CN101759181A - Method for producing activated carbon for super capacitors - Google Patents
Method for producing activated carbon for super capacitors Download PDFInfo
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- CN101759181A CN101759181A CN200910227472A CN200910227472A CN101759181A CN 101759181 A CN101759181 A CN 101759181A CN 200910227472 A CN200910227472 A CN 200910227472A CN 200910227472 A CN200910227472 A CN 200910227472A CN 101759181 A CN101759181 A CN 101759181A
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Abstract
The invention discloses a method for producing activated carbon for super capacitors and relates to activated carbon. The method comprises the following steps: a, selecting materials; b, steaming the materials and phosphoric acid by the weight ratio being 1:(2.5-4.0), adding phosphoric acid with the concentration thereof being 30% to 50%, and holding for 1.5 to 3 hours at 120 to 140 DEG C at 0.2MPa to 0.5MPa; c, carbonizing and holding for 0.5 to 1.5 hours at 150 to 300 DEG C; d, activating and holding for 1.5 to 3 hours at 350 to 500 DEG C; e, submerging the carbon surface, soaking for 1 to 2 hours, and recovering the phosphoric acid from the activated material; f, pickling the material, so as to remove the impurities therein, submerging the carbon surface, adding hydrochloric acid with the weight being 5% to 7% of that of the material, and holding for 1 to 2 hours at 70 to 80 DEG C; g, dewatering, drying, pulverizing and packaging separately to obtain the finished product of activated carbon. The invention has the following beneficial effects: the method dispenses with the protective presence of nitrogen, has mild technological conditions and low production cost and is free from environmental pollution; and the method conforms with the requirements for manufacturing super-capacitors: the specific capacitance of the super-capacitor is higher than 200F/g, and the ash content thereof is 0.5% to 1%.
Description
Technical field:
The present invention relates to the activated carbon technology field, further relate to the activated carbon for super capacitors technology, is the production method that activator is produced activated carbon for super capacitors with phosphoric acid especially.
Background technology:
Relevant ultracapacitor (double layer capacitor) is a unusual active subject in recent years.The making of ultracapacitor need be an electrode materials with special gac (being commonly referred to super-activated carbon), super-activated carbon requirement, flourishing effective hole, pore texture distributes rationally, low ash content and good conductivity, apparent density is big, is that other gac is incomparable.
Having with potassium hydroxide, sodium hydroxide at present is additive, because the restriction of manufacture craft requires the carbonization-activation process to carry out under nitrogen protection, investment of production equipment is big, the processing requirement strictness, and production cost improves, and environmental protection has high input the difficult improvement of discharge.
Simultaneously, phosphoric acid manufactured gac is a proven technique, and adopting it is activator, have advantages such as low, the recyclable utilization of production cost, environmental protection, but because the restriction of other technology only limits to produce general gac, as sugar with charcoal, Medicinal Charcoal, chemistry with charcoal etc.
Do not see as yet with phosphoric acid is that activator is used for the public technology that activated carbon for super capacitors is made.
Summary of the invention:
The object of the present invention is to provide a kind of production method of activated carbon for super capacitors, it is raw material that this method adopts wood chip, shell etc., is activator with phosphoric acid, production cost is low, environmental friendliness, and working condition is loose, constant product quality meets the requirement that ultracapacitor is made.
