CN109225137A - A kind of preparation method of the cobalt improved apricot shell active carbon of chlorination - Google Patents
A kind of preparation method of the cobalt improved apricot shell active carbon of chlorination Download PDFInfo
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- CN109225137A CN109225137A CN201811289251.0A CN201811289251A CN109225137A CN 109225137 A CN109225137 A CN 109225137A CN 201811289251 A CN201811289251 A CN 201811289251A CN 109225137 A CN109225137 A CN 109225137A
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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
- B01J20/02—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
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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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0225—Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
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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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0274—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04 characterised by the type of anion
- B01J20/0288—Halides of compounds other than those provided for in B01J20/046
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G25/00—Refining of hydrocarbon oils in the absence of hydrogen, with solid sorbents
- C10G25/003—Specific sorbent material, not covered by C10G25/02 or C10G25/03
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/20—Characteristics of the feedstock or the products
- C10G2300/201—Impurities
- C10G2300/202—Heteroatoms content, i.e. S, N, O, P
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- Inorganic Chemistry (AREA)
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- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a kind of preparation methods of the cobalt improved apricot shell active carbon of chlorination, this method be different from it is traditional by acid or alkali to activated carbon modified, using cobalt chloride to activated carbon modified, whole preparation process mild condition, it is at low cost, easy to implement, have a wide range of application, and substantially increase the utilization rate and adsorption capacity of active carbon；Discovery is verified by being adsorbed with cobalt ions inside the modified active carbon of this method, it is 49.3% that the active carbon for being adsorbed with cobalt ions, which is directed to the desulfurization degree of the mould oil containing benzothiophene, higher than the existing desulfurization degree by sour or alkali modification active carbon；The preparation method expands the scope of application of active carbon, reduces use cost, plays significant effect to desulfurization.
Description
[technical field]
The invention belongs to technical field of desulfurization, and in particular to a kind of preparation method of the cobalt improved apricot shell active carbon of chlorination.
[background technique]
With the rapid development of world economy, referred to as the petroleum of industry blood occupied in entire human society it is extremely heavy
The status wanted constantly pushes the development in the world.However petroleum from exploration, exploitation, storage and transportation, refine, be sold to the process used
In some harmful elements do not removed really so that bringing serious danger to natural environment and human health
Evil.What desulfurization was more difficult in petroleum mainly has the thiophene-baseds such as dibenzothiophenes, alkyl benzothiophenes and methyldibenzothiophene
Compound.
Non-hydrodesulfurization can achieve the purpose of removing benzothiophene kind sulfide；Wherein adsorb desulfurization technology right and wrong
An important branch in hydrodesulfurization technology is logical using the porous masses such as molecular sieve or the metal being supported on inorganic carrier
Cross the technical process of physically or chemically suction-operated removal sulphur compound.
Active carbon has unique pore structure and surface chemistry, is a kind of high-efficiency adsorbent, has to all kinds of chemical substances
There is a preferable adsorption effect, but since active carbon is non-renewable resources, and less varieties, with low content of technology, so constraining
The further development and application of China's activated carbon industry.
Application of the activated carbon adsorption desulfurization in desulfurization still has significant limitation, but can change to active carbon
Property so desulfurization, certain variation can occur in structure for surface treated active carbon, to can change its absorption property.
Acid, alkali are common modifying agent in the prior art, but the active carbon after peracid, alkali modification is not to be readily applicable to desulfurization.
[summary of the invention]
It is an object of the invention to overcome the above-mentioned prior art, a kind of cobalt improved apricot shell active carbon of chlorination is provided
Preparation method, this method are modified active carbon using cobalt chloride, improve active carbon for the oil for including benzothiophene
The removal efficiency of middle sulfur content.
In order to achieve the above objectives, the present invention is achieved by the following scheme:
A kind of preparation method of the cobalt improved apricot shell active carbon of chlorination, includes the following steps, by pretreated apricot shell active carbon
It is mixed with cobalt chloride solution according to solid-liquid ratio 1g:20mL, is stirred at normal temperature after mixing, stand 5h after mixing evenly, be made outstanding
Turbid after suspension is filtered by vacuum, obtains process product；Calcining filters obtained process product, and cobalt chloride is made after cooling
Modified apricot shell active carbon.
