CN104817220A - Sodium 3,5,6-trichloropyridin-2-olate wastewater treatment method - Google Patents

Sodium 3,5,6-trichloropyridin-2-olate wastewater treatment method Download PDF

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Publication number
CN104817220A
CN104817220A CN201510164684.3A CN201510164684A CN104817220A CN 104817220 A CN104817220 A CN 104817220A CN 201510164684 A CN201510164684 A CN 201510164684A CN 104817220 A CN104817220 A CN 104817220A
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Prior art keywords
waste water
sodium alkoxide
suction filtration
trichloropyridine
sodium
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CN201510164684.3A
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CN104817220B (en
Inventor
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 CN201610372053.5A priority Critical patent/CN105967311B/en
Priority to CN201610372055.4A priority patent/CN105967312B/en
Priority to CN201510164684.3A priority patent/CN104817220B/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

Abstract

The present invention discloses a sodium 3,5,6-trichloropyridin-2-olate wastewater treatment method, which comprises carrier pretreatment, supported catalyst preparation, catalytic wet oxidation, distillation, and other steps. According to the present invention, the agriculture and forestry waste is selected as the catalyst carrier, such that the waste is turned into treasure, and the sustainable development can be achieved; the prepared catalyst has a magnetic effect and further has effects of reduction of water surface tension, density and viscosity , increase of the concentration of dissolved oxygen in water, reduction of mass transfer resistance of oxygen in air, significant reduction of reaction temperature and reaction pressure, adsorption of trace copper ions in wastewater, and elimination of heavy metal pollution; and the treatment method has characteristics of simple process, high COD removal rate, small equipment occupation area, no secondary pollution, industrial salt by-production, economy, and environmental protection.

Description

The treatment process of 3,5,6-trichloropyridine-2-sodium alkoxide waste water
Technical field
The present invention relates to a kind for the treatment of process of 3,5,6-trichloropyridine-2-sodium alkoxide waste water.
Background technology
Waste water in 3,5,6-trichloropyridine-2-sodium alkoxide production process mainly comes from mother liquor during alkaline hydrolysis, and complicated component, containing pyridine sodium alkoxide, orthodichlorobenzene, polyacrylonitrile, muriate, heavy metal ion and other impurity.This waste water chocolate, COD 30000 ~ 50000, pH > 12, B/C 0.15 ~ 0.2, content of copper ion 150 ~ 200ppm, sodium chloride content 8 ~ 15%, have the features such as concentration is high, salinity is high, biological degradation is difficult.At present, burning method processes sodium alkoxide waste water in manufacturing enterprise's many employing dilution---biochemical process or underpressure distillation---.The former extension rate, up to 20 ~ 40 times, cause the significant wastage of water resources, 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 a large amount of Dioxins and dense smoke, causes certain harm to air.(pesticide science and the management such as Wang Tongtao, 2013,34(4): 32 ~ 35) adopt Fenton---the mode of oxidizing process sodium alkoxide waste water that ozone combines, COD clearance reaches 89.2%, but this technique can produce the solid wastes such as iron mud, needs to use acid-alkali accommodation pH, additionally introduce a large amount of inorganic salt in waste water, improve the salinity of waste water, for further biochemical treatment brings difficulty.
Catalysis wet-type oxidation technology is a kind of to the effective high-level oxidation technology of high-concentration hardly-degradable poisonous and harmful waste water.It can individual curing waste water, also as the pre-treatment of biochemical treatment, by wet oxidation, can reduce the COD of waste water, remove the poisonous and hazardous material of biochemical bacterium, improve the biodegradability of waste water.Wang great Liu etc. (Chemical Industry in Guangzhou, 2013,41(10): 183 ~ 185) namely adopt the method to process sodium alkoxide waste water.Take CuO-Co3O4-CeO2/TiO2-ZrO2 as catalyzer, COD clearance reaches 97.2%.But this technique does not relate to the process of Cu in waste water and salinity, and the catalyzer more complicated selected, price is more expensive, adds processing cost.Therefore, be necessary that the catalyzer 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
The object of the present invention is to provide the treatment process of a kind of convenience, 3,5,6-effective trichloropyridine-2-sodium alkoxide waste water.
Technical solution of the present invention is:
A kind for the treatment of process of 3,5,6-trichloropyridine-2-sodium alkoxide waste water, is characterized in that: step is as follows:
(1) pre-treatment of carrier: agriculture and forestry organic waste material is pulverized with pulverizer after cleaning and drying, screening 20 ~ 40 orders, put into sulfuric acid (2mol/L)-formaldehyde solution 40 ~ 50 DEG C reflux 1 ~ 2h of mol ratio 5:1, with the NaOH alkalization 1 ~ 2h of 32% after suction filtration cleaning, suction filtration cleaning is for subsequent use to neutral post-drying;
(2) preparation of loaded catalyst: by FeSO 47H 2o and FeCl 36H 2o presses Fe 2+and Fe 3+mol ratio 1:2 is dissolved in distilled water, adds 2 times of FeSO 47H 2the pretreated carrier of O quality, is warming up to 50 ~ 60 DEG C, drips 32% sodium hydroxide solution, 100 DEG C of ageing 2 ~ 3h, and cooling suction filtration is also drying to obtain loaded catalyst with water repetitive scrubbing at product pH is 7,100 ~ 105 DEG C;
(3) Catalytic Wet Oxidation: sodium alkoxide waste water and above-mentioned catalyzer are added in 1L autoclave, are filled with oxygen and stir, be warming up to assigned temperature and react for some time, cooling pressure release, filtration catalizer;
(4) distill: above-mentioned filtrate normal pressure steams the water of 80 ~ 85%, cooling suction filtration obtains white Industrial Salt.
Agriculture and forestry organic waste material refers to wood chip, Pericarppium arachidis hypogaeae or stalk.
In step (3), the add-on of loaded catalyst is 3 ~ 5g/L, and temperature of reaction is 130 ~ 160 DEG C, and the reaction times is 30 ~ 120min, and reaction pressure is 0.5 ~ 3.5MPa.
Catalyzer and mother liquor all overlap in the wet oxidation of using next batch waste water.
The present invention is easy to operate, effective; Advantage of the present invention is: select agriculture and forestry organic waste material as support of the catalyst, turn waste into wealth, be conducive to Sustainable development.Obtained catalyzer has magnetic effect, can make the surface tension of water, density and viscosity degradation, can increase the concentration of oxygen in water, reduce the resistance to mass transfer of oxygen in air, thus can significantly reduce temperature of reaction and pressure, the cupric ion of trace in waste water can also be adsorbed, 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 Industrial Salt, not only economy but also environmental protection.
Below in conjunction with embodiment, the invention will be further described.
Embodiment
Add sulfuric acid (the 2mol/L)-formaldehyde solution of 100g mol ratio 5:1 in 20g wood chip, 50 DEG C of reflux 2h, soak 2h with the NaOH of 50g 32% after suction filtration cleaning, suction filtration cleaning is for subsequent use to neutral post-drying.
By 8g FeSO 47H 2o and 15.6g FeCl 36H 2o is dissolved in 50g distilled water, adds the above-mentioned pre-treatment wood chip of 16g, is warming up to 60 DEG C, slowly drips 50g 32% sodium hydroxide solution, 100 DEG C of ageing 3h, and cooling suction filtration is also drying to obtain loaded catalyst with water repetitive scrubbing at product pH is 7,100 ~ 105 DEG C.
600mL sodium alkoxide waste water (COD 38650, content of copper ion 188ppm) and the above-mentioned catalyzer of 3g be 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, suction filtration obtains 3.8g catalyzer.Above-mentioned 690.2g filtrate (COD 400, cupric ion do not detected) normal pressure steams 555.8g water, and cooling suction filtration obtains white salt 68.3g.The micro-yellow mother liquor of 62.4g and catalyzer cover are used in next batch 600mL waste water.

