CN105540705B - A kind of high concentration NPE waste water thermocatalytic prepares the method and its device of solid adsorbent - Google Patents
A kind of high concentration NPE waste water thermocatalytic prepares the method and its device of solid adsorbent Download PDFInfo
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- CN105540705B CN105540705B CN201610035247.6A CN201610035247A CN105540705B CN 105540705 B CN105540705 B CN 105540705B CN 201610035247 A CN201610035247 A CN 201610035247A CN 105540705 B CN105540705 B CN 105540705B
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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
- C02F1/025—Thermal hydrolysis
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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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3085—Chemical treatments not covered by groups B01J20/3007 - B01J20/3078
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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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
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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
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- Thermal Sciences (AREA)
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The present invention relates to the method and its device that a kind of high concentration NPE waste water thermocatalytic prepares solid adsorbent, method includes：High concentration NPE waste water and water are added in heat catalysis kettle, then add catalyst, reactor is closed, 180~200 DEG C are heated up to, 3.0~4.0h of stirring reaction；Reactor natural cooling, solid-liquid two-phase mixture in reactor is discharged, separation of solid and liquid, obtained solid matter is dried, obtains solid adsorbent.The method of the present invention is simple to operate；Compared with the technologies such as anaerobic methane production, the property of high concentrated organic waste liquid is not only restricted to, it is applied widely, it is easy to be engineered, innoxious and recycling economically viable technical method is provided for difficult and disposal high concentration NPE waste water.
Description
Technical field
It is more particularly to a kind of the invention belongs to high-concentration hardly-degradable industrial wastewater or liquid waste processing and resource technology field
High concentration NPE waste water thermocatalytic prepares the method and its device of solid adsorbent.
Background technology
NPE is widely used in the industries such as printing and dyeing, chemical industry and cleaning, can be used as surfactant, clear
Clean dose.NPE is the generally acknowledged environmental hormone in the whole world.Research shows, even if the concentration of this material discharge is very
It is low, also great harmfulness.NPE is once entered in environment, will resolve into the stronger environment of toxicity rapidly
Hormone-nonyl phenol.Nonyl phenol has persistence and bioconcentration.It can exist for a long time in the environment, and can be with
Into food chain, the normal reproduction of organism and development are influenceed.
NPE belongs to recalcitrant substance, the method for wastewater treatment containing such material have oxidation,
Reduction, coagulation, biochemistry etc. and combinations thereof technique etc..But given up for caused high concentration NPE in industrial production
Water (such as concentrate containing NPE caused by fluoropolymer production technology), because organic concentration is too high,
Conventional combined technology for wastewater treatment can not but prove effective.
In view of the organic matter that contains in these high concentration NPE waste water in a sense, being money
Source, so the processing disposal for such high concentrated organic waste liquid, need to change thinking, will wherein organic matter as resource reclaim,
Pollution reduction requirement can not only be met, and larger economic benefit can be produced by recycling and energy, be the most
Rationally effective processing method of disposal.
At present, the Study of way for the organic resources in high concentrated organic waste liquid and application it is most be that anaerobism disappears
Change methane phase, but anaerobic methane production technology is suitable only for the excess sludge, food industry and poultry that toxicity is smaller, is readily biodegradable
Poultry waster water.For very high concentrations, biodegradability difference and there are the high concentration NPE waste water of certain toxicity, anaerobic bacteria
It is difficult to normal growth metabolism, anaerobic methane production technique effect is limited, can not obtain significant organic resources and total amount emission reduction
Effect.Microbiological fuel cell is the new technology to begin one's study in recent years, and its principle is to accumulate organic matter in waste water or waste liquid
The chemical energy contained is converted into electric energy and realizes recycling, but is limited to microorganism electricity generation limited efficacy and can not obtain higher electric current
Intensity, make it be only capable of resting on the theoretical and laboratory research stage, there is no method to realize engineer applied at present.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of high concentration NPE waste water thermocatalytic system
The method and its device of standby solid adsorbent, this method are simple to operate；Compared with the technologies such as anaerobic methane production, it is not only restricted to highly concentrated
The property of organic liquid waste is spent, it is applied widely, it is easy to be engineered, for difficult and disposal high concentration NPE
Waste water provides innoxious and recycling economically viable technical method.
