CN106185925B - The preparation method of cocoanut active charcoal containing rare earth - Google Patents

The preparation method of cocoanut active charcoal containing rare earth Download PDF

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CN106185925B
CN106185925B CN201610558650.7A CN201610558650A CN106185925B CN 106185925 B CN106185925 B CN 106185925B CN 201610558650 A CN201610558650 A CN 201610558650A CN 106185925 B CN106185925 B CN 106185925B
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宋玉琴
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J20/28057—Surface area, e.g. B.E.T specific surface area
    • B01J20/28066—Surface area, e.g. B.E.T specific surface area being more than 1000 m2/g
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J20/28057—Surface area, e.g. B.E.T specific surface area
    • B01J20/28064—Surface area, e.g. B.E.T specific surface area being in the range 500-1000 m2/g
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/12—Surface area
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/02—Non-contaminated water, e.g. for industrial water supply
    • C02F2103/04—Non-contaminated water, e.g. for industrial water supply for obtaining ultra-pure water

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  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Inorganic Chemistry (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

The invention discloses a kind of preparation methods of the cocoanut active charcoal containing rare earth.The method of the present invention includes following steps：(1) lanthanum earth compounds, cerium compound, alkaline earth metal compound are uniformly mixed with coconut shell powder, obtain mixture；(2) mixture is carbonized at 380~580 DEG C, to obtain the first carbonized product；(3) the first carbonized product is carbonized at 620~780 DEG C, is then cooled to room temperature, to obtain the second carbonized product；(4) the second carbonized product is ground to carbon dust, it is mixed with alkali metal compound, then activated at 350~800 DEG C, to obtain activation products；(5) activation products are obtained into active product char by processing.The method of the present invention directly mixes at least two rare earth compounds with coconut shell powder to manufacture active rare-earth charcoal, significantly improves the stability of active rare-earth Carbon composites.

Description

The preparation method of cocoanut active charcoal containing rare earth
Technical field
The present invention relates to a kind of preparation method of the cocoanut active charcoal containing rare earth, it is particularly useful for filtering containing for tap water The preparation method of the cocoanut active charcoal of rare earth further relates to the cocoanut active charcoal containing rare earth.
Background technology
With the improvement of people ' s living standards and the appearance of water environment pollution, people propose higher want for water quality It asks.Activated carbon has been widely used for as a kind of filtering material in water treatment technology.Activated carbon is a kind of porous material, tool There is huge specific surface area, thus the impurity such as the suspended matter in water can be adsorbed；But for the suction of some organic matters in water Attached ability is then weaker.
Rare earth element is introduced in activated carbon, can improve the ability of its Organic substance in water of degrading.Currently, having occurred The activated carbon of supported rare earth for water treatment technology.For example, CN105214641A discloses a kind of preparation side of RE composite Method：The compound for choosing Ce, Zr, La, Pr, Nd, Yb etc. is presoma, and it is compound to prepare ternary, quaternary and polynary rare earth respectively Object；Powdery porous activated carbon is placed in corresponding precursor solution, is then stirred, precipitating reagent is added in absorption again after a certain period of time Mixture is precipitated, proper pH value is adjusted, after precipitation is complete, ageing is calcined at high temperature after filter washing, drying.
For another example, CN105645558A discloses a kind of catalytic wet oxidation processing method of industrial circulating water, wherein using Catalyst include carrier and active metal component, wherein using transition metal and rare earth metal as active metal component, carrier is Using the activated carbon of the mesh of 150 mesh~300 as core, using amorphous silica-alumina as shell.The catalyst is prepared as follows：Amorphous During sial plastic, the activated carbon for introducing 150~300 mesh is beaten the slurries to be formed, and the material after obtained plastic carries out old Change, be filtered, washed, dry, catalyst carrier is made, on a catalyst support impregnating metal component, then dries, in indifferent gas The lower roasting of body protection, obtains catalytic wet oxidation catalyst.
