CN109534532A - 1-CHLORO-2,4-DINITROBENZENE produces the processing method of waste water and implements the equipment of this method - Google Patents
1-CHLORO-2,4-DINITROBENZENE produces the processing method of waste water and implements the equipment of this method Download PDFInfo
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- CN109534532A CN109534532A CN201811624563.2A CN201811624563A CN109534532A CN 109534532 A CN109534532 A CN 109534532A CN 201811624563 A CN201811624563 A CN 201811624563A CN 109534532 A CN109534532 A CN 109534532A
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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
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C201/00—Preparation of esters of nitric or nitrous acid or of compounds containing nitro or nitroso groups bound to a carbon skeleton
- C07C201/06—Preparation of nitro compounds
- C07C201/12—Preparation of nitro compounds by reactions not involving the formation of nitro groups
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F2001/007—Processes including a sedimentation step
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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
- 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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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2303/00—Specific treatment goals
- C02F2303/16—Regeneration of sorbents, filters
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Abstract
The present invention provides a kind of processing method of 1-CHLORO-2,4-DINITROBENZENE production waste water and implements the equipment of this method.It the treating method comprises following steps: settling step: after 2,4-dinitrochlorobenzene production waste water is precipitated, isolated solid composition and liquid composition；Adsorption step: adsorption treatment is carried out to the liquid component using resin adsorption device；Desorption: after carrying out desorption processing to the resin adsorption device after carrying out adsorption treatment using desorbing agent, separation obtains desorption liquid.The processing method of 2,4-dinitrochlorobenzene production waste water of the invention can recycle to obtain 2,4-DNP sodium, to improve product yield, reduce the load impact to biochemical wastewater treatment.Recycling obtained 2,4- dinitrophenol sodium can be used for the production of black sulfide dye.In addition, waste water is after processing, COD value can be substantially reduced.
Description
Technical field
The present invention relates to a kind of processing method of 2,4-dinitrochlorobenzene production waste water and the equipment of implementation this method, belong to
Field of environment protection.
Background technique
1-CHLORO-2,4-DINITROBENZENE is the important chemical intermediate of one of dyestuff, pesticide, medicine and other fields.It is closed in dyestuff
At aspect, 2,4-dinitrochlorobenzene can be used for preparing chloro- 2, the 4- dinitroaniline of 6-；1-CHLORO-2,4-DINITROBENZENE can be also used for
Synthesize black sulfide dye.Therefore, 2,4-dinitrochlorobenzene is a kind of important dyestuff intermediate.
2,4-dinitrochlorobenzene is mainly using chlorobenzene or paranitrochlorobenzene as raw material, by being nitrified using nitration mixture, through dividing
From, washing obtain 1-CHLORO-2,4-DINITROBENZENE.In water-washing process, there are a small amount of 2,4-dinitrochlorobenzene and 2,4-DNP
Sodium needs to carry out wastewater treatment in waste water.But 2,4-dinitrochlorobenzene and 2,4-DNP sodium biodegradability be not strong,
There are certain toxicity and inhibition to biochemical sludge simultaneously.Therefore, the yield for yet reducing product is not recycled, is increased to environment
Pollution.
With the increase of environmental protection pressure, green, energy conservation, safety, economy, efficient waste water treatment process are developed as urgently
The technical issues of solution.
Summary of the invention
Problems to be solved by the invention
In view of the technical problems existing in the prior art, present invention firstly provides a kind of 2,4-dinitrochlorobenzene to produce waste water
Processing method.The processing method can recycle to obtain 2,4-DNP sodium, to improve product yield, reduce to sewage
The load impact of biochemical treatment.In addition, the 2,4-DNP sodium that recycling obtains can be used for the production of black sulfide dye.
Further, the present invention also provides the equipment for implementing 2,4-dinitrochlorobenzene production waste water, connection type is reasonable,
It allows continuous production.
The solution to the problem
The present invention provides a kind of processing method of 2,4-dinitrochlorobenzene production waste water comprising following steps:
Settling step: after 2,4-dinitrochlorobenzene production waste water is precipitated, isolated solid component and liquid
Body ingredient；
Adsorption step: adsorption treatment is carried out to the liquid component using resin adsorption device；
Desorption: after carrying out desorption processing to the resin adsorption device after carrying out adsorption treatment using desorbing agent, separation
Obtain desorption liquid.
