CN113262757B - Method for preparing furfural simultaneously by regenerating waste activated carbon - Google Patents

Method for preparing furfural simultaneously by regenerating waste activated carbon Download PDF

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CN113262757B
CN113262757B CN202110606733.XA CN202110606733A CN113262757B CN 113262757 B CN113262757 B CN 113262757B CN 202110606733 A CN202110606733 A CN 202110606733A CN 113262757 B CN113262757 B CN 113262757B
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activated carbon
waste
waste activated
catalyst
spray painting
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CN113262757A (en
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李传华
钱光人
卢青
孔旺盛
李玉东
顾佳媛
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Shanghai Solid Waste Disposal Co ltd
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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
    • 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
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/34—Regenerating or reactivating
    • B01J20/3416—Regenerating or reactivating of sorbents or filter aids comprising free carbon, e.g. activated carbon
    • 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
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/34—Regenerating or reactivating
    • B01J20/345—Regenerating or reactivating using a particular desorbing compound or mixture
    • B01J20/3475—Regenerating or reactivating using a particular desorbing compound or mixture in the liquid phase
    • 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
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/34—Regenerating or reactivating
    • B01J20/3483—Regenerating or reactivating by thermal treatment not covered by groups B01J20/3441 - B01J20/3475, e.g. by heating or cooling
    • 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
    • B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/002—Component parts of these vessels not mentioned in B01J3/004, B01J3/006, B01J3/02 - B01J3/08; Measures taken in conjunction with the process to be carried out, e.g. safety measures
    • 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
    • B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/04—Pressure vessels, e.g. autoclaves
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
    • C07D307/02—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
    • C07D307/34—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members
    • C07D307/38—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members with substituted hydrocarbon radicals attached to ring carbon atoms
    • C07D307/40—Radicals substituted by oxygen atoms
    • C07D307/46—Doubly bound oxygen atoms, or two oxygen atoms singly bound to the same carbon atom
    • C07D307/48—Furfural
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/10—Inorganic adsorbents
    • B01D2253/102—Carbon
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/30—Sulfur compounds
    • B01D2257/306—Organic sulfur compounds, e.g. mercaptans
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
    • B01D2257/708—Volatile organic compounds V.O.C.'s
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/584—Recycling of catalysts

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Analytical Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Materials Engineering (AREA)
  • Thermal Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Catalysts (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

The invention belongs to the technical field of waste carbon recycling and hazardous waste recycling, and particularly discloses a method for preparing furfural while regenerating waste activated carbon, which comprises the following steps: s1: adsorbing low-concentration sulfur-containing gas by using the inactivated waste activated carbon at normal temperature until the adsorption is saturated; s2: mixing the waste activated carbon with saturated adsorption, the corn straws and the catalyst obtained in the step S1 in a certain proportion, placing the mixture in a closed pressure-resistant container, and adding a certain volume of solvent into the container for heating and pressurizing treatment, thereby realizing the catalytic activity regeneration of the catalyst; compared with the common dangerous waste treatment methods such as landfill, incineration and the like, the method provided by the invention reuses the waste activated carbon and generates a novel adsorption material, so that the method is environment-friendly, the aim of recycling resources is fulfilled, the operation cost is reduced, and the energy consumption is saved.

