CN117088367A - Activated carbon for sewage treatment and preparation method thereof - Google Patents
Activated carbon for sewage treatment and preparation method thereof Download PDFInfo
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- CN117088367A CN117088367A CN202311355063.4A CN202311355063A CN117088367A CN 117088367 A CN117088367 A CN 117088367A CN 202311355063 A CN202311355063 A CN 202311355063A CN 117088367 A CN117088367 A CN 117088367A
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- activated carbon
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- sewage treatment
- sodium hydroxide
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 125
- 239000010865 sewage Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 129
- 239000003245 coal Substances 0.000 claims abstract description 64
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 49
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims abstract description 42
- 229920002635 polyurethane Polymers 0.000 claims abstract description 36
- 239000004814 polyurethane Substances 0.000 claims abstract description 36
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims abstract description 32
- 239000002994 raw material Substances 0.000 claims abstract description 32
- 239000008367 deionised water Substances 0.000 claims abstract description 30
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 30
- 238000010438 heat treatment Methods 0.000 claims abstract description 30
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims abstract description 28
- URLKBWYHVLBVBO-UHFFFAOYSA-N Para-Xylene Chemical group CC1=CC=C(C)C=C1 URLKBWYHVLBVBO-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000002156 mixing Methods 0.000 claims abstract description 26
- 239000003223 protective agent Substances 0.000 claims abstract description 24
- 238000003756 stirring Methods 0.000 claims abstract description 24
- FRCHKSNAZZFGCA-UHFFFAOYSA-N 1,1-dichloro-1-fluoroethane Chemical compound CC(F)(Cl)Cl FRCHKSNAZZFGCA-UHFFFAOYSA-N 0.000 claims abstract description 16
- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 claims abstract description 16
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 claims abstract description 16
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims abstract description 16
- TVXBFESIOXBWNM-UHFFFAOYSA-N Xylitol Natural products OCCC(O)C(O)C(O)CCO TVXBFESIOXBWNM-UHFFFAOYSA-N 0.000 claims abstract description 16
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims abstract description 16
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052794 bromium Inorganic materials 0.000 claims abstract description 16
- 239000012975 dibutyltin dilaurate Substances 0.000 claims abstract description 16
- 125000005442 diisocyanate group Chemical group 0.000 claims abstract description 16
- HEBKCHPVOIAQTA-UHFFFAOYSA-N meso ribitol Natural products OCC(O)C(O)C(O)CO HEBKCHPVOIAQTA-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000005056 polyisocyanate Substances 0.000 claims abstract description 16
- 229920001228 polyisocyanate Polymers 0.000 claims abstract description 16
- -1 polymethylene Polymers 0.000 claims abstract description 16
- 229920006389 polyphenyl polymer Polymers 0.000 claims abstract description 16
- 229920005749 polyurethane resin Polymers 0.000 claims abstract description 16
- 229920002545 silicone oil Polymers 0.000 claims abstract description 16
- AVWRKZWQTYIKIY-UHFFFAOYSA-N urea-1-carboxylic acid Chemical compound NC(=O)NC(O)=O AVWRKZWQTYIKIY-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000811 xylitol Substances 0.000 claims abstract description 16
- HEBKCHPVOIAQTA-SCDXWVJYSA-N xylitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)CO HEBKCHPVOIAQTA-SCDXWVJYSA-N 0.000 claims abstract description 16
- 229960002675 xylitol Drugs 0.000 claims abstract description 16
- 235000010447 xylitol Nutrition 0.000 claims abstract description 16
- 238000001816 cooling Methods 0.000 claims abstract description 15
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 14
- TXFOLHZMICYNRM-UHFFFAOYSA-N dichlorophosphoryloxybenzene Chemical compound ClP(Cl)(=O)OC1=CC=CC=C1 TXFOLHZMICYNRM-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000010433 feldspar Substances 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 14
- UKODFQOELJFMII-UHFFFAOYSA-N pentamethyldiethylenetriamine Chemical compound CN(C)CCN(C)CCN(C)C UKODFQOELJFMII-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 14
- 238000010000 carbonizing Methods 0.000 claims abstract description 12
- 238000005187 foaming Methods 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 10
- 239000006260 foam Substances 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims description 36
- 239000002245 particle Substances 0.000 claims description 24
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 21
- 238000003763 carbonization Methods 0.000 claims description 20
- RHZUVFJBSILHOK-UHFFFAOYSA-N anthracen-1-ylmethanolate Chemical compound C1=CC=C2C=C3C(C[O-])=CC=CC3=CC2=C1 RHZUVFJBSILHOK-UHFFFAOYSA-N 0.000 claims description 16
- 239000003830 anthracite Substances 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 16
- 238000001994 activation Methods 0.000 claims description 15
- 230000004913 activation Effects 0.000 claims description 13
- 230000015572 biosynthetic process Effects 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 8
- 238000003825 pressing Methods 0.000 claims description 8
- 238000007873 sieving Methods 0.000 claims description 8
- 238000001125 extrusion Methods 0.000 claims description 7
- 238000003786 synthesis reaction Methods 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims 2
- 239000012190 activator Substances 0.000 claims 1
- 230000003213 activating effect Effects 0.000 abstract description 27
- 238000000748 compression moulding Methods 0.000 abstract description 2
- 230000002194 synthesizing effect Effects 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 8
