CN109020032A - A kind of highly concentrated phenol wastewater harmlessness disposing with high salt and high pure sodium chloride recovery process - Google Patents
A kind of highly concentrated phenol wastewater harmlessness disposing with high salt and high pure sodium chloride recovery process Download PDFInfo
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- CN109020032A CN109020032A CN201810994007.8A CN201810994007A CN109020032A CN 109020032 A CN109020032 A CN 109020032A CN 201810994007 A CN201810994007 A CN 201810994007A CN 109020032 A CN109020032 A CN 109020032A
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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
- C02F9/00—Multistage treatment of water, waste water or sewage
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/14—Purification
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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
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
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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
- C02F1/722—Oxidation by peroxides
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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
- C02F1/74—Treatment of water, waste water, or sewage by oxidation with air
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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
- C02F1/76—Treatment of water, waste water, or sewage by oxidation with halogens or compounds of halogens
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/12—Halogens or halogen-containing compounds
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
- C02F2101/345—Phenols
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- Engineering & Computer Science (AREA)
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Abstract
The present invention is to belong to the highly concentrated high-salt wastewater process field of pesticide chemical, more particularly to a kind of highly concentrated phenol wastewater harmlessness disposing with high salt and high pure sodium chloride recovery process.The method that the present invention is combined using physics disposition and chemical disposal, it is oxide target as roadmap using hydroquinone oxidation intermediate product, by the way of multistage combined oxidation stage by stage, level-one uses air oxidation, insoluble precipitate is precipitated, by filters, waste water COD can reduce by 40% or so；Secondary oxidation uses hydrogen peroxide oxidation, controls reaction condition, removes waste water small molecular organic matter, and tertiary oxidation carries out deep oxidation using strong oxidizer.Multi-stage oxidizing treated waste water uses the technique of MVR evaporation, carries out high-purity sodium chloride salt recycling, sodium chloride meets enterprises quality standard, and content reaches 95% or more.Using the present invention, it can be achieved that the recycling of byproduct sodium chloride, achievees the purpose that disposal of resources while reducing phenolic wastewater treatment cost.
Description
Technical field
The invention belongs to the highly concentrated high-salt wastewater process field of pesticide chemical, more particularly to a kind of highly concentrated phenol wastewater with high salt without
Evilization disposition and high pure sodium chloride recovery process.
Background technique
In the production process of pesticide essence Kui He Ling Zhi phenol workshop section, since the excess of hydroquinone adds and product yield
Limitation, generate largely the highly concentrated high-salt wastewater containing hydroquinone, COD may be up to
70000mg/l, total salt are up to 72000mg/l, and product per ton can produce 10 tons of the waste water containing hydroquinone.Waste water
In main component have the organic matters such as hydroquinone and its oxide, cyclocomplex, A3 (a kind of pesticide intermediate), dimethylamine, with
And the inorganic salts such as sodium carbonate, sodium chloride.Current main disposal options are to be evaporated crystallization, are separated by solid-liquid separation, and are generated big
The abraum salt containing organic matter of amount entrusts external disposition as danger wastes, the operating cost of waste water evaporation 120 yuan/it is vertical
Square waste water or so, abraum salt is 4000 yuan/ton of solids as the cost of danger wastes commission disposition, since its processing cost is high,
Evaporate mother liquor simultaneously constantly applies enrichment, and evaporation operating cost constantly rises, therefore finds a kind of newly inexpensive, innoxious
Treatment process it is extremely urgent.
Summary of the invention
Present invention is generally directed to the problem of be: (1) highly concentrated phenolic wastewater treatment difficulty with high salt is big, processing cost is high etc. asks
Topic；(2) existing disposing technique generates a large amount of danger wastes, causes a large amount of wastes of resource.
It is directed to existing problem, the present invention provides a kind of highly concentrated phenol wastewater harmlessness disposing with high salt and high-purity chlorinations
Sodium recovery process, process provides a kind of completely new roadmap and mode, and application which harmless treatment containing pair
Method benzenediol highly concentrated high-salt wastewater and recycle high pure sodium chloride.The method combined using physics disposition and chemical disposal,
It is oxide target as roadmap using hydroquinone oxidation intermediate product, by the way of multistage combined oxidation stage by stage, one
Grade oxidation is passed through a certain amount of air under alkaline condition using air oxidation, then adjusts pH, and insoluble precipitate is precipitated,
Infusible precipitate in waste water is removed by filtering, waste water COD can reduce by 40% or so；Secondary oxidation uses hydrogen peroxide oxidation,
Remove waste water small molecular organic matter；Tertiary oxidation carries out deep oxidation, multi-stage oxidizing treated waste water using strong oxidizer
The technique evaporated using MVR, carries out high-purity sodium chloride salt recycling, sodium chloride meets enterprises quality standard, and content reaches
95% or more.Using this roadmap and technique, is compared with the treatment process of current phenol wastewater, substantially reduce oxidation difficulty
And oxidant cost, while handle after carry out MVR evaporation, it can be achieved that byproduct sodium chloride recycling, reach the mesh of disposal of resources
's.
