CN105906111B - A method of salt is detached from coal chemical industrial waste water by electrodialytic technique - Google Patents
A method of salt is detached from coal chemical industrial waste water by electrodialytic technique Download PDFInfo
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Abstract
The invention discloses a kind of methods detaching salt from coal chemical industrial waste water by electrodialytic technique, it is characterised in that：The raw water of coal chemical industrial waste water is pre-processed first, then pretreated waste water is introduced into level-one electrodialysis, realize the separation of salt and COD, level-one electrodialysis concentrated water is introduced into two level electrodialysis again and is concentrated, gained concentrate is post-treated to isolate sodium sulphate and sodium chloride, i.e. completion is handled.The approach application electrodialysis of the present invention is separable and concentrates the characteristic of salt, COD in coal chemical industrial waste water after pretreatment is separated with salt, the salt after separation is concentrated again, solves the problems, such as that salt separates and recovers in coal chemical industrial waste water, realizes making full use of for solid salt resource；And entire technical process non-pollutant discharge, it is environmentally protective, it can be achieved that coal chemical industrial waste water " zero-emission " truly.
Description
Technical field
The invention belongs to industrial waste water treatments, and in particular to coal chemical wastewater treating technique with high salt.
Background technology
In recent years, with the fast development of coal chemical industry, influence of the waste water that coal chemical industry process generates to environment is more next
Bigger, country also begins to the discharge for going into overdrive to renovate coal chemical industrial waste water, makes " the zero-emission of coal chemical industrial waste water realization truly
It puts ".Coal chemical industrial waste water mainly based on high concentration gas washing wastewater, further include coking wastewater, coal gasified black water, coal directly/
Other waste water such as the waste water generated in indirect liquefaction waste water and syngas conversion catalyst preparation process.Containing a large amount of in waste water
The poisonous and harmful substances such as phenol, cyanogen, oil, ammonia nitrogen, huge discharge of wastewater, which seriously restricts coal chemical industry, to be continued to develop.Mesh
Before, coal chemical industry wastewater treating method includes mainly at preprocessing process, biochemical treatment process, waste water recycling processing and strong brine
Reason.Strong brine processing is generally using concentration, evaporation and drying and other treatment.Reverse osmosis concentration generally can be used in waste water recycling processing,
In this way reverse osmosis freshwater can direct reuse, but in reverse osmosis concentrated water (i.e. strong brine) still contain certain density COD (300-
1200mg/L).And due in concentrated water salt content it is very high, COD is difficult to the removal of the methods of conventional biochemistry in concentrated water.Strong brine is dry
Contain a large amount of COD after change processing in the solid salt that generates, impurity is excessive in salt, the purity of salt is relatively low, industrial application value
It is relatively low, therefore general directly progress solid landfill, the solid waste resource reutilization of coal chemical industrial waste water is cannot achieve, resource is caused
Waste, while certain pollution is also produced to environment.
Chinese patent (105217872 A of CN) reports a kind of processing method of coal chemical industrial waste water, first by coal chemical industrial waste water
It is pre-processed, then reverse osmosis concentration handles to obtain the first separating liquid and the first concentrate；The first separating liquid is returned again
For producing, the first concentrate carries out nanofiltration processing, obtains nanofiltration production water and nanofiltration concentrate；Finally by nanofiltration produce water and
Nanofiltration concentrate concentrates respectively, crystallization treatment obtains solid salt.This method is received with the first concentrate of method pair of nanofiltration
When filter processing, although there is 90% or more sodium chloride that can enter nanofiltration production water side through film, but still there is the chlorination close to 10%
Sodium remains in nanofiltration concentrated water side (salt of nanofiltration concentrated water side is mainly divalent salts), this will cause nanofiltration concentrated water by concentration, crystallization
Divalent purity salt is not high enough in the solid salt obtained after processing, reduces the added value of salt.In addition, pre- in the patent Example 2
Processing stage eliminates divalent magnesium component, remains divalent Calcium compounds, and Calcium compounds in solution mainly with calcium sulfate micro-soluble material
Form exists, and in subsequent nanofiltration concentration, calcium sulfate micro-soluble material easily blocks NF membrane, is unfavorable for serialization concentration.
In view of the above problems, if can the concentrated water after pretreatment, reverse osmosis concentration be carried out COD and mixed salt (1
Valence salt) separation, the salt that this will be fully in reuse coal chemical industrial waste water；In addition, after the salt in concentrated water is detached, in concentrated water
COD can be further processed, and be reduced to discharge standard.The mixed salt being separated in concentrated water can be by being further processed a divalent
Salt separates, and improves the industrial application value of salt.Electroosmose process can be realized by amberplex in material under electric field driven
The separation and concentration of ion to realize the separation and concentration of salt, while can retain molecular state substance.Currently, electrodialysis is
The fields such as sea water desalination, concentration salt manufacturing, industrial material desalination are applied to, and achieve good economic benefit.However, electric osmose
There is presently no application reports in coal chemical industrial waste water desalination field for analysis.