The objective of the invention is to realize by following scheme: a kind of production method of activated carbon for super capacitors, it is characterized in that may further comprise the steps: a selects materials, and selects raw material particle size 10-40 order standby; Bigger as raw material, then pulverize earlier, through broken, screening, forming particle diameter is 10-40 order raw material with raw material; B boiling, raw material by weight: phosphoric acid=1: 2.5-4.0, adding concentration in raw material is the phosphoric acid of 30-50%, mix all, be 120-140 ℃ in temperature, pressure is under the condition of 0.2-0.5MPa, keeps 1.5-3 hour; The c charing is under 150-300 ℃ the condition, to keep 0.5-1.5 hour in temperature; The d activation under temperature 350-500 ℃ condition, kept 1.5-3 hour; E reclaims activator, and the raw material that activation is good is put into pond for recovering (or withdrawing can), adds water logging and does not have the charcoal face, soaks 1-2 hour, the phosphoric acid in the activated material is reclaimed, in order to recycling; F pickling impurity elimination in the e step, when the activation raw material is washed till phosphoric acid concentration less than 0.3% the time, adds water (pure water) and floods the charcoal face and add the hydrochloric acid that concentration is 33-35%, and hydrochloric acid weight is the 5-7% of raw material weight, under 70-80 ℃ situation, keeps 1-2 hour; The g dehydration, oven dry, abrasive dust, packing is finished product.
The present invention can also realize by following scheme:
For the quantity that increases effective hole with enlarge the aperture, during boiling, also can be with phosphoric acid, adding weight in raw material is the 0.5-3% expanding agent of raw material weight, expanding agent can be following a kind of, or the mixing of 2 kinds or 3 kinds: potassium primary phosphate (molecular formula KH
2PO
4) or iron nitrate [molecular formula: Fe (NO
3)
39H
2O] or borax (molecular formula Na
2B
4O
7.10H
2O).
2 kinds when mixing, can be one of following: potassium primary phosphate and iron nitrate be 1 by weight: 1.5-3.5; Potassium primary phosphate and borax are 1 by weight: 1.5-3.5; Iron nitrate and borax are 1 by weight: 1.5-3.5.
During 3 kinds of mixing, can be: by weight, potassium primary phosphate: iron nitrate: borax be 1: 0.5-3.5: 0.5-3.5.
Wherein, potassium primary phosphate (molecular formula KH
2PO
4) can be by SODIUM PHOSPHATE, MONOBASIC (molecular formula: NaH
2PO
4H
2O) substitute.
Carry out calcination process after oven dry, refer to the material after the oven dry is contained in airtight container, place under 800-1000 ℃ the condition, kept 1-2.5 hour, carry out abrasive dust afterwards again, packing is finished product.Calcining can promote even aperture distribution, impels the foreign material volatilization, thereby can make the internal resistance of electrical condenser reduce electric performance stablity.Internal resistance can drop to 300-500m Ω by the 1800-2000m Ω before the calcining.
Charing and activation can be carried out in rotary kiln (being the automatization rotary furnace), to keep continuity; The rotary kiln furnace superintendent is a 15-20 rice, and obliquity is 10-35 °, and rotating speed is adjustable, and the upper end is a feeding mouth, and the lower end is a heating gate, thereby rotary kiln is divided into two portions, i.e. the cold zone on top, and the high-temperature zone of lower section, cold zone is used for charing, and the high-temperature zone is used for activation.
Raw material can be selected one of wood sawdust, apricot shell, peach shell, nut-shell, Exocarpium cocois (Cocos nucifera L), corn cob, cotton stalk; When being raw material with one of apricot shell, peach shell, nut-shell, Exocarpium cocois (Cocos nucifera L), corn cob, cotton stalk, then pulverize earlier, with raw material crushing, screening, forming particle diameter is 10-40 order raw material.
