CN109110757A - A kind of activity bone black and preparation method thereof - Google Patents
A kind of activity bone black and preparation method thereof Download PDFInfo
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- CN109110757A CN109110757A CN201811329401.6A CN201811329401A CN109110757A CN 109110757 A CN109110757 A CN 109110757A CN 201811329401 A CN201811329401 A CN 201811329401A CN 109110757 A CN109110757 A CN 109110757A
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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
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/342—Preparation characterised by non-gaseous activating agents
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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
- C01B32/342—Preparation characterised by non-gaseous activating agents
- C01B32/348—Metallic compounds
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Abstract
The present invention relates to adsorbent material field, a kind of active bone black and preparation method thereof is provided.The preparation method of the activity bone black includes mixing smashed animal waste bone with activator and impregnating 12-20h；60~90min is then activated at a temperature of 500 DEG C~850 DEG C and obtains activated material, and it is 6-8 that activated material to pH value, which is directly washed with water, and active bone black is obtained after dry.The specific surface area of its active bone black is 200-500m2/ g, methylene blue adsorption value 30-130mg/g.The application is advantageously implemented the resource utilization of various animal waste bones, is conducive to save the resources such as timber, coal and coconut husk.Prepared various animal bone matrix activity bone black can be used for substituting the partial use of conventional carbon product；Preparation process is not necessarily to inert gas shielding, simple process, easy to industrialized production.
Description
Technical field
The present invention relates to adsorbent material fields, in particular to a kind of active bone black and preparation method thereof.
Background technique
Charcoal adsorbent material is a kind of porosity contenting carbon material, has the characteristics that pore structure prosperity, large specific surface area, is excellent
Good adsorbent, performance is stablized, and regenerating easily, is a kind of environmentally friendly adsorbent, is widely used in metallurgy, changes
The directions such as work, environmental protection.Currently, in charcoal adsorbent material preparation process, mainly with carbon elements such as timber, coal, various shucks
Substance abundant is raw material, and preparing various charcoal adsorbent materials becomes the research hotspot of domestic and foreign scholars.
It is well known that there is the population more than 1,300,000,000 in China, the amount of consumed various meats is very huge, thus is generated
Various livestocks, the quantity of the useless bone of poultry is also very huge surprising.General bone accounts for the certain proportion of organism, and pig is
12.9%, ox 20.5%, sheep is that 32.2% (the bone ratio of sheep is to take level-one sheep 24.3%, second level sheep 31.8%, thin sheep
40.5% average value), poultry be 30%~45%.For 2015, pig, ox, sheep, poultry meat yield be respectively
5486.5,700.1,440.8,1826.3 ten thousand tons, and then estimating current year pig bone yield is more than 812 ten thousand tons, ox bone yield is 180
Remaining ten thousand tons, more than 209 ten thousand tons of sheep bone, more than 782~1,264 ten thousand tons of poultry bone.The processing of these bones has become a great problem, processing
It is bad just pollute the environment, waste of resource.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of active bone black, and various animal waste bones are prepared into
Absorbent charcoal material is conducive to recycling and the protection environment of resource well using discarded bone.
Another object of the present invention is to provide a kind of active bone black, a variety of absorption of the alternative active carbon of activity bone black
Purposes is not only advantageous to realize the resource utilization of various this wastes of animal waste bone, and be conducive to save timber,
The resources such as coal and coconut husk.
The embodiment of the present invention is achieved in that
A kind of preparation method of activity bone black comprising smashed animal waste bone is mixed and impregnated with activator
12-20h；60~90min is then activated at a temperature of 500 DEG C~850 DEG C and obtains activated material, and activated material is directly washed with water to pH
Value is 6-8, and active bone black is obtained after dry.
A kind of activity bone black is prepared by the preparation method of above-mentioned active bone black；The specific surface area of active bone black
For 200-500m2/ g, methylene blue adsorption value 30-130mg/g.