A further improvement of the present invention is that:
Preferably, the preparation method of pretreated apricot shell active carbon is the following steps are included: crush commercially available apricot shell active carbon,
With the smashed apricot shell active carbon of deionized water repeated flushing, until the deionized water clarification after cleaning；Apricot shell after cleaning is living
Property charcoal is sieved after dry, and pretreated apricot shell active carbon is made.
Preferably, the apricot shell active carbon drying temperature after cleaning is 120 DEG C, and drying time is for 24 hours.
Preferably, the sieving standard of the apricot shell active carbon after cleaning is 60 mesh.
Preferably, the concentration of cobalt chloride solution is 0.5mol/L.
Preferably, after pretreated apricot shell active carbon is mixed with cobalt chloride solution, mixing time >=10h at normal temperature.
Preferably, the calcination temperature of process product is 300 DEG C, calcination time 2h.
Compared with prior art, the invention has the following advantages:
The invention discloses a kind of preparation method of the cobalt improved apricot shell active carbon of chlorination, this method is different from traditional pass through
Acid or alkali are to activated carbon modified, using cobalt chloride to activated carbon modified, whole preparation process mild condition, it is at low cost, be easy to real
It applies, have a wide range of application, and substantially increase the utilization rate and adsorption capacity of active carbon；Verifying discovery is modified by this method
Active carbon inside be adsorbed with cobalt ions, be adsorbed with cobalt ions active carbon be directed to the mould oil containing benzothiophene desulfurization degree
It is 49.3%, higher than the existing desulfurization degree by sour or alkali modification active carbon；The preparation method expands being applicable in for active carbon
Range reduces use cost, plays significant effect to desulfurization.
[Detailed description of the invention]
The SEM that Fig. 1 is commercially available apricot shell active carbon GAC schemes；
Wherein: (a) under 100 μm；(b) under 10 μm；
Fig. 2 is the SEM figure for being chlorinated cobalt improved Co-GAC of the invention；
Wherein: (a) under 100 μm；(b) under 10 μm；
Fig. 3 is the energy spectrum diagram for being chlorinated cobalt improved Co-GAC of the invention；
Fig. 4 is GAC, Co-GAC, 10%HNO3- GAC, 37%HNO3- GAC, 10%HCl-GAC and 40%HCl-GAC's is red
External spectrum figure；
Fig. 5 be include benzothiophene mould oil standard curve；
Fig. 6 is the regression curve of sulfur content in the peak area and mould oil of mould oil.
[specific embodiment]
The invention will be described in further detail with reference to the accompanying drawing:
Embodiment 1
(1) pretreatment and screening of apricot shell active carbon
Apricot shell active carbon is bought in the market, crushes apricot shell active carbon with Miniature universal high speed disintegrator, it will be smashed
Apricot shell active carbon deionized water repeated flushing, until the clarification of active carbon upper liquid.Washed active carbon is placed on air blast to do
Dry in dry case, setting temperature is 120 DEG C, and the time is for 24 hours.The standard inspection sieve of 60 mesh of dried active carbon is screened,
Be placed at dry and ventilated stay it is rear spare, be labeled as GAC.The SEM spectrum prepared is as shown in Figure 1, can from (a) and (b) of Fig. 1
To find out that the surface GAC is attached with small hole.
(2) preparation of modified activated carbon
The cobalt chloride solution for preparing 0.5mol/L weighs 5g active carbon, and 5g active carbon is mixed with 100mL cobalt chloride solution
In beaker, at least stirred 10 hours with magnetic stirring apparatus at normal temperature.After the completion of to be mixed, then stand 5 hours.Then it uses
Vacuum pump is filtered, then filtered sample is calcined 2 hours in tubular heater, and setting temperature is 300 DEG C.Wait calcine
Sample later is cooling, spare, is made and is chlorinated cobalt improved active carbon, is labeled as Co-GAC.The SEM of the Co-GAC prepared
Shown in figure (a) and figure (b) in spectrogram such as Fig. 2, comparison diagram 1 and Fig. 2 it can be found that active carbon be chlorinated it is cobalt improved after, equally
Amplification factor under (10 μm), the density of hole becomes larger, depth down, is further amplified (12 μm) as can be seen that each hole
There is more tiny hole in hole；Fig. 3 is the energy spectrum diagram of Co-GAC, and the following table 1 is the corresponding energy spectrum analysis table of energy spectrum diagram of Fig. 3.