- 239000003795 chemical substances by application Substances 0.000 description 7
- 239000011148 porous material Substances 0.000 description 6
- 238000001179 sorption measurement Methods 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 5
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 4
- 239000002351 wastewater Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 241000195493 Cryptophyta Species 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 241000195628 Chlorophyta Species 0.000 description 1
- 241000282414 Homo sapiens Species 0.000 description 1
- 229910018540 Si C Inorganic materials 0.000 description 1
- 239000002156 adsorbate Substances 0.000 description 1
- 238000005899 aromatization reaction Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000000149 chemical water pollutant Substances 0.000 description 1
- 238000004332 deodorization Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 244000144972 livestock Species 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000008239 natural water Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
-
- 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
- B01J20/28002—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 physical properties
- B01J20/28011—Other properties, e.g. density, crush strength
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/336—Preparation characterised by gaseous activating agents
-
- 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
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses activated carbon for sewage treatment and a preparation method thereof, and belongs to the technical field of activated carbon preparation. The method comprises the following steps: preparing raw material coal; synthesizing polyurethane resin from p-phenylenediamine, xylitol, diisocyanate, deionized water and allophanate; preparing a protective agent by reacting paraxylene, phenyl dichlorophosphate, cetyltrimethylammonium bromide, chloroform and sodium hydroxide solution; reacting polyurethane solution, sodium hydroxide solution, bromine gas, aluminum chloride and a protective agent to prepare a framework; mixing a framework, monofluoro dichloroethane, triethanolamine and dibutyl tin dilaurate to obtain a component A; mixing feldspar powder, hard foam silicone oil, deionized water, pentamethyldiethylenetriamine and triethylamine, stirring to prepare a component B, mixing and stirring a component A, a component B, polyphenyl polymethylene polyisocyanate and raw material coal, heating and foaming, cooling, demolding, compression molding, drying, pre-carbonizing, carbonizing and activating to obtain the high-capacity high-strength activated carbon.
Description
Technical Field
The invention belongs to the technical field of activated carbon preparation, and particularly relates to activated carbon for sewage treatment and a preparation method thereof.
Background
COD is an index showing how much reducing substances in water are contained in the water under a certain condition, but is mainly organic matters, the quantity of the organic matters in sewage is far more than that of inorganic matters, so the total quantity of the organic matters in sewage is generally represented by COD. With the development of Chinese economy in recent years, the problems faced by sewage treatment are more serious due to the gradual increase of high-concentration ammonia nitrogen wastewater such as tanning wastewater, livestock wastewater, landfill leachate and the like, and the environment and living daily life of human beings are seriously harmed by excessive ammonia nitrogen content and COD in water. If the water with high ammonia nitrogen content is discharged into natural water, algae plants such as blue algae, green algae and the like can grow in a large amount, so that dissolved oxygen in the water is consumed in a large amount, aquatic organisms such as fishes and the like in the water are anoxic and dead, if the COD is too high, almost all organisms except microorganisms can die, the ecological system of the water is destroyed, and further the water is subjected to anaerobic deodorization, so that the water loses the use function, the surrounding environment is further influenced, and therefore, the sewage is very necessary to be treated.
Along with the continuous improvement of environmental protection requirements, the sewage purification problem is more and more concerned, and activated carbon is often used as an adsorbate for sewage purification, but the adsorption capacity of the activated carbon is low, and the adsorption capacity is reduced or even eliminated after the adsorption reaches saturation. If the activated carbon is used continuously, the adsorption effect cannot be achieved, and how to prepare activated carbon with large adsorption capacity becomes a technical problem to be solved at present.
Disclosure of Invention
The invention aims to provide a preparation method of activated carbon for sewage treatment, which comprises the following steps: preparing raw material coal; synthesizing polyurethane resin from p-phenylenediamine, xylitol, diisocyanate, deionized water and allophanate; preparing a protective agent by reacting paraxylene, phenyl dichlorophosphate, cetyltrimethylammonium bromide, chloroform and sodium hydroxide solution; reacting polyurethane solution, sodium hydroxide solution, bromine gas, aluminum chloride and a protective agent to prepare a framework; mixing a framework, monofluoro dichloroethane, triethanolamine and dibutyl tin dilaurate to obtain a component A; mixing feldspar powder, hard foam silicone oil, deionized water, pentamethyldiethylenetriamine and triethylamine, stirring to prepare a component B, mixing and stirring a component A, a component B, polyphenyl polymethylene polyisocyanate and raw material coal, heating and foaming, cooling, demolding, compression molding, drying, pre-carbonizing, carbonizing and activating to obtain the high-capacity high-strength activated carbon.
