CN107902655A - A kind of method for preparing nitrating activated carbon using discarded activated carbon - Google Patents
A kind of method for preparing nitrating activated carbon using discarded activated carbon Download PDFInfo
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- CN107902655A CN107902655A CN201711187796.6A CN201711187796A CN107902655A CN 107902655 A CN107902655 A CN 107902655A CN 201711187796 A CN201711187796 A CN 201711187796A CN 107902655 A CN107902655 A CN 107902655A
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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- C07C17/08—Preparation of halogenated hydrocarbons by addition of hydrogen halides to unsaturated hydrocarbons
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Abstract
The invention discloses a kind of method for preparing nitrating Carbon Materials using discarded activated carbon, using useless charcoal as raw material, the itrogenous organic substance such as amino acid, paracetamol or protein etc. that useless charcoal saturation is adsorbed are nitrogen source, after two-step carbonization under inert atmosphere, you can obtain the nitrating Carbon Materials.The processing cost that the present invention greatly reduces this kind of high-risk discarded object of Industry Waste charcoal realizes recycling, and the nitrogen modified activated carbon of high added value can be obtained with a step.The preparation method is simple to operation, can directly utilize existing activated carbon generation technique, and the Carbon Materials that recycling obtains can prepare vinyl chloride monomer directly as catalyst, catalyzing acetylene hydrogen chloride, greatly improve the added value of waste active carbon.
Description
Technical field
The invention belongs to discarded activated carbon reclaiming to prepare field of new materials, is specifically related to one kind and utilizes food service industry
Activated carbon is discarded caused by refinery decolorization process and prepares nitrating Carbon Materials and its application.
Background technology
The grain conversion industry such as fermentation industry in China is developed rapidly, wherein starch candy output it is 2,000,000 tons about nearly/
Year, 400,000 tons/year of citric acid, 1,000,000 tons of msg output, these products are producing and certainly will need to use activity in subtractive process
Charcoal.According to rough Statistics, only monosodium glutamate subtractive process charcoal amount 1 year will be 3.5 ten thousand~4.0 ten thousand tons, in addition sorbic acid, citric acid, doctor
Medicine intermediate, food additives and dyestuff intermediate etc., need the annual consumption of wood activated charcoal also of about 3.0 ten thousand~3.5 ten thousand tons.
Activated carbon after these adsorption saturations is directly abandoned or burned mostly as discarded object, landfill disposal, this not only increases life
Production cost also creates the very big pollution of environment, wherein the organic substance adsorbed is not also reasonably handled and recycled profit
With, while also result in the waste of resource.
Activated carbon has acid-alkali-corrosive-resisting, cheap etc. as a kind of material with high-specific surface area, hole prosperity
Advantage.In industrial production food, medicine and other fields, bleaching process is essential link, and activated carbon has as a kind of
The adsorbent for having high absorption capacity is even more to be widely used, and such as in production monosodium glutamate field, activated carbon is commonly used to adsorb
Pigment, iron ion, its surface can also adsorb the nitrogen substances such as sodium glutamate, protein, amino acid；Pyrogen (pyrogen) conduct
The pathogenic bacteria of association in a kind of pharmaceutical product, are decolourizing usually through needle-use activated carbon (injection active carbon, medicinal carbon)
While adsorbing and removing；L-Trp is humans and animals essential amino acid, and the growth and development, metabolism to humans and animals play
Important function, at present the extraction process of tryptophan include micro-filtration, ion exchange, decoloration, evaporation, crystallization, wherein bleaching process is more
Decolourized using activated carbon adsorption.Activated carbon after these adsorption saturations is directly abandoned or burned, filled out mostly as discarded object
Processing is buried, this not only increases the very big pollution that production cost also creates environment, wherein the nitrogen substance adsorbed does not also obtain
Rational processing and recycling, while also result in the waste of resource.
