CN108191105A - A kind of Shu Zhi Jing Hua processing method of chlorinated exhaust wastewater eluting - Google Patents
A kind of Shu Zhi Jing Hua processing method of chlorinated exhaust wastewater eluting Download PDFInfo
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- CN108191105A CN108191105A CN201711463123.9A CN201711463123A CN108191105A CN 108191105 A CN108191105 A CN 108191105A CN 201711463123 A CN201711463123 A CN 201711463123A CN 108191105 A CN108191105 A CN 108191105A
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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
- 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
- C02F1/42—Treatment of water, waste water, or sewage by ion-exchange
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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
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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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
- C02F1/42—Treatment of water, waste water, or sewage by ion-exchange
- C02F2001/422—Treatment of water, waste water, or sewage by ion-exchange using anionic exchangers
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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
- C02F2103/18—Nature of the water, waste water, sewage or sludge to be treated from the purification of gaseous effluents
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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
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/29—Chlorine 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
- C02F2301/00—General aspects of water treatment
- C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
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- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
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Abstract
The invention belongs to industrial waste water treatments, and in particular to a kind of Shu Zhi Jing Hua processing method of chlorinated exhaust wastewater eluting.Technical problem solved by the invention includes the following steps there is provided a kind of Shu Zhi Jing Hua processing method of chlorinated exhaust wastewater eluting：A, hydrochloric acid is added in into waste water, adjustment control system pH is 1~2, stirring removing free chlorine；B, through step a treated waste water through anion exchange resin with the double property metals of adsorbing and removing and acid metal impurity；C, liquid caustic soda is added in the waste water of step b processing, adjustment control system pH is 9~11；D, through step c treated waste water through cation exchange resin with adsorbing and removing residual metallic impurity.Treated that waste water remaining impurity content in addition to containing a large amount of NaCl is extremely low for the method for the present invention, can directly be recycled by chlor-alkali industry, can decrease or even eliminate such waste water to TiCl4The environmental protection pressure that the relevant manufacturers of production are brought, and the production cost of chlor-alkali industry can be reduced.
Description
Technical field
The invention belongs to industrial waste water treatments, and in particular to a kind of Shu Zhi Jing Hua of chlorinated exhaust wastewater eluting
Processing method.
Background technology
TiCl4It is the main intermediate raw material of the Ti industries such as titanium sponge.At present, TiCl is industrially produced4Generally pass through the chlorine that boils
Change and fused salt chlorimation method carry out, in production process due to raw material impurity side reaction, main reaction efficiency is low, subsequent condensation is insufficient etc.
The tail gas that many reasons generate, typically contains HCl, Cl2、CO、CO2、SiCl4、TiCl4And it is mingled with a large amount of solid particles, for purification
Tail gas can generate a large amount of alkaline waste waters, such waste water is also chloride process to reach outer row's standard after liquid caustic soda elutes tail gas
Main waste water, and wastewater flow rate increases with yield and is increased.In this waste water in addition to the complete NaOH of unreacted, also containing NaClO,
NaClO3、Na2CO3、TiO2Hydrate and various metals hydroxide.At present, such waste water generally using dechlorination → neutralization →
Filtering → outer row or the process of slag sprinkling, waste water fail to realize comprehensive utilization.Due to complicated component, impurity kind in waste water
Class is more, and impurity most of in waste water can not be removed by directly carrying out neutralizing.Due in the waste water after dechlorinated neutralisation treatment
NaCl contents ＞ 15% sprays processing influence operation for slag and brings impurity into again simultaneously.With the raising year by year of environmental requirement,
Such wastewater eluting urgently carries out harmless recycling using new method.
Chloride process generally provides chlorine by neighbouring chlor-alkali plant, and chlor-alkali plant produces liquid caustic soda by electrolysis NaCl solution, together
When will be electrolysed generate H2With part Cl2(it is besides sold) synthesizes hydrochloric acid, needs largely to supplement what is taken out of by liquid caustic soda in production process
Water, while outsourcing raw material NaCl.
Meaning of the present invention is to distinguish impurity different in adsorbing separation waste water by two kinds of resins, treated waste water
In addition to containing a large amount of NaCl, remaining impurity content is extremely low, can be directly by chlor-alkali close to drinking water standard (in addition to pH value and NaCl)
Industry recycles, and can decrease or even eliminate environmental protection pressure and reduce chlor-alkali row that such waste water brought to relevant manufacturers
The production cost of industry.Resin adsorption method is industrial common purification and impurity removal means, and resin therein can be repeatedly in lifetime
It uses, advantageously reduces production cost, while convenient for automation control.The metal impurities that resin is adsorbed can in regenerating resin
It desorbs and is discharged for high concentration metal chloride waste solution, can be recycled as raw material.