The invention aims to solve the technical problems: and producing high-capacity high-strength activated carbon.
The aim of the invention can be achieved by the following technical scheme:
an activated carbon for sewage treatment and a preparation method thereof, wherein the preparation of the activated carbon comprises the following steps:
(1) Grinding anthracite, fat coal and sulfonated coal in a vertical mill, and sieving with a 200-mesh sieve to obtain raw material coal;
(2) One-step synthesis of polyurethane resin by p-phenylenediamine, xylitol, diisocyanate, deionized water and allophanate in a double-screw extruder, crushing and dissolving the polyurethane resin in dimethylformamide to prepare polyurethane solution;
(3) Adding paraxylene, phenyl dichlorophosphate, cetyl trimethyl ammonium bromide, chloroform and sodium hydroxide solution into a reaction kettle, and heating at 60 ℃ for reaction for 4-6 hours to prepare a protective agent;
(4) Adding the polyurethane solution, sodium hydroxide solution, bromine gas and aluminum chloride into a reaction kettle, heating at 70 ℃ for reaction for 4-8 hours, adding the protective agent into the reaction kettle, cooling to 0-5 ℃ for reaction for 15-20 hours, and obtaining a framework;
(5) Mixing and stirring the framework, the monofluoro-dichloroethane, the triethanolamine and the dibutyl tin dilaurate uniformly to obtain a component A;
(6) Mixing feldspar powder, hard bubble silicone oil, deionized water, pentamethyldiethylenetriamine and triethylamine, and stirring for 1min at 500-600r/min to obtain a component B;
(7) Mixing the component A, the component B, the polyphenyl polymethylene polyisocyanate and the raw material coal, stirring for 15min, pouring into a mould, heating at 35-45 ℃ for 0.5h for foaming, cooling, and demoulding to obtain a mixture;
(8) Pressing the mixture to form columnar particles, drying, pre-carbonizing the dried columnar particles in a carbonization furnace at 270 ℃ for 2 hours, and gradually heating the temperature in the carbonization furnace from 270 ℃ to 550 ℃ for 40 minutes to carbonize;
(9) And (3) putting the carbonized particles into an activation furnace for activation to obtain the activated carbon.
As a preferable technical scheme of the invention, in the step (1), the mass ratio of the anthracite, the fat coal and the sulfonated coal is 1-2:0.5-0.8:0.2-0.3.
As a preferable technical scheme of the invention, in the step (2), the mass ratio of the p-phenylenediamine, the xylitol, the diisocyanate, the deionized water and the allophanate is 0.1-0.3:1-2:1:10:0.5-0.8; the extrusion temperature of the extruder is 165-240 ℃.
As a preferable technical scheme of the invention, in the step (3), the mass ratio of the paraxylene, the phenyl dichlorophosphate, the cetyltrimethylammonium bromide, the chloroform and the sodium hydroxide solution is 1-2:1-1.5:0.1-0.25:0.8:8-10; the concentration of the sodium hydroxide solution is 1mol/L.
As a preferable technical scheme of the invention, in the step (4), the mass ratio of the polyurethane solution to the sodium hydroxide solution to the bromine gas to the aluminum chloride to the protective agent is 5-8:10-20:1-2:0.1-0.3:2-5; the concentration of the sodium hydroxide solution is 1mol/L.
As a preferable technical scheme of the invention, in the step (5), the mass ratio of the framework, the monofluoro dichloroethane, the triethanolamine and the dibutyl tin dilaurate is 10-15:0.2-0.4:0.3-0.5:4-6.
In the step (6), the mass ratio of feldspar powder, hard foam silicone oil, deionized water, pentamethyldiethylenetriamine and triethylamine is 110:25-45:200-400:1-3:2.54-4.72.
In the step (7), the mass ratio of the component A to the component B to the polyphenyl polymethylene polyisocyanate to the raw material coal is 1-2:1.2-1.8:0.05-0.09:4-6.
As a preferable technical scheme of the invention, in the step (9), the activation refers to the adoption of water vapor as an activating agent, and the activation temperature is controlled to be 750-850 ℃ and maintained for 7-15h.
The activated carbon for sewage treatment prepared by the preparation method is provided.