It is to leach organic matter, decompose or charcoal in situ that the waste active carbon for having adsorbed organic matter is carried out regenerated method
Change.At present, the common regeneration of such useless charcoal is high temperature method, acid-alkali washing method, oxidation reclaiming process, microwave radiation method, solvent
Method of reproduction, bio-regeneration method etc., these types of method can be such that useless charcoal is regenerated to a certain extent, but there is also certain to ask
Topic, the regeneration rate such as high temperature method is not high, and there are certain etching problem, solvent regeneration process can produce at the same time to equipment for acid-alkali washing method
Raw substantial amounts of waste liquid, microwave reclaiming method are difficult to realize industrialized production, and bio-regeneration method is retained there is also the surface of activated carbon to be had
The shortcomings of machine thing.In addition, the processing of high temperature method, acid-alkali washing method can not fundamentally solve the problems, such as " danger is solid ", and simply by it
It is changed into " danger gas ", " danger liquid " etc., still lacks a kind of means of the effective discarded activated carbon of processing industry decoloration at present.Absorption exists
Complicated components on activated carbon are greatly improved, it is necessary to can be purified using the technique of substantial amounts of organic solvent and complexity
Energy consumption and environmentally friendly cost.Directly if discarded activated carbon can be converted into and can on the one hand can with the activated carbon of functionalization
The skeleton structure of activity recovery charcoal, on the other hand can be modified activated carbon during regenerated, improve its added value,
Catalyst carrier is such as used as, this can also substantially reduce production cost, realize the recycling of resource.
Nitrating Carbon Materials have shown excellent performance in absorption and catalytic field as a kind of novel alkaline Carbon Materials,
Nitrating Carbon Materials not yet realize industrialization production at present, and the preparation method in document on nitrating Carbon Materials is more, but mostly
It is by impregnating extra organic or inorganic nitrogen-sourced such as ammonium hydroxide, urea, ammonium hydrogen carbonate, melamine to synthetic Carbon Materials
Amine etc. is modified and obtains, and such method is required to extra consumption nitrogenous reagent, such as patent of invention [application publication number
CN106115698A] using useless charcoal as carbon source, ammonium oxalate is nitrogen source, and nitrating Carbon Materials are prepared through mechanical lapping and charing.Invention
Patent [application publication number CN105819443A] selects discarded plant based biomass to be mixed for raw material with activator, nitrogenous phosphate
Dipping is closed, nitrating Carbon Materials are prepared through drying, charing.Patent of invention [application publication number CN103922306A] selects biomass
Raw material is carbon source, after being carbonized under an inert atmosphere, and secondary charing process is carried out under ammonia atmosphere, obtained high nitrogen doped
The modified porous Carbon Materials of amount.Patent of invention [application publication number CN105948045A] uses starch to be passed through for carbon source and additional nitrogen source
After hydro-thermal, activation, nitrating activated carbon nanoparticle is obtained by high temperature carbonization.These methods all to a certain extent there is into
This height, complex process, the shortcomings of additionally consuming substantial amounts of Organic Ingredients, while to reactor there are certain etching problem, it is difficult
To realize industrialization production.
The present invention in view of the above problems, propose it is a kind of turn waste into wealth prepare the basic activated carbon thinking of N doping, utilize
The organic matter (glutamic acid, glycine, paracetamol, vinasse etc.) adsorbed in discarded activated carbon is used as nitrogen source, by owing
Heat treatment cracks itrogenous organic substance under the conditions of oxygen, and a step obtains the activated carbon of nitrating.The present invention is carrying out resource to discarded object
Circulationization realizes the modification of activated carbon while utilization, introduce nitrogen while the pore structure of activity recovery charcoal
The surface of activated carbon, obtains the basic activated carbon of nitrating,
A kind of method that nitrating activated carbon is prepared using discarded activated carbon of the present invention can be with killing three birds with one stone, in the useless charcoal of processing
Meanwhile recovered pore structure, while activated centre is introduced, a step realizes the recycling of useless charcoal；It can save into
This, reduces three waste discharge, turns waste into wealth, be the new way that an environmentally protective solid waste resource recovery utilizes.