The highly concentrated phenol wastewater harmlessness disposing with high salt of one kind of the present invention and high pure sodium chloride recovery process are specific to walk
Suddenly include:
(1) air is passed through under stair oxidation normal temperature and pressure into highly concentrated phenol wastewater with high salt and carries out air oxidation；It has aoxidized
Finish, adjusting water sample pH value is 3-4, and filtering removes precipitating, obtains acid waste water；
(2) secondary oxidation will be added hydrogen peroxide and carry out hydrogen peroxide oxidation in the acid waste water after stair oxidation, and oxidation finishes,
Zhi≤12 water sample pH are adjusted, alkaline waste water is obtained；
(3) tertiary oxidation will be added strong oxidizer and carry out deep oxidation in alkaline waste water, and oxidation finishes, and it is useless to obtain deep oxidation
Water；
(4) it adjusts deep oxidation pH value of waste water and carries out the recycling of sodium chloride salt into MVR vapo(u)rization system for 6-8, obtain high
Pure sodium chloride salt.
The highly concentrated phenol wastewater pH value with high salt is usually between 10-12, using air compressor into reaction system
Be passed through air, control air mass flow and oxidization time, using the oxygen in air, by the highly concentrated high-salt wastewater to benzene two
Phenol is oxidized to 1,4-benzoquinone.Alkaline condition, hydroquinone form phenol sodium, are easily oxidized, therefore the oxygen in air is entirely capable of completely
Foot oxidation demand.It after air oxidation, is acidified using hydrochloric acid, adjusts water sample pH value between 3-4, water sample is generated in after acid
A large amount of sediments, sediment includes the acid insoluble matter and 1,4-benzoquinone contained in waste water, because 1,4-benzoquinone is insoluble in cold water, mistake
Filter, waste water COD are reduced with the removal of sediment, and after measured, the removal rate of COD is up to 40%；It is empty during stair oxidation
Throughput is 20-30L/min, oxidization time 4-5h, hydrochloric acid generally use mass fraction for 30% hydrochloric acid.It is of the present invention
Room temperature refer to 20-25 DEG C, normal pressure refers to a standard atmospheric pressure.
Hydroquinone sloughs hydrogen ion and forms 1,4-benzoquinone, and hydroquinone is soluble in hot water, can be dissolved in cold water, and 1,4-benzoquinone is molten
It is insoluble in cold water in hot water, using the difference of hydroquinone and 1,4-benzoquinone dissolution properties, carries out the removal of hydroquinone.
Hydrogen peroxide is added in the acid waste water generated after to stair oxidation and carries out hydrogen peroxide oxidation, removes waste water small molecular
Organic matter；Air is difficult to the small molecule straight chain organic matter aoxidized, predominantly monohydric alcohol, dihydric alcohol etc. during stair oxidation, double
Oxygen water can achieve good oxidation effectiveness, and the product after hydrogen peroxide oxidation is mainly water, will not bring secondary pollution into.Second level oxygen
During change, hydrogen peroxide 8-10ml is added in every liter of acid waste water, oxidization time 2-3h, hydrogen peroxide is that mass fraction is 32%
Hydrogen peroxide.
After secondary oxidation, the liquid alkaline alkaline hydrolysis for being 30% using mass fraction adjusts Zhi≤12 waste water pH, obtains alkaline waste water.
Then solid sodium hypochlorite strong oxidizer is added, aoxidizes 2-3h, solid sodium hypochlorite additional amount is the 3- of alkaline waste water quality
5‰；Zhi≤12 waste water pH are adjusted, are to provide a kind of suitable oxidizing condition to strong oxidizer.Hypochlorite oxidation agent tool
There is very strong broken ring ability, for the organic matter for having phenyl ring, there is very high oxidation efficiency.Sodium hypochlorite is as strong oxidizer
Product be sodium chloride, other inorganic ions in waste water will not be brought into.
