CN109133056A - A kind of high anticracking material of active carbon - Google Patents
A kind of high anticracking material of active carbon Download PDFInfo
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- CN109133056A CN109133056A CN201810995487.XA CN201810995487A CN109133056A CN 109133056 A CN109133056 A CN 109133056A CN 201810995487 A CN201810995487 A CN 201810995487A CN 109133056 A CN109133056 A CN 109133056A
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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
- C01B32/354—After-treatment
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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
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- C01B32/312—Preparation
- C01B32/342—Preparation characterised by non-gaseous activating agents
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Abstract
The invention discloses a kind of high anticracking materials of active carbon, belong to chemical field.The present invention is using coconut husk as raw material, in glycerol, rilanit special mechanical milling process, can sufficiently expose organic principle therein such as glucose, pentosan, can cooperate rigid Nano-meter SiO_22It is coupled this material system with the sodium humate of high activity, the flexural strength of system can be effectively improved；The present invention using bacteria cellulose, starch octenyl succinate anhydride etc. be wall material, oil plant is core material, calcium bicarbonate solution is inorganic flocculating agent, and terephthalaldehyde is crosslinking agent, the Nano-meter SiO_2 of addition2With great specific surface area, surface atom has high unsaturation again, improves the dispersibility of this material impact energy and absorbability, so that flexural strength, compression strength is improved.The present invention solves the problems, such as that the flexural strength of common absorbent charcoal material, compression strength are poor at present.
Description
Technical field
The invention belongs to chemical fields, and in particular to a kind of high anticracking material of active carbon.
Background technique
With the implementation and development of building energy conservation, environment-friendly materials and product are increasingly valued by people.And make at present
Environment-friendly materials are not ideal enough in various performances, especially on environment-friendly insulating construction material.
Active carbon is also known as activated carbon black, is one of common adsorbent, is widely used in all trades and professions.Active carbon has very
Strong physical absorption and chemisorption function.Its absorption property is largely decided by its pore property.Active carbon hole
Gap distribution is distributed in three, i.e., macropore, mesoporous and micropore account for certain proportion.Demand with society to Special adsorbent increases
Add, therefore aperture is carried out effectively to control the target just pursued at Carbon Materials researcher.
Active carbon is the carbonaceous adsorbent material for having pore structure prosperity, large specific surface area, selective adsorption capacity strong.?
Under conditions of certain, adsorbing and removing, purification, purification or recycling are carried out to a certain or Cucumber of liquid or gas, thus real
The purification of existing product and the purification of environment.It is generally acknowledged that the hole of active carbon is made of macropore, mesoporous and micropore, macropore diameter is big
In 50nm, mesoporous is 2~50nm, and micropore size is less than 2nm.
Preparing the common method of active carbon at present has physical activation method, chemical activation method or physically activated and chemical activation knot
The method of conjunction.It is vapor, carbon dioxide and their mixed gas that activated gas is commonly used in physical activation method, i.e., will carbonize
Carbon material afterwards is reacted with activated gas to form the technique of hole.Chemical activation method is by various carbon raw materials and chemistry
After drug is uniformly mixed or impregnated, at a suitable temperature, activity is produced with processes such as recycling chemicals by carbonizing, activating
A kind of method of charcoal.Chemical activating agent used is usually zinc chloride, phosphoric acid or alkali.It is physically activated to be with chemical activation combined techniques
Finger is first carbonized carbon raw material, after chemical activation, then carries out the further reaming of gas activation.
Current absorbent charcoal material existing on the market be applied to in compression strength, the building of High anti bending strength there is also
Insufficient problem.Therefore a kind of high anticracking material of the active carbon that bending and compressive strength is high need to be developed.
Summary of the invention
The technical problems to be solved by the invention: poor for the flexural strength of current common absorbent charcoal material, compression strength
The problem of, a kind of high anticracking material of active carbon is provided.
In order to solve the above technical problems, the present invention is using technical solution as described below:
A kind of high anticracking material of active carbon, including following component: 10 ~ 15 parts of lignite, 6 ~ 10 parts of pitch cokes, 5 ~ 10 parts of hydroxides
Iron, 2 ~ 5 parts of NaH2PO4, 4 ~ 8 parts of auxiliary agents, further includes: 20 ~ 45 parts of composite activated carbon substrates, 15 ~ 30 parts of multiple emulsions.