The content of the invention
The invention discloses a kind of using having adsorbed the method that the discarded activated carbon of nitrogenous compound prepared nitrating Carbon Materials,
To have adsorbed the activated carbon of nitrogen substance in food service industry subtractive process as raw material, using the nitrogenous compound in the charcoal that gives up as nitrogen source,
Through impregnating charing catalyst, carbonized under an inert atmosphere after dry, you can obtain the nitrating Carbon Materials.
Regenerated present invention also offers a kind of using industry decoloration waste active carbon, original position obtains the nitrating charcoal of functionalization
The method of material, greatly reduces the processing cost of this kind of high-risk discarded object of the useless charcoal of industry decoloration.The preparation method is simply easily grasped
Make, can directly utilize existing activated carbon generation technique, and the Carbon Materials that recycling obtains not only show in absorption waste water from dyestuff
Excellent absorption property is gone out, moreover it is possible to which, directly as catalyst, catalyzing acetylene hydrogen chloride, greatly improves the attached of waste active carbon
It is value added.
The present invention uses following technical scheme：
A kind of method for preparing nitrating activated carbon using discarded activated carbon, the method are：Discarded activated carbon is done
Dry, drying temperature is 80~110 DEG C, and drying time is 12~24h, and charing catalysis is added dropwise on discarded activated carbon after the drying
Agent, stands, and dwell temperature is 25~50 DEG C, and time of repose is 8~24h, is then carbonized in advance under atmosphere of inert gases, temperature
Degree control is between 150~350 DEG C, and the retention time is 1~10h, then temperature is warming up to 400~850 DEG C, the retention time 1
~20h, up to the nitrating activated carbon；The discarded activated carbon for absorption itrogenous organic substance discarded activated carbon, the charcoal
It is the concentrated sulfuric acid or oxalic acid solution to change catalyst.
In the above method, the quality of the charing catalyst is the 1~5% of the discarded quality of activated carbon.Oxalic acid solution
Mass fraction be 10-30wt%.The concentrated sulfuric acid refers to the pure H that mass fraction is more than or equal to 70%2SO4Aqueous solution.
In the above method, the discarded activated carbon of the itrogenous organic substance, the itrogenous organic substance is amino acid, to acetyl
One or more in amino phenols or protein.
In the above method, the amino acid is glutamic acid, alanine, arginine, winter propylhomoserin, histidine, lysine, color
One or more in propylhomoserin or L glycine.
In the above method, the discarded activated carbon is selected from discarded activated carbon caused by food, medical synthesis field industry
In one or more.
In the above method, the food service industry discards activated carbon and is selected from the decoloration discarded caused by glutamate production industry
Waste active carbon, waste active carbon, soy sauce brewing industry institute caused by starch sugaring industry caused by activated carbon, glycine production
One or more in the waste active carbon or drinks brewing industry of generation in caused waste active carbon.
In the above method, the inert gas is nitrogen or argon gas.
In the above method, by two-step carbonization, the itrogenous organic substance adsorbed on activated carbon surface is cracked and surface
Reaction, first step charcoal, which turns to, " to be added dropwise charing catalyst on discarded activated carbon after the drying, stands, dwell temperature is 25~50
DEG C, time of repose is 8~24h, is then carbonized in advance under atmosphere of inert gases, temperature control between 150~350 DEG C,
Retention time is 1~10h ", second step charcoal turn to " temperature is warming up to 400~850 DEG C, the retention time is 1~20h ", you can
Obtain modified activated carbon, namely nitrating activated carbon.
The above method carries out preferably in tube furnace.
Further, the nitrating activated carbon prepared by the present invention can be directly used as the catalyst of acetylene hydrochlorination, can also use
Make the carrier of catalyst without mercury.By obtained nitrating activated carbon, using dipping or other conventional method for preparing catalyst, draw
Enter active component, be dried to obtain modified activated carbon supported catalyst.Activated carbon composition described here can be RuCl3、
HAuCl4、HgCl2Deng.