The beneficial effect of the embodiment of the present invention for example,
For the application using animal waste bone as raw material, phosphoric acid or potassium hydroxide or zinc chloride or magnesium chloride are activator preparation
Large specific surface area out, the high active bone black of absorption property；It is advantageously implemented the resource utilization of various animal waste bones, favorably
In resources such as saving timber, coal and coconut husks.Prepared various animal bone matrix activity bone black can be used for substituting conventional carbon
The partial use of product；Preparation process is not necessarily to inert gas shielding, simple process, easy to industrialized production.
Specific embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will
Understand, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the invention.It is not specified in embodiment specific
Condition person carries out according to conventional conditions or manufacturer's recommended conditions.Reagents or instruments used without specified manufacturer is
The conventional products that can be obtained by commercially available purchase.
Active bone black of the embodiment of the present invention and preparation method thereof is specifically described below.
There is also differences for the complicated composition of bone, beast bone and fowl bone composed structure, chemical component, also produce to reasonable utilize
Challenge.At present useless bone by the way of mainly have bone mud (first hot mastication, then high power crush), gelatine (high pressure be made in bone black
Boiling proposes marrow, reheats dissolution bleaching, then in vacuum evaporating pot inspissation, goes out finished product after finally drying), animal oil is (by bone
Crush, boiling added to boil to bone powdering, the oil taken out on pot face is condensed into animal oil), bone meal (mentions the remaining bone meal of Wangue oil to add
Water, a small amount of potassium carbonate heat 24~30 hours, after dry be crushed and screened into bone meal), bone fat (bone is put into boiling in pressure cooker
It 10 hours, then takes out upper liquid and is contained in water-bath and heat repeatedly, rear to extract upper layer faint yellow, transparent, no moisture impurity
Bone fat), bone ash (live stock and fowl bone is burnt until at ash), shine bone and (bone scraped off interior muscle to be immersed in lime water 20~30 days
Then take out to be exposed to the sun finally rub to be trimmed to and shine bone) and bone black (by bone destructive distillation acquirement grease, then increase temperature and make its carbon
Change, taking-up crushes to obtain bone black), these products food, chemical industry, daily necessity manufacture, medicine, in terms of have it is wide
General purposes.
Various animal waste bones are innovatively prepared into absorbent charcoal material in the application, discarded bone is utilized well
Head is conducive to recycling and the protection environment of resource.
Specifically, this application provides a kind of preparation methods of active bone black comprising following steps:
S1, dry: it is 5-15% that animal waste bone, which is dried to moisture,.
S2, crushing: animal waste bone is crushed according to process requirement.
S3, activator dipping: smashed animal waste bone is mixed with activator and impregnates 12-20h.Wherein, living
The mass ratio of agent and animal waste bone is 1.5-3:1, and activator includes in potassium hydroxide, phosphoric acid, zinc chloride and magnesium chloride
It is one or more.
By impregnating animal waste bone with activator, these usual activators have dehydration to carbonaceous organic material
Effect, run-inflation effect can come into full contact with discarded bone, at a certain temperature (different activators require temperature range different)
Make its activation, activator interacts with material at high temperature in the process, and the carbon in organic matter is made to be fixed up (such as phosphorus
Acid), corrode and aoxidize unsetting part formation micropore, mesoporous, so that specific surface area be significantly greatly increased), so that discarded bone is activated
For the adsorbent material with stronger adsorption capacity.
It is worth noting that, its mass ratio with animal waste bone of different activator is selected to have difference slightly, and
And the concentration of activator also has difference.
Such as: in the other embodiments of the application, when activator is potassium hydroxide, potassium hydroxide and animal waste
The mass ratio of bone is 1.5-2.5:1, and the concentration of potassium hydroxide is greater than 50%；In the other embodiments of the application, work as work
When agent is phosphoric acid, the mass ratio of phosphoric acid and animal waste bone is 2-3:1, the concentration 50-85% of phosphoric acid；In its of the application
In his embodiment, when activator is zinc chloride, the mass ratio of zinc chloride and animal waste bone is 2-3:1, zinc chloride
Concentration is greater than 60%；In the other embodiments of the application, when activator is magnesium chloride, magnesium chloride and animal waste bone
Mass ratio be 2-3:1, the concentration of magnesium chloride is greater than 60%.