The processing method of 2,4-dinitrochlorobenzene production waste water according to the present invention, wherein in the settling step: adjustment
The pH value of the 2,4-dinitrochlorobenzene production waste water is 0.5~8, preferably 1~6.5, is then precipitated.
The processing method of 2,4-dinitrochlorobenzene production waste water according to the present invention, wherein the adsorption step further include:
Adsorption treatment is carried out to the liquid component using desorption treated resin adsorption device；And/or
The flow for flowing through the liquid component of the resin adsorption device is 0.3~10BV/h.
The processing method of 2,4-dinitrochlorobenzene production waste water according to the present invention, wherein described in the adsorption step
Resin in resin adsorption device includes macroporous type nonpolar adsorption resin, it is preferable that the resin includes D101 macroporous absorption
Resin, DA201 macroporous absorbent resin, XDA resin, 106 macroreticular resins, Amberlite XAD04 resin, Amberlite
The combination of one or more of XAD16HP resin and Amberlite XAD1600 resin.
The processing method of 2,4-dinitrochlorobenzene production waste water according to the present invention, wherein the desorbing agent includes hydrogen-oxygen
Change the combination of one or more of sodium, methanol and ethyl alcohol, it is preferable that the desorbing agent includes sodium hydroxide；And/or
The flow for flowing through the desorbing agent of the resin adsorption device is 0.3~2BV/h.
The processing method of 2,4-dinitrochlorobenzene according to the present invention production waste water, wherein before the desorption and/
Or after the desorption, further includes:
Water-washing step: first with progress adsorption treatment described in water washing and/or desorption treated resin adsorption device；It is excellent
Selection of land,
The flow for flowing through the water of the resin adsorption device is 0.3~2BV/h.
The present invention also provides a kind of equipment of processing method for implementing 2,4-dinitrochlorobenzene production waste water of the invention,
It include: the settler being connected, the first separator, resin adsorption device and the second separator；Preferably,
First separator and/or the second separator include: 2-4 micro-filter being sequentially connected in series, it is described
Micro-filter is equipped with the filter screen that aperture is 30~80 μm.
Equipment according to the present invention, wherein between the settler and first separator, be provided with solid at
Divide collecting tank.
Equipment according to the present invention, wherein the resin adsorption device includes: that 3-5 be sequentially connected in series are filled with resin
The adsorption tower of column is recycled the adsorption tower and carries out adsorption treatment and desorption processing；Preferably,
The adsorption tower be connected with one of desorbing agent storage tank, water tank, cleaning solution recycling can, desorbed solution recycling can or
Two or more combinations.
Equipment according to the present invention, wherein after second separator, be connected with processing water collecting tank.
The effect of invention
The processing method of 2,4-dinitrochlorobenzene production waste water of the invention can recycle to obtain 2,4-DNP sodium,
To improve product yield, the load impact to biochemical wastewater treatment is reduced.It is available to recycle obtained 2,4- dinitrophenol sodium
In the production of black sulfide dye.In addition, waste water is after processing, COD value can be substantially reduced.
Further, the processing equipment of 2,4-dinitrochlorobenzene production waste water of the invention, connection type is reasonable, can be with
Realize continuous production.
Specific embodiment
It will be detailed below various exemplary embodiments, feature and aspect of the invention.Dedicated word " example herein
Property " mean " being used as example, embodiment or illustrative ".Here as any embodiment illustrated by " exemplary " should not necessarily be construed as
Preferred or advantageous over other embodiments.
In addition, in order to better illustrate the present invention, numerous details is given in specific embodiment below.
It will be appreciated by those skilled in the art that without certain details, the present invention equally be can be implemented.In other example,
Method well known to those skilled in the art, means, equipment and step are not described in detail, in order to highlight master of the invention
Purport.