For another example, CN104496011B discloses a kind of preparation method of rare earth-activated carbon bio-catalytical oxidation sludge：It takes dilute The waste residue and concentrations by weight be by the waste residue of alloy containing mixed rare earth oxide 5wt%~10wt% in the production of native ore 10%~60% hydrochloric acid is mixed according to weight ratio 1: 1~4, is sufficiently stirred activation 6~12 hours, is staticly settled, and is separated by solid-liquid separation, The solid is mixed rare-earth oxide；Activated sludge is taken, active carbon powder and mixed rare-earth oxide, stirring is added 2.5~3.5h stops 1.5~2.5h of stirring, and when stopping stirring, active carbon powder and mixed rare-earth oxide swim in the water surface, The step of repeating to stir and stop stirring, after 2~7 days, when stopping stirring, active carbon powder and mixed rare-earth oxide are not It floats again, removes water layer above, obtain rare earth-activated carbon bio-catalytical oxidation sludge.
The above method is all that will contain the compound of rare earth element to mix with active carbon finished products or by the change containing rare earth element Object is closed to be impregnated in active carbon finished products, thus the adhesive force of rare earth element and activated carbon is not strong, and rare earth element is caused to be easy from work It is oozed out in property charcoal, thus its stability is not high.
Invention content
In order to overcome drawbacks described above, present inventor to have made intensive studies, find at least two rare earth chemical combination Object is directly mixed with coconut shell powder can significantly improve the stability of rare earth-activity Carbon composites to manufacture rare earth-activated carbon, from And complete the present invention.
It is simple for process the purpose of the present invention is to provide a kind of preparation method of rare earth-activated carbon, stabilization can be obtained Higher rare earth-activity the Carbon composites of property.It is another object of the present invention to provide rare earth-activated carbons prepared by the above method Compound, rare earth element therein are not easy to ooze out from activated carbon.In addition, rare earth-activity Carbon composites mistake through the present invention Drinking water after filter has better mouthfeel.Above-mentioned purpose may be implemented in the following technical solution of the present invention.
The present invention provides a kind of preparation method of the cocoanut active charcoal containing rare earth, includes the following steps：
(1) rare earth compound, alkaline earth metal compound are uniformly mixed with coconut shell powder, obtain mixture, described is dilute Earth compounds include cerium compound and lanthanum compound；
(2) mixture is carbonized at 380~580 DEG C, to obtain the first carbonized product；
(3) the first carbonized product is carbonized at 620~780 DEG C, is then cooled to room temperature, to obtain the second carbonization Product；
(4) the second carbonized product is ground to carbon dust, it is mixed with alkali metal compound, then in 350~800 DEG C of work Change, to obtain activation products；
(5) activation products are obtained into activated carbon by processing.
Preparation in accordance with the present invention, it is preferable that in step (1), rare earth compound, alkaline earth metal compound and coconut palm The weight ratio of shell powder is 0.2~8：2~10：100；Wherein, the weight ratio of the cerium compound and the lanthanum compound is 0.5 ~5：1.
Preparation in accordance with the present invention, it is preferable that in step (1), the cerium compound is selected from ammonium ceric nitrate, nitre Sour cerium, cerous sulfate, cerous sulfate, cerous carbonate, cerium oxide, cerous acetate or cerium oxalate it is one or more；The lanthanum compound Selected from the one or more of lanthanum chloride, lanthanum nitrate, lanthanum sulfate, lanthanum carbonate or lanthana.
Preparation in accordance with the present invention, it is preferable that in step (1), the alkaline earth metal compound is selected from alkaline earth Oxide, hydroxide, chloride, bromide, iodide, fluoride, phosphate, carbonate, sulfide, the sulfate of metal Or nitrate.
Preparation in accordance with the present invention, it is preferable that in step (1), the average grain diameter of the coconut shell powder is 5~ 500 mesh.
Preparation in accordance with the present invention, it is preferable that in step (4), the alkali metal compound is selected from hydroxide Sodium or potassium hydroxide；The dosage of the alkali metal compound is 2~5 times of carbon dust weight.
Preparation in accordance with the present invention, it is preferable that in step (2), which is heated up with 6~20 DEG C/h To 380~580 DEG C, the first carbonized product is obtained after keeping the temperature 5~20 hours at such a temperature；In step (3), by described One carbonized product is warming up to 620~780 DEG C with 30~80 DEG C/h, keeps the temperature 0.5~3 hour, then cooled to room temperature, Obtain the second carbonized product.