The invention has the beneficial effects that:
according to the activated carbon for sewage treatment and the preparation method thereof disclosed by the invention, the polyurethane skeleton with high elasticity is prepared, more raw material coal can be fixed and wrapped by the polyurethane skeleton, and pressure is applied to enable the polyurethane skeleton to be tightly embedded into polyurethane, and in the embedding process, the polyurethane skeleton is deformed, and the deformation process enables the raw material coal to be tightly filled in all gaps of the polyurethane skeleton, so that the raw material coal is distributed in the polyurethane more uniformly, and the contact area between the polyurethane skeleton and the raw material coal is effectively increased;
further, the polyurethane-coated raw material coal is adhered to the surface of the activated carbon through an open-network pore structure formed after foaming and solidification of the hard foam silicone oil, and Si-C bonds formed between the hard foam silicone oil and the activated carbon firmly link the pore structure together in the high-temperature carbonization and activation processes of the activated carbon, so that the pore space of the activated carbon is increased;
further, in the carbonization and activation processes of the activated carbon, polyurethane is gradually burned out at high temperature to provide channels for gaps of the activated carbon, so that the formation and expansion of the pores of the activated carbon are promoted, a carbon-containing main chain of the polyurethane is gradually concentrated, and a regular carbon-based structure with condensed rings aromatization is formed, so that the activated carbon has a rich pore structure and a higher specific surface area, the mechanical strength and stability of the activated carbon are enhanced, and the service life of the activated carbon is prolonged;
further, a protective agent is introduced into the main carbon chain of polyurethane to prevent the polyurethane from moving and sliding prematurely, delay the structural damage in the carbonization process, and reduce the rate of decomposing, gasifying and volatilizing to take away the active carbon, thereby improving the carbonization yield, protecting the integrity of the carbon structure and improving the density and strength of the carbon material.
Detailed Description
In order to further describe the technical means and effects adopted by the present invention for achieving the intended purpose, the following detailed description is given below with reference to the embodiments, structures, features and effects according to the present invention.
Example 1
The preparation of the activated carbon comprises the following steps:
(1) Grinding anthracite, fat coal and sulfonated coal in a vertical mill, and sieving with a 200-mesh sieve to obtain raw material coal; the mass ratio of the anthracite, the fat coal and the sulfonated coal is 1:0.5:0.2;
(2) One-step synthesis of polyurethane resin by p-phenylenediamine, xylitol, diisocyanate, deionized water and allophanate in a double-screw extruder, crushing and dissolving the polyurethane resin in dimethylformamide to prepare polyurethane solution; the mass ratio of the p-phenylenediamine, the xylitol, the diisocyanate, the deionized water and the allophanate is 0.1:1:1:10:0.5; the extrusion temperature of the extruder is 165 ℃;
(3) Adding paraxylene, phenyl dichlorophosphate, cetyl trimethyl ammonium bromide, chloroform and sodium hydroxide solution into a reaction kettle, and heating at 60 ℃ for reaction for 4 hours to prepare a protective agent; the mass ratio of the p-xylene, phenyl dichlorophosphate, cetyl trimethyl ammonium bromide, chloroform and sodium hydroxide solution is 1:1:0.1:0.8:8, 8; the concentration of the sodium hydroxide solution is 1mol/L;
(4) Adding the polyurethane solution, sodium hydroxide solution, bromine gas and aluminum chloride into a reaction kettle, heating at 70 ℃ for reaction for 4 hours, adding the protective agent into the reaction kettle, cooling to 0 ℃ for reaction for 15 hours, and obtaining a framework; the mass ratio of the polyurethane solution to the sodium hydroxide solution to the bromine gas to the aluminum chloride to the protective agent is 5:10:1:0.1:2; the concentration of the sodium hydroxide solution is 1mol/L;
(5) Mixing and stirring the framework, the monofluoro-dichloroethane, the triethanolamine and the dibutyl tin dilaurate uniformly to obtain a component A; the mass ratio of the framework to the monofluoro dichloroethane to the triethanolamine to the dibutyl tin dilaurate is 10:0.2:0.3:4, a step of;
(6) Mixing feldspar powder, hard bubble silicone oil, deionized water, pentamethyldiethylenetriamine and triethylamine, and stirring for 1min at 500r/min to obtain a component B, wherein the mass ratio of the feldspar powder to the hard bubble silicone oil to the deionized water to the pentamethyldiethylenetriamine to the triethylamine is 110:25:200:1:2.54;
(7) Mixing the component A, the component B, the polyphenyl polymethylene polyisocyanate and the raw material coal, stirring for 15min, pouring into a mould, heating at 35 ℃ for 0.5h for foaming, cooling, and demoulding to obtain a mixture; the mass ratio of the component A to the component B to the polyphenyl polymethylene polyisocyanate to the raw material coal is 1:1.2:0.05:4, a step of;
(8) Pressing the mixture to form columnar particles, drying, pre-carbonizing the dried columnar particles in a carbonization furnace at 270 ℃ for 2 hours, and gradually heating the temperature in the carbonization furnace from 270 ℃ to 550 ℃ for 40 minutes to carbonize;
(9) And (3) putting the carbonized particles into an activating furnace for activating, adopting water vapor as an activating agent, controlling the activating temperature to be 750 ℃, and keeping for 7 hours to obtain the activated carbon.