Waste water after deep oxidation adjusts pH value between 6-8, and filtering, filtrate enters MVR vapo(u)rization system, carries out high-purity chlorine
Change the recycling of sodium salt；Into when MVR evaporation, pressure is -0.08~-0.05Mpa, and temperature is 80-100 DEG C.Chlorination after the recovery
Sodium reaches enterprises quality requirement: sodium chloride content>95%, sulfate radical content<0.5%, aqueous<4%.
In conclusion the present invention provides a kind of removal techniques of organic matter in completely new highly concentrated phenol wastewater with high salt: the
One, for the hydroquinone organic matter for having phenyl ring in waste water, it is difficult to which exhaustive oxidation will be to benzene by the way of intermediate oxidation
Diphenol is converted into 1,4-benzoquinone, in the dissolution properties different according to two kinds of substances, by the means of physical filtering by waste water to benzene
Diphenol removal, reduces the processing difficulty and Material Cost of exhaustive oxidation；Second, it is physical according to the difference of useless Organic substance in water
Matter is carried out at oxidation for small organic molecule using green oxidation agent hydrogen peroxide using multistage combined oxidation mode stage by stage
It sets, does not generate secondary pollution；The organic matter with phenyl ring contained in waste water is carried out using sodium hypochlorite strong oxidizer
Deep oxidation processing, while not bringing other inorganic ions into, meet the requirement that subsequent technique recycles high pure sodium chloride.The present invention
The advantages of giving full play to various oxidants, oxidant not will cause secondary pollution, and simultaneous oxidation agent is cheap and easy to get, and reaction condition is slow
With, high temperature and pressure is not needed, it is easy to operate；And treated that highly concentrated high-salt wastewater utilizes the recyclable height of conventional vaporising device
Pure sodium chloride realizes the purpose of recycling.
Detailed description of the invention
Fig. 1 is the flow chart of technique of the present invention.
Specific embodiment
Embodiment 1:
Take the highly concentrated phenol wastewater (COD with high salt of 500mlCr: 65736mg/L, ammonia nitrogen: 1419.2mg/L, total salt: 69460mg/
L, pH=11.8), it is placed in the vertical-type air-flotation device of laboratory, opens air compressor,
At 20 DEG C, it is passed through air into waste water and carries out stair oxidation, during stair oxidation, air mass flow 22L/
Min, oxidization time 5h.Oxidation finishes, and the waste water in air-floating apparatus is transferred in four-hole boiling flask, is adjusted using 30% hydrochloric acid
Water sample pH value is 3.2, stirs 10min, and filtering removes precipitating, obtains acid waste water, water-quality CODCrIt is reduced to 37287mg/L；
Hydrogen peroxide will be added in acid waste water after stair oxidation and carry out hydrogen peroxide oxidation, during secondary oxidation, every liter
Hydrogen peroxide 8ml, oxidization time 3h are added in acid waste water.Secondary oxidation terminates, and adjusts water sample pH using 30% sodium hydroxide
Value is 12.9, obtains alkaline waste water；
Deep oxidation is carried out by solid sodium hypochlorite strong oxidizer is added in alkaline waste water, oxidation finishes, and obtains deep oxidation
Waste water, wherein the additional amount of solid sodium hypochlorite is the 3 ‰ of alkaline waste water quality, stirring oxidation, oxidization time 3h.
Adjusting deep oxidation pH value of waste water using 30% hydrochloric acid is 6.8, after filtering, into MVR vapo(u)rization system ,-
0.08Mpa under 80 degrees celsius, is evaporated crystallization, recycles high pure sodium chloride: sodium chloride content content: 98.8%,
SO4 2-: 0.4%, insoluble substance: 0.1%.
Embodiment 2:
Take the highly concentrated phenol wastewater (COD with high salt of 500mlCr: 57321mg/L, ammonia nitrogen: 1273.2mg/L, total salt: 47683mg/
L, pH=12.1), it is placed in the vertical-type air-flotation device of laboratory, opens air compressor,
At 20 DEG C, it is passed through air into waste water and carries out stair oxidation, during stair oxidation, air mass flow 26L/
Min, oxidization time 4.5h.Oxidation finishes, and the waste water in air-floating apparatus is transferred in four-hole boiling flask, utilizes 30% hydrochloric acid tune
Water-saving sample pH value is 3.8, stirs 10min, and filtering removes precipitating, obtains acid waste water, water-quality CODCrIt is reduced to 23563mg/L；
Hydrogen peroxide will be added in acid waste water after stair oxidation and carry out hydrogen peroxide oxidation, during secondary oxidation, every liter
Hydrogen peroxide 10ml, oxidization time 2h are added in acid waste water.Secondary oxidation terminates, and adjusts water sample pH using 30% sodium hydroxide
Value is 12.3, obtains alkaline waste water；
Deep oxidation is carried out by solid sodium hypochlorite strong oxidizer is added in alkaline waste water, oxidation finishes, and obtains deep oxidation
Waste water, wherein the additional amount of solid sodium hypochlorite is the 4 ‰ of alkaline waste water quality, stirring oxidation, oxidization time 2.5h.