The preparation method of the composite activated carbon substrate, includes the following steps:
(1) it takes coconut husk to wash, dries, pulverize and sieve, in 40 ~ 55 DEG C, take sieving particle 1:8 in mass ratio ~ 15 that reagent A is added mixed
Stirring is closed, is stored at room temperature, mixed gas, HIGH PRESSURE TREATMENT are passed through, pressure release discharges, must pre-process coconut husk particle, take pretreatment coconut husk
Rilanit special, glycerol mixing is added in particle 10:1 ~ 3:1 in mass ratio, and zirconium oxide ball milling pearl is added by 20 ~ 30:1 of ratio of grinding media to material,
Ball milling obtains ball milling material, and ball milling material ethanol solution is taken to clean, dry, obtains dried object, takes dried object in 550 ~ 750 DEG C of high temperature pyrolysis,
It must be pyrolyzed material, take pyrolysis material 1:10 in mass ratio ~ 15 that HCl solution is added and impregnate, be warming up to 90 ~ 100 DEG C, keep the temperature, filtering takes filter
Slag washes with water, dry, obtains active carbon base-material；
(2) take active carbon base-material 1:4 in mass ratio ~ 6 that KOH mixing is added, grinding leads to argon gas protection, is warming up to 400 ~ 500 DEG C,
Heat preservation is warming up to 800 ~ 1000 DEG C, keeps the temperature, cooling, obtains activation products, takes activation products 1:12 in mass ratio ~ 18 that reagent B is added
It is mixed, is stored at room temperature, filter, take filter residue and drying to get composite activated carbon substrate.
Mixed gas in the step (1): 5:1 ~ 3 take oxygen, carbon dioxide mix to get gaseous mixture by volume
Body.
Reagent A in the step (1): in mass ratio 1:3 ~ 6:1:20 ~ 40 take glucose, citric acid, sodium bicarbonate,
NaH2PO4Solution mixes to get reagent A.
Reagent B in the step (2): 5:1 ~ 3:1:15 ~ 25 take ethylenediamine, urea, hydrazine hydrate, deionization in mass ratio
Water mixes to get reagent B.
The preparation of the multiple emulsion: in 30 ~ 45 DEG C, according to parts by weight, 10 ~ 15 parts of bacteria celluloses, 8 ~ 12 parts are taken
Starch octenyl succinate anhydride, 6 ~ 10 parts of auxiliary materials, 80 ~ 100 parts of water are mixed in container, are stored at room temperature swelling, it is warming up to 85 ~
95 DEG C, heating stirring obtains mixed liquor, takes mixed liquor that the oil plant of mixed liquor quality 2 ~ 5% is added, and is cooled to 35 ~ 45 DEG C, is added mixed
The calcium bicarbonate solution for closing liquid quality 6 ~ 10%, is stirred, and the ethyl alcohol that the terephthalaldehyde of mixed liquor quality 6 ~ 10% is added is molten
Liquid is stirred to react, and adjusts pH to get multiple emulsion.
The auxiliary material: 8:1 ~ 3:1 in mass ratio takes carboxymethyl cellulose, Nano-meter SiO_22, microcrystalline wax mixing to get auxiliary
Material.
The oil plant: 4:1 ~ 3 take linseed oil, rilanit special mixing to get oil plant in mass ratio.
The water-reducing agent: any one in poly carboxylic acid series water reducer TH-928, XBW-10.
The auxiliary agent: 8:1 ~ 3 take polyvinylpyrrolidone, sodium humate mixing to get auxiliary agent in mass ratio.
The present invention is compared with other methods, and advantageous effects are:
(1) for the present invention using coconut husk as raw material, crushing is dipped in solvent A, then puts into autoclave and is pressurizeed using mixed gas, so that
Ingredient in solvent A penetrates sufficiently into inside coconut husk particle, in glycerol, rilanit special mechanical milling process, can sufficiently expose
Organic principle therein such as glucose, pentosan increase the ratio of carbon distribution material by pyrolysis, KOH activation grinding, high-temperature roasting
Surface area and aperture, then mix with solvent B, impregnate and can access nitrogen-atoms well, material can be improved in the introducing of nitrogen-containing functional group
The absorption property on surface, and rigid Nano-meter SiO_2 can be cooperated2It is coupled this material system with the sodium humate of high activity, it can be effective
The flexural strength of raising system；
(2) present invention using bacteria cellulose, starch octenyl succinate anhydride etc. be wall material, oil plant is core material, calcium bicarbonate solution
For inorganic flocculating agent, terephthalaldehyde is crosslinking agent, multiple emulsion processed, during the preparation process, the use of calcium bicarbonate, and on the one hand
Bacteria cellulose and starch octenyl succinate anhydride in system can be made to be precipitated, generation mutually separates, and coat core material oil plant formed it is micro-
Capsule, and calcium bicarbonate is heated in subsequent processes and decomposes, the calcium bicarbonate of generation can be used as filler and be adsorbed by system
It is fixed, and carbon dioxide can further strengthen emulsification dispersion effect, in use, as there is fine fisssure in absorbent charcoal material
Line, linseed oil, rilanit special exudation in oil plant can form film after dry solidification, and the calcium carbonate wherein dispersed can be with
Linseed oil forms a film jointly, realizes the reinforcing to micro-crack, and Crack prevention further expands, realizes the self-healing of micro-crack, play
Crack resistence effect, the Nano-meter SiO_2 of addition2With great specific surface area, surface atom has high unsaturation, micro-crack again
Nano-meter SiO_2 is encountered in extension2Can occur sheaths of bamboo shoots to or deflection, absorb energy and have the function that cracking resistance, Nano-meter SiO_22Itself also have
Good compatibility improves the dispersibility of this material impact energy and absorbability, so that flexural strength, compression strength
It is improved.
