CN108114728A - A kind of method that catalytic wet oxidation catalyst is prepared with waste acetic acid - Google Patents

A kind of method that catalytic wet oxidation catalyst is prepared with waste acetic acid Download PDF

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CN108114728A
CN108114728A CN201711465696.5A CN201711465696A CN108114728A CN 108114728 A CN108114728 A CN 108114728A CN 201711465696 A CN201711465696 A CN 201711465696A CN 108114728 A CN108114728 A CN 108114728A
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wet oxidation
acetic acid
oxidation catalyst
catalytic wet
phase material
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CN108114728B (en
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孙鹏
张皓
徐燕
李杨军
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Zhongke Yuenengjing Shandong New Material Co ltd
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Guangdong Guangdong Energy Net Environmental Protection Technology Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J38/00Regeneration or reactivation of catalysts, in general
    • B01J38/48Liquid treating or treating in liquid phase, e.g. dissolved or suspended
    • B01J38/485Impregnating or reimpregnating with, or deposition of metal compounds or catalytically active elements
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/002Mixed oxides other than spinels, e.g. perovskite
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/76Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/84Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/889Manganese, technetium or rhenium
    • B01J23/8892Manganese
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J38/00Regeneration or reactivation of catalysts, in general
    • B01J38/48Liquid treating or treating in liquid phase, e.g. dissolved or suspended
    • B01J38/68Liquid treating or treating in liquid phase, e.g. dissolved or suspended including substantial dissolution or chemical precipitation of a catalyst component in the ultimate reconstitution of the catalyst
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/72Treatment of water, waste water, or sewage by oxidation
    • C02F1/725Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2523/00Constitutive chemical elements of heterogeneous catalysts
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/34Organic compounds containing oxygen
    • C02F2101/345Phenols

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Catalysts (AREA)

Abstract

The invention discloses a kind of methods that catalytic wet oxidation catalyst is prepared using waste acetic acid.This method includes:(1)Waste acetic acid adds in titaniferous solution and is handled, and then obtains liquid phase material A and solid-phase material after filtering;(2)Step(1)Manganese source is added in the liquid phase material A, obtains liquid phase material B;(3)Step(2)The liquid phase material B of gained is added to step with precipitating reagent cocurrent(1)In the solid-phase material of gained, burin-in process is carried out;(4)Step(3)Catalytic wet oxidation catalyst is made through drying, roasting in material and activated carbon, kaolin, adhesive kneading and compacting after the aging of gained.This method is not only able to turn waste into wealth waste acetic acid, and the manufacturing cost of catalytic wet oxidation catalyst can also be made low, functional.

Description

A kind of method that catalytic wet oxidation catalyst is prepared with waste acetic acid
Technical field
The present invention relates to field of waste water treatment and field of catalyst preparation, and in particular to a kind of to use waste acetic acid The method for preparing catalytic wet oxidation catalyst.
Background technology
Catalytic cracking is catalyzed in one of light materialization of heavy oil processing technology that oil plant generally uses and petroleum refining industry The secondary operation technique of agent dosage maximum.With the heaviness and in poor quality of world's crude quality and to clear gusoline demand In the case that amount constantly increase and environmental requirement are increasingly stringent, the replacement rate of catalytic cracking catalyst increases, because heavy metal deposition, Waste acetic acid amount increasingly increases caused by the reasons such as coking.At present, the mode of generally use buried under ground is handled, no Only seriously pollution air, soil and water resource, and also result in the wasting of resources, add entreprise cost.Therefore, how effectively to locate It manages and becomes the emphasis problem currently to receive much attention using waste acetic acid.
Catalytic cracking catalyst be aluminium oxide and silicon oxide series catalyst, generally natural aluminium silicate, synthetic aluminium silicate and Molecular sieve catalyst, also containing a small amount of rare earth oxide.During catalyzed cracking processing, the weight such as Ni, V, Ca in raw material Largely on a catalyst, the carbonaceous material generated during catalytic cracking reaction can also be deposited on catalyst table to deposition to metal Face covers the activated centre of catalyst or activated centre poisoning, catalyst is finally made to lose activity and regenerate and is also unable to reach Requirement becomes dead catalyst.