The method that a kind of high concentration NPE waste water thermocatalytic of the present invention prepares solid adsorbent, bag
Include：
(1) high concentration NPE waste water and water are added in heat catalysis device, then add catalysis
Agent, reactor is closed, 180~200 DEG C are heated up to, 3.0~4.0h of stirring reaction；Wherein, H2O addition and high concentration nonyl
Base phenol polyethenoxy ether wastewater volume ratio is 1:5~1:6；
(2) after reaction terminates, reactor natural cooling, solid-liquid two-phase mixture in reactor is discharged, separation of solid and liquid, will
Obtained solid matter is dried, and obtains solid adsorbent.
Waste water is to be produced in industrial production, thick organic liquid waste is presented in the step (1), and is difficult to conventional useless
Method for treating water processing is up to standard.
Step (1) the middle and high concentration NPE waste water addition accounts for the 1/2 of reactor dischargeable capacity.
Catalyst is 98% concentrated sulfuric acid and ground hematite in the step (1)；Wherein, the throwing amount of ground hematite is 1.0
~2.0g/ (L waste water), 98% concentrated sulfuric acid throwing amount are 0.1g/ (L waste water).
Solid-liquid two-phase mixture is the mixture of solid adsorbent and reaction residue in the step (2).
The raffinate that separation of solid and liquid obtains in the step (2) is the organic wastewater that COD is less than 500mg/L.
Solid matter is powdered in the step (2).
Solid absorbent adsorption capacity is 0.1~0.2g COD/ (g adsorbents) in the step (2).
A kind of high concentration NPE waste water thermocatalytic of the present invention prepares the device of solid adsorbent, including
Heat catalysis kettle, wherein being provided with heat catalysis kettle agitator, lower end and solid-liquid among described heat catalysis kettle upper end
Two phase reaction product discharge line is connected, and described heat catalysis kettle agitator side, heat catalysis kettle upper end are provided with
Line pressure meter and pressure alarm, opposite side are provided with online thermometer and temperature alarm, described heat catalysis kettle side,
Lower end is provided with and overhauled into hole, and described heat catalysis kettle inner side is provided with electric heater, described heat catalysis kettle
Two sides upper end is respectively equipped with decompression outgassing pipe and feeding liquid pipeline, and described decompression outgassing pipe is provided with decompression releasing valve, institute
On the heat catalysis kettle stated, decompression outgassing pipe lower end be provided with overflowing liquid delivery pipe, described overflowing liquid delivery pipe is provided with excessive
Flow liquid drain valve, described overflowing liquid delivery pipe lower end be provided with overflowing liquid accept pond, described feeding liquid pipeline by catalyst,
Acid add pipe respectively drug slot molten with ground hematite catalyst and sulfuric acid dispensing groove be connected and described feeding liquid pipeline be catalyzed
Agent, acid add pipe connection both sides and are respectively equipped with feeding liquid regulating valve, described feeding liquid pipeline be connected with running water water inlet pipe and
Between feeding liquid regulating valve, described running water water inlet pipe is provided with running water inlet regulating valve, described red iron for junction
The molten drug slot of catalyst and sulfuric acid dispensing groove upper end are respectively equipped with molten drug slot mixer and dosing pump.
A kind of a kind of high concentration NPE waste water thermocatalytic described in use prepares the dress of solid adsorbent
The method put, wherein described device use the interval batch-type course of work, comprise the following steps：
(a) waste liquid inlet valve, control valve, outgassing valve, overflow pipe control valve are opened；Close draining valve, originally
Water water intaking valve；Open waste liquid intake pump and pending waste liquid is conveyed into heat catalysis device, have waste liquid outflow into overflow pipe, then
Show that waste liquid amount has reached specified treating capacity in reactor；Close waste liquid inlet valve, overflow pipe control valve；Open running water
Water intaking valve, mixer is opened, open catalyst and alkali chemicals feed pump, until amount of water and chemical feeding quantity reach design parameter；Closing is urged
Agent and acid add pump；Close running water water intaking valve, regulating valve, releasing valve；So far fill process is completed；
(b) reaction mechanical stirrer, electric heater are opened, stirs simultaneously 3.0~4.0h of heating response；Be then shut off mixer,
Electric heater, complete natural cooling after heat catalysis；So far course of reaction is completed；
(c) open draining valve and discharge solid-liquid two phase reaction product, the solid product warp through precipitating or being centrifugally separating to obtain
It is prepared solid adsorbent after drying.
