说明。本领域技术人员应当理解，下面所具体描述的内容是说明性的而非限制性的，不应以此限制本发明的保护范围。为了避免混淆本发明的实质，公知的方法和过程并没有详细的叙述。In order to illustrate the present invention more clearly, the present invention will be further described below with reference to the preferred embodiments. Those skilled in the art should understand that the content specifically described below is illustrative rather than restrictive, and should not limit the protection scope of the present invention. In order to avoid obscuring the essence of the present invention, well-known methods and procedures have not been described in detail.
实施例1Example 1
步骤一、生物质热解：Step 1. Biomass pyrolysis:
生物质粉碎至粒径30mm～100mm，经斗氏提升机加入热解塔，调整进入热解区的氧含量，使热解段温度保持在650℃，热解1.0h，生物质分解为热解气和热解炭；The biomass is pulverized to a particle size of 30mm-100mm, and is added to the pyrolysis tower through a bucket elevator to adjust the oxygen content entering the pyrolysis zone, so that the temperature of the pyrolysis section is maintained at 650 °C for 1.0h, and the biomass is decomposed into pyrolysis. Gas and pyrolysis carbon;
步骤二、热解气生产高温蒸汽：Step 2. Pyrolysis gas to produce high temperature steam:
将所述步骤一中得到的650℃的热解气引入中温蒸汽锅炉间接加热生产温度为150℃的中温蒸汽，再同时将热解气和中温蒸汽引入高温蒸汽锅炉，燃烧加热至900℃，生产高温蒸汽；The pyrolysis gas at 650°C obtained in the step 1 is introduced into a medium-temperature steam boiler to indirectly heat the medium-temperature steam with a production temperature of 150°C, and then the pyrolysis gas and the medium-temperature steam are introduced into a high-temperature steam boiler at the same time, and the combustion is heated to 900°C. high temperature steam;
步骤三、活化剂浸渍：Step three, activator impregnation:
按质量比为100：3将生物质炭与活化剂溶液喷淋混合均匀，再浸渍8h，制备浸渍生物质炭；According to the mass ratio of 100:3, the biomass charcoal and the activator solution are sprayed and mixed evenly, and then impregnated for 8 hours to prepare the impregnated biomass charcoal;
步骤四、生物质炭活化：Step 4. Biochar activation:
将步骤二制备的高温蒸汽从带有倾角的回转活化炉炉底部加入，逆流上行，到达活化区；将步骤三制备的浸渍生物质炭从回转活化炉顶部加入，顺流下行，到达反应区，在温度为900℃的条件下，进行活化反应，产物气体经过上部反应物加入区，加热浸渍生物质炭，引入燃烧炉燃烧制备高温蒸汽；粗品活性炭从回转活化炉底部排出；The high-temperature steam prepared in step 2 is added from the bottom of the rotary activation furnace with an inclination angle, and the upstream is countercurrent to reach the activation zone; the impregnated biomass charcoal prepared in step 3 is added from the top of the rotary activation furnace, and flows downstream to reach the reaction zone, Under the condition of temperature of 900℃, the activation reaction is carried out. The product gas passes through the upper reactant addition zone, heats and impregnates the biomass carbon, and is introduced into the combustion furnace for combustion to prepare high-temperature steam; the crude activated carbon is discharged from the bottom of the rotary activation furnace;
步骤五、水洗干燥：Step 5. Wash and dry:
按照质量比为1：10将步骤四的粗品活性炭和去离子水加入到水洗釜中，第一次水洗、过滤，收集滤液返回步骤三循环利用，滤饼再水洗、过滤，至pH值为7，转移到干燥炉，在120℃干燥12h，活性炭出料、降温、包装。According to the mass ratio of 1:10, the crude activated carbon and deionized water of step 4 are added to the washing kettle, the first time washing and filtration, the filtrate is collected and returned to step 3 for recycling, and the filter cake is washed and filtered again to pH 7 , transferred to a drying oven, dried at 120 ℃ for 12h, activated carbon was discharged, cooled and packaged.
其中，所述热解塔、中温蒸汽锅炉、高温蒸汽锅炉及回转活化炉首尾相连，紧密衔接，反应连续进行，避免能量损失。Among them, the pyrolysis tower, the medium temperature steam boiler, the high temperature steam boiler and the rotary activation furnace are connected end to end and are closely connected, and the reaction is carried out continuously to avoid energy loss.
其中，所述步骤四中从浸渍生物质炭加入到粗品活性炭从底部排出的时间为1h～2h。Wherein, in the step 4, the time from adding the impregnated biomass carbon to the crude activated carbon being discharged from the bottom is 1 h to 2 h.