Claims (4)

1. the treatment process of a trichloropyridine-2-sodium alkoxide waste water, is characterized in that: step is as follows:
(1) pre-treatment of carrier: agriculture and forestry organic waste material is pulverized with pulverizer after cleaning and drying, screening 20 ~ 40 orders, put into sulfuric acid-formaldehyde solution 40 ~ 50 DEG C of reflux 1 ~ 2h of mol ratio 5:1, with the NaOH alkalization 1 ~ 2h of 32% after suction filtration cleaning, suction filtration cleaning is for subsequent use to neutral post-drying;
(2) preparation of loaded catalyst: by FeSO 47H 2o and FeCl 36H 2o presses Fe 2+and Fe 3+mol ratio 1:2 is dissolved in distilled water, adds 2 times of FeSO 47H 2the pretreated carrier of O quality, is warming up to 50 ~ 60 DEG C, drips 32% sodium hydroxide solution, 100 DEG C of ageing 2 ~ 3h, and cooling suction filtration is also drying to obtain loaded catalyst with water repetitive scrubbing at product pH is 7,100 ~ 105 DEG C;
(3) Catalytic Wet Oxidation: sodium alkoxide waste water and above-mentioned catalyzer are added in 1L autoclave, are filled with oxygen and stir, be warming up to assigned temperature and react for some time, cooling pressure release, filtration catalizer;
(4) distill: above-mentioned filtrate normal pressure steams the water of 80 ~ 85%, cooling suction filtration obtains white Industrial Salt.
2. the treatment process of 3,5,6-trichloropyridine-2-sodium alkoxide waste water according to claim 1, is characterized in that: agriculture and forestry organic waste material refers to wood chip, Pericarppium arachidis hypogaeae or stalk.
3. the treatment process of 3,5,6-trichloropyridine-2-sodium alkoxide waste water according to claim 1, it is characterized in that: in step (3), the add-on of loaded catalyst is 3 ~ 5g/L, and temperature of reaction is 130 ~ 160 DEG C, reaction times is 30 ~ 120min, and reaction pressure is 0.5 ~ 3.5MPa.
4. the treatment process of 3,5,6-trichloropyridine-2-sodium alkoxide waste water according to claim 1, is characterized in that: catalyzer and mother liquor all overlap in the wet oxidation of using next batch waste water.
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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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
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

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CN105967312B (en) 2018-10-02
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CN105967311B (en) 2018-09-11
CN104817220B (en) 2016-08-17

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