<first embodiment>
First embodiment of the invention provides a kind of processing method of 2,4-dinitrochlorobenzene production waste water, including following
Step:
Settling step: after 2,4-dinitrochlorobenzene production waste water is precipitated, isolated solid component and liquid
Body ingredient recycles the solid component；
Wherein, the solid component contains 2,4-dinitrochlorobenzene, and the liquid component contains water, acid and is dissolved in acid
A small amount of 1-CHLORO-2,4-DINITROBENZENE.
Adsorption step: adsorption treatment is carried out to the liquid component using resin adsorption device；
Desorption: after carrying out desorption processing to the resin adsorption device after carrying out adsorption treatment using desorbing agent, separation
Obtain desorption liquid.
In the desorption liquid that the present invention obtains, according to the difference of desorbing agent, it can obtain containing heterogeneity.For example, using
When sodium hydroxide is as desorbing agent, 2,4-DNP sodium, sodium hydroxide and water can be contained in desorption liquid, as sulphur black
The raw material of the alkalization process of production, reaches comprehensive utilization.
In the present invention, precipitating refers to that three-level precipitates, and three-level precipitating refers to that there are three made of the connection of sedimentation basin side by side.It is logical
It crosses and is precipitated using three-level, a part of 2,4-dinitrochlorobenzene reuse 2,4-dinitrochlorobenzene production can be recycled.The precipitating step
In rapid, the pH value of the adjustable 2,4-dinitrochlorobenzene production waste water is 0.5~8, preferably 1~6.5, is then sunk
It forms sediment.
The adsorption step can also include: to be carried out using desorption treated resin adsorption device to the liquid component
Adsorption treatment.In the present invention, the resin adsorption device in the adsorption step can be the series connection of N (N >=2) grade adsorption tower
Resin adsorption device.By taking 3 tower, 2 grades of series models as an example, wherein third adsorption tower can be used as spare adsorption tower.First by first
Adsorption tower carries out waste water absorption at two-stage tandem resin adsorption device to the second adsorption tower group.After the first adsorption tower adsorption saturation
It switches to third adsorption tower (i.e. spare adsorption tower) to continue to adsorb, i.e., by the second adsorption tower to third adsorption tower group Cheng Xin's
Two-stage tandem resin adsorption device continues charging and carries out waste water absorption.As standby after the first adsorption tower is desorbed using desorbing agent simultaneously
Use adsorption tower.And so on, the continual progress adsorption treatment of entire resin adsorption device and desorption processing can obtain after separation
Obtain desorption liquid, also referred to as desorbed solution.In the present invention, the flow for flowing through the liquid component of the resin adsorption device is
0.3~10BV/h can effectively realize adsorption treatment under the flow, wherein BV is the resin admission space in resin column.
In the adsorption step, the resin in the resin adsorption device includes macroporous type nonpolar adsorption resin, preferably
Ground, the resin include D101 macroporous absorbent resin, DA201 macroporous absorbent resin, XDA macroporous absorbent resin, 106 macropore trees
Rouge, Amberlite XAD-4 macroporous absorbent resin, Amberlite XAD16HP macroporous absorbent resin and Amberlite
The combination of one or more of XAD1600 macroporous absorbent resin.Wherein, it is big to can be XDA-1 for XDA macroporous absorbent resin
Macroporous adsorbent resin, XDA-4 macroporous absorbent resin, XDA-5 macroporous absorbent resin, XDA-6 macroporous absorbent resin, XDA-8 macropore are inhaled
The macroporous absorbent resins such as attached resin.
In the present invention, the desorbing agent includes the combination of one or more of sodium hydroxide, methanol and ethyl alcohol,
Preferably, the desorbing agent includes sodium hydroxide, other impurity can not be introduced using sodium hydroxide, so that containing in desorption liquid
2,4-DNP sodium, sodium hydroxide and the water of proper ratio, the original for the alkalization process that can be produced directly as sulphur black
Material；And/or flowing through the flow of the desorbing agent of the resin adsorption device is 0.3~2BV/h.