Preparation in accordance with the present invention, it is preferable that in step (4), second carbonized product is ground to put down The carbon dust that equal grain size is 20~500 microns, which is uniformly mixed with alkali metal compound, and is fitted into container；By the appearance Device heats in activation furnace, and 350~550 DEG C are warming up to 3~10 DEG C/min of the rate of heat addition, at such a temperature keep 30~ It 100 minutes, is heated 10~60 minutes at 750~850 DEG C, is then cooled to room temperature, is lived under the protection of protective gas Change product.
Preparation in accordance with the present invention, it is preferable that in step (5), the processing is：The activation products are used The hydrochloric acid of 0.6~3mol/L neutralizes, and then with the salt acid elution of 0.06~0.3mol/L, is washed with water and washs；The washing is produced Object is dried with stream of hot air, and activated carbon is obtained after sieving.
The present invention also provides the activated carbon that above-mentioned preparation method obtains, the average grain diameter of the activated carbon is 20~500 micro- Rice, specific surface area are 500~2800m2/ g, and the lanthanum of the cerium containing 0.1~0.8wt% and 0.1~0.9wt%.
The present invention directly mixes at least two rare earth compounds with the raw material of manufacture activated carbon to manufacture rare earth-activated carbon Rare earth element is just placed in the forming process of activated carbon in the agent structure of activated carbon by compound in this way.With traditional system Standby technique is compared with using the preparation process of Rare Earth Elements Determination, and method of the invention can make rare earth element and activated carbon In conjunction with more securely, thus the stability of rare earth-activity Carbon composites is significantly improved.In addition, by the coconut activated of the present invention The mouthfeel of the drinking water of charcoal filtering is more preferable.
Specific implementation mode
With reference to specific embodiment, the present invention is further illustrated, but protection scope of the present invention is not limited to This.
<The preparation method of activated carbon>
The preparation method of the cocoanut active charcoal containing rare earth of the present invention includes multiple steps：(1) mixing step；(2) first Carburising step；(3) second carburising steps；(4) activation step；(5) post-processing step.
The step (1) of the present invention is mixing step：Rare earth compound, alkaline earth metal compound are mixed with coconut shell powder It is even, obtain mixture.The rare earth compound of the present invention includes cerium compound and lanthanum compound.Preferably, the rare earth Object is closed to be made of cerium compound and lanthanum compound.The average grain diameter of the coconut shell powder of the present invention can be 5~500 mesh；Preferably 50~350 mesh；More preferably 100~300 mesh.Mixed mode is not particularly limited, as long as they are uniformly mixed.Example Such as, rare earth compound powder, alkaline earth metal compound powder are added in coconut shell powder, then stirring to obtain mixture.Stirring Mode is not particularly limited, and can use Henschel mixer, V-Mixer etc..A specific implementation according to the present invention Mode mixes rare earth compound, alkaline earth metal compound with coconut shell powder under the inert gas shieldings such as nitrogen, argon gas It is even, obtain mixture.
In above-mentioned steps, the weight ratio of rare earth compound, alkaline earth metal compound and coconut shell powder can be 0.2~8： 2~10：100；That is, in terms of 100 parts by weight coconut shell powders, rare earth compound is 0.2~8 parts by weight, alkaline-earth metal Conjunction object is 2~10 parts by weight.Preferably, the weight ratio of rare earth compound, alkaline earth metal compound and coconut shell powder can be 0.3~7：2~10：100；More preferably, the weight ratio of rare earth compound, alkaline earth metal compound and coconut shell powder can be 0.35~6：2~10：100.When the content of alkaline earth metal compound is too low, it is not enough to play the catalytic action of activation step, When the content of alkaline earth metal compound is too high, it is unfavorable for rare earth element being stabilized in activated carbon.
In above-mentioned steps, the weight ratio of the cerium compound and the lanthanum compound is 0.5~5：1, preferably 0.6~ 3：1, more preferably 0.7~2：1.When rare earth compound selects above range, the combination of rare earth element and activated carbon is more secured, Thus it is not easy to ooze out.