Have in the prior art and recover waste acetic acid activity using distinct methods, but its is ineffective, such as CN104801353A, CN104841495A, CN104815704A etc. recover catalyst using the methods of being reacted with silicon tetrachloride Activity, but heavy metal removing rate therein is relatively low, so that the activation recovering of catalyst is limited.
It, so can be with if producing the catalyst of good performance of other purposes using waste acetic acid as raw material The problem of environmental pollution brought by dead catalyst is solved, and certain economic benefit can also be created.Therefore, split with useless catalysis It is one of important channel turned waste into wealth to change catalyst as the catalyst that raw material prepares other purposes.
The content of the invention
In order to overcome shortcoming of the prior art, the present invention provides it is a kind of prepared with waste acetic acid it is wet The method of formula catalyst for catalytic oxidation.This method is not only able to turn waste into wealth waste acetic acid, and can also make wet The manufacturing cost of formula catalyst for catalytic oxidation is low, functional.
A kind of method that catalytic wet oxidation catalyst is prepared with waste acetic acid provided by the invention, including:
(1)Waste acetic acid adds in titaniferous solution and is handled, and then obtains liquid phase material A and solid formation after filtering Material;
(2)Step(1)Manganese source is added in the liquid phase material A, obtains liquid phase material B;
(3)Step(2)The liquid phase material B of gained is added to step with precipitating reagent cocurrent(1)In the solid-phase material of gained, aging is carried out Processing;
(4)Step(3)Material and activated carbon, kaolin, adhesive kneading and compacting after the aging of gained, are made through drying, roasting Catalytic wet oxidation catalyst.
In the method for the present invention, waste acetic acid can first pass through pretreatment to remove the oil on catalyst surface And/or carbon distribution.Extraction process, washing method etc. may be employed in the oil removed on catalyst surface.Carbon distribution is removed generally to roast using high temperature Burning method, roasting condition are:Calcination temperature is 500 ~ 900 DEG C, when roasting time is 1 ~ 5 small.
Step(1)The waste acetic acid derives from catalytic cracking unit, and performance has been not achieved former anti- It should require.The waste acetic acid is aluminium oxide and/or silicon oxide series catalyst, generally natural aluminium silicate, conjunction Into alumina silicate and molecular sieve catalyst, the particularly catalytic cracking catalyst containing rare earth.It is former due in catalytic cracking process The metal deposits such as nickel, vanadium in material are in catalytic cracking catalyst, therefore, in waste acetic acid usually contain nickel, vanadium Wait metals.Step(1)In the waste acetic acid final gained is accounted for containing nickel oxide and/or vanadium oxide, total content Less than the 4.0% of catalytic wet oxidation catalyst weight.
Step(1)The titaniferous solution is typically to be prepared by titanium-containing compound dissolving, and titanium-containing compound is selected from sulphur One or more in sour titanium, titanium chloride, Titanium Nitrate.In the titaniferous solution, 0.5~25g/100mL is calculated as with titanium elements, Preferably 1~20g/100mL.Waste acetic acid is added in the condition handled in titaniferous solution is:Processing time For 1 ~ 5 it is small when, treatment temperature be room temperature ~ 60 DEG C.
Step(2)Conventional contain in manganese compound, such as manganese nitrate, manganese chloride, manganese acetate can be used in the manganese source It is one or more.Step(2)The manganese source, which is added in the liquid phase material A, to be made according to actual requirement addition water equal solvent It is fully dissolved, and the manganese source can be separately added into water equal solvent in the liquid phase material A, can also first with water equal solvent After mixing, add in together in the liquid phase material A, to obtain liquid phase material B.
Step(3)Alkaline precipitating agent can be used in the precipitating reagent, it is preferred to use carbonate deposition agent, such as ammonium carbonate, One or more in sodium carbonate, potassium carbonate.Step(3)The reaction condition of the cocurrent reaction controlling is as follows:PH value for 6 ~ 10, temperature is room temperature ~ 80 DEG C.Step(3)The aging condition is as follows:PH is 6.0 ~ 10.0, is preferably 7.0 ~ 9.5, aging When time is 0.5 ~ 5 small, when being preferably 1 ~ 3 small, aging temperature is room temperature ~ 80 DEG C.
