CN101289183A - Method for preparing starch based active carbon microballoons with high specific surface area - Google Patents
Method for preparing starch based active carbon microballoons with high specific surface area Download PDFInfo
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- CN101289183A CN101289183A CNA2008100534179A CN200810053417A CN101289183A CN 101289183 A CN101289183 A CN 101289183A CN A2008100534179 A CNA2008100534179 A CN A2008100534179A CN 200810053417 A CN200810053417 A CN 200810053417A CN 101289183 A CN101289183 A CN 101289183A
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Abstract
The invention discloses a method for preparing starch-based activated carbon microsphere with high specific surface area, which pertains to the technology of preparing activated carbon microsphere. The process of the method comprises: cereal starch, potato starch, pea starch and banana and plantain fruit starch are taken as raw material, which is oxidized under constant temperature in an oxidizing atmosphere; oxidized starch, under the protection of nitrogen, is carbonized in a carbonization furnace, and starched-based carbon microsphere with the original shape of starch granules is produced; the prepared carbon microsphere and activating agent are mixed and dipped and dried, and the mixture obtained, under the protection of nitrogen, is activated in an activating furnace; the activated product is washed and centrifugally separated and dried, and the starch-based activated carbon microsphere with high specific surface area is obtained. The method of the invention has the advantages of simple process, low price for raw material and wide raw material source, and can realize large-scale production easily.
Description
Technical field
The present invention relates to a kind of preparation of starch based active carbon microballoons with high specific surface area, belong to the technology of preparing of activated carbon microballon.
Background technology
Activated carbon microballon has a series of premium propertiess such as the impurity the ash content of coal is low, physical strength is high, pore size distribution is easily controlled, specific surface area is big, absorption property is good, good sphericity, smooth surface, and extremely common people pay close attention to.In recent years, activated carbon microballon has obtained in fields such as environment protection, chemical protection, biomedicine, support of the catalyst, the energy, electronics using widely.Can be divided three classes by raw material different activities carbon microspheres: coal-based, polymer-based and asphalt based active carbon microballoon.In general, the activated carbon microballon material is along with the increase of its mesopore content, and specific surface area can reduce, and the successful preparation that therefore has the mesothyrid activated carbon microballon of high-specific surface area will be played very important meaning to its application.Xue Ruisheng etc. pass through Powdered carbon microspheres and tackiness agent mixing moulding, and the activated carbon microballon specific surface area of preparing through Overheating Treatment reaches 2800m again
2/ g, total hole volume reaches 2.9cm
3/ g, and mesopore content reaches 50-70% (ZL200610141086.5).Guo Chunyu etc. also prepare the activated carbon microballon (ZL200610053552.4) of high-specific surface area senior middle school porosity by the method for adding ferrocene in pitch.At present, the preparation of activated carbon microballon also comprises some other methods, as being raw material with resinous material (as: resol, styrene resin), add properties-correcting agent or pore-forming material (as arene material, organometallic compound), adopt the emulsion process balling-up, prepare activated carbon microballon by conventional carbonization-activation.And also do not see about the report of starch base activated carbon microballon.In these above-mentioned preparation methods, the method that has is subjected to the restriction of raw material, causes product price higher; Though the method raw material abundance that has because of the limitation of method itself and there is severe contamination, is lacked competitiveness on market.And the used starting material of these technologies are Nonrenewable resources (as: refinery coke, pitch) and the serious organic compound of environmental pollution, can not satisfy the requirement of " green chemical industry ".
Summary of the invention
The object of the present invention is to provide a kind of preparation method of starch based active carbon microballoons with high specific surface area.This method has the advantages that raw material sources are extensive, cheap, production cost is low.
The present invention is realized that by the following technical programs a kind of preparation method of starch based active carbon microballoons with high specific surface area is characterized in that comprising following process:
(1) be that cereal kind of starch, potato starch, legume starch and the banana of 2-120 μ m and the fruit kind of starch of bajiao banana are raw material with the particle diameter; Raw material is added in the process furnace, in the atmosphere of air, oxygen, ozone, sulfurous gas, nitrogen peroxide or sulphur trioxide, is that 0.5-20 ℃/min is warming up to 60-300 ℃ with the temperature rise rate, carries out oxide treatment in constant temperature 2-72 hour.
(2) step (1) is added in the charring furnace through the starch of peroxidation, under protection of nitrogen gas, rise to 600 ℃-1500 ℃ with the temperature rise rate of 0.5-20 ℃/min, constant temperature thermal treatment 0.5-10 hour is cooled to room temperature, makes starch-based carbon microsphere.