The gac that adopts method provided by the invention to produce has the following advantages: 1, manufacturing process is simple, environmental friendliness.Selection phosphoric acid is activator, and without nitrogen protection, working condition is loose, the equipment less investment.2, cost is low, is activator with phosphoric acid, and when comparing potassium hydroxide and being activator, general consumption is 1 of raw material weight: 4-6, and phosphoric acid only is 1 of raw material weight: 2.5-4.0, and consumption is few; And price difference is big, and potassium hydroxide is 10,000 yuan/ton, and only 0.3 ten thousand yuan/ton of phosphoric acid, so production cost significantly reduces, and the phosphoric acid method is the 1/3-1/5 of potassium hydroxide method production cost.3, the activator loss is little, because low-temperature activation, the activator loss is little.And reclaim and to reuse.4, phosphoric acid environmentally safe, a spot of phosphoric acid is also favourable to plant growth.Refuse is easily handled.5, specific surface area is big, in, micropore is abundant.Ratio can reach more than 90%; 6, get the charcoal rate and improve, proportion is bigger.Proportion reaches 0.48-0.55g/ml usually; 7, meet the requirement of ultracapacitor.Its ash is 0.5-1%, and internal resistance is little, electric performance stablity, and specific capacitance can reach more than the 200F/g.
Embodiment:
In order to make those skilled in the art person understand the present invention program better, and above-mentioned purpose of the present invention, feature and advantage can be become apparent more, the present invention is described in further detail below in conjunction with embodiment.
Embodiment 1:
A kind of production method of activated carbon for super capacitors is characterized in that may further comprise the steps:
A selects materials, and selects raw material particle size 10-40 order standby; Wherein raw material can be selected wood sawdust, also can be one of apricot shell, peach shell, nut-shell, Exocarpium cocois (Cocos nucifera L), corn cob, cotton stalk, and is bigger as raw material, then pulverizes earlier, and with raw material crushing, screening, forming particle diameter is 10-40 order raw material;
B boiling, raw material by weight: phosphoric acid=1: 2.8, adding concentration is 35% phosphoric acid in raw material, mix all, be 125 ℃ in temperature, pressure is under the condition of 0.3MPa, keeps 2.2-2.8 hour, is preferably 2.6 hours, boiling makes phosphoric acid quicken infiltration; For increasing the quantity in hole, also can be with phosphoric acid, adding weight in raw material is 1.5% expanding agent of raw material weight, expanding agent is selected potassium primary phosphate;
The c charing is under 180 ℃ the condition, to keep 1.1-1.4 hour in temperature, is preferably 1.3 hours;
The d activation under 320 ℃ of conditions of temperature, kept 2.3-2.9 hour, was preferably 2.6 hours; Charing and activation are carried out in rotary kiln, and the rotary kiln furnace superintendent is a 15-20 rice, and obliquity is 10-35 °, and rotating speed is adjustable, the upper end is a feeding mouth, and the lower end is a heating gate, thereby rotary kiln is divided into two portions, i.e. the cold zone on top, the high-temperature zone of lower section, cold zone is used for charing, and the high-temperature zone is used for activation;
E reclaims activator, and the raw material that activation is good is put into pond for recovering, adds water logging and does not have the charcoal face, soaks 1.1-1.5 hour, is preferably 1.3 hours, and the phosphoric acid washing in the activated material is reclaimed;
F pickling impurity elimination in the e step, when the activation raw material is washed till phosphoric acid concentration less than 0.3% the time, adds water logging and there is not the charcoal face, and to add concentration be 435% hydrochloric acid, and hydrochloric acid weight is 5.5% of raw material weight, under 72 ℃ situation, keeps 1.6-2 hour, is preferably 1.8 hours;
The g dehydration, oven dry;
H calcining is about to raw material and contains in airtight container, places under 850 ℃ the condition, keeps 2.1-2.5 hour, is preferably 2.3 hours, and calcining can promote even aperture distribution, impels foreign material to volatilize, thereby can make the internal resistance of electrical condenser reduce electric performance stablity.Internal resistance can drop to 300-500m Ω by the 1800-2000m Ω before the calcining.
The i abrasive dust, the granularity of gac can be the 800-1500 order behind the abrasive dust, also can determine the granularity of powder according to customer need;
The j packing is finished product.
