CN111013571A - Preparation method of modified ozone catalyst suitable for high-salinity wastewater in coal chemical industry - Google Patents

Preparation method of modified ozone catalyst suitable for high-salinity wastewater in coal chemical industry Download PDF

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CN111013571A
CN111013571A CN201911181406.3A CN201911181406A CN111013571A CN 111013571 A CN111013571 A CN 111013571A CN 201911181406 A CN201911181406 A CN 201911181406A CN 111013571 A CN111013571 A CN 111013571A
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ozone catalyst
preparation
modified
chemical industry
salinity wastewater
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王吉坤
杜松
牟子申
黄荣法
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Pingxiang Coal Science Environmental Protection Technology Co ltd
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Pingxiang Coal Science Environmental Protection Technology 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
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/32—Manganese, technetium or rhenium
    • B01J23/34—Manganese
    • 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
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/002—Mixed oxides other than spinels, e.g. perovskite
    • 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
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
    • B01J37/0018—Addition of a binding agent or of material, later completely removed among others as result of heat treatment, leaching or washing,(e.g. forming of pores; protective layer, desintegrating by heat)
    • 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
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02—Impregnation, coating or precipitation
    • B01J37/0201—Impregnation
    • B01J37/0203—Impregnation the impregnation liquid containing organic compounds
    • 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
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/08—Heat treatment
    • B01J37/082—Decomposition and pyrolysis
    • 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
    • C02F1/72—Treatment of water, waste water, or sewage by oxidation
    • C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
    • 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
    • C02F1/72—Treatment of water, waste water, or sewage by oxidation
    • C02F1/78—Treatment of water, waste water, or sewage by oxidation with ozone
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2209/00—Controlling or monitoring parameters in water treatment
    • C02F2209/08—Chemical Oxygen Demand [COD]; Biological Oxygen Demand [BOD]
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2305/00—Use of specific compounds during water treatment
    • C02F2305/02—Specific form of oxidant
    • C02F2305/023—Reactive oxygen species, singlet oxygen, OH radical

Abstract

A preparation method of a modified ozone catalyst suitable for high-salinity wastewater in coal chemical industry overcomes the defect of low efficiency of removing COD in the high-salinity wastewater by using the ozone catalyst in the prior art, and provides a preparation method of the modified ozone catalyst suitable for the high-salinity wastewater in coal chemical industry for adapting to different production processes and application environments, wherein the method is based on a preparation method of an ozone catalyst formed by roasting, and comprises the following steps: soaking the roasted and molded ozone catalyst in a non-polar reagent for 12-24h, and then filtering; and drying and roasting the filtered ozone catalyst to obtain the modified ozone catalyst. The surface of the modified ozone catalyst is loaded with the non-polar reagent, and in an ozone oxidation experiment, the modified ozone catalyst can specifically attract heterocyclic compounds to the surface of the catalyst to perform an oxidation reaction with hydroxyl radicals, and is particularly suitable for removing COD (chemical oxygen demand) of waste water with complex and turbid water quality.