In the method for the present invention, through step(3)Step is carried out again after material after aging is preferably washed(4), mode of washing It is known in those skilled in the art, it is therefore an objective to remove heteroion, make the close neutrality of pH value of material.
Step(4)The activated carbon is conventional powdered active carbon, 150 ~ 300 mesh of granularity, specific surface area 500 ~ 3000m2/g.The adhesive is organic binder bond, is preferably hydroxymethyl cellulose, one kind in polyacrylamide or more Kind.
Step(4)The dosage of the activated carbon accounts for the 20% ~ 50% of final gained catalytic wet oxidation catalyst weight, preferably For 30% ~ 40%.The kaolinic dosage accounts for the 1% ~ 15% of final gained catalytic wet oxidation catalyst weight.Described adhesive Total dosage account for the 5% ~ 20% of final gained catalytic wet oxidation catalyst weight.
Step(4)During described kneading and compacting, shaping assistant, such as extrusion aid etc. are added according to actual conditions.
Step(4)The drying condition is as follows:When drying 1 ~ 15 is small at 50 ~ 150 DEG C, conventional drying may be employed Method carries out.The shaping can carry out as needed, generally strip, spherical shape etc., and granularity can determine as needed.
Step(4)In, the roasting carries out under non-oxygen atmosphere, such as the one or more in nitrogen, inert gas. The roasting condition is as follows:Calcination temperature is 500 ~ 750 DEG C, when roasting time is 1 ~ 10 small.
In the method for the present invention, the addition of the waste acetic acid accounts for gained catalytic wet oxidation catalyst weight 20% ~ 50%, be preferably 30% ~ 40%.Step(4)In the catalytic wet oxidation catalyst, it is catalyzed with catalytic wet oxidation On the basis of the weight of agent, the content of manganese oxide is 3% ~ 15%, rare earth metal using the content that oxide is counted as 1% ~ 10%, titanium oxide Content is 1% ~ 15%.
In the method for the present invention, volume can be added using this field conventional technical means in preparation process according to actual needs At least one of outer rare earth metal, the preferred lanthanum of rare earth metal, cerium, such as in step(4)After kneading and compacting, drying, first soak Stain supported rare earth metal is dried again afterwards, calcination process prepares catalytic wet oxidation catalyst.
Wet oxidizing catalyst prepared by the method for the present invention can be used in the processing procedure containing organic wastewater, suitable for controlling Contain high chemical oxygen demand (COD) in the industry such as reason coking, dyestuff, pesticide, printing and dyeing, petrochemical industry, leather or cannot be dropped containing biochemical process The compound of solution(Such as ammonia nitrogen, polycyclic aromatic hydrocarbon)Various industrial organic waste waters.Continuous operation may be employed in treatment of Organic Wastewater Formula reactor can also use intermittently operated formula reactor.During using continuous operation type reactor, fixed bed reaction may be employed Device can also use fluidized-bed reactor.
The catalytic wet oxidation catalyst prepared using the method for the present invention, can be used conventional operating condition and is reacted, By air or oxygen rich gas for exemplified by oxide isolation, specific operating condition is preferably:Reaction temperature is 120 ~ 260 DEG C, reaction Pressure is 0.3 ~ 9.0MPa, and the introduction volume of oxygen is 1~3 times of theoretical requirement needed for waste water complete oxidation, preferably 1.1~ 1.8 times, 0.5 ~ 3.0h of reaction time.During using intermittently operated formula reactor, the dosage of catalyst is given up for 1 ~ 10g catalyst/L Water.
The method of the present invention has the following advantages that:
1st, the method for the present invention can make full use of waste acetic acid that catalytic wet oxidation catalyst is made, and realize useless catalysis Comprehensive utilization of metal and carrier, improves resource utilization in Cracking catalyst, has saved great amount of cost, realizes dead catalyst Turn waste into wealth.