The safe operation protection technique measure of described heat catalysis kettle 2 is：Signal is fed back to by online thermometer
PLC automatic control system, electric heater is controlled by automatic control system, reactor temperature is maintained normal working temperature
Scope；When reactor temperature exceedes the scope of safe working temperature, temperature alarm is alarmed and automatically cuts off heating power supply；
When reactor pressure exceedes safe-working pressure scope, pressure alarm is alarmed and automatically cuts off heating power supply, and is passed through
Automatic control system opens releasing valve, quickly to reduce reactor pressure.
The principle of the present invention is under certain temperature and pressure condition in heat catalysis kettle, in ferriferous oxide, acid
The NPE in high-concentration waste water is carbonized under co-catalysis effect, being converted into it has stronger adsorption capacity
Solid adsorbent, thermocatalytic raffinate is converted into low-concentration organic waste water, realizes innoxious and recycling.The present invention can solve the problem that
The processing of the insoluble high concentration base phenol polyethenoxy ether wastewater of Conventional waste water treatment technology and handling problems, and pass through preparation
The higher adsorbent of added value creates larger benefits of environment and economy.
The scope of application of the present invention is caused high concentration NPE waste water in industrial production, due to organic
Thing concentration is higher and NPE is hard-degraded substance, can not use Conventional waste water processing method processing qualified discharge.
, can such is difficult and disposal high concentrated organic waste liquid be innoxious and recycling by method proposed by the present invention.
Being mainly characterized by for the present invention is simple to operate；Compared with the technologies such as anaerobic methane production, it is organic to be not only restricted to high concentration
The property of waste liquid, it is applied widely；It is easy to be engineered.The present invention is harmless for difficult high concentration NPE waste water
Change and recycling provides a kind of economically viable method, meet the developing direction of industrial circle energy-saving and emission-reduction.
The present invention is directed to caused high-concentration hardly-degradable NPE waste water in industrial production, it is proposed that a kind of
Waste liquid middle and high concentration NPE is converted into the method and reactor of solid adsorbent by thermocatalytic.This method
The solid matter of generation can do water treatment absorbent；The liquid content of organics of generation is relatively low, through materialization, biochemical waste water group
Secondary pollution can will not be caused to environment with qualified discharge after closing PROCESS FOR TREATMENT.
Beneficial effect
(1) the high concentration nonyl phenol that the present invention can solve the insurmountable high concentrated organic waste liquid of conventional waste water processing gathers
Oxygen vinethene wastewater treatment and handling problems；
(2) in method of the invention after heat catalysis, NPE organics dehydration is carbonized in waste liquid
The stronger solid adsorbent of adsorption capacity is formed afterwards, available for wastewater treatment；
(3) present invention is catalyzed in carbonisation in caused secondary liquid waste because organic matter majority is by carbon in waste liquid hydro-thermal
Change, it is very low (between 100~500mg/L) containing COD concentration, it is entirely capable of meeting after materialization, the processing of biochemical waste water group technology
Qualified discharge requirement；Secondary pollution will not be produced.
Brief description of the drawings
Fig. 1 is the installation drawing that middle and high concentration NPE waste water thermocatalytic of the present invention prepares solid adsorbent；
Fig. 2 is the workflow diagram of heat catalysis device when method is implemented in the present invention.
Embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate the present invention
Rather than limitation the scope of the present invention.In addition, it is to be understood that after the content of the invention lectured has been read, people in the art
Member can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited
Scope.
Embodiment 1
High concentration NPE waste water in the present embodiment is derived from certain fluoropolymer company production technology, COD
Up to 200000mg/L, early stage once can not obtain with advanced oxidization methods such as ozone, Fentons and its with the group technology of biology
Notable treatment effect.Using the present embodiment propose thermocatalytic technology this kind of high concentration raffinate is handled, specific method and
Step is：(1) high concentration NPE waste water is injected in heat catalysis device；(2) by catalyst ground hematite
Injected respectively by 1.5g/ (L waste liquids), 0.1g/ (L waste liquids) dosage in reactor with 98% concentrated sulfuric acid, closed reactor；
(3) reactor is heated up to 190 DEG C, stirring reaction 3.0h；(4) after cooling down, discharge residue in reactor and carry out solid-liquid point
From, by obtained black powder solid matter after drying be solid adsorbent, can be used for the other low concentrations of company and give up
Water adsorption treatment.Reaction residue COD is only 300~400mg/L, can be discharged into company's centralized wastewater treatment station be uniformly processed it is rear up to standard
Discharge.
