CN103112853B - Technology for preparing high nitrogenous functional group activated carbon through phosphoguanidine activation method - Google Patents

Technology for preparing high nitrogenous functional group activated carbon through phosphoguanidine activation method Download PDF

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CN103112853B
CN103112853B CN201310088266.1A CN201310088266A CN103112853B CN 103112853 B CN103112853 B CN 103112853B CN 201310088266 A CN201310088266 A CN 201310088266A CN 103112853 B CN103112853 B CN 103112853B
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phosphoguanidine
functional group
degree
activated carbon
dry
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CN103112853A (en
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张建
刘海
张成禄
程呈
李一冉
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Shandong University
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Shandong University
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Abstract

The invention relates to a technology for preparing a high nitrogenous functional group activated carbon through a phosphoguanidine activation method. The technology comprises the following steps of: mixing lotus stem powder with phosphoguanidine powder according to different mass ratios, adding the mixture into deionized water, uniformly stirring, drying at high temperature, putting the mixture into a muffle furnace, carbonizing and activating for 40-60 minutes at the temperature of 450 DEG C-550 DEG C, taking out and cleaning the carbonized and activated mixture to be neutral, filtering and drying a cleaned sample. The preparation technology is simple and has high activated carbon yield; and the activated carbon has developed pores, is rich in nitrogenous functional group, has strong absorption property and is contributed to absorption of heavy metal ions.

Description

A kind of phosphoguanidine activation method prepares the technique of high nitrogen-containing functional group gac
One, technical field
The invention belongs to gac preparing technical field, relate to the technique that a kind of phosphoguanidine activation method prepares gac.
Two, background technology
Gac is that a kind of internal voids structure is flourishing, specific surface area is large, the microcrystalline carbon material of high adsorption capacity.Gac has very strong absorption property, is widely used in the fields such as chemical industry, food, medicine, environmental protection.The absorption property of gac determines primarily of its pore texture, specific surface area and surface functional group three factors, and wherein pore texture and specific surface area determine its physical adsorption performance, its chemisorption performance of surface functional group decision.The activator that conventional chemical activation method adopts is mainly phosphoric acid, potassium hydroxide and zinc chloride, and the surface functional group of obtained gac is mainly oxygen-containing functional group.A lot of research increases gac to removal effect that is organic and inorganic pollution material by load nitrogen-containing functional group.Phosphoguanidine contains guanidine radicals (CH 4n 3), there is strong basicity.In heat treatment process, phosphoguanidine can decompose, and discharges nitrogenous gas, can play pore-creating and fire retardation; And it can also react with lignocellulose, introduce nitrogen-containing functional group at activated carbon surface, improve its adsorptive power.Not yet discovery phosphoguanidine activation method prepares the report of gac at present.
Three, summary of the invention
The object of this invention is to provide a kind of be activator with phosphoguanidine, stalk is raw material, prepares the technique of high nitrogen-containing functional group gac.In preparation process, phosphoguanidine can play fire-retardant, pore-creating and introducing nitrogen-containing functional group.
The phosphoguanidine activation method that the present invention proposes prepares high nitrogen-containing functional group activated carbon process, and take phosphoguanidine as activator, ligno-cellulosic materials used is lotus bar, and preparation technology is as follows:
(1) with tap water, lotus bar is cleaned, dry 6 hours at 100 degree of temperature, removing moisture, the lotus bar after drying is crushed to 60 ~ 120 orders;
(2) by lotus bar powder in mass ratio 1:1 ~ 1:4 ratio mix with phosphoguanidine powder, then add in 50ml deionized water and stir evenly, in 80 ~ 110 degree dry 6 ~ 8 hours;
(3) above-mentioned dry sample is placed in retort furnace, carbonization-activation 40 ~ 60 minutes at 450 degree ~ 550 degree temperature, boils in a covered pot over a slow fire 1 ~ 1.5 hour in stove after powered-down;
(4) sample is taken out, with deionized water wash to PH=6.5 ~ 7.5, refilter, dry, be i.e. obtained high nitrogen-containing functional group gac.
The present invention prepares high nitrogen-containing functional group gac with phosphoguanidine activation method, and preparation technology is simple, and gac yield is high, hole is flourishing, and obtained activated carbon surface nitrogen content is 15% ~ 30%, is mainly amino and amide group, absorption property is strong, is conducive to heavy metal ion adsorbed.
The present invention also can adopt potato stalk as raw material, also can obtain high nitrogen-containing functional group gac.
Four, embodiment
Embodiment 1
Cleaned up by lotus bar with tap water, dry 6 hours under 100 degree, removing moisture, is crushed to 60 ~ 120 orders; Mix with phosphoguanidine powder by impregnating ratio 1:1, then add 50mL deionized water and stir evenly, in 70 ~ 80 degree dry 8 hours; The sample of above-mentioned drying is moved in retort furnace, carbonization-activation 60 minutes under 450 degree, stewing taking-up after 1.5 hours in stove after powered-down; Again with deionized water wash to pH=6.5 ~ 7.0, filter, dry, be i.e. obtained high nitrogen-containing functional group gac.
Embodiment 2
Cleaned up by lotus bar with tap water, dry 6 hours under 100 degree, removing moisture, is crushed to 60 ~ 120 orders; Mix with phosphoguanidine powder by impregnating ratio 1:2, then add 50mL deionized water and stir evenly, in 90 ~ 100 degree dry 7 hours; The sample of above-mentioned drying is moved in retort furnace, carbonization-activation 50 minutes under 500 degree, stewing taking-up after 1.5 hours in stove after powered-down; Again with deionized water wash to pH=6.5 ~ 7.0, filter, dry, be i.e. obtained high nitrogen-containing functional group gac.
Embodiment 3
Cleaned up by lotus bar with tap water, dry 6 hours under 100 degree, removing moisture, is crushed to 60 ~ 120 orders; Mix with phosphoguanidine powder by impregnating ratio 1:3, then add 50mL deionized water and stir evenly, in 100 ~ 110 degree dry 6 hours; The sample of above-mentioned drying is moved in retort furnace, carbonization-activation 40 minutes under 550 degree, stewing taking-up after 1.5 hours in stove after powered-down; Again with deionized water wash to pH=6.5 ~ 7.0, filter, dry, be i.e. obtained high nitrogen-containing functional group gac.