In conjunction with Fig. 3 and table 1 as can be seen that being attached with a small amount of cobalt in modified active carbon, illustrate being modified to for Supported Co active carbon
Function, in addition by the absorption property of active carbon it is found that Metal Supported ion can be attached in the aperture of active carbon under normal circumstances.
The energy spectrum analysis table of table 1Co-GAC
Comparative example:
68% nitric acid is diluted to the 10% of 100mL and 40% nitric acid of 100mL respectively, by 40% hydrochloric acid
At 10% hydrochloric acid of 100mL, 40% hydrochloric acid of 100mL is separately taken.The active carbon after screening is divided into 5 parts again, every portion
30g chooses 4 parts and comes out, is added separately in four kinds of acid, and using reflux unit heating stirring, temperature is set as 75 DEG C, when reflux
Between 2h.After reflux, be cooled to room temperature, after wash modified active carbon repeatedly with deionized water, until the pH of cleaning solution exists
Between 6-7.Then it is dried with constant temperature blast drying oven, air dry oven temperature is 120 DEG C, drying time 5h.It will do
Active carbon after dry is respectively labeled as 10%HNO3- GAC, 37%HNO3- GAC, 10%HCl-GAC, 40%HCl-GAC are placed on dry
Stay rear spare in dry ventilation.
Fig. 4 is unmodified active carbon, and embodiment 1 is chlorinated in cobalt improved active carbon and comparative example four kinds and is modified
The infrared spectrogram of active carbon, it can be seen from the figure that in wavelength in 750cm-1There is different vibration peaks, this is mainly the face C-H
Outside sweep vibration, in 1500cm-1Also there is different vibration peaks, this is mainly C=C skeletal vibration, in 2800-3000cm-1Also have
Different vibration peaks, this is mainly that C-H stretching vibration absorbs, it can be seen that Co/GAC is in 500-1500cm-1With other four kinds
Sour modified activated carbon and unmodified activity have certain difference between wavelength 1250-1500 on absorbance, peak area,
Illustrate there are further micronization processes to the surface of active carbon by modification, obtains different surface textures.
The preparation of mould oil
Use n-hexane as solvent, benzothiophene is solute, and the mould oil for configuring 1000ppm is mother liquor, and is diluted to
The sub- liquid of 200ppm, 400ppm, 600ppm, 800ppm are respectively placed in in labelled volumetric flask, spare.By above-mentioned
The mother liquor of 200ppm, 400ppm, 600ppm, 800ppm and 1000ppm obtain standard curve such as Fig. 5 through chromatographic
It is shown, using the sulfur content in mould oil as abscissa, scatter plot is drawn by ordinate of benzothiophene chromatographic peak area, passes through line
Property returns to obtain standard curve, fit equation are as follows:
Y=0.0095X-0.183, R2=0.9983 (1)
In formula, X is concentration/ppm, and Y is peak area/106。
The calculation formula of desulfurization degree η are as follows:
In formula, η is desulfurization degree/%, and c is sulfur content/ppm.
Four kinds of active carbons of the active carbon and comparative example preparation that take unmodified active carbon (GAC), embodiment 1 to prepare are each
The mould oil 25mL of 1g, mother liquor 1000ppm take 6 parts, and six kinds of activated carbon are added in mould oil respectively, stand and inhale at 20 DEG C
After attached 2h, is first tentatively filtered with recirculated water and vacuum pump, obtain filtrate.It filters, obtains again using sand core funnel
Filtrate.Test sample finally is obtained by filtration with 0.45 micrometer Millipore membrane filtration vacuum pump.By Shimadzu chromatographic
Benzothiophene chromatographic peak area is obtained, is analyzed by measurement, obtains GAC, 10%HNO3- GAC, 40%HNO3- GAC, 10%HCl-
Chromatographic peak area after GAC, 40%HCl-GAC, Co-GAC absorption is successively 6.85 × 105、6.76×105、5.24×105、
5.32×105、5.77×105、4.68×105, according to formula (1) obtain sulfur content be followed successively by 745ppm, 727ppm, 566ppm,
575ppm,622ppm,507ppm.Show that desulfurization degree is followed successively by 25.5% according to formula (2), 27.3%, 43.4%, 42.5%,
37.8%, 49.3%, the type and desulfurization degree of the corresponding active carbon being modified are as shown in table 2 below, are chlorinated cobalt as known from Table 2
The desulfurization degree of modified active carbon is much larger than by the desulfurization degree of the active carbon after acid or alkali modification, illustrate to be chlorinated it is cobalt improved after
Active carbon removing oil in sulphur excellent effect.