S4, high-temperature activation: 60~90min is then activated at a temperature of 500 DEG C~850 DEG C and obtains activated material.
Specifically, the first activation temperature is warming up to the heating rate of 15-25 DEG C/min, activates 20-30min, then with
The heating rate of 5-10 DEG C/min is warming up to the second activation temperature, continues to activate 40-60min；Wherein, the first activation temperature is
500 DEG C~750 DEG C, the second activation temperature is 600 DEG C~850 DEG C；First activation temperature is lower than the second activation temperature.
In the application, high-temperature activation is carried out to the animal waste bone after dipping by stepped activation temperature, first
It is warming up to the first activation temperature with the heating rate of 15-25 DEG C/min, and is activated under the first activation temperature, is realized to dynamic
Object discards the preheating and charing of bone, while being attached to the activator of animal waste bone surface by high temperature evaporation part after impregnating
Gas is formed, portion gas enters with the charing of animal waste bone inside carbon material at this time, when under the first activation temperature
Activation after, the second activation temperature is warming up to the heating rate of 5-10 DEG C/min, it can be seen that living being warming up to second
Heating rate when changing temperature is significantly lower than heating rate when being warming up to the first activation temperature, this is because first with higher liter
Warm speed is warming up to the first activation temperature, is activated, as early as possible the charing of animal waste bone, and then with lower heating speed
Degree is warming up to the second activation temperature, so that the animal waste bone carbonized constantly opens hole in the state of continuous activation,
It is easy to the gas reaction generated with activator high temperature, in turn results in constantly expanding and develop in depth for hole.As activation is anti-
The continuous progress answered, activation temperature are increased to the second activation temperature, and new unsaturated carbon atom or active site are then exposed to crystallite
Surface, then these new active sites can be reacted again with other molecules of activated gas, microporous surface it is this uneven
Burning just constantly lead to the formation of new hole, activation effect is more preferably.
It is worth noting that, activation temperature also slightly has difference when selecting different activators.Such as: in its of the application
In his embodiment, when activator is potassium hydroxide, activation temperature is 750 DEG C~850 DEG C；In other embodiment party of the application
In formula, when activator is phosphoric acid, zinc chloride or magnesium chloride, activation temperature is 500 DEG C~600 DEG C.
S5, cooling: the cooling rate by activated material in 8-11 DEG C/min is cooled to room temperature.By specific cooling rate into
Row cooling down reduces the time that activated material is contacted with air, so that the porous structure on the surface of activated material is in temperature-fall period
Middle sizing is not easy the influence again by oxygen, carbon dioxide or vapor in air, is conducive to the property for keeping activated material.
S6, water washing: it is 6-8 that activated material to pH value, which is directly washed with water,.
Directly be washed with water in the application, without use acid elution, the surface texture of maximum protection activity material, together
When during being washed with water, the activator not with animal waste aggregate reaction can be recycled.
It is worth noting that, the pH value that activated material acquisition is washed with water slightly has difference when selecting different activators.Example
Such as: in the other embodiments of the application, when activator is potassium hydroxide, being directly washed with water to pH value is 7-8；At this
In the other embodiments of application, when activator is phosphoric acid, zinc chloride or magnesium chloride, being directly washed with water to pH value is 6-7.
S7, drying: obtaining active bone black after 100-120 DEG C of dry 8-12h, passes through dry removal active bone carbon surface
Moisture.
After drying, the quality percentage that over dry material quality is accounted for by calculating the quality of active bone black, can be obtained
The yield of active bone black, the specific surface area of the active bone black obtained by the above method are 200-500m2/ g, methylene blue adsorption number
Value is 30-130mg/g.
Wherein, the specific area measuring of active bone black is using Tristar3000analyzer specific surface area analysis instrument
(Micromeritics, USA) measurement.The calculating of specific surface area is according to Brunaue-Emmett-Teller (BET) equation.It is sub-
The measuring method of methyl blue adsorptive value are as follows: the measurement of methylene blue adsorption value is according to national standard GB/T 12496.10-1999 " wood
Activated carbon test method: the measurement of methylene blue adsorption value ".