(3) starch-based carbon microsphere that step (2) is made and activator KOH are 1 by mass ratio: 1-10: 1 mixes, and adds water simultaneously and carries out hybrid infusion, dries moisture then.Again the mixture of gained is risen to 500-1000 ℃ with the temperature rise rate of 0.5-20 ℃/min under inert atmosphere and activate, soak time is 0.5-10 hour, is cooled to room temperature then under inert atmosphere.Products therefrom washs with hydrochloric acid soln, is washed to neutrality with deionized water at last, centrifugation, and drying promptly gets starch based active carbon microballoons with high specific surface area.
The cereal kind of starch that said process adopts is a W-Gum, and potato starch is a yam starch.
The present invention has following advantage:
(1) raw materials used is the fruit kind of starch of cereal kind of starch, potato starch, legume starch and banana and bajiao banana, has advantage cheap, wide material sources, and is to be renewable resources.The farm crop that are used for Starch Production at present mainly contain corn, cassava, potato, wheat etc.China is agriculture production big country, so starch resource is very abundant and cheap.
(2) production technique is simple, saves time, and is laborsaving, easily realizes scale operation;
(3) starch according to different varieties exists difference in granular size and vpg connection, can select for use different sorts starch to prepare the activated carbon microballon of different shape as requested.
Description of drawings
The stereoscan photograph of the yam starch based active carbon microballoons with high specific surface area that Fig. 1-be embodiment of the invention 4 makes.
Embodiment
Embodiment 1
In process furnace, in air atmosphere, add the W-Gum of the spherical in shape and polygon bodily form of 100g, with the temperature rise rate of 5 ℃/min process furnace is risen to 200 ℃ after, constant temperature oxide treatment 48h is cooled to room temperature.Obtain the 67.8g product.Then the 20g Sumstar 190 is put into charring furnace, at N
2Protection rises to 600 ℃ with the temperature rise rate of 2 ℃/min down, and constant temperature processing 1h, and carbonization yield is 29.8%.Get 5g carbonizing production and 15gKOH, add less water simultaneously and carry out hybrid infusion.In 120 ℃ baking oven, dry moisture.Then at N
2The following temperature rise rate with 2 ℃/min of protection rises to 700 ℃ and activates, and soak time is 1h.Take out after being cooled to room temperature, with the washing of the hydrochloric acid soln of 1mol/L, again with deionized water wash to neutral, centrifugation in rotating speed is 2000 rev/mins whizzer.With product dry 24h under 120 ℃ that separation obtains, obtaining specific surface area is 1751m
2/ g, total hole volume are 0.91cm
3The corn starch base activated carbon microballon of/g, the activation yield is 66.1%.
Embodiment 2
In process furnace, in air atmosphere, add the W-Gum of the spherical in shape and polygonal bodily form of 100g, with the temperature rise rate of 10 ℃/min process furnace is risen to 220 ℃ after, constant temperature oxide treatment 36h is cooled to room temperature.Obtain the 65.7g product.Then the 20g Sumstar 190 is put into charring furnace, at N
2Protection rises to 650 ℃ with the temperature rise rate of 2 ℃/min down, and constant temperature processing 1h, and carbonization yield is 29.2%.Get 5g carbonizing production and 15gKOH, add less water simultaneously and carry out hybrid infusion.In 120 ℃ baking oven, dry moisture.Then at N
2The following temperature rise rate with 2 ℃/min of protection rises to 800 ℃ and activates, and soak time is 1h.Take out after being cooled to room temperature, with the washing of the hydrochloric acid soln of 1mol/L, again with deionized water wash to neutral, centrifugation in rotating speed is 2000 rev/mins whizzer.With product dry 24h under 120 ℃ that separation obtains, obtaining specific surface area is 2103m
2/ g, total hole volume are 1.11cm
3The corn starch base activated carbon microballon of/g, the activation yield is 62.0%.
Embodiment 3
In process furnace, in air atmosphere, add the yam starch of the spherical in shape and elliposoidal of 100g, with the temperature rise rate of 15 ℃/min process furnace is risen to 240 ℃ after, constant temperature oxide treatment 18h is cooled to room temperature.Obtain the 66.2g product.Then the 20g Sumstar 190 is put into charring furnace, at N
2Protection rises to 700 ℃ with the temperature rise rate of 5 ℃/min down, and constant temperature processing 1h, and carbonization yield is 31.2%.Get 5g carbonizing production and 20gKOH, add less water simultaneously and carry out hybrid infusion.In 120 ℃ baking oven, dry moisture.Then at N
2The following temperature rise rate with 5 ℃/min of protection rises to 600 ℃ and activates, and soak time is 1h.Take out after being cooled to room temperature, with the washing of the hydrochloric acid soln of 1mol/L, again with deionized water wash to neutral, centrifugation in rotating speed is 2000 rev/mins whizzer.With product dry 24h under 120 ℃ that separation obtains, obtaining specific surface area is 1943m
2/ g, total hole volume are 1.03cm
3The yam starch matrix activated carbon microballoon of/g, the activation yield is 68.9%.