Specific embodiment
Reagent A: 1:3 ~ 6:1:20 ~ 40 take glucose, citric acid, sodium bicarbonate, concentration 0.1mol/L in mass ratio
NaH2PO4Solution mixes to get reagent A；
Reagent B: 5:1 ~ 3:1:15 ~ 25 take ethylenediamine, urea, hydrazine hydrate, deionized water mixing to get reagent B in mass ratio；
Mixed gas: 5:1 ~ 3 take oxygen, carbon dioxide mix to get mixed gas by volume；
Auxiliary agent: 8:1 ~ 3 take polyvinylpyrrolidone, sodium humate mixing to get auxiliary agent in mass ratio；
Water-reducing agent: any one in poly carboxylic acid series water reducer TH-928, XBW-10；
Oil plant: 4:1 ~ 3 take linseed oil, rilanit special mixing to get oil plant in mass ratio；
Auxiliary material: 8:1 ~ 3:1 in mass ratio takes carboxymethyl cellulose, Nano-meter SiO_22, microcrystalline wax mixing to get auxiliary material；
The preparation method of composite activated carbon substrate, includes the following steps:
(1) coconut husk is taken to be cleaned with 3 ~ 6 times of coconut husk quality of water, naturally dry crushed 120 meshes, in 40 ~ 55 DEG C of water-bath, take
Reagent A mixing is added in the particle 1:8 in mass ratio ~ 15 that is sieved, and stirs 30 ~ 50min with 400 ~ 600r/min, is stored at room temperature 2 ~ 5h
Afterwards, autoclave is moved into, is passed through mixed gas, controlling pressure in kettle is 8.2 ~ 9.5MPa, 20 ~ 45min of HIGH PRESSURE TREATMENT, with 0.05 ~
0.09MPa/s pressure release to normal pressure, discharging must pre-process coconut husk particle, and pretreatment coconut husk particle 10:1 ~ 3:1 in mass ratio is taken to add
Enter rilanit special, glycerol mixing, by 20 ~ 30:1 of ratio of grinding media to material addition zirconium oxide ball milling pearl, with 350 ~ 600r/min, 1 ~ 3h of ball milling,
Ball milling material, after taking ball milling material to clean 3 ~ 5 times with the ethanol solution of volume fraction 60%, in 60 ~ 80 DEG C of oven dryings to constant weight,
Dried object, take dried object in the tube furnace of argon atmosphere, be warming up to 550 ~ 750 DEG C with 5 ~ 8 DEG C/min, high temperature pyrolysis 3 ~
5h must be pyrolyzed material, and the HCl solution for taking pyrolysis material 1:10 in mass ratio ~ 15 that mass fraction 10% is added impregnates, and be warming up to 90 ~ 100
DEG C, 20 ~ 45min is kept the temperature, filtering moves to 100 ~ 110 DEG C of oven dryings 12 after taking filter residue to be neutral to washing lotion wash with distilled water
~ 15h obtains active carbon base-material；
(2) it takes active carbon base-material 1:4 in mass ratio ~ 6 that KOH mixing is added, 20 ~ 45min is ground with 300 ~ 500r/min, moves to earthenware
Crucible is put into tube furnace, leads to argon gas protection, is warming up to 400 ~ 500 DEG C with 5 ~ 8 DEG C/min rate, keeps the temperature 35 ~ 60min, then be warming up to
800 ~ 1000 DEG C, 45 ~ 60min is kept the temperature, cooled to room temperature obtains activation products, and activation products 1:12 ~ 18 in mass ratio is taken to add
Enter reagent B mixing, 30 ~ 50min is stirred with 400 ~ 600r/min, is stored at room temperature 1 ~ 3h, is filtered, filter residue is taken to dry in 100 ~ 120 DEG C
Case drying is to constant weight to get composite activated carbon substrate；
The preparation of multiple emulsion: in 30 ~ 45 DEG C, according to parts by weight, 10 ~ 15 parts of bacteria celluloses, 8 ~ 12 parts of octenyl ambers are taken
Amber acid-starch ester, 6 ~ 10 parts of auxiliary materials, 80 ~ 100 parts of water are mixed in container, after stirring 10 ~ 25min with 400 ~ 600r/min, room temperature
Stand swelling 4 ~ 6h, be warming up to 85 ~ 95 DEG C, 20 ~ 35min of heating stirring obtains mixed liquor, take mixed liquor be added mixed liquor quality 2 ~
5% oil plant is cooled to 35 ~ 45 DEG C, and the mass fraction that mixed liquor quality 6 ~ 10% is added is 20% calcium bicarbonate solution, and stirring is mixed
20 ~ 30min is closed, the ethanol solution of the terephthalaldehyde of the concentration 0.3mol/L of mixed liquor quality 6 ~ 10% is added, it is stirred to react 2 ~
After 5h, pH to 8.5 ~ 9.0 is adjusted to get multiple emulsion with the sodium hydroxide solution of concentration 0.1mol/L；
A kind of high anticracking material of active carbon, according to the mass fraction, including following component: 10 ~ 15 parts of lignite, 6 ~ 10 parts of pitch cokes, 5
