CN105967311B - The processing method of the simple 3,5,6- trichloropyridines -2- sodium alkoxide waste water of flow - Google Patents

The processing method of the simple 3,5,6- trichloropyridines -2- sodium alkoxide waste water of flow Download PDF

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Publication number
CN105967311B
CN105967311B CN201610372053.5A CN201610372053A CN105967311B CN 105967311 B CN105967311 B CN 105967311B CN 201610372053 A CN201610372053 A CN 201610372053A CN 105967311 B CN105967311 B CN 105967311B
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waste water
water
catalyst
sodium alkoxide
flow
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CN105967311A (en
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周新基
朱建军
李珣珣
夏俊维
陈俊明
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Jiangsu nine Jiangsu jiujiujiu Technology Co. Ltd.
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Jiangsu Nine Jiangsu Jiujiujiu Technology Co Ltd
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    • 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
    • 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
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/74—Iron group metals
    • B01J23/745—Iron
    • 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
    • C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • 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
    • C02F2101/10—Inorganic compounds
    • C02F2101/20—Heavy metals or heavy metal compounds
    • 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
    • C02F2101/34—Organic compounds containing oxygen
    • 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
    • C02F2101/36—Organic compounds containing halogen
    • 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
    • C02F2101/38—Organic compounds containing nitrogen
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
    • C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds

Abstract

The invention discloses a kind of flow simple 3, the processing method of 5,6 trichloropyridine, 2 sodium alkoxide waste water, including the pretreatment of carrier, the preparation of loaded catalyst, catalytic wet oxidation, distillation.The present invention selects agriculture and forestry organic waste material as catalyst carrier, turns waste into wealth, and is conducive to sustainable development.Catalyst obtained has magnetic effect, and the surface tension, density and viscosity of water can be made to decline, can increase the concentration of oxygen in water, reduce the resistance to mass tranfer of oxygen in air, thus it can significantly reduce reaction temperature and pressure, moreover it is possible to adsorb copper ion micro in waste water, eliminate heavy metal pollution problem.Flow of the present invention is simple, and COD removal rates are high, and occupation area of equipment is small, non-secondary pollution, while by-product Nacl, both economically and environmentally beneficial.