2nd, catalytic wet oxidation catalyst of the invention, using the original vector in waste acetic acid with afterwards adding in The carrier component of activated carbon, kaolin as the catalytic wet oxidation catalyst, by the manganese of rear addition, titanium and useless catalytic cracking The metals such as rare earth metal and nickel, vanadium in catalyst make its mutual cooperation, on the one hand increase the steady of manganese as active metal component It is qualitative, it is made to not easily run off during the reaction, on the other hand improves the activity of catalyst, increases the removal efficiency of organic matter.
Specific embodiment
Technical scheme is described in further detail with reference to embodiment.But implementation described herein Example is only to explain the present invention, the protection domain being not intended to limit the present invention.
The main composition of waste acetic acid used in following embodiment of the present invention and comparative example is as follows by weight:Oxygen SiClx content is 35.8%, and the content of aluminium oxide is 50.9%, and rare earth metal is calculated as 6.0% with oxide, and the content of nickel is 1.3%th, the content of vanadium is 0.4%.
Waste acetic acid used in the embodiment of the present invention and comparative example is by extraction process oil removing and 700 DEG C of high temperature roastings Burn off charcoal is handled.
The granularity of activated carbon used in the embodiment of the present invention and comparative example is 200 mesh, and specific surface area is 2100 m2/g。
Embodiment 1
The preparation process of the present embodiment catalytic wet oxidation catalyst A, it is specific as follows:
(1)Waste acetic acid 100g adds in titanium sulfate solution 200mL(Ti content is 8g/100mL)In, at 46 DEG C Handle 3.5 it is small when, then filter, obtain liquid phase material A and solid-phase material;
(2)Step(1)Manganese nitrate 65g is added in the liquid phase material A and suitable water is uniformly mixed, and obtains liquid phase material B;
(3)Step(2)The liquid phase material B of gained is added to step with sal volatile cocurrent(1)In the solid-phase material of gained, control System pH is 9.0, and reaction temperature is 50 DEG C, carries out aging, aging condition after reaction:PH is 9.0, aging temperature 65 DEG C, when the time is 2.0 small;
(4)Step(3)After the aging of gained material spend after ion-cleaning to neutrality with activated carbon 85g, kaolin 13g, hydroxyl first Base cellulose 16g, kneading and compacting when drying 5 is small at 100 DEG C, are roasted in the presence of nitrogen, when 720 DEG C of roastings 5 are small, Obtain catalytic wet oxidation catalyst A.In the catalytic wet oxidation catalyst A of gained, mainly form as follows by weight:Oxygen Change the content of manganese as 12%, the content of rare-earth oxide is 2.3%, and the content of titanium oxide is 7%, nickel oxide and vanadium oxide Total content is 0.6%.
Embodiment 2
The preparation process of the present embodiment catalytic wet oxidation catalyst B, it is specific as follows:
(1)Waste acetic acid 100g adds in nitric acid titanium solution 210mL(Ti content is 12g/100mL)In, at 40 DEG C Handle 3.0 it is small when, then filter, obtain liquid phase material A and solid-phase material;
(2)Step(1)Manganese nitrate 60g is added in the liquid phase material A and suitable quantity of water is uniformly mixed, and obtains liquid phase material B;
(3)Step(2)The liquid phase material B of gained is added to step with sodium carbonate liquor cocurrent(1)In the solid-phase material of gained, control System pH is 9.5, and reaction temperature is 40 DEG C, carries out aging, aging condition after reaction:PH is 9.5, aging temperature 75 DEG C, when the time is 1.5 small;
(4)Step(3)After the aging of gained material spend after ion-cleaning to neutrality with activated carbon 80g, kaolin 15g, hydroxyl first Base cellulose 19g, kneading and compacting when drying 7 is small at 110 DEG C, are roasted in the presence of nitrogen, when 550 DEG C of roastings 6 are small, Obtain catalytic wet oxidation catalyst B.In the catalytic wet oxidation catalyst B of gained, mainly form as follows by weight:Oxygen Change the content of manganese as 11%, the content of rare-earth oxide is 2.6%, and the content of titanium oxide is 8%, nickel oxide and vanadium oxide Total content is 0.6%.
