CN104817220B - The processing method of 3,5,6-trichloropyridine-2-sodium alkoxide waste water - Google Patents

The processing method of 3,5,6-trichloropyridine-2-sodium alkoxide waste water Download PDF

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Publication number
CN104817220B
CN104817220B CN201510164684.3A CN201510164684A CN104817220B CN 104817220 B CN104817220 B CN 104817220B CN 201510164684 A CN201510164684 A CN 201510164684A CN 104817220 B CN104817220 B CN 104817220B
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waste water
catalyst
water
trichloropyridine
sodium alkoxide
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CN104817220A (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 JIUJIUJIU TECHNOLOGY Co Ltd
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Priority to CN201510164684.3A priority patent/CN104817220B/en
Priority to CN201610372053.5A priority patent/CN105967311B/en
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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

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

Abstract

The invention discloses the processing method of a kind of 3,5,6 trichloropyridine 2 sodium alkoxide waste water, the step such as including the pretreatment of carrier, the preparation of loaded catalyst, CWO, distillation.The present invention selects agriculture and forestry organic waste material as catalyst carrier, turns waste into wealth, beneficially sustainable development.The catalyst prepared has magnetic effect, the surface tension of water, density and viscosity can be made to decline, can increase the concentration of oxygen in water, reduce the resistance to mass tranfer of oxygen in air, thus reaction temperature and pressure can be significantly reduced, moreover it is possible to and the copper ion of trace in absorption waste water, eliminate heavy metal pollution problem.Flow process of the present invention is simple, and COD clearance is high, and occupation area of equipment is little, non-secondary pollution, simultaneously by-product Nacl, both economically and environmentally beneficial.

Description

The processing method of 3,5,6-trichloropyridine-2-sodium alkoxide waste water
Technical field
The present invention relates to the processing method of a kind of 3,5,6-trichloropyridine-2-sodium alkoxide waste water.
Background technology
Waste water in 3,5,6-trichloropyridine-2-sodium alkoxide production processes mostlys come from mother solution during alkaline hydrolysis, and complicated component, containing pyridine sodium alkoxide, o-dichlorohenzene, polyacrylonitrile, chloride, heavy metal ion and other impurity.This waste water pitchy, COD 30000～50000, pH ＞ 12, B/C 0.15～0.2, content of copper ion 150～200ppm, sodium chloride content 8～15%, there is the features such as concentration is high, salinity is high, biodegradation is difficult.At present, manufacturing enterprise uses dilution biochemical process or decompression distillation burning method to process 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 energy consumption is high, and cost for wastewater treatment per ton is up to 200～400 yuan, and the burning of residue can produce substantial amounts of dioxin and dense smoke, and air causes certain harm.(pesticide science and the management such as Wang Tongtao, 2013, mode of oxidizing 34(4): 32～35) using Fenton ozone to combine processes sodium alkoxide waste water, COD clearance reaches 89.2%, but this technique can produce the solid wastes such as iron cement, need to use acid-alkali accommodation pH, in waste water, additionally introduce a large amount of inorganic salt, improve the salinity of waste water, bring difficulty for further biochemical treatment.
Catalysis wet-type oxidation technology is a kind of to the high-concentration hardly-degradable effective high-level oxidation technology of poisonous and harmful waste water.It can be with individual processing waste water, it is also possible to as the pretreatment of biochemical treatment, by wet oxidation, reduces the COD of waste water, removes the biochemical poisonous and hazardous material of antibacterial, improve the biodegradability of waste water.Wang great Liu etc. (Chemical Industry in Guangzhou, 2013,41(10): 183～185) i.e. use the method to process sodium alkoxide waste water.With CuO-Co3O4-CeO2/TiO2-ZrO2 as catalyst, COD clearance reaches 97.2%.But this technique is not directed to the process of Cu in waste water and salinity, and the catalyst selected is more complicated, expensive, adds processing cost.Therefore, it is necessary to the catalyst seeking a kind of high efficiency low cost carries out wet oxidation to sodium alkoxide waste water, remove the copper in waste water simultaneously.
Summary of the invention
It is an object of the invention to provide a kind of convenience, the processing method of effective 3,5,6-trichloropyridine-2-sodium alkoxide waste water.
The technical solution of the present invention is:
A kind of 3,5, the processing method of 6-trichloropyridine-2-sodium alkoxide waste water, it is characterized in that: step is as follows:
(1) pretreatment of carrier: agriculture and forestry organic waste material is cleaned after drying and pulverized with pulverizer, screening 20～40 mesh, put in sulphuric acid (the 2mol/L)-formalin of mol ratio 5:1 40～50 DEG C and be heated to reflux 1～2h, sucking filtration clean after with 32% NaOH alkalization 1～2h, sucking filtration clean to neutrality post-drying standby；
(2) preparation of loaded catalyst: by FeSO4•7H2O and FeCl3•6H2O presses Fe2+And Fe3+Mol ratio 1:2 is dissolved in distilled water, adds 2 times of FeSO4•7H2The pretreated carrier of O mass, is warming up to 50 ~ 60 DEG C, drips 32% sodium hydroxide solution, 100 DEG C of ageings 2～3h, cooling sucking filtration be to be drying to obtain loaded catalyst at 7,100～105 DEG C with water cyclic washing to product pH；
(3) CWO: sodium alkoxide waste water and above-mentioned catalyst are added in 1L autoclave, are filled with oxygen and stir, being warming up to assigned temperature and react a period of time, pressure release of lowering the temperature, filter catalyst；
(4) distillation: above-mentioned filtrate normal pressure steams the water of 80～85%, cooling sucking filtration obtains white Nacl.
Agriculture and forestry organic waste material refers to wood flour, Pericarppium arachidis hypogaeae or straw.
In step (3), the addition of loaded catalyst is 3～5g/L, and reaction temperature is 130～160 DEG C, and the response time is 30～120min, and reaction pressure is 0.5～3.5MPa.
Catalyst and mother solution all overlap in the wet oxidation using next group waste water.
The present invention is easy to operate, effective；Present invention have an advantage that selection agriculture and forestry organic waste material, as catalyst carrier, is turned waste into wealth, beneficially sustainable development.The catalyst prepared has magnetic effect, the surface tension of water, density and viscosity can be made to decline, can increase the concentration of oxygen in water, reduce the resistance to mass tranfer of oxygen in air, thus reaction temperature and pressure can be significantly reduced, moreover it is possible to and the copper ion of trace in absorption waste water, eliminate heavy metal pollution problem.Flow process of the present invention is simple, and COD clearance is high, and occupation area of equipment is little, non-secondary pollution, simultaneously by-product Nacl, both economically and environmentally beneficial.
Below in conjunction with embodiment, the invention will be further described.
Detailed description of the invention
Adding sulphuric acid (the 2mol/L)-formalin of 100g mol ratio 5:1 in 20g wood flour, 50 DEG C are heated to reflux 2h, and sucking filtration uses 50g after cleaning The NaOH of 32% soaks 2h, and sucking filtration cleans to neutral post-drying standby.
By 8g FeSO4•7H2O Yu 15.6g FeCl3•6H2O is dissolved in 50g distilled water, adds 16g above-mentioned pretreatment wood flour, is warming up to 60 DEG C, is slowly added dropwise 50g 32% sodium hydroxide solution, 100 DEG C of ageing 3h, cooling sucking filtration be to be drying to obtain loaded catalyst at 7,100～105 DEG C with water cyclic washing to product pH.
600mL sodium alkoxide waste water (COD 38650, content of copper ion 188ppm) and the above-mentioned catalyst of 3g being added in 1L autoclave, be filled with 1MPa air and stir, be warming up to 160 DEG C of reaction 120min, be down to pressure release after room temperature, sucking filtration obtains 3.8g catalyst.Above-mentioned 690.2g filtrate (COD 400, be not detected by copper ion) normal pressure steams 555.8g water, and cooling sucking filtration obtains white salt 68.3g.62.4g micro-HUANGMU liquid and catalyst set are used in next group 600mL waste water.