Description

Preparation method of modified ozone catalyst suitable for high-salinity wastewater in coal chemical industry
Technical Field
The invention relates to the field of preparation of modified ozone catalysts, in particular to a preparation method of a modified ozone catalyst suitable for high-salinity wastewater in coal chemical industry.
Background
The modern coal chemical industry is an important way for realizing clean and efficient utilization of coal, but coal chemical industry enterprises are mostly in northwest areas with more coal and less water, local ecology is fragile, environmental bearing capacity is poor, no sewage containing body is provided, and zero discharge of waste water is required. The treatment of high-concentration brine is a bottleneck problem which restricts the zero discharge of waste water. The high-concentration brine is mainly derived from concentrated water generated by a reverse osmosis device and a heat concentration device, the Total Dissolved Solids (TDS) content reaches more than 10g/L, COD is generally 300-500 mg/L or higher, and as the COD content is high, regenerated salt obtained by crystallization of the high-concentration brine cannot be recycled as dangerous waste, the key technology for efficiently removing COD by catalytic oxidation of the high-concentration brine is urgently needed to be developed; however, COD in high-salinity water is mostly a heterocyclic compound which is difficult to degrade. Therefore, the key point for effectively reducing COD in the wastewater lies in the efficient oxidation removal of heterocyclic compounds in the water.
According to the running condition of the existing ozone catalytic oxidation technology, the ozone catalyst has poor effect of removing organic matters in the high-salinity wastewater in the coal chemical industry, and COD is even lower than 30%. The analysis reasons are mainly as follows: because the high-salinity wastewater has complex components and high contents of turbidity, suspended matters and the like, a path for a heterocyclic compound to enter an ozone catalyst pore channel is blocked, the contact probability and the contact time of the heterocyclic compound in the high-salinity wastewater and hydroxyl radicals on the surface of an ozone catalyst are influenced, and the COD removal efficiency of the hydroxyl radicals is influenced.
Patent CN 106732792B proposes a catalyst for treating high-salt wastewater in coal chemical industry and a preparation method thereof, wherein the calcined catalyst is subjected to hydrophobic modification, so as to reduce salt ions in high-salt water occupying active sites and prevent the salt ions from contacting catalyst pore channels to indirectly improve the removal rate of COD by an ozone catalyst. Patent CN106881090B proposes a method for modifying an ozone catalytic oxidation catalyst, in which a calcined catalyst is immersed in a hydroxylation reagent, in order to increase the number of hydroxyl radicals and further increase the removal efficiency of the ozone catalyst on COD.
In order to improve the efficiency of removing COD in high-salinity wastewater by using the ozone catalyst, the invention provides a new solution to adapt to different production processes and application environments.
Disclosure of Invention
The invention overcomes the defect of low efficiency of removing COD in high-salinity wastewater by using an ozone catalyst in the prior art, and provides a preparation method of a modified ozone catalyst suitable for high-salinity wastewater in coal chemical industry for adapting to different production processes and application environments.
The technical scheme adopted for realizing the aim of the invention is as follows: a preparation method of a modified ozone catalyst suitable for high-salinity wastewater in coal chemical industry is obtained based on a roasted and formed ozone catalyst, and comprises the following steps: step A, soaking a roasted and molded ozone catalyst in a non-polar reagent for 12-24 hours, and then filtering; and step B, drying and roasting the ozone catalyst obtained by filtering in the step A to obtain the modified ozone catalyst.
Further, the impregnation temperature of the ozone catalyst formed by roasting in the step A and the nonpolar reagent is 20-70 ℃.
Further, the volume ratio of the baked and molded ozone catalyst to the nonpolar reagent in the step A is 1: 1-1: 10.
Further, the nonpolar reagent in the step A is any one of dichloromethane, chloroform, carbon tetrachloride, acetone, tributylamine, trioctylamine, benzene, petroleum ether and cyclohexane.
Further, the drying temperature of the ozone catalyst washed in the step B is 50-100 ℃, and the drying time is 10-30 h.
Further, the roasting conditions of the ozone catalyst dried in the step B are as follows: the muffle furnace adopts programmed heating, the heating rate is 2.5-5.5 ℃/min, the temperature is 600 ℃ to 500 ℃, and the roasting time is 3-6 h.
Further, the raw materials of the calcined and molded ozone catalyst comprise: an ozone catalyst carrier and an active component solution; the ozone catalyst carrier is one of alumina, activated carbon and ceramsite; the active component solution is a solution containing any one or more ions of manganese, iron, cobalt, nickel, magnesium, zinc, copper and the like.
Furthermore, the preparation method of the baked and molded ozone catalyst is one of a mixing method, an impregnation method and a coprecipitation method.