Example 2
The preparation of the activated carbon comprises the following steps:
(1) Grinding anthracite, fat coal and sulfonated coal in a vertical mill, and sieving with a 200-mesh sieve to obtain raw material coal; the mass ratio of the anthracite, the fat coal and the sulfonated coal is 1.5:0.7:0.25;
(2) One-step synthesis of polyurethane resin by p-phenylenediamine, xylitol, diisocyanate, deionized water and allophanate in a double-screw extruder, crushing and dissolving the polyurethane resin in dimethylformamide to prepare polyurethane solution; the mass ratio of the p-phenylenediamine, the xylitol, the diisocyanate, the deionized water and the allophanate is 0.2:1.5:1:10:0.7; the extrusion temperature of the extruder is 200 ℃;
(3) Adding paraxylene, phenyl dichlorophosphate, cetyl trimethyl ammonium bromide, chloroform and sodium hydroxide solution into a reaction kettle, and heating at 60 ℃ for reaction for 5 hours to prepare a protective agent; the mass ratio of the p-xylene, phenyl dichlorophosphate, cetyl trimethyl ammonium bromide, chloroform and sodium hydroxide solution is 1.5:1.2:0.2:0.8:9, a step of performing the process; the concentration of the sodium hydroxide solution is 1mol/L;
(4) Adding the polyurethane solution, sodium hydroxide solution, bromine gas and aluminum chloride into a reaction kettle, heating at 70 ℃ for reaction for 6 hours, adding the protective agent into the reaction kettle, cooling to 2.5 ℃ and reacting for 17 hours to obtain a framework; the mass ratio of the polyurethane solution to the sodium hydroxide solution to the bromine gas to the aluminum chloride to the protective agent is 7:15:1.5:0.2:3.5; the concentration of the sodium hydroxide solution is 1mol/L;
(5) Mixing and stirring the framework, the monofluoro-dichloroethane, the triethanolamine and the dibutyl tin dilaurate uniformly to obtain a component A; the mass ratio of the framework to the monofluoro dichloroethane to the triethanolamine to the dibutyl tin dilaurate is 13:0.3:0.4:5, a step of;
(6) Mixing feldspar powder, hard bubble silicone oil, deionized water, pentamethyldiethylenetriamine and triethylamine, and stirring for 1min at 550r/min to obtain a component B, wherein the mass ratio of the feldspar powder to the hard bubble silicone oil to the deionized water to the pentamethyldiethylenetriamine to the triethylamine is 110:35:300:2:3.5;
(7) Mixing the component A, the component B, the polyphenyl polymethylene polyisocyanate and the raw material coal, stirring for 15min, pouring into a mould, heating at 37 ℃ for 0.5h for foaming, cooling, and demoulding to obtain a mixture; the mass ratio of the component A to the component B to the polyphenyl polymethylene polyisocyanate to the raw material coal is 1.5:1.5:0.07:5, a step of;
(8) Pressing the mixture to form columnar particles, drying, pre-carbonizing the dried columnar particles in a carbonization furnace at 270 ℃ for 2 hours, and gradually heating the temperature in the carbonization furnace from 270 ℃ to 550 ℃ for 40 minutes to carbonize;
(9) And (3) putting the carbonized particles into an activating furnace for activation, adopting water vapor as an activating agent, controlling the activating temperature to be 800 ℃, and keeping the activating temperature for 10 hours to obtain the activated carbon.