The high concentration NPE waste water thermocatalytic used in the present embodiment prepares the device of solid adsorbent,
As shown in figure 1, including heat catalysis kettle 2, wherein being stirred among the described upper end of heat catalysis kettle 2 provided with heat catalysis kettle
Mix device 1, lower end and solid-liquid two phase reaction product discharge line 25 to connect, the described side of heat catalysis kettle agitator 1, heat are urged
Change the upper end of reactor 2 and be provided with online thermometer 10 and temperature alarm provided with online pressure gauge 3 and pressure alarm 4, opposite side
11, the described side of heat catalysis kettle 2, lower end, which are provided with, overhauls into hole 22, is set in the described inner side of heat catalysis kettle 2
There is electric heater 21, the described two sides upper end of heat catalysis kettle 2 is respectively equipped with decompression outgassing pipe 6 and feeding liquid pipeline 13,
Described decompression outgassing pipe 6 is provided with decompression releasing valve 5, and on described heat catalysis kettle 2, the lower end of decompression outgassing pipe 6 is provided with
Overflowing liquid delivery pipe 8, described overflowing liquid delivery pipe 8 are provided with overflowing liquid drain valve 7, the described lower end of overflowing liquid delivery pipe 8
Pond 9 is accepted provided with overflowing liquid, described feeding liquid pipeline 13 adds pipe 17,26 by catalyst, acid and urged respectively with ground hematite
The molten drug slot 19 of agent and sulfuric acid dispensing groove 20 connect and described feeding liquid pipeline 13 adds pipe 17,26 with catalyst, acid and is connected
Both sides are respectively equipped with feeding liquid regulating valve 12,16, and described feeding liquid pipeline 13 is connected with running water water inlet pipe 14 and junction
Between feeding liquid regulating valve 12,16, described running water water inlet pipe 14 is provided with running water inlet regulating valve 15, and described is red
The molten drug slot 19 of Iron Ore Powder catalyst and sulfuric acid dispensing groove 20 upper end are respectively equipped with molten drug slot mixer 18,27 and dosing pump
28、23。
Claims (8)
1. a kind of high concentration NPE waste water thermocatalytic prepares the device of solid adsorbent, including heat catalysis
Kettle (2), it is characterised in that：Heat catalysis kettle agitator (1), lower end are provided among described heat catalysis kettle (2) upper end
It is connected with solid-liquid two phase reaction product discharge line (25), described heat catalysis kettle agitator (1) side, heat catalysis
Kettle (2) upper end is provided with online pressure gauge (3) and pressure alarm (4), opposite side are provided with online thermometer (10) and temperature alarming
Device (11), described heat catalysis kettle (2) side, lower end are interior into hole (22), described heat catalysis kettle (2) provided with overhauling
Portion side is provided with electric heater (21), and described heat catalysis kettle (2) two sides upper end is respectively equipped with decompression outgassing pipe (6)
With feeding liquid pipeline (13), described decompression outgassing pipe (6) is provided with decompression releasing valve (5), described heat catalysis kettle (2)
Upper, decompression outgassing pipe (6) lower end is provided with overflowing liquid delivery pipe (8), and described overflowing liquid delivery pipe (8) discharges provided with overflowing liquid
Valve (7), described overflowing liquid delivery pipe (8) lower end are provided with overflowing liquid and accept pond (9), and described feeding liquid pipeline (13) is by urging
Agent, acid add pipe (17,26) and are connected and described with the molten drug slot of ground hematite catalyst (19) and sulfuric acid dispensing groove (20) respectively
Feeding liquid pipeline (13) with catalyst, acid add pipe (17,26) and be connected both sides and be respectively equipped with feeding liquid regulating valve (12,16),
Described feeding liquid pipeline (13) is connected with running water water inlet pipe (14) and junction is between feeding liquid regulating valve (12,16),
Described running water water inlet pipe (14) is provided with running water inlet regulating valve (15), the described molten drug slot of ground hematite catalyst
(19) and sulfuric acid dispensing groove (20) upper end is respectively equipped with molten drug slot mixer (18,27) and dosing pump (28,23).