Embodiment 4
In process furnace, in air atmosphere, add the yam starch of the spherical in shape and elliposoidal of 100g, with the temperature rise rate of 20 ℃/min process furnace is risen to 240 ℃ after, constant temperature oxide treatment 18h is cooled to room temperature.Obtain the 66.2g product.Then the 20g Sumstar 190 is put into charring furnace, at N
2Protection rises to 700 ℃ with the temperature rise rate of 5 ℃/min down, and constant temperature processing 1h, and carbonization yield is 31.2%.Get 5g carbonizing production and 20gKOH, add less water simultaneously and carry out hybrid infusion.In 120 ℃ baking oven, dry moisture.Then at N
2The following temperature rise rate with 5 ℃/min of protection rises to 800 ℃ and activates, and soak time is 1h.Take out after being cooled to room temperature, with the washing of the hydrochloric acid soln of 1mol/L, again with deionized water wash to neutral, centrifugation in rotating speed is 2000 rev/mins whizzer.With product dry 24h under 120 ℃ that separation obtains, obtaining specific surface area is 2520m
2/ g, total hole volume are 1.33cm
3The yam starch matrix activated carbon microballoon of/g, the activation yield is 61.4%.
Embodiment 5
In process furnace, in air atmosphere, add the yam starch of the spherical in shape and elliposoidal of 100g, with the temperature rise rate of 20 ℃/min process furnace is risen to 260 ℃ after, constant temperature oxide treatment 12h is cooled to room temperature.Obtain the 62.8g product.Then the 20g Sumstar 190 is put into charring furnace, at N
2Protection rises to 750 ℃ with the temperature rise rate of 5 ℃/min down, and constant temperature processing 1h, and carbonization yield is 29.3%.Get 5g carbonizing production and 20gKOH, add less water simultaneously and carry out hybrid infusion.In 120 ℃ baking oven, dry moisture.Then at N
2The following temperature rise rate with 5 ℃/min of protection rises to 900 ℃ and activates, and soak time is 1h.Take out after being cooled to room temperature, with the washing of the hydrochloric acid soln of 1mol/L, again with deionized water wash to neutral, centrifugation in rotating speed is 2000 rev/mins whizzer.With product dry 24h under 120 ℃ that separation obtains, obtaining specific surface area is 2835m
2/ g, total hole volume are 1.59cm
3The yam starch matrix activated carbon microballoon of/g, the activation yield is 42.1%.
Claims (2)
1. the preparation method of a starch based active carbon microballoons with high specific surface area is characterized in that comprising following process:
(1) be that cereal kind of starch, potato starch, legume starch and the banana of 2-120 μ m and the fruit kind of starch of bajiao banana are raw material with the particle diameter; Raw material is added in the process furnace, in the atmosphere of air, oxygen, ozone, sulfurous gas, nitrogen peroxide or sulphur trioxide, is that 0.5-20 ℃/min is warming up to 60-300 ℃ with the temperature rise rate, carries out oxide treatment in constant temperature 2-72 hour;
(2) step (1) is added in the charring furnace through the starch of peroxidation, under protection of nitrogen gas, rise to 600 ℃-1500 ℃ with the temperature rise rate of 0.5-20 ℃/min, constant temperature thermal treatment 0.5-10 hour is cooled to room temperature, makes starch-based carbon microsphere;
(3) starch-based carbon microsphere that step (2) is made and activator KOH are 1 by mass ratio: 1-10: 1 mixes, add water simultaneously and carry out hybrid infusion, dry moisture then, again the mixture of gained being risen to 500-1000 ℃ with the temperature rise rate of 0.5-20 ℃/min under inert atmosphere activates, soak time is 0.5-10 hour, is cooled to room temperature then under inert atmosphere.Products therefrom washs with hydrochloric acid soln, is washed to neutrality with deionized water at last, centrifugation, and drying promptly gets starch based active carbon microballoons with high specific surface area.
2. by the preparation method of the described starch based active carbon microballoons with high specific surface area of claim 1, it is characterized in that the cereal kind of starch is a W-Gum, potato starch is a yam starch.
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Open date: 20081022 |