Invention content
To overcome the drawbacks described above of the prior art, the present invention is intended to provide it is a kind of by electrodialytic technique from coal chemical industrial waste water
The method of middle separation salt improves the secondary of salt in waste water to can effectively realize the separation of salt and COD in coal chemical industrial waste water
Utility value.
For achieving the above object, the present invention adopts the following technical scheme that：
The method that the present invention detaches salt by electrodialytic technique from coal chemical industrial waste water, feature are：First to coalification
The raw water of work waste water is pre-processed, and then pretreated waste water is introduced into level-one electrodialysis, realizes salt and point of COD
From, then level-one electrodialysis concentrated water is introduced into two level electrodialysis and is concentrated, gained concentrate is post-treated to isolate sodium sulphate
And sodium chloride, i.e. completion are handled.Specifically comprise the following steps：
(1) raw water of coal chemical industrial waste water is pre-processed, including organics removal, goes removing heavy metals, sofening treatment, mistake
Filter, RO concentrations so that for RO concentrates TDS in 30000-60000mg/L, COD content in 300-1200mg/L, gained RO fresh water is straight
It takes back and is used for production process；
(2) RO concentrates obtained by step (1) are passed through the electrodialytic diluting compartment of level-one, then to the electrodialytic enriched chamber of level-one
In be passed through distilled water, carry out electrodialysis, the salt in RO concentrates made to enter enriched chamber, realize the separation of salt and COD；
After separation, level-one electrodialysis concentrated water side is mainly mixed salt solution, and level-one electrodialysis fresh water side salt content is relatively low, master
Will group be divided into COD；
When level-one electrodialysis concentrated water TDS reaches 90000-100000mg/L, step (4) is carried out to it, and electric to level-one
Two level electrodialysis fresh water obtained by a certain amount of distilled water and/or step (4) is filled into dialysis enriched chamber；
When level-one electrodialysis fresh water TDS is down to 8000-10000mg/L, step (3) is carried out to it, and replaces level-one electricity
Dialysis diluting compartment feeding liquid；
(3) level-one electrodialysis fresh water is subjected to RO concentrations, makes gained RO concentrates TDS in 30000-60000mg/L, then will
Gained RO concentrates are back to further desalination in the electrodialytic diluting compartment of level-one, and gained RO desalination solutions direct reuse was in producing
Journey；
(4) by level-one electrodialysis concentrated water by volume 3~6:1 each leads into the electrodialytic diluting compartment of two level and concentration
Room carries out two level electrodialysis concentration, two level electrodialysis concentrated water TDS is improved, when two level electrodialysis fresh water TDS is down to 30000mg/L
When following, stop concentration；Two level electrodialysis fresh water returns to the electrodialytic enriched chamber of level-one, supplement charging；
(5) two level electrodialysis concentrated water is post-processed, isolates sodium sulphate and sodium chloride, that is, completed in coal chemical industrial waste water
The separation of salt.Two level electrodialysis concentrated water TDS may be up to 150000-200000mg/L, be conducive to subsequent separation salt process.
In step (2), in order to make level-one electrodialysis concentrated water TDS reach high value, can be arranged level-one electrodialysis diluting compartment and
Enriched chamber's input material volume ratio is 2~4:1.
The mode of step (5) described post-processing is：Two level electric osmose is detached using cryogenic freezing sodium sulfate crystal method first
The sodium sulphate in concentrated water is analysed, after filtering sodium sulphate, being evaporated again to filtrate makes sodium chloride be precipitated, and sodium chloride is obtained after filtering,
Filtrate may return in level-one electrodialysis diluting compartment and handle again.
Compared with prior art, the beneficial effects of the present invention are：
The present invention, can be by COD and mixed salt when to carrying out level-one electrodialysis separation by pretreated coal chemical industrial waste water
It is sufficiently separated out, the salt rate of recovery may be up to 99% or more, COD rejections and be up to 85%-95%, this solves with high salt useless well
The problem of salt recycles in water improves the secondary use value of salt in waste water；Level-one electrodialysis fresh water is passed through after repeatedly cycle,
Salt content therein can be reduced to 1000mg/L hereinafter, again handling the fresh water again by level-one electrodialysis, removed
COD realizes the recycling of water resource；Level-one electrodialysis concentrated water is concentrated using two level electrodialysis, and energy consumption is steamed than common multiple-effect
Hair and MVR are relatively low, have saved the cost of subsequent evaporation separation salt；In subsequent divalent salts separation process, first use low
Warm Refrigeration Technique separates sodium sulphate, then isolates sodium chloride by evaporation, and the sodium sulphate and sodium chloride obtained in this way is thick
The purity of product is higher, increases the added value of salt, avoids the solid waste landfill in conventional method, economical and environmentally friendly.Therefore, lead to
The salt crossed in electroosmose process separation coal chemical industrial waste water can realize " zero-emission " of coal chemical industrial waste water truly, realize salt and water
Recycling.