For the application using animal waste bone as raw material, phosphoric acid or potassium hydroxide or zinc chloride or magnesium chloride are activator preparation
Large specific surface area out, the high active bone black of absorption property；It is advantageously implemented the resource utilization of various animal waste bones, favorably
In resources such as saving timber, coal and coconut husks.Prepared various animal bone matrix activity bone black can be used for substituting conventional carbon
The partial use of product；Preparation process is not necessarily to inert gas shielding, simple process, easy to industrialized production.
Active bone black of the invention and preparation method thereof further progress is illustrated with reference to embodiments.
Embodiment 1
A kind of active aggregates (phosphoric acid activation discards pig bone charcoal adsorbent material) is present embodiments provided, preparation method is such as
Under:
The discarded pig bone raw material for weighing 20g is mixed with 50g phosphoric acid (concentration 85%) activator, impregnates 15h.It will impregnate
Full material is put into chamber type electric resistance furnace, is warming up to 550 DEG C of activation 60min with 20 DEG C/min, is taken out after cooled to room temperature,
Sufficiently washing 5 times is washed with water, through filtering, 110 DEG C of dry 10h are powder activated by what is prepared after taking out ground, sieving
It is spare that pig bone charcoal adsorbent material sample is packed into sample sack.
Embodiment 2-5
Embodiment 2-5 provides a kind of active aggregates (phosphoric acid activation discards pig bone charcoal adsorbent material), preparation method with
Embodiment 1 is essentially identical, and distinctive points are:
In embodiment 2,500 DEG C of activation 20min are warming up to 20 DEG C/min, are then heated up with the heating rate of 10 DEG C/min
To 600 DEG C, continue to activate 40min；
In embodiment 3, after activation, the cooling rate by activated material in 10 DEG C/min is cooled to room temperature.
In embodiment 4,500 DEG C of activation 20min are warming up to 20 DEG C/min, are then heated up with the heating rate of 10 DEG C/min
To 600 DEG C, continue to activate 40min；Then the cooling rate by activated material in 10 DEG C/min is cooled to room temperature.
In embodiment 5, raw material is discarded Os Bovis seu Bubali raw material.
The product that above-described embodiment 1-5 is obtained tests its yield, specific surface area and methylene blue adsorption value, and
And the activation parameter by changing above-described embodiment 1 obtains comparative example 1-5, while to comparative example 1-5 yield, specific surface area and
Methylene blue adsorption value is tested, and test result please refers to table 1.
1. phosphoric acid activation of table discards pig bone charcoal properties of product
As it can be seen from table 1 activator level, activation temperature and activation time have more important shadow to activation results
It rings, too high or too low for temperature, activator level is impossible to obtain ideal activation product when being lower than 2:1.Pass through setting simultaneously
Staged activation temperature, and control activation time and rate of temperature fall in activation, are conducive to the performance for promoting product.
Embodiment 6
A kind of active bone black (activation of potassium hydroxide discards pig bone charcoal) is present embodiments provided, preparation method includes:
The discarded pig bone raw material for weighing 20g is mixed with 30g pure cerium hydroxide potassium (aqueous solution for being made into concentration 50%) activator,
Impregnate 20h.Complete material will be impregnated to be put into chamber type electric resistance furnace, 800 DEG C of activation 60min are warming up to 15 DEG C/min, it is cooling
It is taken out after to room temperature, sufficiently washing 5 times is washed with water, through filtering, 110 DEG C of dry 10h will be prepared after taking out ground, sieving
Powder activated discarded pig bone charcoal adsorbent material sample to be packed into sample sack spare.
Embodiment 7-10
Embodiment 7-10 provides a kind of active aggregates (phosphoric acid activation discards pig bone charcoal adsorbent material), preparation method with
Embodiment 1 is essentially identical, and distinctive points are:
In embodiment 7,750 DEG C of activation 20min are warming up to 15 DEG C/min, are then heated up with the heating rate of 5 DEG C/min
To 800 DEG C, continue to activate 40min；
In embodiment 8, after activation, the cooling rate by activated material in 8 DEG C/min is cooled to room temperature.