In the present invention, before the desorption and/or after the desorption, further includes: water-washing step: first benefit
The progress adsorption treatment and/or desorption treated resin adsorption device is washed with water, to wash off in resin adsorption device
Remaining adsorbent and/or desorbing agent, when recycling, can effectively improve the adsorption effect of resin.Washing after washing simultaneously
Water can be washed with circulating sleeve, reduce the water of washing.Furthermore it is also possible to carry out one or many washings using clear water, washing is generated
Water can be recycled, such as: the washing water that upper level adsorption tower washs can be used as the washing water of next stage adsorption tower.
Specifically, adsorption tower is carried out 1 time before desorption or repeatedly washing when, wash for the 1st time obtained washing water into
Enter and refine pond, subsequent 2nd time or repeatedly washs obtained washing water and enter cleaning solution recycling can.To adsorption tower after desorption
When carrying out 1 time or repeatedly washing, the remaining desorbing agent on resin column can be eluted in the 1st washing water, wherein 2,4- dinitros
When the concentration of sodium phenate is higher, when being greater than 300ppm, desorbed solution recycling can be directly entered, subsequent 2nd time or repeatedly
It washs in obtained washing water, when the concentration of 2,4-DNP sodium is lower, when for example, 300ppm or less, into cleaning solution
Recycling can.
Preferably, the flow for flowing through the water of the resin adsorption device is 0.3~2BV/h.
The processing water that 2,4-dinitrochlorobenzene production waste water obtains after adsorption/desorption, is transported at sewage treatment
Reason.
<second embodiment>
Second embodiment of the present invention provides a kind of processing for implementing 1-CHLORO-2,4-DINITROBENZENE production waste water of the invention
The equipment of method, comprising: settler, the first separator, resin adsorption device and the second separator being connected.
First separator and/or the second separator include: 2-4 micro-filter being sequentially connected in series, it is described
Micro-filter is equipped with the filter screen that aperture is 30~80 μm；Preferably, first separator and the second separator
It include 2-4 micro-filter being sequentially connected in series, the outlet of usually upper level micro-filter connects next stage micro-filter
Import, and so on.In general, the entrance of first separator or the second separator, that is, first order micro-filter
The outlet of entrance, first separator or the second separator is the outlet of afterbody micro-filter.
The resin adsorption device, which can be, (is denoted as adsorption tower 1 to adsorption tower by the N+1 adsorption towers filled with resin column
N+1 N grades of series connection resin adsorption devices of the N+1 tower) being composed in series, one of adsorption tower are stand-by still, upper level adsorption tower
The entrance of outlet connection next stage adsorption tower.
Preferably, the resin adsorption device may include: a adsorption tower for being filled with resin column of 3-5 being sequentially connected in series,
That is: N takes 2-4, specifically, using 4 grades of 3 tower, 2 grades of series models, 4 tower, 3 grades of series models or 5 towers series models.It is recycled
The adsorption tower carries out adsorption treatment and desorption processing.It is preferred that the resin adsorption device is by 4 tower, 3 grades of concatenated adsorption tower groups
At.By taking 3 grades of 4 towers (being denoted as adsorption tower A, B, C, D) series connection as an example, the specific steps are as follows:
It is adsorbed 1. waste water enters after three-level precipitates by the thtee-stage shiplock resin adsorption device that adsorption tower A, B, C are formed, when
After adsorption tower A adsorption saturation, adsorption tower A stops into waste water and starts to be desorbed with desorbing agent, while adsorption tower B is as first
Adsorption tower is continued to adsorb waste water by 3 grades of series connection resin adsorption devices that adsorption tower B, C, D are formed；
2. after adsorption tower B adsorption saturation, adsorption tower B stops into waste water and starts to be desorbed with desorbing agent, while adsorption tower C makees
For first adsorption tower, the thtee-stage shiplock resin adsorption device being made of adsorption tower C, D, A continues to adsorb waste water；
3. after adsorption tower C adsorption saturation, adsorption tower C stops into waste water and starts to be desorbed with desorbing agent, while adsorption tower D makees
For first adsorption tower, the thtee-stage shiplock resin adsorption device being made of adsorption tower D, A, B continues to adsorb waste water；
4. after adsorption tower D adsorption saturation, adsorption tower D stops into waste water and starts to be desorbed with desorbing agent, while adsorption tower A makees
For first adsorption tower, the thtee-stage shiplock resin adsorption device being made of adsorption tower A, B, C continues to adsorb waste water.