Claims (1)

1. phosphoguanidine activation method prepares the technique of high nitrogen-containing functional group gac, and it is characterized in that taking phosphoguanidine as activator, with ligno-cellulosic materials lotus bar for raw material, preparation technology is as follows:
(1) with tap water, lotus bar is cleaned, dry 6 hours at 100 degree of temperature, removing moisture, the lotus bar after drying is crushed to 60 ~ 120 orders;
(2) by lotus bar powder in mass ratio 1:1 ~ 1:4 ratio mix with phosphoguanidine powder, then add in 50ml deionized water and stir evenly, in 80 degree ~ 110 degree dry 6 ~ 8 hours;
(3) above-mentioned dry sample is placed in retort furnace, carbonization-activation 40 ~ 60 minutes at 450 degree ~ 550 degree temperature, boils in a covered pot over a slow fire 1 ~ 1.5 hour in stove after powered-down;
(4) sample is taken out, with deionized water wash to PH=6.5 ~ 7.5, refilter, dry, be i.e. obtained high nitrogen-containing functional group gac.
CN201310088266.1A 2013-03-19 2013-03-19 Technology for preparing high nitrogenous functional group activated carbon through phosphoguanidine activation method Active CN103112853B (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105819443B (en) * 2016-03-04 2019-03-26 四川大学 It is a kind of to prepare active carbon and method using discarded plant based biomass
CN106495149B (en) * 2016-11-18 2018-10-12 刘春明 A kind of technique that biomass prepares high absorption property activated carbon

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3527564A (en) * 1968-04-15 1970-09-08 Stevens & Co Inc J P Process for carbonizing fibrous materials
CN101112983A (en) * 2007-06-08 2008-01-30 山东大学 Preparation method of mizue brocade straw activated charcoal
CN101219787A (en) * 2008-01-25 2008-07-16 山东大学 Method for preparing bean tendril absorbent charcoal
EP2478957A1 (en) * 2011-01-25 2012-07-25 Norit Nederland B.V. Production of catalytically active activated carbon

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3527564A (en) * 1968-04-15 1970-09-08 Stevens & Co Inc J P Process for carbonizing fibrous materials
CN101112983A (en) * 2007-06-08 2008-01-30 山东大学 Preparation method of mizue brocade straw activated charcoal
CN101219787A (en) * 2008-01-25 2008-07-16 山东大学 Method for preparing bean tendril absorbent charcoal
EP2478957A1 (en) * 2011-01-25 2012-07-25 Norit Nederland B.V. Production of catalytically active activated carbon

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