Present invention also offers application of the nitrating activated carbon as catalyst in acetylene hydrochlorination reaction, the second
Alkynes hydrochlorination uses routine operation, such as by being carried out as follows operation：
Acetylene hydrochlorination reaction carries out in the glass fixed bed reactors of internal diameter 20mm, loaded catalyst 1-4mL,
Acetylene and chlorination hydrogen pressure are all 0.1MPa, V (C2H2):V (HCl)=1:1.05~1.2, control acetylene flow air speed is in 30h-1, 180 DEG C of reaction temperature, acetylene gas removes H by concentrated sulfuric acid purification first2S and H3The impurity such as P, HCl gases are done in silica gel
Dry device removes moisture.N is used before reaction2Moisture and air in removing system are purged, is then first passed through HCl gas activation 0.5h, then
Acetylene gas is passed through to be reacted.Gas flow is controlled with mass flowmenter.Reaction product NaOH solution absorb HCl gases it
Laggard promoting the circulation of qi analysis of hplc, usable floor area normalization method measure each component content.
The present invention has the following advantages compared with prior art：
1. the present invention is using industry decoloration waste active carbon as raw material, using the rich nitrogen material of absorption as nitrogen source, need not be additional
In the case of additional nitrogen source, one-step method fabricated in situ nitrating Carbon Materials are realized；
2. the present invention uses discarded activated carbon of the raw material for food service industry, with using timber, coconut husk and coal as raw material
Production activated carbon is compared, and has the features such as of low cost, technique is simple.Contain nitrogen in the activated carbon of preparation, for being catalyzed
Agent need not be handled early period when preparing.
3. catalyst prepared by the present invention can both be reacted as catalyst for acetylene hydrochlorination, very high urge is shown
Change activity and stability, while can also be prepared as the carrier of catalyst without mercury using infusion process after loading other components, i.e.,
It can obtain catalyst without mercury.
4. the method for production modified alkaline activated carbon proposed by the present invention, can not only turn waste into wealth, and production process
Simply, aneroid gives up and solid waste discharge, is a kind of environmentally protective technology, meets policy of the country on utilization of waste as resource
It is oriented to, there is preferable industrialization prospect.
5. basic activated carbon produced by the invention also has extensive in basins such as capacitor, electrode material and sorbing materials
Purposes.It is not limited solely to catalytic field of the present invention.
Brief description of the drawings
Fig. 1 is that regenerated carbon prepared by embodiment 1 and the nitrogen adsorption as the fresh activity charcoal of contrast sample are desorbed
Curve (left side) and graph of pore diameter distribution (right side)
Fig. 2 is the regenerated nitrating absorbent charcoal material sample of embodiment 1 and is catalyzed as the fresh activity charcoal of contrast sample
The conversion of alkyne figure of acetylene hydrochlorination.
Embodiment
With reference to specific embodiment, the present invention is described further, but protection scope of the present invention is not limited in
This.The concentrated sulfuric acid is purchased from Quzhou Ju Hua groups, and mass fraction is more than or equal to 70%.
Embodiment 1
The discarded activated carbon used in bleaching workshop section during 20g glutamate productions is weighed, dry 24h, passes through leaching at 110 DEG C
The 2g concentrated sulfuric acids are added drop-wise to the surface of activated carbon by the method for stain, and 25 DEG C of standing 10h, transfer the sample into porcelain boat, then in pipe
Carbonized in formula stove.Carbonization condition is：Nitrogen flow rate is warming up at 250 DEG C in advance for 30mL/min, by 30 DEG C with 3.4 DEG C/min
Charing 2h, carbonize 3h, cooled to room temperature at 850 DEG C, you can obtains the nitrating regeneration Carbon Materials.