~ 10 parts of iron hydroxides, 2 ~ 5 parts of NaH2PO4, 4 ~ 8 parts of auxiliary agent, 20 ~ 45 parts of composite activated carbon substrates, 15 ~ 30 parts of multiple emulsions；
A kind of preparation method of the high anticracking material of active carbon, includes the following steps:
(1) according to the mass fraction, including following component: 10 ~ 15 parts of lignite, 6 ~ 10 parts of pitch cokes, 5 ~ 10 parts of iron hydroxides, 2 ~ 5
Part NaH2PO4, 4 ~ 8 parts of auxiliary agent, 20 ~ 45 parts of composite activated carbon substrates, 15 ~ 30 parts of multiple emulsions；
(2) it takes pitch coke, lignite, composite activated carbon substrate to mix in pulverizer, crushed 150 meshes, in high-temperature activation furnace
650 ~ 850 DEG C of 4 ~ 8h of heat treatment, must be heat-treated material, take heat treatment material in N2Under atmosphere, iron hydroxide, NaH is added2PO4, auxiliary agent,
Multiple emulsion mixing after stirring 30 ~ 50min with 400 ~ 600r/min, is evaporated in vacuo to constant weight in 70 ~ 90 DEG C, obtains concentrate, take
Concentrate crushed 800 meshes in micronizer, collect sieving particle to get the high anticracking material of active carbon.
Embodiment 1
Reagent A: 1:6:1:40 in mass ratio takes the NaH of glucose, citric acid, sodium bicarbonate, concentration 0.1mol/L2PO4Solution
Mixing is to get reagent A；
Reagent B: 5:3:1:25 in mass ratio takes ethylenediamine, urea, hydrazine hydrate, deionized water mixing to get reagent B；
Mixed gas: 5:3 takes oxygen, carbon dioxide mix to get mixed gas by volume；
Auxiliary agent: 8:3 in mass ratio takes polyvinylpyrrolidone, sodium humate mixing to get auxiliary agent；
Water-reducing agent: poly carboxylic acid series water reducer TH-928；
Oil plant: 4:3 in mass ratio takes linseed oil, rilanit special mixing to get oil plant；
Auxiliary material: 8:3:1 in mass ratio takes carboxymethyl cellulose, Nano-meter SiO_22, microcrystalline wax mixing to get auxiliary material；
The preparation method of composite activated carbon substrate, includes the following steps:
(1) coconut husk is taken to be cleaned with 3 times of coconut husk quality of water, naturally dry crushed 120 meshes, in 40 DEG C of water-bath, take sieving
Reagent A mixing is added in grain 1:8 in mass ratio, stirs 30min with 400r/min, after being stored at room temperature 2h, moves into autoclave, is passed through mixed
Gas is closed, controlling pressure in kettle is 8.2MPa, HIGH PRESSURE TREATMENT 20min, and with 0.05MPa/s pressure release to normal pressure, discharging must be pre-processed
Coconut husk particle takes pretreatment coconut husk particle 10:1:1 in mass ratio that rilanit special, glycerol mixing is added, adds by ratio of grinding media to material 20:1
Enter zirconium oxide ball milling pearl, with 350r/min ball milling 1h, obtains ball milling material, ball milling material is taken to clean 3 with the ethanol solution of volume fraction 60%
After secondary, in 60 DEG C of oven dryings to constant weight, dried object is obtained, takes dried object in the tube furnace of argon atmosphere, with 5 DEG C/min heating
To 550 DEG C, high temperature pyrolysis 3h must be pyrolyzed material, and the HCl solution for taking pyrolysis material 1:10 in mass ratio that mass fraction 10% is added impregnates,
90 DEG C are warming up to, 20min is kept the temperature, filtering moves to 100 DEG C of oven dryings after taking filter residue to be neutral to washing lotion wash with distilled water
12h obtains active carbon base-material；
(2) it takes active carbon base-material 1:4 in mass ratio that KOH mixing is added, 20min is ground with 300r/min, crucible is moved to, is put into pipe
Formula furnace, leads to argon gas protection, is warming up to 400 DEG C with 5 DEG C/min rate, keeps the temperature 35min, then be warming up to 800 DEG C, keeps the temperature 45min, from
It is so cooled to room temperature, obtains activation products, take activation products 1:12 in mass ratio that reagent B mixing is added, stirred with 400r/min
30min is stored at room temperature 1h, and filtering takes filter residue in 100 DEG C of oven dryings to constant weight to get composite activated carbon substrate；
The preparation of multiple emulsion: in 30 DEG C, according to parts by weight, 10 parts of bacteria celluloses, 8 parts of octenyl succinic acid starch are taken
Ester, 6 parts of auxiliary materials, 80 parts of water are mixed in container, after stirring 10min with 400r/min, are stored at room temperature swelling 4h, are warming up to 85 DEG C,
