CN109264715A

CN109264715A - A kind of method that step heating prepares active carbon

Info

Publication number: CN109264715A
Application number: CN201811137553.6A
Authority: CN
Inventors: 李大伟; 王宇
Original assignee: China University of Petroleum East China
Current assignee: China University of Petroleum East China
Priority date: 2018-09-28
Filing date: 2018-09-28
Publication date: 2019-01-25

Abstract

The present invention relates to the methods that one step heating of one kind prepares active carbon.Its technical solution is the following steps are included: reactor bottom shown in Fig. 1 places CaCO₃, it is laid with stainless (steel) wire thereon, 0.25-2 times of CaCO is pressed on stainless (steel) wire₃Quality places shell, then places lid, but endless hermetically sealed reactor naturally in reactor head.Then, reactor is put into Muffle furnace, is warming up to 800-950 DEG C with the rate of 2-40 DEG C/min, keep the temperature after 2-7h natural cooling to get active carbon is arrived.The beneficial effects of the present invention are: 1) specific surface area of gained active carbon is 1000-2500m²/ g, yield 5-35%；2) in whole preparation process, without being passed through protection gas or activation gas；3) priming reaction occurs under normal pressure, is not necessarily to high pressure resistant equipment；4) activators such as additional addition acid, alkali are not had in activation process；5) without being washed or being dried after activation products are cooling.

Description

A kind of method that step heating prepares active carbon

Technical field

The present invention relates to technical field of active carbon, in particular to a kind of method that a step heating prepares active carbon.

Background technique

Active carbon has flourishing pore structure and is easy to the surface chemical property of modulation, be widely used in sewage treatment, The fields such as gas purification, electrode material.The traditional preparation methods of active carbon are physical method and chemical method.Physical method need to consume fluidised form Gas or activation gas, chemical method is protected to need to wash or dry repeatedly.In recent years, researcher develops some novel porous charcoal preparations Technology.

For example, the reactor equipped with shell is full of air simultaneously by the scholars such as Jiang Jianchun (Patent publication No CN102627276A) It is completely closed, carries out hot high pressure priming reaction later, then washed, dried, active carbon has been made.Zou Qingli (patent disclosure Number CN101880037A) by Nano-meter CaCO3₃Aqueous gelatin solution is added, then is carbonized, pickling, washing, active carbon is made. AngGao etc. (Microporous and Mesoporous Materials, 2018,260,172-179) is by Ca (NO₃)₂With K₂CO₃Collagen gel is added, obtains CaCO₃Collagen-based composite goes template, washing that activity has been made through high-temperature heating, pickling Charcoal.Shaojin Qiu etc. (Chemical Engineering Journal, 2017,321, P301-313) will contain CaCO₃Template Presoma mixed with KOH, by heat-activated and washing, active carbon has been made.

The studies above provides of great value thinking for the preparation of active carbon, but still has the following disadvantages: that 1) activation needs It to carry out under high pressure, lead to high equipment cost, and there are security risks；2) it needs to wash repeatedly, causes to take a long time, And there may be waste liquids；3) drying process is needed, causes activation post-processing that need to consume energy；4) it needs to be passed through fluid gas, from And cause to consume the auxiliary facilities such as pipeline, flowmeter, gas cylinder, increase investment cost；5) it needs to consume a variety of activators.

Summary of the invention

The purpose of the present invention is in view of the foregoing defects the prior art has, provide one step heating of one kind to prepare active carbon Method, without high-pressure activated, without washing repeatedly, is not necessarily to without dry link without being passed through fluid gas using this method A variety of chemical reagent are consumed, and gained active carbon specific surface area is 1000-2500m²/ g, yield 5-35%.

Its technical solution is: placing CaCO in reactor bottom₃, it is laid with stainless (steel) wire thereon, presses 0.25- on stainless (steel) wire 2 times of CaCO₃Quality places shell, then places lid, but incomplete closed reactor naturally in reactor head.Then, will Reactor is put into Muffle furnace, is warming up to 800-950 DEG C with the rate of 2-40 DEG C/min, natural cooling is after keeping the temperature 2-7h to get work Property charcoal.

Above-mentioned shell partial size≤15mm, moisture content≤10%.

Above-mentioned CaCO₃Moisture content is lower than 10%, for CO needed for providing activation₂。

Above-mentioned stainless (steel) wire, effect are barrier active carbon and CaCO₃Contact, prevent CaCO₃Powder pollutes active carbon.

Above-mentioned heat-activated refers to and is heated to 800-950 DEG C with the heating rate of 2-40 DEG C/min and keeps the temperature 2-7h.