Embodiment 2
The discarded activated carbon used in bleaching workshop section during 20g glutamate productions is weighed, dry 24h, passes through leaching at 110 DEG C
The 2g concentrated sulfuric acids are added drop-wise to the surface of activated carbon by the method for stain, and 25 DEG C of standing 10h, transfer the sample into porcelain boat, then in pipe
Carbonized in formula stove.Carbonization condition is：Nitrogen flow rate is warming up at 250 DEG C in advance for 30mL/min, by 30 DEG C with 3.4 DEG C/min
Charing 2h, carbonize 10h, cooled to room temperature at 850 DEG C, you can obtains the nitrating Carbon Materials.
Embodiment 3
The discarded activated carbon used in bleaching workshop section during 20g glutamate productions is weighed, dry 24h, passes through leaching at 110 DEG C
2g oxalic acid solutions (15wt%) are added drop-wise to the surface of activated carbon by the method for stain, and 30 DEG C of standing 10h, transfer the sample into porcelain boat
In, then carbonized in tube furnace.Carbonization condition is：Nitrogen flow rate heats up for 30mL/min, by 30 DEG C with 3.4 DEG C/min
At to 250 DEG C in advance charing 2h, carbonize 3h, cooled to room temperature at 400 DEG C, you can obtain the nitrating Carbon Materials.
Embodiment 4
The discarded activated carbon produced in the production of 20g glycine is weighed, the dry 24h at 110 DEG C will by the method for dipping
The 2g concentrated sulfuric acids are added drop-wise to the surface of activated carbon, and 30 DEG C of standing 15h, transfer the sample into porcelain boat, then carried out in tube furnace
Charing.Carbonization condition is：Nitrogen flow rate is warming up at 250 DEG C pre- charing 2h, 850 for 30mL/min, by 30 DEG C with 3.4 DEG C/min
3h, cooled to room temperature are carbonized at DEG C, you can obtain the nitrating Carbon Materials.
Embodiment 5
Weigh waste active carbon caused by 100g soy sauce brewing processes, dry 24h, passes through the side of dipping at 110 DEG C
The 2g concentrated sulfuric acids are added drop-wise to the surface of activated carbon by method, and 50 DEG C of standing 15h, transfer the sample into porcelain boat, then in tube furnace
Carbonized.Carbonization condition is：Nitrogen flow rate is 30mL/min, is warming up at 250 DEG C with 3.4 DEG C/min by 30 DEG C and carbonizes in advance
2h, carbonize 3h, cooled to room temperature at 850 DEG C, you can obtains the nitrating Carbon Materials.
The physical parameter and nitrogen content of 1 various Carbon Materials of table
The nitrogen in the product prepared in above-described embodiment as the waste active carbon of raw material with embodiment 1-5 is listed in table 1
Constituent content.The specific surface area and pore volume and nitrogen of activated carbon after the fresh activity charcoal provided by table 1, waste active carbon and regeneration
Content value can be seen that the specific surface area of waste active carbon and pore volume is substantially reduced than fresh activity charcoal, most activated carbon
Hole adsorbed material blocks, and after the method by the present invention is handled and regenerated, specific surface area returns to 1000m2/ g with
On, pore volume returns to 0.97cm3/ g, illustrates that the method that the present invention provides can not only realize the regeneration of activated carbon, while goes back real
The nitrogen for having showed activated carbon is modified, and successfully nitrogen is incorporated into activated carbon.
The nitrogen adsorption desorption curve (left side) and pore size distribution curve of the nitrating Carbon Materials of the preparation of embodiment 1 are provided in Fig. 1
(right side), and provide fresh activity charcoal nitrogen adsorption desorption curve without decolorization and pore size distribution curve as a comparison.By
Figure understands that nitrating Carbon Materials manufactured in the present embodiment have a larger specific surface area, while comprising micropore and mesoporous, passes through at the same time
Substantially the pore structure of fresh activity charcoal can be returned to after high temperature carbonization.