Heating stirring 20min, obtains mixed liquor, takes mixed liquor that the oil plant of mixed liquor quality 2% is added, and is cooled to 35 DEG C, and mixed liquor matter is added
The mass fraction of amount 6% is 20% calcium bicarbonate solution, is stirred 20min, and the concentration 0.3mol/L of mixed liquor quality 6% is added
Terephthalaldehyde ethanol solution, after being stirred to react 2h, adjust pH to 8.5 with the sodium hydroxide solution of concentration 0.1mol/L,
Up to multiple emulsion；
A kind of high anticracking material of active carbon, according to the mass fraction, including following component: 10 parts of lignite, 6 parts of pitch cokes, 5 parts of hydrogen-oxygens
Change iron, 2 parts of NaH2PO4, 4 parts of auxiliary agent, 20 parts of composite activated carbon substrates, 15 parts of multiple emulsions；
A kind of preparation method of the high anticracking material of active carbon, includes the following steps:
(1) according to the mass fraction, including following component: 10 parts of lignite, 6 parts of pitch cokes, 5 parts of iron hydroxides, 2 parts of NaH2PO4、4
Part auxiliary agent, 20 parts of composite activated carbon substrates, 15 parts of multiple emulsions；
(2) it takes pitch coke, lignite, composite activated carbon substrate to mix in pulverizer, crushed 150 meshes, in high-temperature activation furnace
650 DEG C of heat treatment 4h, must be heat-treated material, take heat treatment material in N2Under atmosphere, iron hydroxide, NaH is added2PO4, auxiliary agent, Composite Milk
Liquid mixing after stirring 30min with 400r/min, is evaporated in vacuo to constant weight in 70 DEG C, obtains concentrate, take concentrate in ultramicro grinding
Machine crushed 800 meshes, collect sieving particle to get the high anticracking material of active carbon.
Embodiment 2
Reagent A: 1:5:1:30 in mass ratio takes the NaH of glucose, citric acid, sodium bicarbonate, concentration 0.1mol/L2PO4Solution
Mixing is to get reagent A；
Reagent B: 5:2:1:18 in mass ratio takes ethylenediamine, urea, hydrazine hydrate, deionized water mixing to get reagent B；
Mixed gas: 5:2 takes oxygen, carbon dioxide mix to get mixed gas by volume；
Auxiliary agent: 8:2 in mass ratio takes polyvinylpyrrolidone, sodium humate mixing to get auxiliary agent；
Water-reducing agent: poly carboxylic acid series water reducer XBW-10；
Oil plant: 4:2 in mass ratio takes linseed oil, rilanit special mixing to get oil plant；
Auxiliary material: 8:2:1 in mass ratio takes carboxymethyl cellulose, Nano-meter SiO_22, microcrystalline wax mixing to get auxiliary material；
The preparation method of composite activated carbon substrate, includes the following steps:
(1) coconut husk is taken to be cleaned with 5 times of coconut husk quality of water, naturally dry crushed 120 meshes, in 45 DEG C of water-bath, take sieving
Reagent A mixing is added in grain 1:13 in mass ratio, stirs 40min with 500r/min, after being stored at room temperature 4h, moves into autoclave, is passed through
Mixed gas, controlling pressure in kettle is 8.9MPa, HIGH PRESSURE TREATMENT 35min, and with 0.08MPa/s pressure release to normal pressure, discharging obtains pre- place
Coconut husk particle is managed, takes pretreatment coconut husk particle 10:2:1 in mass ratio that rilanit special, glycerol mixing is added, by ratio of grinding media to material 25:1
Zirconium oxide ball milling pearl is added, ball milling material is obtained with 500r/min ball milling 2h, takes the ethanol solution of ball milling material volume fraction 60% clear
After washing 4 times, in 70 DEG C of oven dryings to constant weight, dried object is obtained, takes dried object in the tube furnace of argon atmosphere, with 6 DEG C/min
650 DEG C are warming up to, high temperature pyrolysis 4h must be pyrolyzed material, take pyrolysis material 1:13 in mass ratio that the HCl solution of mass fraction 10% is added
It impregnates, is warming up to 95 DEG C, keep the temperature 35min, filtering moves to 105 DEG C of baking ovens after taking filter residue to be neutral to washing lotion wash with distilled water
Dry 13h, obtains active carbon base-material；
(2) it takes active carbon base-material 1:5 in mass ratio that KOH mixing is added, 35min is ground with 400r/min, crucible is moved to, is put into pipe
Formula furnace, leads to argon gas protection, is warming up to 450 DEG C with 6 DEG C/min rate, keeps the temperature 50min, then be warming up to 900 DEG C, keeps the temperature 50min, from