Description

Method for preparing furfural simultaneously by regenerating waste activated carbon
Technical Field
The invention relates to the technical field of recycling of waste carbon and recycling of hazardous wastes, in particular to a method for preparing furfural while regenerating waste activated carbon.
Background
With the development of modern industry, Volatile Organic Compounds (VOCs) emitted from chemical plants are important pollutants, and even at low concentrations, cause environmental pollution. Most volatile organic compounds are toxic and long term exposure can be detrimental to human health, damage the nervous system, increase psychological stress, damage the ozone stratosphere, and cause photochemical smog. Therefore, the control of the discharge of VOCs is of great concern.
From the viewpoint of classification, VOCs are classified into alkanes, alkenes, aromatics, oxygen-containing VOCs, nitrogen-containing VOCs, sulfur-containing VOCs, and the like. As a branch of volatile organic compounds, sulfur-containing compounds from printing plants, sewage treatment plants, waste treatment plants, pharmaceutical plants and paper mills may cause odor problems and health hazards, such as respiratory diseases, headaches, nausea and even cancer. Therefore, it is very necessary to remove these compounds. Currently, methods for removing toxic emissions are cryocondensation, catalytic oxidation, biological treatment, and adsorption. Among these methods, the adsorption method has been widely used because of its advantages such as simple operation, low energy consumption, high purification efficiency, and the like.
The activated carbon is black powdery or granular amorphous carbon, contains a large number of micropores and a large specific surface area, and is an adsorbent widely used for gas adsorption. Most of the adsorbed or decolored waste activated carbon in the chemical industry is treated as waste, is usually used for incineration and landfill treatment, and greatly improves the production cost. The waste of the saturated activated carbon causes problems of resource waste, secondary pollution and the like, and the application scale of the activated carbon is greatly limited. Research on methods of reusing or regenerating waste activated carbon has drawn increasing attention from researchers.
Therefore, a new technical means for regenerating the waste activated carbon is urgently needed to be found, and the new technical means is used for solving the problems of environmental pollution, high treatment cost, incomplete treatment technology and resource waste.
Disclosure of Invention
The invention aims to provide a method for preparing furfural while regenerating waste activated carbon, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: the method for preparing furfural while regenerating waste activated carbon comprises the following steps:
s1: adsorbing low-concentration sulfur-containing gas by using the inactivated waste activated carbon at a proper temperature until the adsorption is saturated;
s2: and (2) mixing the waste activated carbon with saturated adsorption obtained in the step S1, corn stalks and the catalyst according to a certain proportion, placing the mixture in a closed pressure-resistant container, and simultaneously adding a certain volume of solvent into the container to carry out heating and pressurizing treatment, thereby realizing the regeneration of the catalytic activity of the catalyst.
Preferably, the waste activated carbon in the step of S1 is waste lacquer activated carbon.
Preferably, the sulfur-containing gas in the step S1 is a gas containing one or more of methyl mercaptan, hydrogen sulfide, thiophene, carbonyl sulfide, etc. in a total concentration of 100-500 ppm.
Preferably, the temperature condition in the step S1 is lower than 150 ℃, and the space velocity is kept for 1000-3000 h -1 Adsorbing for 2-3h under the condition of (1).
Preferably, when the reaction is carried out in the vessel in the step S2, the reaction temperature is controlled to be 150-200 ℃, the regeneration treatment pressure is 50MPa, and the reaction time is 1.5-7.5 h.
Preferably, the catalyst in the step of S2 may be ZnCl 2 、KOH、FeCl 3 One or more of (a) and (b).
Preferably, in the reaction, the catalyst, the waste activated carbon, the corn stalks and the solvent are uniformly mixed and then are put into an autoclave for heating and pressurizing treatment, and the autoclave is continuously turned over in the treatment process to ensure that the catalyst is uniformly contacted with the waste activated carbon; and after the reaction is finished, carrying out solid-liquid separation, calcining the solid obtained by separation after the reaction in a nitrogen atmosphere at the temperature of 500-800 ℃ for 1-2h, and circularly regenerating the regenerated waste activated carbon until the weight of the dried waste activated carbon is less than 3-5%, increasing the measured iodine value by 200-250% and obtaining the regenerated spray painting activated carbon.
Compared with the prior art, the invention has the beneficial effects that: (1) compared with the common dangerous waste treatment methods such as landfill and incineration, the method of the invention regenerates the waste spray painting activated carbon after catalytic inactivation into a new carbon adsorbent, which is environment-friendly, achieves the purpose of resource recycling, and reduces the operation cost;
(2) the method utilizes the waste spray painting activated carbon to absorb sulfur-containing gas at normal temperature, and the reacted solid matter can regenerate a new carbonaceous adsorbent after being activated at high temperature, thereby having breakthrough advantage, greatly reducing the operation cost of chemical enterprises, and being beneficial to circular economy and hazardous waste management and disposal;
(3) the method is simple and easy to implement, low in cost and suitable for popularization and application.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the invention provides a method for preparing furfural while regenerating waste activated carbon, which comprises the following steps:
s1: adsorbing low-concentration sulfur-containing gas by using the inactivated waste activated carbon at normal temperature until the adsorption is saturated;
s2: and (2) mixing the waste activated carbon with saturated adsorption obtained in the step S1, corn stalks and the catalyst according to a certain proportion, placing the mixture in a closed pressure-resistant container, and simultaneously adding a certain volume of solvent into the container to carry out heating and pressurizing treatment, thereby realizing the regeneration of the catalytic activity of the catalyst.
Further, the waste activated carbon in the step S1 is waste lacquer activated carbon.
Further, in the step S1, the sulfur-containing gas is a gas containing one or more of methyl mercaptan, hydrogen sulfide, thiophene, carbonyl sulfide, etc. with a total concentration of 100-500 ppm.
Further, the temperature condition in the step S1 is lower than 150 ℃, and the space velocity is kept for 1000-3000 h -1 Adsorbing for 2-3h under the condition of (1).
Further, when the reaction is carried out in the vessel in the step S2, the reaction temperature is controlled to be 150-200 ℃, the regeneration treatment pressure is 50MPa, and the reaction time is 1.5-7.5 h.
Further, the catalyst in the step of S2 may be ZnCl 2 、KOH、FeCl 3 One or more of (a) and (b).
Further, in the reaction, the catalyst, the waste activated carbon, the corn straw and the solvent are uniformly mixed and then are put into a high-pressure kettle for heating and pressurizing treatment, and the high-pressure kettle is continuously turned over in the treatment process to ensure that the catalyst is uniformly contacted with the waste activated carbon; and (3) after the reaction is finished, carrying out solid-liquid separation, calcining the solid obtained by separation after the reaction in a nitrogen atmosphere at 800 ℃ for 1-2h, circularly regenerating the regenerated waste activated carbon until the weight of the dried waste activated carbon is less than 3-5%, and increasing the measured iodine value by 200-250% to obtain the regenerated spray painting activated carbon.
Example 1:
(1) in the embodiment, the used waste activated carbon is spray painting activated carbon, a certain amount of samples to be treated are put into a vertical tubular furnace reactor, and 100 ppm of methyl mercaptan gas is adsorbed for 3 hours under the conditions that the reaction temperature is controlled at 100 ℃ and the space velocity is 2000h < -1 >;
(2) the solvent is ionized water, ZnCl 2 The corn straw and the waste spray painting active carbon which adsorbs the methyl mercaptan are put into a high-pressure reaction kettle, and simultaneously, the deionized water and the ZnCl are put into the high-pressure reaction kettle 2 The proportion of the corn stalks to the waste active carbon is 1: 2: 3, overturning under the conditions of 50MPa pressure and 180 ℃ for 3 hours, standing at room temperature, and filtering; the filtered waste spray-painting activated carbon is calcined for 2 hours at 800 ℃ under nitrogen, and is dried for 12 hours in an oven at 105 ℃.
Experimental test analysis:
the waste spray painting activated carbon regenerated in the experiment is weighed, and compared with the original waste spray painting activated carbon, the weight is reduced by 4%.
The iodine value of the regenerated waste spray painting activated carbon is subjected to adsorption analysis, and compared with the original waste spray painting activated carbon, the iodine value is increased by 200%.
Example 2:
this embodiment is substantially the same as embodiment 1, and is characterized in that:
in this embodiment, a method for regenerating waste spray activated carbon comprises the following steps:
(1) this procedure is the same as in example 1.
(2) The solvent is deionized water, and KOH, corn stalks and waste spray painting activated carbon which adsorbs methyl mercaptan are put into a high-pressure reaction kettle, and the deionized water is simultaneously put into the high-pressure reaction kettle, wherein the proportion of the KOH, the corn stalks and the waste activated carbon is 1: 2: 3, overturning and heating for 3 hours under the conditions of 50MPa of pressure and 180 ℃, standing at room temperature and filtering; the filtered waste spray-painting activated carbon is calcined for 2 hours at 800 ℃ under nitrogen, and is dried for 12 hours in an oven at 105 ℃.
Carrying out test analysis:
the waste spray painting activated carbon regenerated in the experiment is weighed, and compared with the original waste spray painting activated carbon, the weight is reduced by 3%.
The regenerated waste spray painting activated carbon of the experiment is subjected to iodine value adsorption analysis, and compared with the original waste spray painting activated carbon, the iodine value is increased by 230%.
Example 3:
this embodiment is substantially the same as embodiment 1, and is characterized in that:
in this embodiment, a method for regenerating waste spray activated carbon comprises the following steps:
(1) this procedure is the same as in example 1.
(2) Solvent is deionized water, FeCl is added 3 The corn straw and the waste spray painting active carbon which adsorbs the methyl mercaptan are put into a high-pressure reaction kettle, and simultaneously, deionized water and FeCl are put into the high-pressure reaction kettle 3 The proportion of the corn straw and the waste activated carbon is 1: 2: 3, overturning and heating for 3 hours under the conditions of 50MPa of pressure and 180 ℃, standing at room temperature and filtering; the filtered waste spray-painting activated carbon is calcined for 2 hours at 800 ℃ under nitrogen, and is placed in an oven at 105 ℃ for drying for 12 hours.
Test analysis was performed:
the waste spray painting activated carbon regenerated in the experiment is weighed, and compared with the original waste spray painting activated carbon, the weight is reduced by 5%.
The iodine value of the waste spray paint activated carbon regenerated in the experiment is adsorbed and analyzed, and compared with the original waste spray paint activated carbon, the iodine value is increased by 250 percent
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (2)