其中，所述步骤四中回转活化炉采用变频调节的方式回转，转速为10r/min～15r/min。Wherein, in the step 4, the rotary activation furnace is rotated by means of frequency conversion adjustment, and the rotating speed is 10r/min～15r/min.
其中，所述步骤四中回转活化炉升降角度为10°～30°。Wherein, in the step 4, the lifting angle of the rotary activation furnace is 10°˜30°.
其中，所述步骤四中用于活化的生物质炭是稻壳热解炭、酸处理除氧化物的净化稻壳热解炭或稻壳热解炭脱硅后炭粉。Wherein, the biomass char used for activation in the step 4 is rice husk pyrolysis charcoal, acid-treated deoxidized purified rice husk pyrolysis charcoal or rice husk pyrolysis charcoal desiliconized carbon powder.
其中，所述步骤四中用于活化的生物质炭是糠醛渣经水洗、干燥、炭化处理后的炭粉，或木糖渣经水洗、干燥、炭化处理后的炭粉。Wherein, the biomass carbon used for activation in the step 4 is the carbon powder after the furfural residue is washed, dried and carbonized, or the carbon powder after the xylose residue is washed, dried and carbonized.
其中，所述步骤三中的活化剂是含有钾离子的碱金属和碱土金属氢氧化物的混合物。Wherein, the activator in the third step is a mixture of alkali metal and alkaline earth metal hydroxides containing potassium ions.
实施例2Example 2
步骤一、生物质热解：Step 1. Biomass pyrolysis:
生物质粉碎至粒径30mm～100mm，经斗氏提升机加入热解塔，调整进入热解区的氧含量，使热解段温度保持在600℃，热解0.5h，生物质分解为热解气和热解炭；The biomass is pulverized to a particle size of 30mm-100mm, and is added to the pyrolysis tower through a bucket elevator to adjust the oxygen content entering the pyrolysis zone, so that the temperature of the pyrolysis section is kept at 600 °C, and the pyrolysis is 0.5h. The biomass is decomposed into pyrolysis Gas and pyrolysis carbon;
步骤二、热解气生产高温蒸汽：Step 2. Pyrolysis gas to produce high temperature steam:
将所述步骤一中得到的600℃的热解气引入中温蒸汽锅炉间接加热生产温度为160℃的中温蒸汽，再同时将热解气和中温蒸汽引入高温蒸汽锅炉，燃烧加热至850℃，生产高温蒸汽；The pyrolysis gas at 600°C obtained in the step 1 is introduced into a medium-temperature steam boiler for indirect heating to produce medium-temperature steam with a temperature of 160°C, and the pyrolysis gas and the medium-temperature steam are introduced into a high-temperature steam boiler at the same time, and the combustion is heated to 850°C. high temperature steam;
步骤三、活化剂浸渍：Step three, activator impregnation:
按质量比为100：1将生物质炭与活化剂溶液喷淋混合均匀，再浸渍6h，制备浸渍生物质炭；According to the mass ratio of 100:1, the biomass charcoal and the activator solution are sprayed and mixed evenly, and then impregnated for 6 hours to prepare the impregnated biomass charcoal;
步骤四、生物质炭活化：Step 4. Biochar activation:
将步骤二制备的高温蒸汽从带有倾角的回转活化炉炉底部加入，逆流上行，到达活化区；将步骤三制备的浸渍生物质炭从回转活化炉顶部加入，顺流下行，到达反应区，在温度为850℃的条件下，进行活化反应，产物气体经过上部反应物加入区，加热浸渍生物质炭，引入燃烧炉燃烧制备高温蒸汽；粗品活性炭从回转活化炉底部排出；The high-temperature steam prepared in step 2 is added from the bottom of the rotary activation furnace with an inclination angle, and the upstream is countercurrent to reach the activation zone; the impregnated biomass charcoal prepared in step 3 is added from the top of the rotary activation furnace, and flows downstream to reach the reaction zone, Under the condition of temperature of 850℃, the activation reaction is carried out. The product gas passes through the upper reactant addition zone, heats and impregnates the biomass carbon, and is introduced into the combustion furnace for combustion to prepare high-temperature steam; the crude activated carbon is discharged from the bottom of the rotary activation furnace;
步骤五、水洗干燥：Step 5. Wash and dry:
按照质量比为1：10将步骤四的粗品活性炭和去离子水加入到水洗釜中，第一次水洗、过滤，收集滤液返回步骤三循环利用，滤饼再水洗、过滤，至pH值为7，转移到干燥炉，在120℃干燥12h，活性炭出料、降温、包装。According to the mass ratio of 1:10, the crude activated carbon and deionized water of step 4 are added to the washing kettle, the first time washing and filtration, the filtrate is collected and returned to step 3 for recycling, and the filter cake is washed and filtered again to pH 7 , transferred to a drying oven, dried at 120 ℃ for 12h, activated carbon was discharged, cooled and packaged.