The active carbon and desulfurization degree that table 2 is modified
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (7)
1. a kind of preparation method of the cobalt improved apricot shell active carbon of chlorination, which is characterized in that include the following steps, by pretreated apricot
Shell active carbon is mixed with cobalt chloride solution according to solid-liquid ratio 1g:20mL, is stirred after mixing, is stood at normal temperature after mixing evenly
5h is made suspension, after suspension is filtered by vacuum, obtains process product；Calcining filters obtained process product, makes after cooling
Obtain the cobalt improved apricot shell active carbon of chlorination.
2. a kind of preparation method of the cobalt improved apricot shell active carbon of chlorination according to claim 1, which is characterized in that pretreatment
Apricot shell active carbon preparation method the following steps are included: commercially available apricot shell active carbon is crushed, with deionized water repeated flushing powder
Apricot shell active carbon after broken, until the deionized water clarification after cleaning；Apricot shell active carbon after cleaning is sieved after dry, is made pre-
The apricot shell active carbon of processing.
3. a kind of preparation method of the cobalt improved apricot shell active carbon of chlorination according to claim 2, which is characterized in that after cleaning
Apricot shell active carbon drying temperature be 120 DEG C, drying time be for 24 hours.
4. a kind of preparation method of the cobalt improved apricot shell active carbon of chlorination according to claim 2, which is characterized in that after cleaning
Apricot shell active carbon sieving standard be 60 mesh.
5. a kind of preparation method of the cobalt improved apricot shell active carbon of chlorination according to claim 1, which is characterized in that cobalt chloride
The concentration of solution is 0.5mol/L.
6. a kind of preparation method of the cobalt improved apricot shell active carbon of chlorination according to claim 1, which is characterized in that pretreatment
Apricot shell active carbon mixed with cobalt chloride solution after, mixing time >=10h at normal temperature.
7. a kind of preparation method of the cobalt improved apricot shell active carbon of chlorination according to claim 1, which is characterized in that process produces
The calcination temperature of object is 300 DEG C, calcination time 2h.
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Citations (5)
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| CN1135456A (en) * | 1996-01-11 | 1996-11-13 | 湖北省化学研究所 | Active-carbon finely sweetening agent and preparation thereof |
| US20100025301A1 (en) * | 2004-05-31 | 2010-02-04 | Agency For Science, Technology And Research | Novel process for removing sulfur from fuels |
| CN101747931A (en) * | 2010-01-12 | 2010-06-23 | 华烁科技股份有限公司 | Fine desulfurizing agent for transforming thioalcohol in liquid hydrocarbons at normal temperature and preparation and application methods thereof |
| CN102500362A (en) * | 2011-12-02 | 2012-06-20 | 中国科学院山西煤炭化学研究所 | Catalyst for removing H2S from gas by catalytic oxidation, preparation method and application |
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2018
- 2018-10-31 CN CN201811289251.0A patent/CN109225137A/en active Pending
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| CN1135456A (en) * | 1996-01-11 | 1996-11-13 | 湖北省化学研究所 | Active-carbon finely sweetening agent and preparation thereof |
| US20100025301A1 (en) * | 2004-05-31 | 2010-02-04 | Agency For Science, Technology And Research | Novel process for removing sulfur from fuels |
| CN101747931A (en) * | 2010-01-12 | 2010-06-23 | 华烁科技股份有限公司 | Fine desulfurizing agent for transforming thioalcohol in liquid hydrocarbons at normal temperature and preparation and application methods thereof |
| CN102500362A (en) * | 2011-12-02 | 2012-06-20 | 中国科学院山西煤炭化学研究所 | Catalyst for removing H2S from gas by catalytic oxidation, preparation method and application |
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