The invention has the beneficial effects that: (1) the surface of the modified ozone catalyst obtained by the preparation method of the invention is loaded with the nonpolar reagent, and in an ozone catalysis experiment, the modified ozone catalyst can attract the heterocyclic compound to the surface of the catalyst in a specific way to perform an oxidation reaction with the hydroxyl radical, so that the phenomenon that the heterocyclic compound cannot be directly contacted with the surface of the catalyst and further cannot be effectively directly contacted with the hydroxyl radical to perform an oxidation reaction due to the fact that a large amount of impurities such as salt ions and the like are attached to the surface of the unmodified catalyst except the heterocyclic compound is avoided.
(2) In an ozone oxidation experiment, the modified ozone catalyst prepared by the invention opens a green channel for a heterocyclic compound in wastewater to enter a catalyst pore channel, and realizes zero-distance contact of the heterocyclic compound and the catalyst, so that the catalytic performance of the ozone catalyst cannot be directly influenced by the types and contents of other impurities in the wastewater, and the ozone catalyst prepared by the invention is particularly suitable for wastewater with complex and turbid water quality.
The invention is further described below by means of specific embodiments.
Detailed Description
Argil and aluminum trioxide are respectively used as carriers, and an ozone catalyst is prepared by adopting a mixing-roasting process to obtain a sample 1 and a sample 2.
Sample 1
The preparation steps are as follows: the preparation method comprises the steps of taking argil as a carrier and manganese nitrate as an active component precursor, mixing the manganese nitrate, the argil, polyethylene glycol and an alumina sol adhesive according to the mass ratio of 20:70:5:5, adding the mixture into a ball forming machine to prepare a catalyst forming ball body with the diameter of 3-6mm, and then placing the catalyst forming ball body in a muffle furnace to be roasted for 4 hours at the temperature of 550 ℃ to obtain the target catalyst.
Sample 2
The preparation steps are as follows: the method comprises the steps of taking aluminum trioxide as a carrier, taking manganese nitrate as an active component precursor, impregnating the carrier and the active component according to the volume ratio of 1:1, wherein the loading amount of the manganese nitrate is 10%, the impregnating time is 12h, then drying the carrier in an oven at 100 ℃ for 10h, and finally roasting the carrier in a muffle furnace at 550 ℃ for 4h to obtain the target catalyst.
Dichloromethane and trioctylamine are respectively used as modifying reagents, and the sample 1 is modified by the preparation method to obtain a comparative sample 1 and a comparative sample 2.
Comparative sample 1
The preparation steps are as follows: soaking the sample 1 and a dichloromethane solution for 12 hours according to the volume ratio of 1:2.5, filtering, placing in an oven, drying at 50-80 ℃ for 24 hours, and finally placing in a muffle furnace, and roasting at 550 ℃ for 4 hours to obtain the modified ozone catalyst.
Comparative sample 2
The preparation steps are as follows: soaking the sample 1 and trioctylamine solution according to the volume ratio of 1:3 for 12h, filtering, placing in an oven, drying at 50-80 ℃ for 24h, and finally placing in a muffle furnace, and roasting at 550 ℃ for 4h to obtain the modified ozone catalyst.
Dichloromethane and carbon tetrachloride are respectively used as modifying reagents, and the sample 2 is modified by the preparation method of the modified ozone catalyst to obtain a comparative sample 3 and a comparative sample 4.
Comparative sample 3
The preparation steps are as follows: soaking a comparative sample 2 and a dichloromethane solution for 12 hours according to the volume ratio of 1:2.5, filtering, placing in an oven, drying at 50-80 ℃ for 24 hours, and finally placing in a muffle furnace, and roasting at 550 ℃ for 4 hours to obtain the modified ozone catalyst.
Comparative sample 4
The preparation steps are as follows: soaking a comparative sample 2 and a carbon tetrachloride solution for 12 hours according to the volume ratio of 1:5, filtering, placing in an oven, drying at 50-80 ℃ for 24 hours, and finally placing in a muffle furnace, and roasting at 550 ℃ for 4 hours to obtain the modified ozone catalyst.
The catalytic effect of the sample prepared above was evaluated by the following experiment: adopt laboratory ozone oxidation reaction column to handle the coal chemical industry high salt waste water that TDS is 60000mg/L, COD is 850mg/L, and the experimental condition is: the ozone concentration is 100mg/L, the ozone adding amount is 350mg/L, the reaction time is 2h, and then sampling is carried out to detect COD.
Figure BDA0002291372220000051
The above table was analyzed: the COD removal rates of sample 1, comparative sample 1 and comparative sample 2 were: 32%, 39.1% and 40%; the COD removal rates for sample 2, comparative sample 3 and comparative sample 4 were 38%, 47.5% and 48%, respectively, and the comparison found: the removal rate of COD of the modified ozone catalyst obtained by impregnating the catalyst with a nonpolar reagent is higher than that of the unmodified ozone catalyst.