In above-mentioned steps, the cerium compound can be ammonium ceric nitrate, cerous nitrate, cerous sulfate, cerous sulfate, carbonic acid Cerium, cerium oxide, cerous acetate or cerium oxalate；Preferably cerous sulfate, cerous carbonate or cerium oxide.The lanthanum compound of the present invention can be selected from Lanthanum chloride, lanthanum nitrate, lanthanum sulfate, lanthanum carbonate or lanthana it is one or more；Preferably lanthanum chloride, lanthanum carbonate or lanthana It is one or more.
In above-mentioned steps, the alkaline earth metal compound can be selected from oxide, hydroxide, the chlorine of alkaline-earth metal Compound, bromide, iodide, fluoride, phosphate, carbonate, sulfide, sulfate or nitrate.Preferably, of the invention Alkaline earth metal compound can be selected from oxide, hydroxide, carbonate or the nitrate of alkaline-earth metal；It is highly preferred that it is Carbonate.The alkali earth metal of the present invention is the 2nd race's element of periodic table, such as Be, Mg, Ca, Sr, Ba and Ra；Preferably Mg And Ca.The specific example of the alkaline earth metal compound of the present invention includes but not limited to calcium carbonate, calcium oxide etc..These alkaline-earth metal Compound can be used alone or two or more combined uses.
The step (2) of the present invention is the first carburising step：The mixture is carbonized at 380~580 DEG C, to obtain First carbonized product.A specific implementation mode according to the present invention, by the mixture with 6~20 DEG C/h of the first heating Rate is warming up to 380~580 DEG C of the first carburizing temperature, and keep the temperature 5~20 hours at such a temperature obtains after (the first soaking time) First carbonized product.The mixture can be begun to warm up from room temperature.The first heating rate is preferably 8~15 DEG C/h, more preferably It is 10~12 DEG C/h.First carburizing temperature is preferably 450~560 DEG C, preferably 500~550 DEG C.First soaking time is excellent It is selected as 8~15 hours, preferably 10~12 hours.
The step (3) of the present invention is the second carburising step：First carbonized product is carbonized at 620~780 DEG C, so Postcooling is to room temperature, to obtain the second carbonized product.A specific implementation mode according to the present invention, by first carbonization Product is warming up to 620~780 DEG C of the second carburizing temperature with 30~80 DEG C/h of the second heating rate, keeps the temperature 0.5~3 hour (the second soaking time), then cooled to room temperature, obtains the second carbonized product.First carbonized product can be from the first carbonization Temperature starts to warm up.Second heating rate is preferably 35~70 DEG C/h, more preferably 50~60 DEG C/h.Second carbonization temperature Preferably 680~760 DEG C, preferably 700~750 DEG C of degree.Second soaking time is preferably 0.8~2 hour, preferably 1~1.5 Hour.
In step (2)~(3) of the present invention, coconut shell powder is carbonized, so as to cause pyrolytic reaction.The carbonization of the present invention Step determines the structure of activated carbon, and ensures rare earth element being stabilized in activated carbon.First carburizing temperature 380~ Between 580 DEG C, the second carburizing temperature is at 620~780 DEG C, it is ensured that the carbonization of coconut shell powder is abundant.By the first heating rate, Second heating rate is controlled in the scope of the present invention, can further increase stability of the rare earth element in activated carbon so that Rare earth element is combined more closely with activated carbon.By the activated carbon natural cooling (Slow cooling) after carbonization, activity can be improved The intensity of charcoal, and rare earth element is tightly combined with activated carbon.