Description

The processing method of the simple 3,5,6- trichloropyridines -2- sodium alkoxide waste water of flow
The application is application number：201510164684.3, the applying date：2015-04-09, title " 3,5,6- trichloropyridines- The divisional application of the processing method of 2- sodium alkoxide waste water ".
Technical field
The present invention relates to a kind of processing methods of 3,5,6- trichloropyridines -2- sodium alkoxide waste water.
Background technology
Waste water in 3,5,6- trichloropyridine -2- sodium alkoxide production processes mostlys come from mother liquor when alkaline hydrolysis, complicated component, Contain pyridine sodium alkoxide, o-dichlorohenzene, polyacrylonitrile, chloride, heavy metal ion and other impurities.The waste water dark brown, COD 30000~50000, pH ＞ 12, B/C 0.15~0.2,150~200ppm of content of copper ion, sodium chloride content 8~15%, have The features such as concentration is high, salinity is high, biodegradable difficult.Currently, manufacturing enterprise mostly uses dilution --- biochemical process or decompression are steamed Evaporating --- burning method handles sodium alkoxide waste water.The former extension rate is up to 20~40 times, causes the significant wastage of water resource, and Effluent quality is unstable.The latter's high energy consumption, cost for wastewater treatment per ton is up to 200~400 yuan, and the burning of residue will produce greatly The dioxin and dense smoke of amount, cause air certain harm.Wang Tongtao etc.（Pesticide science and management, 2013,34（4）：32~ 35）Using Fenton --- the mode of oxidizing that ozone is combined handles sodium alkoxide waste water, and COD removal rates reach 89.2%, but the technique meeting The solid wastes such as iron cement are generated, needs to use acid-base accommodation pH, a large amount of inorganic salts is additionally introduced into waste water, improve the salinity of waste water, Difficulty is brought for further biochemical treatment.
Catalysis wet-type oxidation technology is a kind of to the effective high-level oxidation technology of the poisonous and harmful waste water of high-concentration hardly-degradable.It Waste water can be individually handled, the pretreatment of biochemical treatment is can also be used as, by wet oxidation, reduces the COD of waste water, removal pair The biochemical poisonous and hazardous substance of bacterium, improves the biodegradability of waste water.Wang great Liu etc.（Chemical Industry in Guangzhou, 2013,41（10）：183~ 185）Sodium alkoxide waste water is handled using this method.Using CuO-Co3O4-CeO2/TiO2-ZrO2 as catalyst, COD removal rates reach To 97.2%.But the technique is not directed to the processing of Cu in waste water and salinity, and the catalyst selected is more complicated, expensive, Increase processing cost.Therefore, it is necessary to seek a kind of catalyst of high efficiency low cost to carry out wet oxidation to sodium alkoxide waste water, together When remove waste water in copper.
Invention content
The purpose of the present invention is to provide a kind of processing of the good 3,5,6- trichloropyridine -2- sodium alkoxide waste water of convenience, effect Method.
Technical solution of the invention is：
The processing method of one kind 3,5,6- trichloropyridine -2- sodium alkoxide waste water, it is characterized in that：Steps are as follows：
（1）The pretreatment of carrier：Agriculture and forestry organic waste material is crushed after cleaning drying with pulverizer, is screened 20~40 mesh, is put into and rubs That ratio 5:1 sulfuric acid（2mol/L）It is heated to reflux 1~2h for 40~50 DEG C in formalin, filters the NaOH alkali with 32% after cleaning Change 1~2h, is dried for standby after filtering cleaning to neutrality；
（2）The preparation of loaded catalyst：By FeSO4•7H2O and FeCl3•6H2O presses Fe2+And Fe3+Molar ratio 1:2 are dissolved in In distilled water, 2 times of FeSO are added4•7H2The pretreated carrier of O mass is warming up to 50 ~ 60 DEG C, and 32% sodium hydroxide solution is added dropwise, 100 DEG C of 2~3h of ageing, it is to be drying to obtain support type at 7,100~105 DEG C to urge that cooling, which is filtered and washed repeatedly with water to product pH, Agent；
（3）Catalytic wet oxidation：Sodium alkoxide waste water and above-mentioned catalyst are added in 1L autoclaves, oxygen is filled with and stirs It mixes, is warming up to assigned temperature reaction a period of time, cool down pressure release, filters out catalyst；
（4）Distillation：Above-mentioned filtrate normal pressure steams 80~85% water, and cool down the Nacl for filtering white.
Agriculture and forestry organic waste material refers to sawdust, peanut shell or stalk.
Step（3）In, the addition of loaded catalyst is 3~5g/L, and reaction temperature is 130~160 DEG C, the reaction time For 30~120min, reaction pressure is 0.5~3.5MPa.
Catalyst and mother liquor cover in the wet oxidation for using next group waste water.
The present invention is easy to operate, effect is good；Advantage of the invention is that：Select agriculture and forestry organic waste material as catalyst carrier, Turn waste into wealth, is conducive to sustainable development.Catalyst obtained has magnetic effect, can make the surface tension, density and viscosity of water Decline, the concentration of oxygen in water can be increased, reduce the resistance to mass tranfer of oxygen in air, thus can significantly reduce reaction temperature and pressure Power, moreover it is possible to adsorb copper ion micro in waste water, eliminate heavy metal pollution problem.Flow of the present invention is simple, and COD removal rates are high, Occupation area of equipment is small, non-secondary pollution, while by-product Nacl, both economically and environmentally beneficial.
With reference to embodiment, the invention will be further described.
Specific implementation mode
100g molar ratios 5 are added in 20g sawdusts:1 sulfuric acid（2mol/L）Formalin, 50 DEG C are heated to reflux 2h, filter 2h is impregnated with the NaOH of 50g 32% after cleaning, is dried for standby after filtering cleaning to neutrality.
By 8g FeSO4•7H2O and 15.6g FeCl3•6H2O is dissolved in 50g distilled water, and the above-mentioned pretreatment wood of 16g is added Bits, are warming up to 60 DEG C, and 32% sodium hydroxide solutions of 50g, 100 DEG C of ageing 3h is slowly added dropwise, and cooling is filtered and washed repeatedly with water It is to be drying to obtain loaded catalyst at 7,100~105 DEG C to product pH.
By 600mL sodium alkoxide waste water（COD 38650, content of copper ion 188ppm）It is anti-it to be added to 1L high pressures with the above-mentioned catalyst of 3g It answers in kettle, be filled with 1MPa air and stir, be warming up to 160 DEG C of reaction 120min, be cooled to room temperature pressure release, filter to obtain 3.8g catalysis Agent.Above-mentioned 690.2g filtrates（COD 400, copper ion is not detected）Normal pressure steams 555.8g water, and cooling filters to obtain white salt 68.3g.The micro- yellow mother liquors of 62.4g and catalyst set are used in next group 600mL waste water.

Claims (1)

1. a kind of processing method of simple 3,5,6- trichloropyridine -2- sodium alkoxide waste water of flow, it is characterized in that：Steps are as follows：
100g molar ratios 5 are added in 20g sawdusts:1 sulfuric acid-formalin, a concentration of 2mol/L of sulfuric acid；50 DEG C are heated back 2h is flowed, uses the NaOH of 50g 32% to impregnate 2h after filtering cleaning, is dried for standby after filtering cleaning to neutrality；
By 8g FeSO4•7H2O and 15.6g FeCl3•6H2O is dissolved in 50g distilled water, and the above-mentioned pretreatment sawdusts of 16g, heating is added To 60 DEG C, 32% sodium hydroxide solutions of 50g, 100 DEG C of ageing 3h is slowly added dropwise, cooling is filtered and washed repeatedly with water to product pH It is to be drying to obtain loaded catalyst at 7,100~105 DEG C；
By 600mL3,5,6- trichloropyridine -2- sodium alkoxide waste water are added in 1L autoclaves with the above-mentioned loaded catalysts of 3g, fill Enter 1MPa air and stir, is warming up to 160 DEG C of reaction 120min, is cooled to room temperature pressure release, filters to obtain 3.8g catalyst；It is described COD 38650, the content of copper ion 188ppm of 600mL sodium alkoxide waste water；Above-mentioned suction filtration filters out the 690.2g filters obtained after catalyst Liquid normal pressure steams 555.8g water, and cooling filters to obtain white salt 68.3g；The COD 400 of the 690.2g filtrates, be not detected copper from Son.
CN201610372053.5A 2015-04-09 2015-04-09 The processing method of the simple 3,5,6- trichloropyridines -2- sodium alkoxide waste water of flow Active CN105967311B (en)

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CN102101053A (en) * 2009-12-18 2011-06-22 中国科学院兰州化学物理研究所 Catalyst for treating organic wastewater and preparation method thereof
CN103962116A (en) * 2014-04-25 2014-08-06 南开大学 Preparation method of solid catalyst loaded with cellulose aiding body

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