Claims (8)

1. A preparation method of a modified ozone catalyst suitable for high-salinity wastewater in coal chemical industry is a preparation method of an ozone catalyst based on roasting forming, and is characterized by comprising the following steps:
step A, soaking a roasted and molded ozone catalyst in a non-polar reagent for 12-24 hours, and then filtering;
and step B, drying and roasting the ozone catalyst obtained by filtering in the step A to obtain the modified ozone catalyst.
2. The preparation method of the modified ozone catalyst suitable for the high-salinity wastewater in the coal chemical industry according to claim 1, wherein the impregnation temperature of the baked and molded ozone catalyst and the nonpolar reagent in the step A is 20-70 ℃.
3. The preparation method of the modified ozone catalyst suitable for the high-salinity wastewater in the coal chemical industry according to claim 1, wherein the volume ratio of the baked and molded ozone catalyst to the nonpolar reagent in the step A is 1: 1-1: 10.
4. The method as claimed in claim 1, wherein the non-polar reagent in step A is any one of dichloromethane, chloroform, carbon tetrachloride, acetone, tributylamine, trioctylamine, benzene, petroleum ether, and cyclohexane.
5. The preparation method of the modified ozone catalyst suitable for the high-salinity wastewater in the coal chemical industry according to claim 1, wherein the drying temperature of the ozone catalyst washed in the step B is 50-100 ℃, and the drying time is 10-30 h.
6. The preparation method of the modified ozone catalyst suitable for the high-salinity wastewater in the coal chemical industry according to claim 1, wherein the roasting conditions of the dried ozone catalyst in the step B are as follows: the muffle furnace adopts the programmed temperature rise to 500-600 ℃, the temperature rise rate is 2.5-5.5 ℃/min, and the roasting time is 3-6 h.
7. The preparation method of the modified ozone catalyst suitable for the high-salinity wastewater in the coal chemical industry according to claim 1, wherein the raw materials of the calcined and molded ozone catalyst comprise: an ozone catalyst carrier and an active component solution; the ozone catalyst carrier is one of alumina, activated carbon and ceramsite; the active component solution is a solution containing any one or more ions of manganese, iron, cobalt, nickel, magnesium, zinc, copper and the like.
8. The method for preparing the modified ozone catalyst suitable for the high-salinity wastewater in the coal chemical industry according to claim 7, wherein the preparation method of the baked and molded ozone catalyst is one of a mixing method, an impregnation method and a coprecipitation method.
CN201911181406.3A 2019-11-27 2019-11-27 Preparation method of modified ozone catalyst suitable for high-salinity wastewater in coal chemical industry Withdrawn CN111013571A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6387278B1 (en) * 2000-02-16 2002-05-14 The Regents Of The University Of California Increasing subterranean mobilization of organic contaminants and petroleum by aqueous thermal oxidation
CN102001765A (en) * 2010-10-21 2011-04-06 东莞市汇赋节能电子有限公司 Method for deeply treating sewage containing phenol and aniline
CN102059146A (en) * 2010-12-08 2011-05-18 重庆理工大学 Catalyst for further treating coking wastewater and preparation method thereof
JP2012217988A (en) * 2011-04-13 2012-11-12 Umekita Atsuo Simplified wastewater treatment apparatus and wastewater treatment method
CN103145266A (en) * 2013-03-20 2013-06-12 上海大学 Method for treating coking wastewater by using ozone under catalysis of activated carbon
CN104891713A (en) * 2015-06-23 2015-09-09 杭州大地环保工程有限公司 Catalytic ozonation process for treatment of organic wastewater
CN106732792A (en) * 2016-12-16 2017-05-31 煤炭科学技术研究院有限公司 One kind treatment Coal Chemical Industry high-salt wastewater catalyst and preparation method thereof

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6387278B1 (en) * 2000-02-16 2002-05-14 The Regents Of The University Of California Increasing subterranean mobilization of organic contaminants and petroleum by aqueous thermal oxidation
CN102001765A (en) * 2010-10-21 2011-04-06 东莞市汇赋节能电子有限公司 Method for deeply treating sewage containing phenol and aniline
CN102059146A (en) * 2010-12-08 2011-05-18 重庆理工大学 Catalyst for further treating coking wastewater and preparation method thereof
JP2012217988A (en) * 2011-04-13 2012-11-12 Umekita Atsuo Simplified wastewater treatment apparatus and wastewater treatment method
CN103145266A (en) * 2013-03-20 2013-06-12 上海大学 Method for treating coking wastewater by using ozone under catalysis of activated carbon
CN104891713A (en) * 2015-06-23 2015-09-09 杭州大地环保工程有限公司 Catalytic ozonation process for treatment of organic wastewater
CN106732792A (en) * 2016-12-16 2017-05-31 煤炭科学技术研究院有限公司 One kind treatment Coal Chemical Industry high-salt wastewater catalyst and preparation method thereof

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Application publication date: 20200417