Embodiment 3
The preparation process of the present embodiment catalytic wet oxidation catalyst C, it is specific as follows:
(1)Waste acetic acid 100g adds in titanium chloride solution 195mL(Ti content is 12g/100mL)In, at 39 DEG C Handle 4.5 it is small when, then filter afterwards, obtain liquid phase material A and solid-phase material;
(2)Step(1)Manganese acetate 58g is added in the liquid phase material A and suitable quantity of water is uniformly mixed, and obtains liquid phase material B;
(3)Step(2)The liquid phase material B of gained is added to step with solution of potassium carbonate cocurrent(1)In the solid-phase material of gained, control System pH is 9.0, and reaction temperature is 62 DEG C, carries out aging, aging condition after reaction:PH is 9.0, reaction temperature 69 DEG C, when the time is 2.5 small;
(4)Step(3)After the aging of gained material spend after ion-cleaning to neutrality with activated carbon 81g, kaolin 16g, hydroxyl first Base cellulose 20g, kneading and compacting when drying 6 is small at 80 DEG C, are roasted in the presence of nitrogen, and 600 DEG C of roastings 6.5 are small When, obtain catalytic wet oxidation catalyst C.In the catalytic wet oxidation catalyst C of gained, mainly form by weight such as Under:The content of manganese oxide is 13%, and the content of rare-earth oxide is 3.0%, and the content of titanium oxide is 9%, nickel oxide and oxidation The total content of vanadium is 0.7%.
Embodiment 4
Catalytic wet oxidation catalyst A, B, C of gained are respectively used to treatment of Organic Wastewater experiment, taken respectively prepared by 20g Catalytic wet oxidation catalyst A, B, C degradation 4L phenolic waste waters, waste water COD 17750mg/L, 167 DEG C of reaction temperature, reaction Stagnation pressure 4.5MPa, reaction 2.0 it is small when after, water outlet COD removal rates are respectively 94.2%, 95.0%, 94.1%, show good urge Change activity.It reuses the catalyst 10 times, to COD removal rates still more than 93%, illustrates having good stability for catalyst.
Comparative example 1
The preparation process of this comparative example catalytic wet oxidation catalyst DA, it is specific as follows:
(1)Waste acetic acid 100g and activated carbon 85g, kaolin 13g, hydroxymethyl cellulose 25g, kneading and compacting, system Into carrier;
(2)Manganese nitrate 65g and suitable quantity of water are made into dipping solution A;
(3)Carrier is immersed in dipping solution A, when drying 5 is small at 100 DEG C, is roasted in the presence of nitrogen, 720 DEG C of roastings 5 Hour, obtain catalytic wet oxidation catalyst DA.In the catalytic wet oxidation catalyst DA of gained, mainly form by weight It is as follows:The content of manganese oxide is 13%, and the content of rare-earth oxide is 2.5%, and the total content of nickel oxide and vanadium oxide is 0.7%。
Comparative example 2
The catalytic wet oxidation catalyst DA of gained for treatment of Organic Wastewater is tested, takes the catalytic wet oxygen prepared by 20g Change catalyst DA degradation 4L phenolic waste waters, waste water COD 17750mg/L, 167 DEG C of reaction temperature reacts stagnation pressure 4.5MPa, instead Answer 2.0 it is small when after, water outlet COD removal rates be 69.7%.Reuse the catalyst 4 times, COD removal rates are substantially reduced 20% with On, illustrate that the stability of catalyst is poor.

Claims (10)

1. a kind of method that catalytic wet oxidation catalyst is prepared with waste acetic acid, including:
(1)Waste acetic acid adds in titaniferous solution and is handled, and then obtains liquid phase material A and solid formation after filtering Material;
(2)Step(1)Manganese source is added in the liquid phase material A, obtains liquid phase material B;
(3)Step(2)The liquid phase material B of gained is added to step with precipitating reagent cocurrent(1)In the solid-phase material of gained, aging is carried out Processing;
(4)Step(3)Material and activated carbon, kaolin, adhesive kneading and compacting after the aging of gained, are made through drying, roasting Catalytic wet oxidation catalyst.