Embodiment 2:
A kind of production method of activated carbon for super capacitors is characterized in that comprising the following step:
A selects materials, and selects raw material particle size 10-40 order standby; Wherein raw material can be selected wood sawdust, also can be one of apricot shell, peach shell, nut-shell, Exocarpium cocois (Cocos nucifera L), corn cob, cotton stalk, and is bigger as raw material, then pulverizes earlier, and with raw material crushing, screening, forming particle diameter is 10-40 order raw material;
B boiling, raw material by weight: phosphoric acid=1: 3.2, adding concentration is 40% phosphoric acid in raw material, mix all, be 130 ℃ in temperature, pressure is under the condition of 0.4MPa, keeps 1.8-2.6 hour, is preferably 2.2 hours; Adding weight in raw material is 2% expanding agent of raw material weight, and expanding agent is to be 1 by weight by potassium primary phosphate and iron nitrate: 1.5-3.5 mixes;
The c charing is under 220 ℃ the condition, to keep 0.9-1.3 hour in temperature, is preferably 1.1 hours;
The d activation under 420 ℃ of conditions of temperature, kept 1.9-2.5 hour, was preferably 2.2 hours;
E reclaims activator, and the raw material that activation is good is put into pond for recovering, adds water logging and does not have the charcoal face, soaks 1.3-1.7 hour, is preferably 1.5 hours, and the phosphoric acid in the activated material is reclaimed;
F pickling impurity elimination in the e step, when the activation raw material is washed till phosphoric acid concentration less than 0.3% the time, adds water logging and there is not the charcoal face, and to add concentration be 34% hydrochloric acid, and hydrochloric acid weight is 6% of raw material weight, under 75 ℃ situation, keeps 1.2-1.8 hour, is preferably 1.5 hours;
The g dehydration, oven dry;
H calcining is about to raw material and contains in airtight container, places under 900 ℃ the condition, keeps 1.8-2.2 hour, is preferably 2 hours;
The i abrasive dust, the granularity of gac can be the 800-1500 order behind the abrasive dust, also can determine the granularity of powder according to customer need;
The j packing is finished product.
Embodiment 3:
A kind of production method of activated carbon for super capacitors is characterized in that may further comprise the steps:
A selects materials, and selects raw material particle size 10-40 order standby; Wherein raw material can be selected wood sawdust, also can be one of apricot shell, peach shell, nut-shell, Exocarpium cocois (Cocos nucifera L), corn cob, cotton stalk, and is bigger as raw material, then pulverizes earlier, and with raw material crushing, screening, forming particle diameter is 10-40 order raw material;
B boiling, raw material by weight: phosphoric acid=1: 3.6, adding concentration is 45% phosphoric acid in raw material, mix all, be 135 ℃ in temperature, pressure is under the condition of 0.45MPa, keeps 1.5-2.2 hour, is preferably 1.8 hours; Adding weight in raw material is 2.5% expanding agent of raw material weight, and expanding agent is by potassium primary phosphate, iron nitrate, borax by weight, potassium primary phosphate: iron nitrate: borax is 1: 0.5-3.5: 0.5-3. mixes;
The c charing is under 260 ℃ the condition, to keep 0.6-1.0 hour in temperature, is preferably 0.8 hour;
The d activation under 460 ℃ of conditions of temperature, kept 1.5-2.2 hour, was preferably 1.8 hours;
E reclaims activator, and the raw material that activation is good is put into pond for recovering, adds water logging and does not have the charcoal face, soaks 1.5-1.9 hour, is preferably 1.7 hours, and the phosphoric acid in the activated material is reclaimed;
F pickling impurity elimination is in the e step, when the activation raw material is washed till phosphoric acid concentration less than 0.3% the time, add water logging and do not have the charcoal face, and to add concentration be 33% hydrochloric acid that hydrochloric acid weight is 6.5% of raw material weight, under 77 ℃ situation, kept 1.0-1.5 hour, be preferably 1.2 hours;
The g dehydration, oven dry;
Carry out abrasive dust again after the h calcining, the granularity of gac can be the 800-1500 order behind the abrasive dust, also can determine the granularity of powder according to customer need;
The i packing is finished product.