In embodiment 9,750 DEG C of activation 20min are warming up to 15 DEG C/min, are then heated up with the heating rate of 5 DEG C/min
To 800 DEG C, continue to activate 40min；Then the cooling rate by activated material in 8 DEG C/min is cooled to room temperature.
In embodiment 10, raw material is discarded Os Bovis seu Bubali raw material.
The product that above-described embodiment 7-10 is obtained tests its yield, specific surface area and methylene blue adsorption value,
And the activation temperature by changing above-described embodiment 7 obtains comparative example 6-8, while to comparative example 6-8 yield, specific surface area
It is tested with methylene blue adsorption value, test result please refers to table 2.
2. activation of potassium hydroxide of table discards pig bone charcoal properties of product
Embodiment 11
Present embodiments provide a kind of active bone black (zinc chloride activation discards pig bone charcoal adsorbent material), preparation method packet
It includes:
The discarded pig bone raw material for weighing 20g is mixed with the pure zinc chloride of 60g (aqueous solution for being made into concentration 60%) activator, leaching
Stain is for 24 hours.Complete material will be impregnated to be put into chamber type electric resistance furnace, 500 DEG C of activation 90min are warming up to 20 DEG C/min, are cooled to
It is taken out after room temperature, sufficiently washing 5 times is washed with water, through filtering, 110 DEG C of dry 10h, after taking out ground, sieving, by what is prepared
It is spare that powder activated discarded pig bone charcoal adsorbent material sample is packed into sample sack.
Embodiment 12-15
Embodiment 12-15 provides a kind of active aggregates (zinc chloride activation discards pig bone charcoal adsorbent material), preparation side
Method is substantially the same manner as Example 1, and distinctive points are:
In embodiment 12,500 DEG C of activation 30min are warming up to 25 DEG C/min, then with the heating rate liter of 15 DEG C/min
Temperature continues to activate 60min to 600 DEG C；
In embodiment 13, after activation, the cooling rate by activated material in 11 DEG C/min is cooled to room temperature.
In embodiment 14,500 DEG C of activation 30min are warming up to 25 DEG C/min, then with the heating rate liter of 15 DEG C/min
Temperature continues to activate 60min to 600 DEG C；Then the cooling rate by activated material in 11 DEG C/min is cooled to room temperature.
In embodiment 15, raw material is discarded Os Bovis seu Bubali raw material.
The product that above-described embodiment 11-15 is obtained tests its yield, specific surface area and methylene blue adsorption value,
And by change above-described embodiment 11 activation parameter obtain comparative example 9-12, while to comparative example 9-12 yield, compare table
Area and methylene blue adsorption value are tested, and test result please refers to table 3.
3. zinc chloride activation of table discards pig bone charcoal properties of product
Embodiment 16
A kind of active bone black (magnesium chloride activates discarded pig bone charcoal) is present embodiments provided, preparation method includes:
The discarded pig bone raw material for weighing 20g is mixed with the pure magnesium chloride of 60g (aqueous solution for being made into concentration 60%) activator, leaching
Stain is for 24 hours.Complete material will be impregnated to be put into chamber type electric resistance furnace, 500 DEG C of activation 90min are warming up to 20 DEG C/min, are cooled to
It is taken out after room temperature, sufficiently washing 5 times is washed with water, through filtering, 110 DEG C of dry 10h, after taking out ground, sieving, by what is prepared
It is spare that powder activated discarded pig bone charcoal sample is packed into sample sack.
Embodiment 17-20
Embodiment 17-20 provides a kind of active aggregates (phosphoric acid activation discards pig bone charcoal adsorbent material), preparation method
Substantially the same manner as Example 1, distinctive points are:
In embodiment 17,500 DEG C of activation 30min are warming up to 20 DEG C/min, then with the heating rate liter of 10 DEG C/min
Temperature continues to activate 60min to 600 DEG C；
In embodiment 18, after activation, the cooling rate by activated material in 9 DEG C/min is cooled to room temperature.