The step (4) of the present invention is activation step：Second carbonized product is ground to carbon dust, by itself and alkali metal compound Mixing, then activates under 350~800 DEG C of activation temperature, to obtain activation products.A specific implementation according to the present invention Second carbonized product is ground to the carbon dust that average grain diameter is 20~500 microns, by the carbon dust and alkali metal by mode It closes object to be uniformly mixed, and is fitted into container；The container is heated in activation furnace, is heated up with 3~10 DEG C/min of the rate of heat addition To 350~550 DEG C, is kept for 30~100 minutes at such a temperature, heat 10~60 minutes at 750~850 DEG C, then protecting It protects under the protection of gas and is cooled to room temperature, obtain activation products.The average grain diameter of carbon dust after grinding is preferably 30~350 micro- Rice, more preferably 50~300 microns.The lapping mode of the present invention is not particularly limited, and jet mill, vibromill can be used for example Deng conventional milling apparatus.Carbon dust is ground to above-mentioned particle size range, can extend and live to avoid the stripping of rare earth element and activated carbon Service life of the property charcoal as adsorbent.
In the step (4) of the present invention, the alkali metal compound can be selected from sodium hydroxide or potassium hydroxide；It is preferred that For potassium hydroxide.The dosage of the alkali metal compound can be 2~5 times, preferably 2~3 times of carbon dust weight.Aforementioned carbon Change the carbon dust that step obtains to activate in the presence of alkali metal compound, for example, carbon dust and alkali metal compound are formed into mixture, Then it fills this blend into nickel container and is heated.It heats the activation furnace used to be not particularly limited, this can be used Those of known to field.
In the step (4) of the present invention, activation temperature can be 350~800 DEG C, preferably 400~750 DEG C.The present invention's Activation process can carry out in the inert atmospheres such as nitrogen, argon gas.Furthermore it is possible to introduce carbon dioxide etc..To fill carbon dust with The container of alkali metal compound is warming up in activation furnace with 3~10 DEG C/min, preferably 5~8 DEG C/min of the rate of heat addition It 350~550 DEG C, preferably 400~500 DEG C, is kept for 30~100 minutes, preferably 50~80 minutes at such a temperature, 750~850 DEG C, heat 10~60 minutes, preferably 20~30 minutes at preferably 750~800 DEG C, then in protective gas such as nitrogen, argon gas It is cooled to room temperature under protection, obtains activation products.
In activation process, alkali metal compound is reacted with the substance in carbon dust, and the gas of formation can make carbon Powder foams, and the alkali metal of formation then enters in carbon-coating, to form many gaps.
The step (5) of the present invention is post-processing step：Activation products are obtained into active product char by processing.According to this hair A bright specific implementation mode, the processing are：The activation products hydrochloric acid of 0.6~3mol/L is neutralized, then With the salt acid elution of 0.06~0.3mol/L, it is washed with water and washs；The washed product is dried with stream of hot air, and is sieved and obtains Activated carbon.Preferably, salt acid elution and water washing carry out under boiling conditions.
In the step (5) of the present invention, is neutralized and washed using hydrochloric acid, detersive efficiency, and hydrochloric acid can be improved It easily removes.The concentration of neutralization hydrochloric acid can be 0.6~3mol/L, preferably 0.8~2.5mol/L, more preferably 1.0~ 2mol/L.The concentration of washing hydrochloric acid can be 0.06~0.3mol/L, preferably 0.08~0.25mol/L, more preferably 0.1 ~0.2mol/L.The hydrochloric acid of suitable concentration can prevent rare earth element from being oozed out from activated carbon, in addition can also wash away combination Unstable rare earth element.By activation products and mixed in hydrochloric acid so that acid-base neutralization, and then remove alkali metal compound.It will neutralize Activation products afterwards and mixed in hydrochloric acid, washed under 55~105 DEG C, preferably 80~100 DEG C of heating condition 1~24 hour, it is excellent It is selected as 2~15 hours, more preferably 2~5 hours；Washing times are 2~5 times.Washing the water used can be distilled water or go Ionized water etc. is preferably washed under boiling conditions.
In the step (5) of the present invention, the washed product stream of hot air is dried to obtain desciccate, dry temperature Degree can be 110~180 DEG C, preferably 120~150 DEG C.After desciccate is sieved, activated carbon is obtained.Sieve used Mesh number is 32~800 mesh, preferably 45~460 mesh, more preferably 50~350 mesh.