1. A method for preparing furfural while regenerating waste activated carbon is characterized by comprising the following steps:
s1: the inactivated waste spray painting active carbon is kept at the temperature of less than 150 ℃ for 1000-3000 h -1 Adsorbing the sulfur-containing gas with low concentration for 2-3h under the condition until the adsorption is saturated; the sulfur-containing gas is methyl mercaptan and/or hydrogen sulfide;
s2: during the reaction, uniformly mixing a catalyst, waste spray paint active carbon with saturated adsorption, corn straws and a solvent, putting the mixture into a high-pressure kettle, and heating and pressurizing the mixture; controlling the reaction temperature at 150-; in the treatment process, the high-pressure kettle is continuously turned over to ensure that the catalyst is uniformly contacted with the waste spray painting active carbon; after the reaction is finished, carrying out solid-liquid separation, calcining the solid obtained by separation after the reaction in a nitrogen atmosphere at 800 ℃ for 1-2h, circularly regenerating the regenerated waste spray painting activated carbon until the weight of the dried waste activated carbon is less than 3-5%, and increasing the measured iodine value by 200-250% to obtain the regenerated spray painting activated carbon; the catalyst is ZnCl 2 、KOH、FeCl 3 One or more of (a).
2. The method for regenerating the waste activated carbon and simultaneously preparing the furfural according to claim 1, wherein: the total concentration of the sulfur-containing gas is 100-500 ppm.
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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000350932A (en) * 1999-06-11 2000-12-19 Daido Steel Co Ltd Regenerating process for used active carbon and treatment process for exhaust gas
CN103143336A (en) * 2011-12-07 2013-06-12 中国中化股份有限公司 Regeneration method of activated carbon catalyst used for preparing glyphosate
CN103551135A (en) * 2013-11-19 2014-02-05 太原理工大学 Regenerative activated carbon as well as preparation method and application thereof
CN106602013A (en) * 2016-12-19 2017-04-26 中国科学院山西煤炭化学研究所 Preparation method of sulfur-active carbon/graphene composite material
KR20170127683A (en) * 2016-05-12 2017-11-22 주식회사 이에스티 Regenerable adsorbent and method for producing same
CN108745328A (en) * 2018-05-28 2018-11-06 上海大学 A kind of New Regenerated method of volatile organic contaminant adsorbent

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Publication number Priority date Publication date Assignee Title
JP2000350932A (en) * 1999-06-11 2000-12-19 Daido Steel Co Ltd Regenerating process for used active carbon and treatment process for exhaust gas
CN103143336A (en) * 2011-12-07 2013-06-12 中国中化股份有限公司 Regeneration method of activated carbon catalyst used for preparing glyphosate
CN103551135A (en) * 2013-11-19 2014-02-05 太原理工大学 Regenerative activated carbon as well as preparation method and application thereof
KR20170127683A (en) * 2016-05-12 2017-11-22 주식회사 이에스티 Regenerable adsorbent and method for producing same
CN106602013A (en) * 2016-12-19 2017-04-26 中国科学院山西煤炭化学研究所 Preparation method of sulfur-active carbon/graphene composite material
CN108745328A (en) * 2018-05-28 2018-11-06 上海大学 A kind of New Regenerated method of volatile organic contaminant adsorbent

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Title
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龚建平等."玉米芯水解制糠醛的废渣制备活性炭新工艺研究".《林产化学与工业》.2010,第30卷(第6期), *

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