Claims (3)

1. one kind 3, the processing method of 5,6-trichloropyridine-2-sodium alkoxide waste water, it is characterized in that: step As follows:
(1) pretreatment of carrier: agriculture and forestry organic waste material is cleaned and pulverized with pulverizer after drying, sieve Select 20～40 mesh, put in the sulphuric acid-formalin of mol ratio 5:1 40～50 DEG C and be heated to reflux 1～2h, sucking filtration clean after with 32% NaOH alkalization 1～2h, sucking filtration cleaning is to after neutrality Dry for standby；
(2) preparation of loaded catalyst: by FeSO4·7H2O and FeCl3·6H2O presses Fe2+ And Fe3+Mol ratio 1:2 is dissolved in distilled water, adds 2 times of FeSO4·7H2The pre-place of O mass Reason carrier, is warming up to 50～60 DEG C, drips 32% sodium hydroxide solution, and 100 DEG C are aged 2～3h, Cooling sucking filtration and with water cyclic washing to product pH be drying to obtain at 7,100～105 DEG C negative Supported catalyst；
(3) CWO: by 3,5,6-trichloropyridine-2-sodium alkoxide waste water and above-mentioned load Type catalyst is added in 1L autoclave, is filled with oxygen and stirs, being warming up to assigned temperature Reaction a period of time, pressure release of lowering the temperature, filter catalyst；
(4) distillation: the filtrate normal pressure after step (3) filters catalyst steams 80～85% Water, cooling sucking filtration obtains white Nacl.
The process side of 3,5,6-trichloropyridine-2-sodium alkoxide waste water the most according to claim 1 Method, is characterized in that: agriculture and forestry organic waste material refers to wood flour, Pericarppium arachidis hypogaeae or straw.
The process side of 3,5,6-trichloropyridine-2-sodium alkoxide waste water the most according to claim 1 Method, is characterized in that: in step (3), and the addition of loaded catalyst is 3～5g/L, instead Answering temperature is 130～160 DEG C, and the response time is 30～120min, reaction pressure be 0.5～ 3.5MPa。
CN201510164684.3A 2015-04-09 2015-04-09 The processing method of 3,5,6-trichloropyridine-2-sodium alkoxide waste water Active CN104817220B (en)

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CN201610372055.4A CN105967312B (en) 2015-04-09 2015-04-09 A kind of processing method of 3,5,6- trichloropyridines -2- sodium alkoxide waste water
CN201510164684.3A CN104817220B (en) 2015-04-09 2015-04-09 The processing method of 3,5,6-trichloropyridine-2-sodium alkoxide waste water
CN201610372053.5A CN105967311B (en) 2015-04-09 2015-04-09 The processing method of the simple 3,5,6- trichloropyridines -2- sodium alkoxide waste water of flow

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