<Cocoanut active charcoal>
The average grain diameter of the cocoanut active charcoal of the present invention is 20~500 microns, preferably 30~350 microns, is preferably 50 ~300 microns.Its specific surface area is 500~2800m2/ g, preferably 1000~2500m2/g.It can be in the activated carbon of the present invention The cerium of cerium containing 0.1~0.8wt%, the preferably cerium of 0.2~0.75wt%, more preferably 0.5~0.7wt%.The present invention Activated carbon in can the lanthanum containing 0.1~0.9wt%, preferably 0.2~0.8wt% lanthanum, more preferably 0.3~ The lanthanum of 0.7wt%.Rare earth element is introduced into activated carbon by the present invention, and in above-mentioned content range, rare earth element more stable can be deposited It is in activated carbon, and good catalytic action can be played.
The activated carbon of the present invention can be used as adsorbent, preferably as the adsorbent of water process, more preferably be drunk The adsorbent of water process.The drinking water mouthfeel obtained in this way is more preferable.
<Performance test methods>
Rare earth element content is measured using the NexION 300X type sense couple plasma mass spectrometers of PE companies of the U.S..Its In, the rare earth element assay in water refers to following document：" ICP-MS methods measure 17 kinds of rare earth elements in source water simultaneously ", Square swallow etc., Shandong chemical industry, the 1st phase of volume 42, the 43-44 pages, 2013 years.
It is (logical using the high-speed automated specific surface area of NOVA-1000e types and lacunarity analysis instrument of Kang Ta instrument companies of the U.S. Cross BET method) measure BET specific surface area.
Average grain diameter is measured using U.S.'s Beckman Kurt LS13-320 series laser Particle Size Analyzers.
Embodiment 1
By 4 grams of cerium chloride (CeCl3), 3.5 grams of lanthanum chloride (LaCl3), 30 grams of calcium carbonate 1000 grams of coconut shell powders (200 are added Mesh) be uniformly mixed obtain mixture.The mixture is warming up to 530 DEG C with 10 DEG C/h, heat preservation obtains the first carbon after 10 hours Change product.First carbonized product is warming up to 720 DEG C with 60 DEG C/h from 530 DEG C, 1 hour is kept the temperature, then naturally cools to room Temperature obtains the second carbonized product.Second carbonized product is ground, is 75 microns to obtain average grain diameter by 200 mesh screens Carbon dust, by itself and potassium hydroxide (mass ratio 1：3) it is uniformly mixed, and is fitted into nickel matter container；The container is continuously being activated Stove heat is warming up to 400 DEG C with 5 DEG C/min of the rate of heat addition, is kept for 60 minutes at such a temperature, then heat 20 at 720 DEG C Minute, it is then cooled to room temperature under nitrogen protection, obtains activation products.The activation products hydrochloric acid of 1mol/L is neutralized, so It is washed three times with the hydrochloric acid of 0.1mol/L (boiling) afterwards, then is washed with distilled water (boiling) and obtain washed product three times；It will washing Product is dried at 120 DEG C with stream of hot air, and by 200 mesh screens, obtains active product char A1.After testing, the activated carbon The average grain diameter of product is 75 microns, specific surface area 2020m2/ g, and the lanthanum of the cerium containing 0.6wt% and 0.5wt%.
Active product char A1 is placed in as adsorbent in water-purifying filter, processing is filtered to tap water, is run After 2000 hours, cerium and lanthanum element is not detected in water after filtration.It randomly selects 50 moral standings and tastes filtered water and originally Water, it is believed that the ratio that the former mouthfeel is better than the latter is 95%.
Embodiment 2
Other than replacing 4 grams of cerium chlorides, 1.5 grams of lanthanas 3.5 grams of lanthanum chlorides of replacement using 3 grams of cerium oxide, other Part and parameter are same as Example 1, obtain active product char A2.After testing, the average grain diameter of the activity product char be 75 microns, Specific surface area is 2080m2/ g, and the lanthanum of the cerium containing 0.65wt% and 0.3wt%.
Active product char A2 is placed in as adsorbent in water-purifying filter, processing is filtered to tap water, is run After 2000 hours, cerium and lanthanum element is not detected in water after filtration.It randomly selects 50 moral standings and tastes filtered water and originally Water, it is believed that the ratio that the former mouthfeel is better than the latter is 98%.