Adjusting deep oxidation pH value of waste water using 30% hydrochloric acid is 7.2, after filtering, into MVR vapo(u)rization system ,-
0.08Mpa under 80 degrees celsius, is evaporated crystallization, recycles high pure sodium chloride: sodium chloride content content: 98.1%,
SO4 2-: 0.3%, insoluble substance: 0.2%.
Embodiment 3:
By the highly concentrated phenol wastewater (COD with high salt of 1000LCr: 42400mg/L, ammonia nitrogen: 1018mg/L, total salt: 4592.0mg/L,
PH=10.5), workshop enlarged experiment is carried out, is transferred in R105A reaction kettle using pump, reaction kettle stirring is opened and carries out waste water system
Workshop wind line is opened in stirring, is passed through air to R105A reaction kettle at 20 °C, carries out stair oxidation, stair oxidation process
In, air mass flow 30L/min, oxidization time 4h.Stair oxidation terminates, and the waste water in R105A reaction kettle is transferred to
In R105B reaction kettle, adjusting water sample pH value using 30% hydrochloric acid in the storage tank of workshop is 3.5, opens R105B and stirs 10min, then
Waste water in R105B kettle is squeezed into M105A sheet frame to be filtered, water-quality COD after filteringCrIt is reduced to 24245mg/L.
Filtered acid waste water is subjected to secondary oxidation, hydrogen peroxide, every liter of acid waste water are added into R105A reaction kettle
Middle addition hydrogen peroxide 10ml opens stirring, aoxidizes 2h, and secondary oxidation terminates, and adjusts water sample pH value using 30% sodium hydroxide and is
13.2, obtain alkaline waste water；
Deep oxidation is carried out by strong oxidizer is added in alkaline waste water, oxidation finishes, and obtains deep oxidation waste water；Described is strong
Oxidant is solid sodium hypochlorite, and additional amount is the 5 ‰ of alkaline waste water quality, oxidization time 2h.
Deep oxidation terminates, and the pH value of waste water of R105A reaction kettle after deep oxidation is adjusted using 30% hydrochloric acid of workshop storage tank
To between 7.5, waste water is then squeezed into M105B sheet frame and is filtered, the waste water generated after filtering enters workshop MVR evaporation dress
It sets, at -0.08Mpa, 80 degrees celsius, is evaporated crystallization, recycle high pure sodium chloride: sodium chloride content content:
97.1%, SO4 2-: 0.4%, insoluble matter: 0.3%.
Claims (6)
1. a kind of highly concentrated phenol wastewater harmlessness disposing with high salt and high pure sodium chloride recovery process, it is characterised in that: by highly concentrated height
Salt phenol wastewater is handled using multi-stage oxidizing, then using the technique of MVR evaporation, carries out high-purity sodium chloride salt recycling.
2. the highly concentrated phenol wastewater harmlessness disposing with high salt of one kind according to claim 1 and high pure sodium chloride recovery process,
It is characterized by: specific steps include:
(1) air is passed through under stair oxidation normal temperature and pressure into highly concentrated phenol wastewater with high salt and carries out air oxidation；Oxidation finishes, and adjusts
Water-saving sample pH value is 3-4, and filtering removes precipitating, obtains acid waste water；
(2) secondary oxidation will be added hydrogen peroxide and carry out hydrogen peroxide oxidation in the acid waste water after stair oxidation, and oxidation finishes, and adjusts
Zhi≤12 water sample pH, obtain alkaline waste water；
(3) tertiary oxidation will be added strong oxidizer and carry out deep oxidation in alkaline waste water, and oxidation finishes, and obtains deep oxidation waste water；
(4) it adjusts deep oxidation pH value of waste water and carries out the recycling of sodium chloride salt into MVR vapo(u)rization system for 6-8, obtain high-purity chlorine
Change sodium salt.