Description of the drawings
Fig. 1 is the process flow chart that electrodialytic technique of the present invention detaches salt from coal chemical industrial waste water.
Specific implementation mode
Present invention be described in more detail by the following examples, and electrodialytic technique detaches the side of salt from coal chemical industrial waste water
Method.
Embodiment 1
Electrodialysis plant used in the present embodiment is the CJED-90* of Hefei Ke Jia high molecular materials Science and Technology Ltd. production
The equipment of 210-5 models, used electrodialysis cation-exchange membrane and anion-exchange membrane are respectively the good macromolecule of Hefei section
CJMC the and CJMA films of material Science and Technology Ltd. production.
The raw water of coal chemical industrial waste water is pre-processed, including organics removal, go removing heavy metals, sofening treatment, filtering,
RO is concentrated so that RO concentrates TDS is in 45000-55000mg/L, COD content in 550-700mg/L.
The electrodialysis experiment of the present embodiment is the COD and salt in level-one electrodialysis separation waste water, specifically takes various concentration
Waste water carry out batch processing, per batch processing waste water (electrodialysis diluting compartment) 6L, for improve detach after salt content in concentrate,
It is 2L that the initial liquid in electrodialysis enriched chamber (distilled water), which is arranged,.Constant voltage mode, voltage is used to be fixed as 6V, experiment temperature in experimentation
Degree is 15-25 DEG C.Every batch of is tested in operational process, and when enriched chamber TDS rises to 90000-100000mg/L, enriched chamber is expected
Fluid exchange is new distilled water or two level electrodialysis fresh water；When diluting compartment TDS is down to 8000-10000mg/L, terminate batch reality
It tests, replaces diluting compartment feeding liquid, while initial liquid of the enriched chamber's solution of the batch as next batch enriched chamber.Again repeatedly into
Row next batch is tested, and has carried out the processing of 10 various concentration waste water altogether, related data is as shown in table 1.
1. level-one electrodialysis diluting compartment of table feeds TDS, COD variation, COD rejections, energy consumption
As can be known from Table 1, after the waste water of level-one electrodialysis process various concentration, the COD of level-one electrodialysis diluting compartment water outlet
It is above the COD of diluting compartment water inlet, this is because electrodialytic membranes has very strong crown_interception to COD, in addition, being run in electrodialysis
In the process, due to diluting compartment intermediate ion in the form of hydrated ion by amberplex, it is light so before and after electrodialysis operation
Change building volume opposite to reduce, has~20% water in this system in diluting compartment with Ion transfer to enriched chamber.Under every batch of,
COD rejections can reach 85-92%, and retention COD effects are preferable.In addition, energy consumption maintains essentially in electrodialysis operational process
8.5-11.5kWh/m3Between, operation energy consumption is relatively low, can save operating cost well.It is worth noting that, COD and salt
Separation is that other chemical engineering unit operations cannot achieve, and therefore, electrodialysis field of COD and salt in detaching coal chemical industrial waste water has
There is irreplaceable status, will also become a kind of indispensable technology in coal chemical industrial waste water processing.
Embodiment 2
It is concentrated again for level-one electrodialysis concentrated water (TDS 91500mg/L) in embodiment 1.Here the side concentrated
Method generally has multiple-effect evaporation and MVR, but the operation energy consumption of both processes is higher, and electrodialysis is a kind of ideal concentration
Method.Therefore, the present embodiment concentrates level-one electrodialysis concentrated water using two level electrodialysis again.Electrodialysis plant and embodiment
Equipment in 1 is identical, and when two level electrodialysis is run, voltage is fixed as 6V, and enriched chamber, diluting compartment charging are that level-one is electrodialytic
Concentrated water, enriched chamber, diluting compartment volume ratio are 1:4 and 1:5, experiment operation to two level electrodialysis fresh water TDS be down to 30000mg/L with
Stop concentration when lower, replaces enriched chamber, diluting compartment charging, carry out next batch concentration.Here two level electrodialysis fresh water can return to
Into the electrodialytic enriched chamber of level-one, for recycling salt；Two level electrodialysis concentrated water is used for postorder separation salt process.Two level electric osmose
The experimental data such as table 2 for analysing concentration indicates.