Present invention is not limited to the embodiments described above, without departing from the essence of the present invention, this field skill Any deformation, improvement, the replacement that art personnel are contemplated that each fall within the scope of the present invention.

Claims (2)

1. a kind of preparation method of the cocoanut active charcoal containing rare earth, which is characterized in that include the following steps：
By 4 grams of cerium chloride CeCl3, 3.5 grams of lanthanum chloride LaCl3The coconut shell powder mixing of 1000 gram of 200 mesh is added with 30 grams of calcium carbonate Uniformly obtain mixture；The mixture is warming up to 530 DEG C with 10 DEG C/h, heat preservation obtains the first carbonized product after 10 hours； First carbonized product is warming up to 720 DEG C with 60 DEG C/h from 530 DEG C, keeps the temperature 1 hour, then cooled to room temperature, obtains Second carbonized product；Second carbonized product is ground, it, will by 200 mesh screens to obtain the carbon dust that average grain diameter is 75 microns Gained carbon dust is 1 according to mass ratio with potassium hydroxide:3 are uniformly mixed, and are fitted into nickel matter container；The container is continuously being activated Stove heat is warming up to 400 DEG C with 5 DEG C/min of the rate of heat addition, is kept for 60 minutes at such a temperature, then heat 20 at 720 DEG C Minute, it is then cooled to room temperature under nitrogen protection, obtains activation products；The activation products hydrochloric acid of 1mol/L is neutralized, so Washed product three times, then with the distillation water washing boiled is obtained three times with the salt acid elution of 0.1mol/L boiled afterwards；It will washing Product is dried at 120 DEG C with stream of hot air, and by 200 mesh screens, obtains active product char；Gained activity product char is put down Equal grain size is 75 microns, specific surface area 2020m2/ g, and the lanthanum of the cerium containing 0.6wt% and 0.5wt%.
2. a kind of preparation method of the cocoanut active charcoal containing rare earth, which is characterized in that include the following steps：
The coconut shell powder of 3 grams of cerium oxide, 1.5 grams of lanthanas and 30 grams of calcium carbonate 1000 gram of 200 mesh of addition is uniformly mixed and is obtained Mixture；The mixture is warming up to 530 DEG C with 10 DEG C/h, heat preservation obtains the first carbonized product after 10 hours；By the first carbon Change product and be warming up to 720 DEG C from 530 DEG C with 60 DEG C/h, keeps the temperature 1 hour, then cooled to room temperature, obtains the second carbonization Product；Second carbonized product is ground, by 200 mesh screens to obtain the carbon dust that average grain diameter is 75 microns, by gained carbon dust With potassium hydroxide according to mass ratio be 1:3 are uniformly mixed, and are fitted into nickel matter container；The container is heated in continuous activating oven, 400 DEG C are warming up to 5 DEG C/min of the rate of heat addition, is kept for 60 minutes at such a temperature, then heat 20 minutes at 720 DEG C, so It is cooled to room temperature under nitrogen protection afterwards, obtains activation products；The activation products hydrochloric acid of 1mol/L is neutralized, is then used The salt acid elution of 0.1mol/L boiled three times, then with the distillation water washing boiled obtains washed product three times；By washed product It is dried with stream of hot air at 120 DEG C, and by 200 mesh screens, obtains active product char；The average grain of gained activity product char Diameter is 75 microns, specific surface area 2080m2/ g, and the lanthanum of the cerium containing 0.65wt% and 0.3wt%.
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CN105268425A (en) * 2014-07-17 2016-01-27 中国科学院大连化学物理研究所 Modified active carbon catalyst, and preparation and application thereof
CN105664928A (en) * 2016-03-21 2016-06-15 张晓菁 Preparation method of platinum-loading citrus grandis peel activated carbon catalyst for room-temperature degradation of formaldehyde in air

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CN105268425A (en) * 2014-07-17 2016-01-27 中国科学院大连化学物理研究所 Modified active carbon catalyst, and preparation and application thereof
CN105664928A (en) * 2016-03-21 2016-06-15 张晓菁 Preparation method of platinum-loading citrus grandis peel activated carbon catalyst for room-temperature degradation of formaldehyde in air

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