Repeat above the 1.~4. step, entire resin adsorption device uninterruptedly carry out waste water absorption and resin desorption.
Preferably, between the settler and first separator, it is provided with solid component collecting tank.It is described solid
Body component collection tank is directly utilized for recycling solid component, i.e. 2,4-dinitrochlorobenzene.
The adsorption tower be connected with one of desorbing agent storage tank, water tank, cleaning solution recycling can, desorbed solution recycling can or
Two or more combinations.For example, the entrance of each adsorption tower can connect going out for the first separator by conversion valve
The outlet of mouth, desorbing agent storage tank；The outlet of each adsorption tower can connect entrance, the solution of the second separator by conversion valve
Analyse the entrance of liquid recycling can；Each adsorption tower and the first separator, desorbing agent storage tank, the second separator, desorbed solution recycle
A valve is both provided between tank.The entrance of each adsorption tower can connect the outlet of water tank by conversion valve, each
The outlet of adsorption tower can connect the entrance of washing water recovery tank by conversion valve.
In addition, it is connected with processing water collecting tank after second separator, to collect finally obtained processing water,
Then the processing water conservancy pump in collecting tank is delivered to sewage treatment processing.
The present invention uses N grades of series connection resin adsorption devices of N+1 tower, and the entrance and exit of each adsorption tower can be equipped with multiple
Valve realizes connection and switching between each adsorption tower, and liquid storage tank, desorbed solution recycling can, water tank and washing water recycling is desorbed
Tank is respectively independent in parallel with adsorption towers at different levels, and the adsorbent equipment is made to also serve as parsing (that is: desorption is handled) device and water washing device, and
And adsorption and desorption can carry out simultaneously, waste water and resin desorption are adsorbed in the entire continual realization of resin adsorption device, the company of realization
Continuous metaplasia produces, and waste water COD after resin adsorption can drop to 0~100ppm from 2000~5000ppm.
1-CHLORO-2,4-DINITROBENZENE production waste water of the invention recycles after processing to be obtained 2,4- dinitrophenol sodium and can be used for
Sulphur black product, it is possible to reduce the consumption of raw material 2,4-dinitrochlorobenzene, sodium hydroxide etc. reduces the discharge of pollutant, reaches
The effect of clean manufacturing, and may be implemented waste water be effectively treated and comprehensive utilization of resources.
Embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will
Understand, the following example is merely to illustrate the present invention, and should not be taken as limiting the scope of the invention.It is not specified in embodiment specific
Condition person carries out according to conventional conditions or manufacturer's recommended conditions.Reagents or instruments used without specified manufacturer is
It can be with conventional products that are commercially available.
Embodiment 1
It measures 1-CHLORO-2,4-DINITROBENZENE of the 26500mL after three-level precipitates and produces waste water (i.e. liquid component, its 2,4- dinitro
Base chlorobenzene content is 390ppm, COD 2650ppm), connection is constantly to equipped with the activated processed D101 macroporous absorption of 70mL
It is adsorbed in resin-column, control absorption flow is 1.0BV/h, and constantly absorption is up to adsorption saturation, to useless after absorption
Water is 15ppm with the content that HPLC is detected as 2,4-dinitrochlorobenzene, and detecting its COD is 50ppm.
By the exchange column equipped with D101 macroporous absorbent resin after absorption, 5% sodium hydroxide solution of 80ml heat is measured
Desorption processing is carried out, control desorption flow is 1.0BV/h, 85ml desorption liquid is obtained, through analyzing 2,4-DNP sodium content
It is 11.5%, is detected through HPLC, 2,4-DNP sodium purity is 97.6%.
Embodiment 2
It measures 1-CHLORO-2,4-DINITROBENZENE of the 24000mL after three-level precipitates and produces waste water (i.e. liquid component, its 2,4- dinitro
Base chlorobenzene content is 390ppm, COD 2650ppm), connection is constantly to equipped with activated processed 106 macroreticular resin of 70mL
It is adsorbed in exchange column, control absorption flow is 1.2BV/h, and constantly absorption is until the waste water after absorption is used in adsorption saturation
The content that HPLC is detected as 2,4-dinitrochlorobenzene is 12ppm, and detecting its COD is 55ppm.