其中，所述热解塔、中温蒸汽锅炉、高温蒸汽锅炉及回转活化炉首尾相连，紧密衔接，反应连续进行，避免能量损失。Among them, the pyrolysis tower, the medium temperature steam boiler, the high temperature steam boiler and the rotary activation furnace are connected end to end and are closely connected, and the reaction is carried out continuously to avoid energy loss.
其中，所述步骤四中从浸渍生物质炭加入到粗品活性炭从底部排出的时间为1h～2h。Wherein, in the step 4, the time from adding the impregnated biomass carbon to the crude activated carbon being discharged from the bottom is 1 h to 2 h.
其中，所述步骤四中回转活化炉采用变频调节的方式回转，转速为10r/min～15r/min。Wherein, in the step 4, the rotary activation furnace is rotated by means of frequency conversion adjustment, and the rotating speed is 10r/min～15r/min.
其中，所述步骤四中回转活化炉升降角度为10°～30°。Wherein, in the step 4, the lifting angle of the rotary activation furnace is 10°˜30°.
其中，所述步骤四中用于活化的生物质炭是稻壳热解炭、酸处理除氧化物的净化稻壳热解炭、稻壳热解炭脱硅后炭粉的一种。Wherein, the biomass carbon used for activation in the step 4 is one of rice husk pyrolysis carbon, acid-treated and deoxidized purified rice husk pyrolysis carbon, and desiliconized carbon powder of rice husk pyrolysis carbon.
其中，所述步骤四中用于活化的生物质炭是糠醛渣经水洗、干燥、炭化处理后的炭粉，或木糖渣经水洗、干燥、炭化处理后的炭粉。Wherein, the biomass carbon used for activation in the step 4 is the carbon powder after the furfural residue is washed, dried and carbonized, or the carbon powder after the xylose residue is washed, dried and carbonized.
其中，所述步骤三中的活化剂是含有钾离子的碱金属和碱土金属氢氧化物的混合物。Wherein, the activator in the third step is a mixture of alkali metal and alkaline earth metal hydroxides containing potassium ions.
实施例3Example 3
步骤一、生物质热解：Step 1. Biomass pyrolysis:
生物质粉碎至粒径30mm～100mm，经斗氏提升机加入热解塔，调整进入热解区的氧含量，使热解段温度保持在700℃，热解1.0h，生物质分解为热解气和热解炭；The biomass is pulverized to a particle size of 30mm-100mm, and is added to the pyrolysis tower through a bucket elevator to adjust the oxygen content entering the pyrolysis zone, so that the temperature of the pyrolysis section is kept at 700 ° C, and the pyrolysis is 1.0h, and the biomass is decomposed into pyrolysis. Gas and pyrolysis carbon;
步骤二、热解气生产高温蒸汽：Step 2. Pyrolysis gas to produce high temperature steam:
将所述步骤一中得到的700℃的热解气引入中温蒸汽锅炉间接加热生产温度为180℃的中温蒸汽，再同时将热解气和中温蒸汽引入高温蒸汽锅炉，燃烧加热至950℃，生产高温蒸汽；The pyrolysis gas at 700°C obtained in the step 1 was introduced into a medium-temperature steam boiler for indirect heating to produce medium-temperature steam with a temperature of 180°C, and the pyrolysis gas and the medium-temperature steam were introduced into a high-temperature steam boiler at the same time, and the combustion was heated to 950°C. high temperature steam;
步骤三、活化剂浸渍：Step three, activator impregnation:
按质量比为100：2将生物质炭与活化剂溶液喷淋混合均匀，再浸渍6h，制备浸渍生物质炭；According to the mass ratio of 100:2, the biomass charcoal and the activator solution are sprayed and mixed evenly, and then impregnated for 6 hours to prepare the impregnated biomass charcoal;
步骤四、生物质炭活化：Step 4. Biochar activation:
将步骤二制备的高温蒸汽从带有倾角的回转活化炉炉底部加入，逆流上行，到达活化区；将步骤三制备的浸渍生物质炭从回转活化炉顶部加入，顺流下行，到达反应区，在温度为950℃的条件下，进行活化反应，产物气体经过上部反应物加入区，加热浸渍生物质炭，引入燃烧炉燃烧制备高温蒸汽；粗品活性炭从回转活化炉底部排出；The high-temperature steam prepared in step 2 is added from the bottom of the rotary activation furnace with an inclination angle, and the upstream is countercurrent to reach the activation zone; the impregnated biomass charcoal prepared in step 3 is added from the top of the rotary activation furnace, and flows downstream to reach the reaction zone, Under the condition of temperature of 950℃, the activation reaction is carried out, and the product gas passes through the upper reactant addition zone, heats and impregnates the biomass carbon, and is introduced into the combustion furnace for combustion to prepare high-temperature steam; the crude activated carbon is discharged from the bottom of the rotary activation furnace;
步骤五、水洗干燥：Step 5. Wash and dry:
按照质量比为1：10将步骤四的粗品活性炭和去离子水加入到水洗釜中，第一次水洗、过滤，收集滤液返回步骤三循环利用，滤饼再水洗、过滤，至pH值为7，转移到干燥炉，在120℃干燥12h，活性炭出料、降温、包装。According to the mass ratio of 1:10, the crude activated carbon and deionized water of step 4 are added to the washing kettle, the first time washing and filtration, the filtrate is collected and returned to step 3 for recycling, and the filter cake is washed and filtered again to pH 7 , transferred to a drying oven, dried at 120 ℃ for 12h, activated carbon was discharged, cooled and packaged.