2. the high concentration NPE waste water thermocatalytic described in a kind of usage right requirement 1 prepares solid adsorbent
The method of device, it is characterised in that described device uses the interval batch-type course of work, comprises the following steps：
(a) waste liquid inlet valve (12), control valve (16), outgassing valve (5), overflow pipe control valve (7) are opened；The row of closing
Water valve (24), running water water intaking valve (15)；Open waste liquid intake pump and pending waste liquid is conveyed into heat catalysis kettle, to overflow
There is waste liquid outflow in pipe (8), then show that waste liquid amount has reached specified treating capacity in reactor；Closing waste liquid inlet valve (12),
Overflow pipe control valve (7)；Running water water intaking valve (15) is opened, opens mixer (18,27), opens catalyst and alkali chemicals feed pump
(28,23), until amount of water and chemical feeding quantity reach design parameter；Close catalyst and acid adds pump (28,23)；Close running water
Water intaking valve (15), regulating valve (16), releasing valve (5)；So far fill process is completed；
(b) reactor mixer (1), electric heater (21) are opened, stirs simultaneously 3.0~4.0h of heating response；It is then shut off stirring
Machine (1), electric heater (21), complete natural cooling after heat catalysis；So far course of reaction is completed；
(c) open draining valve (24) and discharge solid-liquid two phase reaction product, the solid product warp through precipitating or being centrifugally separating to obtain
It is prepared solid adsorbent after drying.
3. the high concentration NPE waste water thermocatalytic described in a kind of usage right requirement 1 prepares solid adsorbent
The method of device, including：
(1) high concentration NPE waste water and water are added in described heat catalysis kettle (2), then added
Catalyst, reactor is closed, 180~200 DEG C are heated up to, 3.0~4.0h of stirring reaction；Wherein, H2O addition with it is highly concentrated
It is 1 to spend NPE wastewater volume ratio:5~1:6；Wherein, catalyst is 98% concentrated sulfuric acid and ground hematite；
(2) after reaction terminates, reactor natural cooling, solid-liquid two-phase mixture in reactor is discharged, separation of solid and liquid, will be obtained
Solid matter dry, obtain solid adsorbent.
4. one kind according to claim 3 prepares solid adsorbant using high concentration NPE waste water thermocatalytic
The method of the device of agent, it is characterised in that in the step (1) waste water be produced in industrial production, present it is thick organic
Waste liquid.
5. one kind according to claim 3 prepares solid adsorbant using high concentration NPE waste water thermocatalytic
The method of the device of agent, it is characterised in that step (1) the middle and high concentration NPE waste water addition accounts for reaction
The 1/2 of kettle dischargeable capacity.
6. one kind according to claim 3 prepares solid adsorbant using high concentration NPE waste water thermocatalytic
The method of the device of agent, it is characterised in that the throwing amount of ground hematite and the ratio of waste water are 1.0~2.0g in the step (1)：
1L；98% concentrated sulfuric acid throwing amount is 0.1g：1L.
7. one kind according to claim 3 prepares solid adsorbant using high concentration NPE waste water thermocatalytic
The method of the device of agent, it is characterised in that the raffinate that separation of solid and liquid obtains in the step (2) is COD having less than 500mg/L
Machine waste water.
8. one kind according to claim 3 prepares solid adsorbant using high concentration NPE waste water thermocatalytic
The method of the device of agent, it is characterised in that solid absorbent adsorption capacity is that (g inhales 0.1~0.2g COD/ in the step (2)
Attached dose).
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| JPS5855030A (en) * | 1981-08-28 | 1983-04-01 | チエスケ・ビソケ・ウセニ・テクニケ・ウ・プラゼ | Separation of isotope |
| JP2000288536A (en) * | 1999-04-08 | 2000-10-17 | Nec Corp | Method and apparatus for treating waste water containing hydrogen peroxide |
| CN104815612A (en) * | 2015-04-28 | 2015-08-05 | 程志宇 | Preparation method of molecular sieve adsorbent for metacresol and paracresol adsorption separation, and adsorbent prepared thereby |
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2016
- 2016-01-19 CN CN201610035247.6A patent/CN105540705B/en active Active
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|---|---|---|---|---|
| JPS5855030A (en) * | 1981-08-28 | 1983-04-01 | チエスケ・ビソケ・ウセニ・テクニケ・ウ・プラゼ | Separation of isotope |
| JP2000288536A (en) * | 1999-04-08 | 2000-10-17 | Nec Corp | Method and apparatus for treating waste water containing hydrogen peroxide |
| CN104815612A (en) * | 2015-04-28 | 2015-08-05 | 程志宇 | Preparation method of molecular sieve adsorbent for metacresol and paracresol adsorption separation, and adsorbent prepared thereby |
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