Example 3
The preparation of the activated carbon comprises the following steps:
(1) Grinding anthracite, fat coal and sulfonated coal in a vertical mill, and sieving with a 200-mesh sieve to obtain raw material coal; the mass ratio of the anthracite, the fat coal and the sulfonated coal is 2:0.8:0.3;
(2) One-step synthesis of polyurethane resin by p-phenylenediamine, xylitol, diisocyanate, deionized water and allophanate in a double-screw extruder, crushing and dissolving the polyurethane resin in dimethylformamide to prepare polyurethane solution; the mass ratio of the p-phenylenediamine, the xylitol, the diisocyanate, the deionized water and the allophanate is 0.3:2:1:10:0.8; the extrusion temperature of the extruder is 240 ℃;
(3) Adding paraxylene, phenyl dichlorophosphate, cetyl trimethyl ammonium bromide, chloroform and sodium hydroxide solution into a reaction kettle, and heating at 60 ℃ for reaction for 6 hours to prepare a protective agent; the mass ratio of the p-xylene, phenyl dichlorophosphate, cetyl trimethyl ammonium bromide, chloroform and sodium hydroxide solution is 2:1.5:0.25:0.8:10; the concentration of the sodium hydroxide solution is 1mol/L;
(4) Adding the polyurethane solution, sodium hydroxide solution, bromine gas and aluminum chloride into a reaction kettle, heating at 70 ℃ for reaction for 8 hours, adding the protective agent into the reaction kettle, cooling to 5 ℃ for reaction for 20 hours, and obtaining a framework; the mass ratio of the polyurethane solution to the sodium hydroxide solution to the bromine gas to the aluminum chloride to the protective agent is 8:20:2:0.3:5, a step of; the concentration of the sodium hydroxide solution is 1mol/L;
(5) Mixing and stirring the framework, the monofluoro-dichloroethane, the triethanolamine and the dibutyl tin dilaurate uniformly to obtain a component A; the mass ratio of the framework to the monofluoro dichloroethane to the triethanolamine to the dibutyl tin dilaurate is 15:0.4:0.5:6, preparing a base material;
(6) Mixing feldspar powder, hard bubble silicone oil, deionized water, pentamethyldiethylenetriamine and triethylamine, and stirring for 1min at 600r/min to obtain a component B, wherein the mass ratio of the feldspar powder to the hard bubble silicone oil to the deionized water to the pentamethyldiethylenetriamine to the triethylamine is 110:45:400:3:4.72;
(7) Mixing the component A, the component B, the polyphenyl polymethylene polyisocyanate and the raw material coal, stirring for 15min, pouring into a mould, heating at 45 ℃ for 0.5h for foaming, cooling, and demoulding to obtain a mixture; the mass ratio of the component A to the component B to the polyphenyl polymethylene polyisocyanate to the raw material coal is 2:1.8:0.09:6, preparing a base material;
(8) Pressing the mixture to form columnar particles, drying, pre-carbonizing the dried columnar particles in a carbonization furnace at 270 ℃ for 2 hours, and gradually heating the temperature in the carbonization furnace from 270 ℃ to 550 ℃ for 40 minutes to carbonize;
(9) And (3) putting the carbonized particles into an activating furnace for activation, adopting water vapor as an activating agent, controlling the activating temperature at 850 ℃, and keeping the activating temperature for 15 hours to obtain the activated carbon.
Comparative example 1
The preparation of the activated carbon comprises the following steps:
(1) Grinding anthracite, fat coal and sulfonated coal in a vertical mill, and sieving with a 200-mesh sieve to obtain raw material coal; the mass ratio of the anthracite, the fat coal and the sulfonated coal is 1.5:0.7:0.25;
(2) Pressing and forming the raw material coal to prepare columnar particles, drying, pre-carbonizing the dried columnar particles in a carbonization furnace at 270 ℃ for 2 hours, and gradually heating the temperature in the carbonization furnace from 270 ℃ to 550 ℃ for 40 minutes to carbonize;
(3) And (3) putting the carbonized particles into an activating furnace for activation, adopting water vapor as an activating agent, controlling the activating temperature to be 800 ℃, and keeping the activating temperature for 10 hours to obtain the activated carbon.
Comparative example 2
The preparation of the activated carbon comprises the following steps:
(1) Grinding anthracite, fat coal and sulfonated coal in a vertical mill, and sieving with a 200-mesh sieve to obtain raw material coal; the mass ratio of the anthracite, the fat coal and the sulfonated coal is 1.5:0.7:0.25;
(2) One-step synthesis of polyurethane resin by p-phenylenediamine, xylitol, diisocyanate, deionized water and allophanate in a double-screw extruder, crushing and dissolving the polyurethane resin in dimethylformamide to prepare polyurethane solution; the mass ratio of the p-phenylenediamine, the xylitol, the diisocyanate, the deionized water and the allophanate is 0.2:1.5:1:10:0.7; the extrusion temperature of the extruder is 200 ℃;
(3) Adding paraxylene, phenyl dichlorophosphate, cetyl trimethyl ammonium bromide, chloroform and sodium hydroxide solution into a reaction kettle, and heating at 60 ℃ for reaction for 5 hours to prepare a protective agent; the mass ratio of the p-xylene, phenyl dichlorophosphate, cetyl trimethyl ammonium bromide, chloroform and sodium hydroxide solution is 1.5:1.2:0.2:0.8:9, a step of performing the process; the concentration of the sodium hydroxide solution is 1mol/L;
(4) Adding the polyurethane solution, sodium hydroxide solution, bromine gas and aluminum chloride into a reaction kettle, heating at 70 ℃ for reaction for 6 hours, adding the protective agent into the reaction kettle, cooling to 2.5 ℃ and reacting for 17 hours to obtain a framework; the mass ratio of the polyurethane solution to the sodium hydroxide solution to the bromine gas to the aluminum chloride to the protective agent is 7:15:1.5:0.2:3.5; the concentration of the sodium hydroxide solution is 1mol/L;
(5) Mixing and stirring the framework, the monofluoro-dichloroethane, the triethanolamine and the dibutyl tin dilaurate uniformly to obtain a component A; the mass ratio of the framework to the monofluoro dichloroethane to the triethanolamine to the dibutyl tin dilaurate is 13:0.3:0.4:5, a step of;
(6) Mixing and stirring the component A, the polyphenyl polymethylene polyisocyanate and the raw material coal for 15min, pouring the mixture into a mould, heating the mixture at 37 ℃ for 0.5h for foaming, cooling and demoulding to obtain a mixture; the mass ratio of the component A to the polyphenyl polymethylene polyisocyanate to the raw material coal is 1.5:0.07:5, a step of;
(7) Pressing the mixture to form columnar particles, drying, pre-carbonizing the dried columnar particles in a carbonization furnace at 270 ℃ for 2 hours, and gradually heating the temperature in the carbonization furnace from 270 ℃ to 550 ℃ for 40 minutes to carbonize;
(8) And (3) putting the carbonized particles into an activating furnace for activation, adopting water vapor as an activating agent, controlling the activating temperature to be 800 ℃, and keeping the activating temperature for 10 hours to obtain the activated carbon.