The above; only be the specific embodiment of the present invention, but protection scope of the present invention is not limited thereto, anyly is familiar with those skilled in the art in the technical scope that the present invention discloses; the variation that can expect easily or replacement all should be encompassed within protection scope of the present invention.
Claims (8)
1. the production method of an activated carbon for super capacitors, it is characterized in that may further comprise the steps: a selects materials, and selects raw material particle size 10-40 order standby; B boiling, raw material by weight: phosphoric acid=1: 2.5-4.0, adding concentration in raw material is the phosphoric acid of 30-50%, mix all, be 120-140 ℃ in temperature, pressure is under the condition of 0.2-0.5MPa, keeps 1.5-3 hour; The c charing is under 150-300 ℃ the condition, to keep 0.5-1.5 hour in temperature; The d activation under temperature 350-500 ℃ condition, kept 1.5-3 hour; E reclaims activator, and the raw material that activation is good is put into pond for recovering, adds water logging and does not have the charcoal face, soaks 1-2 hour, and the phosphoric acid in the activated material is reclaimed; F pickling impurity elimination in the e step, when the activation raw material is washed till phosphoric acid concentration less than 0.3% the time, adds water logging and there is not the charcoal face and adds the hydrochloric acid that concentration is 33-35%, and hydrochloric acid weight is the 5-7% of raw material weight, under 70-80 ℃ situation, keeps 1-2 hour; The g dehydration, oven dry, abrasive dust, packing is finished product.
2. the production method of activated carbon for super capacitors according to claim 1, it is characterized in that: during boiling, also can be with phosphoric acid, adding weight in raw material is the 0.5-3% expanding agent of raw material weight, expanding agent is a kind of of potassium primary phosphate or iron nitrate or borax, or the mixing of 2 kinds or 3 kinds.
3. the production method of activated carbon for super capacitors according to claim 2 is characterized in that: 2 kinds when mixing, be one of following: potassium primary phosphate and iron nitrate are 1 by weight: 1.5-3.5; Potassium primary phosphate and borax are 1 by weight: 1.5-3.5; Iron nitrate and borax are 1 by weight: 1.5-3.5; During 3 kinds of mixing, be: by weight, potassium primary phosphate: iron nitrate: borax is 1: 0.5-3.5: 0.5-3.5.
4. the production method of activated carbon for super capacitors according to claim 3 is characterized in that: potassium primary phosphate is substituted by SODIUM PHOSPHATE, MONOBASIC.
5. the production method of activated carbon for super capacitors according to claim 1, it is characterized in that: after oven dry, carry out calcination process, material after finger will be dried is contained in airtight container, place under 800-1000 ℃ the condition, kept 1-2.5 hour, carry out abrasive dust afterwards again, packing is finished product.
6. the production method of activated carbon for super capacitors according to claim 1, it is characterized in that: charing and activation are carried out in rotary kiln, and the rotary kiln furnace superintendent is a 15-20 rice, and obliquity is 10-35 °, rotating speed is adjustable, the upper end is a feeding mouth, and the lower end is a heating gate, thereby rotary kiln is divided into two portions, it is the cold zone on top, the high-temperature zone of lower section, cold zone is used for charing, and the high-temperature zone is used for activation.
7. the production method of activated carbon for super capacitors according to claim 1, it is characterized in that: raw material is one of wood sawdust, apricot shell, peach shell, nut-shell, Exocarpium cocois (Cocos nucifera L), corn cob, cotton stalk.
8. the production method of activated carbon for super capacitors according to claim 7, it is characterized in that: when being raw material with one of apricot shell, peach shell, nut-shell, Exocarpium cocois (Cocos nucifera L), corn cob, cotton stalk, then pulverize earlier, with raw material crushing, screening, forming particle diameter is 10-40 order raw material.
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Open date: 20100630 |