2. according to the method for claim 1, it is characterised in that:Carrying out step(1)Before, waste acetic acid is first By pretreatment to remove the oil and/or carbon distribution on catalyst surface;The oil on catalyst surface is removed using extraction process or is washed Wash method;Carbon distribution is removed using high-temperature roasting method, roasting condition is:Calcination temperature is 500 ~ 900 DEG C, when roasting time is 1 ~ 5 small.
3. according to the method for claim 1, it is characterised in that:Step(1)The addition of the waste acetic acid The 20% ~ 50% of final gained catalytic wet oxidation catalyst weight is accounted for, is preferably 30% ~ 40%;It is further preferably as follows:Step (1)Containing nickel oxide and/or vanadium oxide in the waste acetic acid, total content accounts for final gained catalytic wet oxidation Less than the 4.0% of catalyst weight.
4. according to the method for claim 1, it is characterised in that:Step(1)The titaniferous solution is by titanium-containing compound Dissolving is prepared, and titanium-containing compound is the one or more in titanium sulfate, titanium chloride and Titanium Nitrate;The titaniferous solution In, 0.5~25g/100mL is calculated as with titanium elements, is preferably 1~20g/100mL;It is molten that waste acetic acid is added in into titaniferous The condition handled in liquid is:When processing time is 1 ~ 5 small, treatment temperature is room temperature ~ 60 DEG C.
5. according to the method for claim 1, it is characterised in that:Step(3)The precipitating reagent is alkaline precipitating agent, preferably Using carbonate deposition agent, the further preferably one or more in ammonium carbonate, sodium carbonate, potassium carbonate;Step(3)Described The reaction condition of cocurrent reaction controlling is as follows:PH value is 6 ~ 10, and temperature is room temperature ~ 80 DEG C;Step(3)The aging condition is such as Under:PH is 6.0 ~ 10.0, is preferably 7.0 ~ 9.5, and when ageing time is 0.5 ~ 5 small, when being preferably 1 ~ 3 small, aging temperature is room Temperature ~ 80 DEG C.
6. according to the method for claim 1, it is characterised in that:Step(2)The manganese source is containing manganese compound, is preferably One or more in manganese nitrate, manganese chloride, manganese acetate;Step(4)The activated carbon be powdered active carbon, granularity 150 ~ 300 mesh, 500 ~ 3000m of specific surface area2/g;The adhesive be organic binder bond, be preferably hydroxymethyl cellulose or One or more in polyacrylamide.
7. according to the method for claim 1, it is characterised in that:Step(4)It is wet that the dosage of the activated carbon accounts for final gained The 20% ~ 50% of formula catalyst for catalytic oxidation weight is preferably 30% ~ 40%;The kaolinic dosage accounts for final gained wet type and urges Change the 1% ~ 15% of oxidation catalyst weight;Total dosage of described adhesive accounts for final gained catalytic wet oxidation catalyst weight 5%~20%。
8. according to the method for claim 1, it is characterised in that:Step(4)The drying condition is as follows:At 50 ~ 150 DEG C When lower drying 1 ~ 15 is small;The roasting carries out under non-oxygen atmosphere, and non-oxygen atmosphere is preferably one in nitrogen, inert gas Kind is a variety of;The roasting condition is as follows:Calcination temperature is 500 ~ 750 DEG C, when roasting time is 1 ~ 10 small.
9. according to the method for claim 1, it is characterised in that:In step(4)After kneading and compacting, drying, first dip loading Rare earth metal, the rare earth metal are at least one of lanthanum, cerium, are dried again afterwards, calcination process prepares catalytic wet Oxidation catalyst.
10. according to any methods of claim 1-9, it is characterised in that:Step(4)The catalytic wet oxidation catalysis In agent, on the basis of the weight of catalytic wet oxidation catalyst, the content of manganese oxide is 3% ~ 15%, and rare earth metal is in terms of oxide Content for 1% ~ 10%, the content of titanium oxide is 1% ~ 15%.
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CN109621976A (en) * 2019-02-27 2019-04-16 广东粤能净环保科技有限公司 A kind of catalyst for catalytic oxidation and preparation method thereof
CN109621976B (en) * 2019-02-27 2022-01-25 广东粤能净环保科技有限公司 Catalytic oxidation catalyst and preparation method thereof

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