其中，所述热解塔、中温蒸汽锅炉、高温蒸汽锅炉及回转活化炉首尾相连，紧密衔接，反应连续进行，避免能量损失。Among them, the pyrolysis tower, the medium temperature steam boiler, the high temperature steam boiler and the rotary activation furnace are connected end to end and are closely connected, and the reaction is carried out continuously to avoid energy loss.
其中，所述步骤四中从浸渍生物质炭加入到粗品活性炭从底部排出的时间为1h～2h。Wherein, in the step 4, the time from adding the impregnated biomass carbon to the crude activated carbon being discharged from the bottom is 1 h to 2 h.
其中，所述步骤四中回转活化炉采用变频调节的方式回转，转速为10r/min～15r/min。Wherein, in the step 4, the rotary activation furnace is rotated by means of frequency conversion adjustment, and the rotating speed is 10r/min～15r/min.
其中，所述步骤四中回转活化炉升降角度为10°～30°。Wherein, in the step 4, the lifting angle of the rotary activation furnace is 10°˜30°.
其中，所述步骤四中用于活化的生物质炭是稻壳热解炭、酸处理除氧化物的净化稻壳热解炭或稻壳热解炭脱硅后炭粉。Wherein, the biomass char used for activation in the step 4 is rice husk pyrolysis charcoal, acid-treated deoxidized purified rice husk pyrolysis charcoal or rice husk pyrolysis charcoal desiliconized carbon powder.
其中所述步骤四中用于活化的生物质炭是糠醛渣经水洗、干燥、炭化处理后的炭粉，或木糖渣经水洗、干燥、炭化处理后的炭粉。Wherein the biomass carbon used for activation in the step 4 is the carbon powder after the furfural residue is washed, dried and carbonized, or the carbon powder after the xylose residue is washed, dried and carbonized.
其中，所述步骤三中的活化剂是含有钾离子的碱金属和碱土金属氢氧化物的混合物。Wherein, the activator in the third step is a mixture of alkali metal and alkaline earth metal hydroxides containing potassium ions.
显然，以上实施例的说明只是用于帮助理解本发明的方法及其核心思想，但是对于本领域的普通技术人员而言，可以在不脱离权利要求所述的本发明的精神和原理的情况下对这些实施例进行多种变化、修改和替换，这些改进和修饰也落入本发明权利要求的保护范围之内。Obviously, the description of the above embodiments is only used to help understand the method and the core idea of the present invention, but for those of ordinary skill in the art, they can do so without departing from the spirit and principle of the present invention described in the claims. Various changes, modifications and substitutions can be made to these embodiments, and these improvements and modifications also fall within the protection scope of the claims of the present invention.
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| CN115893407A (en) * | 2022-11-23 | 2023-04-04 | 北京华能长江环保科技研究院有限公司 | Activated carbon preparation method for nuclear waste gas and activated carbon preparation system for nuclear waste gas |
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| CN110054186A (en) * | 2019-06-06 | 2019-07-26 | 吉林大学 | A method of it producing capacitance carbon desiliconization Sewage treatment and utilizes |
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| CN110054186A (en) * | 2019-06-06 | 2019-07-26 | 吉林大学 | A method of it producing capacitance carbon desiliconization Sewage treatment and utilizes |
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| CN114558547A (en) * | 2022-03-03 | 2022-05-31 | 江西乐博维新材料有限公司 | Biomass air purification columnar activated carbon and forming process thereof |
| CN115893407A (en) * | 2022-11-23 | 2023-04-04 | 北京华能长江环保科技研究院有限公司 | Activated carbon preparation method for nuclear waste gas and activated carbon preparation system for nuclear waste gas |
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