It is so cooled to room temperature, obtains activation products, take activation products 1:15 in mass ratio that reagent B mixing is added, stirred with 500r/min
40min is stored at room temperature 2h, and filtering takes filter residue in 110 DEG C of oven dryings to constant weight to get composite activated carbon substrate；
The preparation of multiple emulsion: in 38 DEG C, according to parts by weight, 13 parts of bacteria celluloses, 10 parts of octenyl succinic acid starch are taken
Ester, 8 parts of auxiliary materials, 90 parts of water are mixed in container, after stirring 18min with 500r/min, are stored at room temperature swelling 5h, are warming up to 90 DEG C,
Heating stirring 28min, obtains mixed liquor, takes mixed liquor that the oil plant of mixed liquor quality 4% is added, and is cooled to 38 DEG C, and mixed liquor matter is added
The mass fraction of amount 8% is 20% calcium bicarbonate solution, is stirred 25min, and the concentration 0.3mol/L of mixed liquor quality 8% is added
Terephthalaldehyde ethanol solution, after being stirred to react 4h, adjust pH to 8.8 with the sodium hydroxide solution of concentration 0.1mol/L,
Up to multiple emulsion；
A kind of high anticracking material of active carbon, according to the mass fraction, including following component: 13 parts of lignite, 8 parts of pitch cokes, 8 parts of hydrogen-oxygens
Change iron, 4 parts of NaH2PO4, 6 parts of auxiliary agent, 35 parts of composite activated carbon substrates, 20 parts of multiple emulsions；
A kind of preparation method of the high anticracking material of active carbon, includes the following steps:
(1) according to the mass fraction, including following component: 13 parts of lignite, 8 parts of pitch cokes, 8 parts of iron hydroxides, 3 parts of NaH2PO4、6
Part auxiliary agent, 40 parts of composite activated carbon substrates, 20 parts of multiple emulsions；
(2) it takes pitch coke, lignite, composite activated carbon substrate to mix in pulverizer, crushed 150 meshes, in high-temperature activation furnace
750 DEG C of heat treatment 6h, must be heat-treated material, take heat treatment material in N2Under atmosphere, iron hydroxide, NaH is added2PO4, auxiliary agent, Composite Milk
Liquid mixing after stirring 40min with 500r/min, is evaporated in vacuo to constant weight in 80 DEG C, obtains concentrate, take concentrate in ultramicro grinding
Machine crushed 800 meshes, collect sieving particle to get the high anticracking material of active carbon.
Embodiment 3
Reagent A: 1:6:1:40 in mass ratio takes the NaH of glucose, citric acid, sodium bicarbonate, concentration 0.1mol/L2PO4Solution
Mixing is to get reagent A；
Reagent B: 5:3:1:25 in mass ratio takes ethylenediamine, urea, hydrazine hydrate, deionized water mixing to get reagent B；
Mixed gas: 5:3 takes oxygen, carbon dioxide mix to get mixed gas by volume；
Auxiliary agent: 8:3 in mass ratio takes polyvinylpyrrolidone, sodium humate mixing to get auxiliary agent；
Water-reducing agent: poly carboxylic acid series water reducer TH-928；
Oil plant: 4:3 in mass ratio takes linseed oil, rilanit special mixing to get oil plant；
Auxiliary material: 8:3:1 in mass ratio takes carboxymethyl cellulose, Nano-meter SiO_22, microcrystalline wax mixing to get auxiliary material；
The preparation method of composite activated carbon substrate, includes the following steps:
(1) coconut husk is taken to be cleaned with 6 times of coconut husk quality of water, naturally dry crushed 120 meshes, in 55 DEG C of water-bath, take sieving
Reagent A mixing is added in grain 1:15 in mass ratio, stirs 50min with 600r/min, after being stored at room temperature 5h, moves into autoclave, is passed through
Mixed gas, controlling pressure in kettle is 9.5MPa, HIGH PRESSURE TREATMENT 45min, and with 0.09MPa/s pressure release to normal pressure, discharging obtains pre- place
Coconut husk particle is managed, takes pretreatment coconut husk particle 10:3:1 in mass ratio that rilanit special, glycerol mixing is added, by ratio of grinding media to material 30:1
Zirconium oxide ball milling pearl is added, ball milling material is obtained with 600r/min ball milling 3h, takes the ethanol solution of ball milling material volume fraction 60% clear
After washing 5 times, in 80 DEG C of oven dryings to constant weight, dried object is obtained, takes dried object in the tube furnace of argon atmosphere, with 8 DEG C/min