By the exchange column equipped with 106 macroreticular resins after absorption, 5% sodium hydroxide solution for measuring 75ml heat is taken off
Attached processing, control desorption flow is 1.0BV/h, obtains 80ml desorption liquid, is analyzed 2,4-DNP sodium content and is
11.4%, it is detected through HPLC, 2,4-DNP sodium purity is 97.4%.
Embodiment 3
It measures 1-CHLORO-2,4-DINITROBENZENE of the 24000mL after three-level precipitates and produces waste water (i.e. liquid component, its 2,4- dinitro
Base chlorobenzene content is 390ppm, COD 2650ppm), connection is constantly to equipped with the activated processed XDA resins exchange of 70mL
It is adsorbed in column, control absorption flow is 1.0BV/h, and constantly absorption is until adsorption saturation uses HPLC to the waste water after absorption
The content for being detected as 2,4-dinitrochlorobenzene is 14ppm, and detecting its COD is 60ppm.
By the exchange column equipped with XDA resin after absorption, 5% sodium hydroxide solution for measuring 75ml heat is carried out at desorption
Reason, control desorption flow is 1.1BV/h, obtains 80ml desorption liquid, is 11.6% through analysis 2,4-DNP sodium content, warp
HPLC detection, 2,4-DNP sodium purity are 97.7%.
Embodiment 4
It measures 1-CHLORO-2,4-DINITROBENZENE of the 23000mL after three-level precipitates and produces waste water (i.e. liquid component, its 2,4- dinitro
Base chlorobenzene content is 390ppm, COD 2650ppm), connection is constantly to equipped with activated processed 106 macroreticular resin of 70mL
It is adsorbed in exchange column, control absorption flow is 1.8BV/h, and constantly absorption is until the waste water after absorption is used in adsorption saturation
The content that HPLC is detected as 2,4-dinitrochlorobenzene is 19ppm, and detecting its COD is 78ppm.
By the exchange column equipped with 106 macroreticular resins after absorption, 5% sodium hydroxide solution for measuring 75ml heat is taken off
Attached processing, control desorption flow is 1.5BV/h, obtains 80ml desorption liquid, is analyzed 2,4-DNP sodium content and is
11.3%, it is detected through HPLC, 2,4-DNP sodium purity is 97.6%.
Embodiment 5
Measure 1-CHLORO-2,4-DINITROBENZENE washing waste water (i.e. liquid component, its 2,4- dinitro of the 21800mL after three-level precipitates
Base chlorobenzene content is 390ppm, COD 2650ppm), connection is constantly to equipped with the activated processed Amberlite of 70mL
It is adsorbed in XAD1600 resin-column, control absorption flow is 0.6BV/h, and constantly absorption is up to adsorption saturation, to absorption
Waste water afterwards is 10ppm with the content that HPLC is detected as 2,4-dinitrochlorobenzene, and detecting its COD is 35ppm.
By the exchange column equipped with Amberlite XAD1600 resin after absorption, 5% sodium hydroxide of 70ml heat is measured
Solution carries out desorption processing, and control desorption flow is 0.8BV/h, 75ml desorption liquid is obtained, through analyzing 2,4-DNP sodium
Content is 11.8%, is detected through HPLC, and 2,4-DNP sodium purity is 97.8%.
The performance test results
By above-described embodiment 1-5 it can be seen that after precipitation 1-CHLORO-2,4-DINITROBENZENE washing waste water (i.e. liquid at
Divide, its 2,4-dinitrochlorobenzene content is 390ppm, COD 2650ppm), it is set by 106 or D, 101 macroporous absorbent resin etc.