The TDS and electrodialysis operation energy consumption of 2. two level electrodialysis fresh water of table, concentrated water
It can be obtained from table 2, two level electrodialysis intakes TDS for 91500mg/L, when diluting compartment and enriched chamber's volume ratio are 4:1
When, when the electrodialytic fresh water TDS of two level is down to 23640mg/L, two level electrodialysis concentrated water TDS can be improved to 159320mg/L, carry
High effect is more apparent；When diluting compartment and enriched chamber's volume ratio are 5:When 1, two level electrodialysis fresh water TDS is down to 24270mg/L
When, two level electrodialysis concentrated water TDS can be improved to 183160mg/L, and concentrated effect has obtained further raising.In addition, two level is electric
The operation energy consumption of dialysis is in 14.31-14.43kWh/m3, operation energy consumption is relatively low, still can be obtained in industrial amplification process into
One step reduces, and therefore, electrodialysis concentration process has very strong Economic competitive.
It is 4 to diluting compartment and enriched chamber's volume ratio:1 two level electrodialysis concentrated water carries out freezing and crystallizing separating sodium sulfate, mistake
After filtering sodium sulphate, being evaporated to filtrate makes sodium chloride be precipitated, and sodium chloride is obtained after filtering.In whole process, the salt rate of recovery can
Reach 99% or more.After analyzing obtained sodium sulphate and sodium chloride crude product, the pure of sodium sulphate in sodium sulphate crude product is obtained
It spends and may be up to 92-98%, the purity of sodium chloride is up to 93-96% in sodium chloride crude product, and purity is higher, can reach Nacl mark
It is accurate.Therefore, for coal chemical industrial waste water with high salt after electrodialysis detaches, abundant recycling can be obtained in the salt in waste water, detaches useless after salt
Water can carry out post-processing and reach direct emission or reuse after discharge standard again, to realize coal chemical industrial waste water Zhong Shui and salt
It fully recycles, realizes coal chemical industrial waste water " zero-emission " truly.
Claims (3)
1. a kind of method detaching salt from coal chemical industrial waste water by electrodialytic technique, it is characterised in that：It is useless to coal chemical industry first
The raw water of water is pre-processed, and then pretreated waste water is introduced into level-one electrodialysis, realizes the separation of salt and COD, then
Level-one electrodialysis concentrated water is introduced into two level electrodialysis and is concentrated, gained concentrate is post-treated to isolate sodium sulphate and chlorination
The processing of sodium, i.e. completion；Specifically comprise the following steps：
(1) raw water of coal chemical industrial waste water is pre-processed, including organics removal, go removing heavy metals, sofening treatment, filtering,
RO is concentrated so that for RO concentrates TDS in 30000-60000mg/L, COD content in 300-1200mg/L, gained RO fresh water is direct
It is back to production process；
(2) RO concentrates obtained by step (1) are passed through the electrodialytic diluting compartment of level-one, then led into the electrodialytic enriched chamber of level-one
Enter distilled water, carry out electrodialysis, the salt in RO concentrates is made to enter enriched chamber, realizes the separation of salt and COD；
When level-one electrodialysis concentrated water TDS reaches 90000-100000mg/L, step (4) is carried out to it, and to level-one electrodialysis
Two level electrodialysis fresh water obtained by a certain amount of distilled water and/or step (4) is filled into enriched chamber；
When level-one electrodialysis fresh water TDS is down to 8000-10000mg/L, step (3) is carried out to it, and replace level-one electrodialysis
Diluting compartment feeding liquid；
(3) level-one electrodialysis fresh water is subjected to RO concentrations, makes gained RO concentrates TDS in 30000-60000mg/L, then by gained
RO concentrates are back to further desalination in the electrodialytic diluting compartment of level-one, and gained RO desalination solution direct reuses are in production process；
(4) by level-one electrodialysis concentrated water by volume 3~6:1 each leads into the electrodialytic diluting compartment of two level and enriched chamber, into
Row two level electrodialysis concentrates, and two level electrodialysis concentrated water TDS is improved, when two level electrodialysis fresh water TDS is down to 30000mg/L or less
When, stop concentration；Two level electrodialysis fresh water returns to the electrodialytic enriched chamber of level-one, supplement charging；
(5) two level electrodialysis concentrated water is post-processed, isolates sodium sulphate and sodium chloride, that is, complete salt in coal chemical industrial waste water
Separation.
2. method according to claim 1, it is characterised in that：In step (2), level-one electrodialysis diluting compartment and enriched chamber's charging
Volume ratio is 2~4:1.
3. method according to claim 1, it is characterised in that：The mode of step (5) described post-processing is：Low temperature is used first
Freezing and crystallizing sodium sulphate method detaches the sodium sulphate in two level electrodialysis concentrated water, after filtering sodium sulphate, is evaporated again to filtrate
So that sodium chloride is precipitated, sodium chloride is obtained after filtering, filtrate may return in level-one electrodialysis diluting compartment and handle again.
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