Embodiment 6
The nitrating Carbon Materials obtained after the fresh activity charcoal in embodiment 1, Regenevating Waste Activated Carbon are crushed respectively, are taken
40-80 mesh sieves point, after 110 DEG C of dry 2h, sample 4mL, are fitted into the stainless steel fixed bed reactors of internal diameter 10mm and carry out acetylene
Hydrochlorination, acetylene and chlorination hydrogen pressure are all 0.1MPa, n (C2H2):N (HCl)=1:1.2, control acetylene flow air speed exists
30h-1, 220 DEG C of reaction temperature, acetylene gas removes H by concentrated sulfuric acid purification first2S and H3The impurity such as P, hydrogen chloride gas exist
Silica gel drier removes moisture.Moisture and air in removing system are purged with nitrogen before reaction, is then first passed through hydrogen chloride gas
0.5h is activated, then is passed through acetylene gas and is reacted.Gas flow is controlled with mass flowmenter.Reaction product sodium hydroxide is molten
Gas chromatographic analysis, usable floor area normalization method measure each component content are carried out after liquid absorbing hydrogen chloride gas.Fig. 2 is with reality
Apply fresh activity charcoal in example 1 and conversion of alkyne figure that nitrating Carbon Materials are catalyst acetylene hydrochlorination.Can by Fig. 2
Know, the conversion of alkyne of fresh activity charcoal only has 15% or so, and the conversion of alkyne of the regenerated nitrating Carbon Materials of embodiment 1 reaches
To more than 60%, illustrate that regenerated nitrating Carbon Materials are compared with fresh activated carbon, its conversion of alkyne obtains larger raising.With
Upper result proves to introduce while can realizing regeneration and the nitrating activated centre of activated carbon at the same time using this technology, has preferable
Novelty.
Claims (8)
- A kind of 1. method for preparing nitrating activated carbon using discarded activated carbon, it is characterised in that the method is：By discarded activity Charcoal is dried, and drying temperature is 80~110 DEG C, and drying time is 12~24h, and charcoal is added dropwise on discarded activated carbon after the drying Change catalyst, stand, dwell temperature is 25~50 DEG C, and time of repose is 8~24h, is then carried out under atmosphere of inert gases pre- Charing, for temperature control between 150~350 DEG C, the retention time is 1~10h, then temperature is warming up to 400~850 DEG C, is kept Time is 1~20h, up to the nitrating activated carbon；The discarded activated carbon is the discarded activated carbon of absorption itrogenous organic substance, The charing catalyst is the concentrated sulfuric acid or oxalic acid solution.
- 2. the method as described in claim 1, it is characterised in that：The quality of the charing catalyst is the discarded active carbonaceous The 1~5% of amount.
- 3. the method as described in claim 1, it is characterised in that：The oxalic acid solution mass fraction is 10-30wt%.
- 4. the method as described in claim 1, it is characterised in that：The discarded activated carbon of the absorption itrogenous organic substance, it is described Itrogenous organic substance is the one or more in amino acid, paracetamol or protein.
- 5. method as claimed in claim 4, it is characterised in that：The amino acid is glutamic acid, alanine, arginine, winter One or more in propylhomoserin, histidine, lysine, tryptophan or L glycine.
- 6. the method as described in claim 1, it is characterised in that：The discarded activated carbon is selected from food, medical synthesis field row The one or more in activated carbon are discarded caused by industry.
- 7. method as claimed in claim 6, it is characterised in that：Activated carbon is discarded caused by the food service industry and is selected from taste Waste active carbon, starch sugaring industry institute caused by the decoloration active carbon discarded caused by smart production industry, glycine production In waste active carbon caused by the waste active carbon of generation, soy sauce brewing industry or drinks brewing industry in caused waste active carbon One or more.
- 8. the method as described in claim 1, it is characterised in that：The inert gas is nitrogen or argon gas.
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| CN108579790A (en) * | 2018-05-25 | 2018-09-28 | 万华化学集团股份有限公司 | A kind of preparation method of porous C catalyst of N doping and preparation method thereof and β-isophorone |
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