After rouge adsorbent equipment adsorption treatment, and controls certain flow and carry out the waste water 2,4-dinitrochlorobenzene after adsorption treatment to it
Content is 10-19ppm, COD 35-78ppm.The sodium hydroxide solution of 5% heat of the resin after absorption is desorbed again, obtains 2,
2, 4-dinitrophenol sodium, detecting its purity through HPLC is 95 or more, reaches as high as 97.94%, 2,4-DNP in solution
Sodium content is 10% or more, can be 11.3%-11.8%.Simultaneously washing waste water COD from 2650ppm drop to 100ppm with
On, 35~78ppm can be dropped to.
The above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be to the present invention
Embodiment restriction.For those of ordinary skill in the art, it can also make on the basis of the above description
Other various forms of variations or variation.There is no necessity and possibility to exhaust all the enbodiments.It is all of the invention
Made any modifications, equivalent replacements, and improvements etc., should be included in the protection of the claims in the present invention within spirit and principle
Within the scope of.
Claims (10)
1. a kind of processing method of 2,4-dinitrochlorobenzene production waste water, which comprises the following steps:
Settling step: after 2,4-dinitrochlorobenzene production waste water is precipitated, isolated solid component and liquid at
Point；
Adsorption step: adsorption treatment is carried out to the liquid component using resin adsorption device；
Desorption: after carrying out desorption processing to the resin adsorption device after carrying out adsorption treatment using desorbing agent, separation is obtained
Desorption liquid.
2. the processing method of 2,4-dinitrochlorobenzene production waste water according to claim 1, which is characterized in that the precipitating
In step: the pH value for adjusting the 2,4-dinitrochlorobenzene production waste water is 0.5~8, preferably 1~6.5, is then sunk
It forms sediment.
3. the processing method of 2,4-dinitrochlorobenzene production waste water according to claim 1 or 2, which is characterized in that described
Adsorption step further include: adsorption treatment is carried out to the liquid component using desorption treated resin adsorption device；And/or
The flow for flowing through the liquid component of the resin adsorption device is 0.3~10BV/h.
4. the processing method of 2,4-dinitrochlorobenzene production waste water according to claim 1-3, which is characterized in that
In the adsorption step, the resin in the resin adsorption device includes macroporous type nonpolar adsorption resin, it is preferable that the tree
Rouge includes D101 macroporous absorbent resin, DA201 macroporous absorbent resin, XDA resin, 106 macroreticular resins, Amberlite XAD04
The combination of one or more of resin, Amberlite XAD16HP resin and Amberlite XAD1600 resin.
5. the processing method of 2,4-dinitrochlorobenzene production waste water according to claim 1-4, which is characterized in that
The desorbing agent includes the combination of one or more of sodium hydroxide, methanol and ethyl alcohol, it is preferable that the desorbing agent packet
Include sodium hydroxide；And/or
The flow for flowing through the desorbing agent of the resin adsorption device is 0.3~2BV/h.
6. the processing method of 2,4-dinitrochlorobenzene production waste water according to claim 1-5, which is characterized in that
Before the desorption and/or after the desorption, further includes:
Water-washing step: adsorption treatment and/or desorption treated resin adsorption device are carried out first with water washing；Preferably,
The flow for flowing through the water of the resin adsorption device is 0.3~2BV/h.
7. a kind of equipment for the processing method for implementing 2,4-dinitrochlorobenzene production waste water described in any one of claims 1-6,
It is characterised by comprising: the settler being connected, the first separator, resin adsorption device and the second separator；It is preferred that
Ground,
First separator and/or the second separator include: 2-4 micro-filter being sequentially connected in series, micro- mistake
Filter is equipped with the filter screen that aperture is 30~80 μm.
8. equipment according to claim 7, which is characterized in that between the settler and first separator,
It is provided with solid component collecting tank.
9. equipment according to claim 7 or 8, which is characterized in that the resin adsorption device includes: the 3- being sequentially connected in series
5 are filled with the adsorption tower of resin column, and the adsorption tower is recycled and carries out adsorption treatment and desorption processing；Preferably,
The adsorption tower is connected with one or both of desorbing agent storage tank, water tank, cleaning solution recycling can, desorbed solution recycling can
Above combination.
10. according to the described in any item equipment of claim 7-9, which is characterized in that after second separator, be connected with
Handle water collecting tank.
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