Comparative example 3
The preparation of the activated carbon comprises the following steps:
(1) Grinding anthracite, fat coal and sulfonated coal in a vertical mill, and sieving with a 200-mesh sieve to obtain raw material coal; the mass ratio of the anthracite, the fat coal and the sulfonated coal is 1.5:0.7:0.25;
(2) One-step synthesis of polyurethane resin by p-phenylenediamine, xylitol, diisocyanate, deionized water and allophanate in a double-screw extruder, crushing and dissolving the polyurethane resin in dimethylformamide to prepare polyurethane solution; the mass ratio of the p-phenylenediamine, the xylitol, the diisocyanate, the deionized water and the allophanate is 0.2:1.5:1:10:0.7; the extrusion temperature is 200 ℃;
(3) Adding the polyurethane solution, sodium hydroxide solution, bromine gas and aluminum chloride into a reaction kettle, and heating at 70 ℃ for reaction for 6 hours to obtain a framework; the mass ratio of the polyurethane solution to the sodium hydroxide solution to the bromine gas to the aluminum chloride is 7:15:1.5:0.2; the concentration of the sodium hydroxide solution is 1mol/L;
(4) Mixing and stirring the framework, the monofluoro-dichloroethane, the triethanolamine and the dibutyl tin dilaurate uniformly to obtain a component A; the mass ratio of the framework to the monofluoro dichloroethane to the triethanolamine to the dibutyl tin dilaurate is 13:0.3:0.4:5, a step of;
(5) Mixing feldspar powder, hard bubble silicone oil, deionized water, pentamethyldiethylenetriamine and triethylamine, and stirring for 1min at 550r/min to obtain a component B, wherein the mass ratio of the feldspar powder to the hard bubble silicone oil to the deionized water to the pentamethyldiethylenetriamine to the triethylamine is 110:35:300:2:3.5;
(6) Mixing the component A, the component B, the polyphenyl polymethylene polyisocyanate and the raw material coal, stirring for 15min, pouring into a mould, heating at 37 ℃ for 0.5h for foaming, cooling, and demoulding to obtain a mixture; the mass ratio of the component A to the component B to the polyphenyl polymethylene polyisocyanate to the raw material coal is 1.5:1.5:0.07:5, a step of;
(7) Pressing the mixture to form columnar particles, drying, pre-carbonizing the dried columnar particles in a carbonization furnace at 270 ℃ for 2 hours, and gradually heating the temperature in the carbonization furnace from 270 ℃ to 550 ℃ for 40 minutes to carbonize;
(8) And (3) putting the carbonized particles into an activating furnace for activation, adopting water vapor as an activating agent, controlling the activating temperature to be 800 ℃, and keeping the activating temperature for 10 hours to obtain the activated carbon.
Performance testing
The sewage sampled on the same day is treated by the active carbon finished products prepared in the examples 1-3 and the comparative examples 1-3 prepared on the basis of the example 2 according to the standard of putting 2g of active carbon finished product into each liter of sewage; according to the test method specified in the water and wastewater monitoring and analyzing method (fourth edition), an ultraviolet-visible spectrophotometer with the model number Q-6 of Shanghai Yuan analytical instruments, inc. is adopted to respectively detect COD and ammonia nitrogen of the water samples of the sewage treated in the examples 1-3 and the comparative examples 1-3, so as to obtain the corresponding removal rate;
the pore volume and specific surface area of the prepared activated carbon are tested according to GB/T7702.20-2008;
the strength of the prepared activated carbon is tested according to GB/T7703-2008;
the results are shown in Table 1 below:
TABLE 1
As can be seen from Table 1, the activated carbon obtained in comparative example 1 is a conventional activated carbon, and each performance is significantly inferior to that of example 2; the activated carbon produced in comparative example 2 was inferior in foaming, resulting in a decrease in the adsorption performance of the produced activated carbon; the activated carbon produced in comparative example 3 was reduced in strength due to the fact that no protective agent was introduced.