3. the highly concentrated phenol wastewater harmlessness disposing with high salt of one kind according to claim 2 and high pure sodium chloride recovery process,
It is characterized by: during stair oxidation, air mass flow 20-30L/min, oxidization time 4-5h.
4. the highly concentrated phenol wastewater harmlessness disposing with high salt of one kind according to claim 2 and high pure sodium chloride recovery process,
It is characterized by: hydrogen peroxide 8-10ml, oxidization time 2-3h are added in every liter of acid waste water during secondary oxidation.
5. the highly concentrated phenol wastewater harmlessness disposing with high salt of one kind according to claim 2 and high pure sodium chloride recovery process,
It is characterized by: the strong oxidizer is solid sodium hypochlorite during tertiary oxidation, additional amount is alkaline waste water quality
3-5 ‰, oxidization time 2-3h.
6. the highly concentrated phenol wastewater harmlessness disposing with high salt of one kind according to claim 2 and high pure sodium chloride recovery process,
It is characterized by: pressure is -0.08~-0.05Mpa into when MVR evaporation, temperature is 80-100 DEG C.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109704492A (en) * | 2019-03-07 | 2019-05-03 | 安徽华星化工有限公司 | A kind of abraum salt harmless resource processing system |
| CN109809434A (en) * | 2019-03-07 | 2019-05-28 | 安徽华星化工有限公司 | A method of production refining industrial salt is recycled based on Cupric sulfate abraum salt |
| CN109848185A (en) * | 2019-03-11 | 2019-06-07 | 安徽华星化工有限公司 | A kind of harmless processing method of Cupric sulfate abraum salt |
| CN110156236A (en) * | 2019-06-27 | 2019-08-23 | 南京大学盐城环保技术与工程研究院 | A kind of method of highly salt containing organic waste water recycling |
| CN111101157A (en) * | 2019-12-27 | 2020-05-05 | 合肥恒力装备有限公司 | Zero-emission treatment process for PCB etching waste liquid |
| CN113173841A (en) * | 2021-04-13 | 2021-07-27 | 宁夏伟创药业有限公司 | Method for preparing p-benzoquinone by catalytic oxidation of 1, 4-benzenediol |
| CN114163036A (en) * | 2021-12-10 | 2022-03-11 | 南京环保产业创新中心有限公司 | Method for treating semi-coke wastewater by pre-oxidation oil removal dephenolization-electro-Fenton technology |
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| CN102815822A (en) * | 2012-08-28 | 2012-12-12 | 无锡晟金环保科技有限公司 | Wastewater purification device |
| CN108191140A (en) * | 2017-12-15 | 2018-06-22 | 江苏湖大化工科技有限公司 | The processing method and device of a kind of phenol wastewater |
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| US20050113534A1 (en) * | 2003-11-21 | 2005-05-26 | Parminder Agarwal | Stabilized polycarbonate polyester composition |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109704492A (en) * | 2019-03-07 | 2019-05-03 | 安徽华星化工有限公司 | A kind of abraum salt harmless resource processing system |
| CN109809434A (en) * | 2019-03-07 | 2019-05-28 | 安徽华星化工有限公司 | A method of production refining industrial salt is recycled based on Cupric sulfate abraum salt |
| CN109848185A (en) * | 2019-03-11 | 2019-06-07 | 安徽华星化工有限公司 | A kind of harmless processing method of Cupric sulfate abraum salt |
| CN109848185B (en) * | 2019-03-11 | 2020-10-27 | 安徽华星化工有限公司 | Monosultap waste salt harmless treatment method |
| CN110156236A (en) * | 2019-06-27 | 2019-08-23 | 南京大学盐城环保技术与工程研究院 | A kind of method of highly salt containing organic waste water recycling |
| CN111101157A (en) * | 2019-12-27 | 2020-05-05 | 合肥恒力装备有限公司 | Zero-emission treatment process for PCB etching waste liquid |
| CN113173841A (en) * | 2021-04-13 | 2021-07-27 | 宁夏伟创药业有限公司 | Method for preparing p-benzoquinone by catalytic oxidation of 1, 4-benzenediol |
| CN114163036A (en) * | 2021-12-10 | 2022-03-11 | 南京环保产业创新中心有限公司 | Method for treating semi-coke wastewater by pre-oxidation oil removal dephenolization-electro-Fenton technology |
| CN114163036B (en) * | 2021-12-10 | 2023-12-05 | 南京环保产业创新中心有限公司 | Method for treating semi-coke wastewater by preoxidation degreasing and dephenolization-electro-Fenton technology |
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Application publication date: 20181218 |