In embodiment 19,500 DEG C of activation 30min are warming up to 20 DEG C/min, then with the heating rate liter of 10 DEG C/min
Temperature continues to activate 60min to 600 DEG C；Then the cooling rate by activated material in 9 DEG C/min is cooled to room temperature.
In embodiment 20, raw material is discarded Os Bovis seu Bubali raw material.
The product that above-described embodiment 16-20 is obtained tests its yield, specific surface area and methylene blue adsorption value,
And the activation parameter by changing above-described embodiment 16 obtains comparative example 13-16, while to comparative example 13-16 yield, ratio
Surface area and methylene blue adsorption value are tested, and test result please refers to table 4.
4. zinc chloride activation of table discards pig bone charcoal properties of product
Experimental example
One, the adsorption bleaching of active bone black and absorption heavy metal experiment
Above-described embodiment 1-20 and comparative example 1-16 are subjected to adsorption bleaching and absorption heavy metal experiment respectively.
(1) adsorption bleaching is detected with the following method:
Methyl orange is a kind of typical dyestuff.This experiment is using active pig bone charcoal adsorbent material prepared by embodiment 1-3
Waste water (containing methyl orange 80mg/L) containing methyl orange is handled.Under room temperature, neutrallty condition, it is living to accurately weigh 0.1g
Property bone black in 250mL conical flask, be added 100mL initial mass concentration be 100mg/L methyl orange solution.Vibrate 30min, quiet
It sets, be centrifuged, supernatant is taken to measure absorbance at maximum wavelength by spectrophotometer, calculate supernatant soln concentration.It repeats
Above-mentioned experiment 3 times, adsorbance (q) is calculated by following formula.
Q=(C0-Ct)V/W
In formula: C0: mass concentration when solution is initial, mg/L；
Ct: the mass concentration of t moment supernatant, mg/L；
W: the quality of adsorbent, g；
V: the volume of dye solution, L.
(2) experiment of absorption heavy metal is detected with the following method:
The amount of industrial wastewater containing heavy metal ion such as zinc, mercury, chromium, lead that countries in the world are discharged every year is huge, wherein inhaling
Attached method is one of effective processing method.With chromium ion Cr (VI) for experimental subjects, the potassium bichromate solution of concentration needed for preparing.
The solution that chromium ion concentration is 5mg/L in conical flask, with 1g activity ox bone charcoal adsorbent material, shakes in 250mL in room temperature constant temperature
It swings and adsorbs 12h in device.Sampling, measures the absorbance of sample, and calculate its adsorbance.
The active bone black adsorbent material decolorizing effect of table 5. and absorption Cr (VI) effect
We, which test, confirms the various activators such as phosphoric acid, potassium hydroxide, relatively low (being lower than 400 DEG C) in activation temperature；Add
It is relatively low (mass ratio of activator and raw material is lower than 1:1) to enter amount, it is right in the case where activation time shorter (being lower than 30min)
The useless bone of various animals is activated, and cannot get the relatively good product of absorption property, (specific surface area is below 75m2/ g, methylene
Indigo plant absorption is below 20mg/g), bone black can only be known as rather than active bone black.
For the application using animal waste bone as raw material, phosphoric acid or potassium hydroxide or zinc chloride or magnesium chloride are activator preparation
Large specific surface area out, the high active bone black of absorption property；It is advantageously implemented the resource utilization of various animal waste bones, favorably
In resources such as saving timber, coal and coconut husks.Prepared various animal bone matrix activity bone black can be used for substituting conventional carbon
The partial use of product；Preparation process is not necessarily to inert gas shielding, simple process, easy to industrialized production.