750 DEG C are warming up to, high temperature pyrolysis 5h must be pyrolyzed material, take pyrolysis material 1:15 in mass ratio that the HCl solution of mass fraction 10% is added
It impregnates, is warming up to 100 DEG C, keep the temperature 45min, filtering moves to 110 DEG C of bakings after taking filter residue to be neutral to washing lotion wash with distilled water
Case dries 15h, obtains active carbon base-material；
(2) it takes active carbon base-material 1:6 in mass ratio that KOH mixing is added, 45min is ground with 500r/min, crucible is moved to, is put into pipe
Formula furnace, leads to argon gas protection, is warming up to 500 DEG C with 8 DEG C/min rate, keeps the temperature 60min, then be warming up to 1000 DEG C, keeps the temperature 60min,
Cooled to room temperature obtains activation products, takes activation products 1:18 in mass ratio that reagent B mixing is added, is stirred with 600r/min
50min is stored at room temperature 3h, and filtering takes filter residue in 120 DEG C of oven dryings to constant weight to get composite activated carbon substrate；
The preparation of multiple emulsion: in 45 DEG C, according to parts by weight, 15 parts of bacteria celluloses, 12 parts of octenyl succinic acid starch are taken
Ester, 10 parts of auxiliary materials, 100 parts of water are mixed in container, after stirring 25min with 600r/min, are stored at room temperature swelling 6h, are warming up to 95
DEG C, heating stirring 35min obtains mixed liquor, takes mixed liquor that the oil plant of mixed liquor quality 5% is added, and is cooled to 45 DEG C, and mixing is added
The mass fraction of liquid quality 10% is 20% calcium bicarbonate solution, is stirred 30min, and the concentration of mixed liquor quality 10% is added
The ethanol solution of the terephthalaldehyde of 0.3mol/L after being stirred to react 5h, is adjusted with the sodium hydroxide solution of concentration 0.1mol/L
PH to 9.0 is to get multiple emulsion；
A kind of high anticracking material of active carbon, according to the mass fraction, including following component: 15 parts of lignite, 10 parts of pitch cokes, 10 parts of hydrogen
Iron oxide, 5 parts of NaH2PO4, 8 parts of auxiliary agent, 45 parts of composite activated carbon substrates, 30 parts of multiple emulsions；
A kind of preparation method of the high anticracking material of active carbon, includes the following steps:
(1) according to the mass fraction, including following component: 15 parts of lignite, 10 parts of pitch cokes, 10 parts of iron hydroxides, 5 parts of NaH2PO4、
8 parts of auxiliary agents, 45 parts of composite activated carbon substrates, 30 parts of multiple emulsions；
(2) it takes pitch coke, lignite, composite activated carbon substrate to mix in pulverizer, crushed 150 meshes, in high-temperature activation furnace
850 DEG C of heat treatment 8h, must be heat-treated material, take heat treatment material in N2Under atmosphere, iron hydroxide, NaH is added2PO4, auxiliary agent, Composite Milk
Liquid mixing after stirring 50min with 600r/min, is evaporated in vacuo to constant weight in 90 DEG C, obtains concentrate, take concentrate in ultramicro grinding
Machine crushed 800 meshes, collect sieving particle to get the high anticracking material of active carbon.
Comparative example 1: it is essentially identical with the preparation method of embodiment 1, it has only the difference is that lacking composite activated carbon substrate.
Comparative example 2: it is essentially identical with the preparation method of embodiment 1, it has only the difference is that lacking multiple emulsion.
Comparative example 3: the high anticracking material of active carbon of Nanjing company production.
Embodiment is compared with the high anticracking material of active carbon obtained by comparative example according to GB/T 7702.3-1997 standard
Test, test result are as shown in table 1.
Table 1
| Test item | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Compression strength (28d/MPa) | 41.3 | 40.8 | 41.1 | 39.4 | 40.1 | 32.3 |
| Flexural strength (MPa) | 22.3 | 21.4 | 21.9 | 20.1 | 20.5 | 16.2 |
| Acoustical ratings (grade) | 1 | 1 | 1 | 1 | 1 | 2 |
| Purifying formaldehyde rate (%) | 95 | 93 | 94 | 92 | 90 | 78 |
In summary, the high anticracking material of active carbon of the invention is more preferable compared to commercial product effect, is worth promoting.