The present invention is not limited to the above embodiments, but is capable of modification and variation in detail, and other modifications and variations can be made by those skilled in the art without departing from the scope of the present invention.
Claims (10)
1. The preparation method of the activated carbon for sewage treatment is characterized by comprising the following steps of:
(1) Grinding anthracite, fat coal and sulfonated coal in a vertical mill, and sieving with a 200-mesh sieve to obtain raw material coal;
(2) One-step synthesis of polyurethane resin by p-phenylenediamine, xylitol, diisocyanate, deionized water and allophanate in a double-screw extruder, crushing and dissolving the polyurethane resin in dimethylformamide to prepare polyurethane solution;
(3) Adding paraxylene, phenyl dichlorophosphate, cetyl trimethyl ammonium bromide, chloroform and sodium hydroxide solution into a reaction kettle, and heating at 60 ℃ for reaction for 4-6 hours to prepare a protective agent;
(4) Adding the polyurethane solution, sodium hydroxide solution, bromine gas and aluminum chloride into a reaction kettle, heating at 70 ℃ for reaction for 4-8 hours, adding the protective agent into the reaction kettle, cooling to 0-5 ℃ for reaction for 15-20 hours, and obtaining a framework;
(5) Mixing and stirring the framework, the monofluoro-dichloroethane, the triethanolamine and the dibutyl tin dilaurate uniformly to obtain a component A;
(6) Mixing feldspar powder, hard bubble silicone oil, deionized water, pentamethyldiethylenetriamine and triethylamine, and stirring for 1min at 500-600r/min to obtain a component B;
(7) Mixing the component A, the component B, the polyphenyl polymethylene polyisocyanate and the raw material coal, stirring for 15min, pouring into a mould, heating at 35-45 ℃ for 0.5h for foaming, cooling, and demoulding to obtain a mixture;
(8) Pressing the mixture to form columnar particles, drying, pre-carbonizing the dried columnar particles in a carbonization furnace at 270 ℃ for 2 hours, and gradually heating the temperature in the carbonization furnace from 270 ℃ to 550 ℃ for 40 minutes to carbonize;
(9) And (3) putting the carbonized particles into an activation furnace for activation to obtain the activated carbon.
2. The method for preparing activated carbon for sewage treatment according to claim 1, wherein in the step (1), the mass ratio of anthracite, fat coal and sulfonated coal is 1-2:0.5-0.8:0.2-0.3.
3. The method for preparing activated carbon for sewage treatment according to claim 1, wherein in the step (2), the mass ratio of p-phenylenediamine, xylitol, diisocyanate, deionized water and allophanate is 0.1-0.3:1-2:1:10:0.5-0.8; the extrusion temperature of the extruder is 165-240 ℃.
4. The method for preparing activated carbon for sewage treatment according to claim 1, wherein in the step (3), the mass ratio of the p-xylene, phenyl dichlorophosphate, cetyltrimethylammonium bromide, chloroform and sodium hydroxide solution is 1-2:1-1.5:0.1-0.25:0.8:8-10; the concentration of the sodium hydroxide solution is 1mol/L.
5. The method for preparing activated carbon for sewage treatment according to claim 1, wherein in the step (4), the mass ratio of the polyurethane solution to the sodium hydroxide solution to the bromine gas to the aluminum chloride to the protective agent is 5-8:10-20:1-2:0.1-0.3:2-5; the concentration of the sodium hydroxide solution is 1mol/L.
6. The method for preparing activated carbon for sewage treatment according to claim 1, wherein in the step (5), the mass ratio of the skeleton to the monofluoro dichloroethane to the triethanolamine to the dibutyl tin dilaurate is 10-15:0.2-0.4:0.3-0.5:4-6.
7. The method for preparing activated carbon for sewage treatment according to claim 1, wherein in the step (6), the mass ratio of feldspar powder, hard foam silicone oil, deionized water, pentamethyldiethylenetriamine and triethylamine is 110:25-45:200-400:1-3:2.54-4.72.
8. The method for preparing activated carbon for sewage treatment according to claim 1, wherein in the step (7), the mass ratio of the component a, the component B, the polyphenyl polymethylene polyisocyanate and the raw material coal is 1-2:1.2-1.8:0.05-0.09:4-6.
9. The method for producing activated carbon for sewage treatment according to claim 1, wherein in the step (9), the activation means that water vapor is used as an activator, and the activation temperature is controlled to be 750-850 ℃ and maintained for 7-15 hours.
10. An activated carbon for sewage treatment produced by the production process according to any one of claims 1 to 9.
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