These are only the preferred embodiment of the present invention, is not intended to restrict the invention, for those skilled in the art
For member, the invention may be variously modified and varied.All within the spirits and principles of the present invention, it is made it is any modification,
Equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of activity bone black, which is characterized in that it includes by smashed animal waste bone and activator
It mixes and impregnates 12-20h；60~90min is then activated at a temperature of 500 DEG C~850 DEG C and obtains activated material, is directly washed with water
The activated material to pH value is 6-8, and active bone black is obtained after dry.
2. the preparation method of activity bone black according to claim 1, which is characterized in that the activator and the animal are useless
The mass ratio for abandoning bone is 1.5-3:1.
3. the preparation method of activity bone black according to claim 2, which is characterized in that the activator includes hydroxide
One of potassium, phosphoric acid, zinc chloride and magnesium chloride are a variety of.
4. the preparation method of activity bone black according to claim 3, which is characterized in that at a temperature of 500 DEG C~850 DEG C
It includes: to be warming up to the first activation temperature with the heating rate of 15-25 DEG C/min that 60~90min of activation, which obtains activated material, activates 20-
30min is then warming up to the second activation temperature with the heating rate of 5-10 DEG C/min, continues to activate 40-60min；
Wherein, first activation temperature is 500 DEG C~750 DEG C, and second activation temperature is 600 DEG C~850 DEG C；Described
One activation temperature is lower than second activation temperature.
5. the preparation method of activity bone black according to claim 3 or 4, which is characterized in that when the activator is hydrogen-oxygen
When changing potassium, the mass ratio of the potassium hydroxide and the animal waste bone is 1.5-2.5:1, and activation temperature is 750 DEG C~850
℃；Directly being washed with water to pH value is 7-8,
Preferably, the concentration of the potassium hydroxide is greater than 50%.
6. it is according to claim 3 or 4 activity bone black preparation method, which is characterized in that when the activator be phosphoric acid,
When zinc chloride or magnesium chloride, the phosphoric acid, the zinc chloride or the magnesium chloride and the mass ratio of the animal waste bone are
2-3:1, activation temperature are 500 DEG C~600 DEG C；Directly being washed with water to pH value is 6-7,
Preferably, the concentration of the phosphoric acid is 50-85%；
Preferably, the chlorination zinc concentration is greater than 60%；
Preferably, the concentration of the magnesium chloride is greater than 60%.
7. the preparation method of activity bone black according to claim 1, which is characterized in that after obtaining the activated material,
It further include that cooling rate by activated material in 8-11 DEG C/min is cooled to room temperature before the activated material is washed with water.
8. the preparation method of activity bone black according to claim 1, which is characterized in that the activated material is directly washed with water
After being 6-8 to pH value, the active bone black is obtained after 100-120 DEG C of dry 8-12h.
9. the preparation method of activity bone black according to claim 1, which is characterized in that by the animal waste bone powder
Before broken, first drying the animal waste bone to moisture is 5-15%.
10. a kind of activity bone black, which is characterized in that it passes through the preparation such as the described in any item active bone black of claim 1-9
Method is prepared；The specific surface area of the activity bone black is 200-500m2/ g, methylene blue adsorption value 30-130mg/g.
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| CN201811329401.6A Active CN109110757B (en) | 2018-11-09 | 2018-11-09 | Activated bone charcoal and preparation method thereof |
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| CN109850893A (en) * | 2019-01-27 | 2019-06-07 | 合肥学院 | A kind of preparation method and application of ox bone active carbon |
| CN110918052A (en) * | 2019-10-28 | 2020-03-27 | 安徽省通源环境节能股份有限公司 | Preparation process of magnetic livestock bone carbonized particle adsorbent |
| CN113264524A (en) * | 2021-05-28 | 2021-08-17 | 河南农业大学 | Pig bone charcoal and preparation method and application thereof |
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| CN110918052A (en) * | 2019-10-28 | 2020-03-27 | 安徽省通源环境节能股份有限公司 | Preparation process of magnetic livestock bone carbonized particle adsorbent |
| CN113264524A (en) * | 2021-05-28 | 2021-08-17 | 河南农业大学 | Pig bone charcoal and preparation method and application thereof |
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| CN109110757B (en) | 2020-05-22 |
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