Claims (10)
1. a kind of high anticracking material of active carbon, according to the mass fraction, including following component: 10 ~ 15 parts of lignite, 6 ~ 10 parts of pitches
Coke, 5 ~ 10 parts of iron hydroxides, 2 ~ 5 parts of NaH2PO4, 4 ~ 8 parts of auxiliary agents, which is characterized in that further include: 20 ~ 45 parts of composite activated carbon bases
Material, 15 ~ 30 parts of multiple emulsions.
2. the high anticracking material of a kind of active carbon according to claim 1, which is characterized in that the system of the composite activated carbon substrate
Preparation Method includes the following steps:
(1) it takes coconut husk to wash, dries, pulverize and sieve, in 40 ~ 55 DEG C, take sieving particle 1:8 in mass ratio ~ 15 that reagent A is added mixed
Stirring is closed, is stored at room temperature, mixed gas, HIGH PRESSURE TREATMENT are passed through, pressure release discharges, must pre-process coconut husk particle, take pretreatment coconut husk
Rilanit special, glycerol mixing is added in particle 10:1 ~ 3:1 in mass ratio, and zirconium oxide ball milling pearl is added by 20 ~ 30:1 of ratio of grinding media to material,
Ball milling obtains ball milling material, and ball milling material ethanol solution is taken to clean, dry, obtains dried object, takes dried object in 550 ~ 750 DEG C of high temperature pyrolysis,
It must be pyrolyzed material, take pyrolysis material 1:10 in mass ratio ~ 15 that HCl solution is added and impregnate, be warming up to 90 ~ 100 DEG C, keep the temperature, filtering takes filter
Slag washes with water, dry, obtains active carbon base-material；
(2) take active carbon base-material 1:4 in mass ratio ~ 6 that KOH mixing is added, grinding leads to argon gas protection, is warming up to 400 ~ 500 DEG C,
Heat preservation is warming up to 800 ~ 1000 DEG C, keeps the temperature, cooling, obtains activation products, takes activation products 1:12 in mass ratio ~ 18 that reagent B is added
It is mixed, is stored at room temperature, filter, take filter residue and drying to get composite activated carbon substrate.
3. the high anticracking material of a kind of active carbon according to claim 2, which is characterized in that the gaseous mixture in the step (1)
Body: 5:1 ~ 3 take oxygen, carbon dioxide mix to get mixed gas by volume.
4. the high anticracking material of a kind of active carbon according to claim 2, which is characterized in that the reagent A in the step (1):
1:3 ~ 6:1:20 ~ 40 take glucose, citric acid, sodium bicarbonate, NaH in mass ratio2PO4Solution mixes to get reagent A.
5. the high anticracking material of a kind of active carbon according to claim 2, which is characterized in that the reagent B in the step (2):
5:1 ~ 3:1:15 ~ 25 take ethylenediamine, urea, hydrazine hydrate, deionized water mixing to get reagent B in mass ratio.
6. the high anticracking material of a kind of active carbon according to claim 1, which is characterized in that the preparation of the multiple emulsion: in
30 ~ 45 DEG C, according to parts by weight, take 10 ~ 15 parts of bacteria celluloses, 8 ~ 12 parts of starch octenyl succinate anhydrides, 6 ~ 10 parts of auxiliary materials,
80 ~ 100 parts of water are mixed in container, are stored at room temperature swelling, are warming up to 85 ~ 95 DEG C, heating stirring obtains mixed liquor, takes mixing
The oil plant of mixed liquor quality 2 ~ 5% is added in liquid, is cooled to 35 ~ 45 DEG C, and the calcium bicarbonate solution of mixed liquor quality 6 ~ 10% is added, stirs
Mixing is mixed, the ethanol solution of the terephthalaldehyde of mixed liquor quality 6 ~ 10% is added, is stirred to react, adjusts pH to get Composite Milk
Liquid.
7. the high anticracking material of a kind of active carbon according to claim 6, which is characterized in that the auxiliary material: 8:1 in mass ratio ~
3:1 takes carboxymethyl cellulose, Nano-meter SiO_22, microcrystalline wax mixing to get auxiliary material.
8. the high anticracking material of a kind of active carbon according to claim 6, which is characterized in that the oil plant: 4:1 ~ 3 in mass ratio
Take linseed oil, rilanit special mixing to get oil plant.
9. the high anticracking material of a kind of active carbon according to claim 1, which is characterized in that the water-reducing agent: polycarboxylic-acid subtracts
Any one in aqua TH-928, XBW-10.
10. the high anticracking material of a kind of active carbon according to claim 1, which is characterized in that the auxiliary agent: 8:1 in mass ratio ~
3 take polyvinylpyrrolidone, sodium humate mixing to get auxiliary agent.
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| CN112537765A (en) * | 2020-11-17 | 2021-03-23 | 浙江大学自贡创新中心 | Preparation method of carbon negative electrode material of lithium ion battery |
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