Compared with existing method prepares activated carbon technology, the invention has the advantages that 1) whole preparation process carries out under normal pressure, Without pressure-resistant equipment；2) it does not need to be passed through fluidised form protection gas or gas activation agent, to save the portions such as pipeline, flowmeter, gas cylinder Part；3) CaCO is used₃The CO that pyrolytic generates₂It is activated, is not consumed the activators such as acid, alkali；4) it is not required to wash, reduction is washed Wash the time of consumption and the generation of waste liquid；5) it does not need to be dried after priming reaction, reduces energy consumption, improve production effect Rate；6) gained active carbon specific surface area is 1000-2500m²/ g, yield 5-35%.

Specific embodiment

Embodiment 1

Reactor bottom shown in Fig. 1 places the CaCO that 6g moisture content is 2%₃, three layers of 310s material are spread above Stainless (steel) wire, places the walnut shell that 1.5g partial size is 3-10mm, moisture content≤5% on stainless (steel) wire, then reactor head from So place lid, but endless hermetically sealed reactor；Reactor is put into Muffle furnace, is warming up to 900 DEG C with the rate of 20 DEG C/min, Keep the temperature 5h after natural cooling to get arrive active carbon.Gained active carbon specific surface area is 1650m²/ g, yield 9.9%.

Embodiment 2

Reactor bottom shown in Fig. 1 places the CaCO that 5g moisture content is 9%₃, four layers of 310s material are spread above Stainless (steel) wire places the walnut shell that 3g partial size is 4-10mm, moisture content≤8% on stainless (steel) wire, then in reactor head nature Place lid, but endless hermetically sealed reactor；Reactor is put into Muffle furnace, is warming up to 870 DEG C with the rate of 10 DEG C/min, Natural cooling after heat preservation 4h.Gained active carbon specific surface area is 1372m²/ g, yield 8.6%.

Embodiment 3

Reactor bottom shown in Fig. 1 places the CaCO that 9g moisture content is 1%₃, four layers of 310s material are spread above Stainless (steel) wire places the Chinese hawthorn seed that 9g partial size is 4-10mm, moisture content≤8% on stainless (steel) wire, then in reactor head nature Place lid, but endless hermetically sealed reactor；Reactor is put into Muffle furnace, is warming up to 900 DEG C with the rate of 30 DEG C/min, Natural cooling after heat preservation 4h.Gained active carbon specific surface area is 1371m²/ g, yield 12.6%.

Embodiment 4

Reactor bottom shown in Fig. 1 places the CaCO that 9g moisture content is 5%₃, five layers of 310s material are spread above Stainless (steel) wire places the hawthorn shell that 6g partial size is 4-10mm, moisture content≤7% on stainless (steel) wire, then in reactor head nature Place lid, but endless hermetically sealed reactor；Reactor is put into Muffle furnace, is warming up to 930 DEG C with the rate of 35 DEG C/min, Natural cooling after heat preservation 4h.Gained active carbon specific surface area is 1371m²/ g, yield 10.6%.

The above is only section Example of the invention, and anyone skilled in the art is possibly also with upper Equivalent technical solution is modified or be revised as to the technical solution for stating elaboration.Therefore, technical solution according to the present invention Any simple modification carried out or substitute equivalents, belong to the greatest extent the scope of protection of present invention.

Detailed description of the invention

Fig. 1 is the reactor used schematic diagram of the present invention.

Claims

1. a kind of method that a step heating prepares active carbon, it is characterized in that: placing CaCO in reactor bottom₃, it is laid with thereon stainless Steel mesh presses 0.25-2 times of CaCO on stainless (steel) wire₃Quality places shell, then places lid but endless naturally in reactor head Reactor is put into Muffle furnace later by totally-enclosed reactor, carries out heat-activated and natural cooling to get active carbon；Entire system Standby process carries out under normal pressure, and obstructed protection gas does not consume the activators such as acid, alkali, is not required to be washed or be dried, and gained is living Property charcoal specific surface area be 1000-2500m²/ g, yield 5-35%.

2. the method that a kind of step heating according to claim 1 prepares active carbon, it is characterized in that: the shell partial size For≤15mm, moisture content≤10%.

3. the method that a kind of step heating according to claim 1 prepares active carbon, it is characterized in that: the CaCO₃It is aqueous Rate is lower than 10%, for CO needed for providing activation₂。

4. the method that a kind of step heating according to claim 1 prepares active carbon, it is characterized in that: the stainless steel Net, effect are barrier active carbon and CaCO₃Contact, prevent CaCO₃Powder pollutes active carbon.

5. the method that a kind of step heating according to claim 1 prepares active carbon, it is characterized in that: the heating is living Change, refers to and be heated to 800-950 DEG C with the heating rate of 2-40 DEG C/min and keep the temperature 2-7h.