Invention content
For existing processing TiCl4Chloride process tail gas elution it is wastewater produced the defects of, the present invention provides one kind
The Shu Zhi Jing Hua processing method of new chlorinated exhaust wastewater eluting.The waste water is production TiCl4Chloride process tail gas elution
Generated alkaline waste water containing free chlorine.The method of the present invention adds hydrochloric acid by elder generation into waste water reduces pH value of waste water, by waste water
In free chlorine be converted into Cl2And removing free chlorine is stirred, partial impurities are then removed using resin anion (R.A.), then adjust system
PH is alkalinity, then removes residual impurity using resin cation, and in addition to containing a large amount of NaCl, remaining impurity contains for treated waste water
It measures extremely low, close to drinking water standard (in addition to pH value and NaCl), can directly be recycled by chlor-alkali industry, can reduce or even disappear
Except the environmental protection pressure that such waste water is brought to relevant manufacturers, and the production cost of chlor-alkali industry can be reduced.
The technical problems to be solved by the invention are to provide a kind of Shu Zhi Jing Hua processing method of chlorinated exhaust wastewater eluting.
This method includes the following steps：
A, hydrochloric acid is added in into waste water, adjustment control system pH is 1~2, stirring removing free chlorine；
B, pass through anion exchange resin through step a treated waste water；
C, liquid caustic soda is added in the waste water of step b processing, adjustment control system pH is 9~11；
D, through step c treated waste water solution after cation exchange resin is to get purification.
Preferably, in the Shu Zhi Jing Hua process method step a of above-mentioned chlorinated exhaust wastewater eluting, the pH is 1.3.
Specifically, in the Shu Zhi Jing Hua process method step b of above-mentioned chlorinated exhaust wastewater eluting, the anion exchange tree
Fat is alkalescent primary amine, secondary amine or tertiary amine based resin.It is preferred that D301 type macroporous type alkalescent tertiary amine groups anion exchange resin.
Preferably, in the Shu Zhi Jing Hua process method step b of above-mentioned chlorinated exhaust wastewater eluting, control fortune during the absorption
Trip temperature is 35~45 DEG C, flow velocity is 1~20BV/h.
Preferably, in the Shu Zhi Jing Hua process method step c of above-mentioned chlorinated exhaust wastewater eluting, the pH is 9.7.
Specifically, in the Shu Zhi Jing Hua process method step d of above-mentioned chlorinated exhaust wastewater eluting, the cation exchange tree
Fat is amine carboxyl chelating resin.It is preferred that D403 type macroporous type imines diacyloxy chelating type cation exchange resins.
Preferably, in the Shu Zhi Jing Hua process method step d of above-mentioned chlorinated exhaust wastewater eluting, control fortune during the absorption
Trip temperature is 60~70 DEG C, flow velocity is 1~15BV/h.
Preferably, in Shu Zhi Jing Hua the process method step b or d of above-mentioned chlorinated exhaust wastewater eluting, multiple absorption are designed
Tower carries out alternate turns absorption, it is described it is multiple be 2 or more.
Specifically, in Shu Zhi Jing Hua the process method step b or d of above-mentioned chlorinated exhaust wastewater eluting, the solution of exchanger resin
Imbibition is hydrochloric acid, and regenerated liquid is liquid caustic soda.
The method of the present invention has the beneficial effect that：
1st, resin adsorption purification process technique it is ripe, using extensive, equipment, instrument are readily available, be easy to continuous production and
Automation control.
2nd, resin can in lifetime Reusability, remaining required raw material hydrochloric acid, liquid caustic soda are cheap, cost of material compared with
It is low.
3rd, good purification, in addition to being 9~11 containing a large amount of NaCl, pH value, remaining metal and nonmetallic inclusion content pole
It is low, close to drinking water standard (in addition to pH value and NaCl).
4th, treated, and waste water can supplement water directly as chlorine feed producer (chlor-alkali plant) raw materials for production and production, no
PH value need to be adjusted again, improve waste resource rate.
Specific embodiment
The present invention provides a kind of Shu Zhi Jing Hua processing method of chlorinated exhaust wastewater eluting, and treated that waste water removes for this method
Outside containing a large amount of NaCl, remaining impurity content is extremely low, can be directly by chlor-alkali row close to drinking water standard (in addition to pH value and NaCl)
Industry recycles.
A kind of Shu Zhi Jing Hua processing method of chlorinated exhaust wastewater eluting, includes the following steps：
(1) hydrochloric acid is added in into the waste water reduces the wastewater pH to 1~2, and stirs to remove free chlorine；
(2) it after removing free chlorine, has reduced pH value and has been added in anion exchange resin tower for acid waste water, to inhale
Double property metals and acid metal impurity in attached removing waste water；
(3) liquid caustic soda is added in into the waste water after anion exchange resin process, improves the wastewater pH to 9~11；
(4) waste water of the pH value for alkalinity will have been improved to be added in cation exchange resin tower, in adsorbing and removing waste water
Residual metallic impurity, the solution after being purified.
Preferably, in the above method, the pH controls of the step (1) are 1.3.
Specifically, in the above method, the step (1) need during hydrochloric acid is added in into the waste water with machinery or
Gas (such as N not reacted with waste component2) be persistently stirred to accelerate chlorine discharge.
Specifically, in the above method, there are a large amount of chlorine to emerge during the step (1), collection need to be carried out, protection is arranged
It applies.
Specifically, in the above method, the anion exchange resin of the step (2) is alkalescent is primary, secondary, tertiary amine groups tree
Fat.It is preferred that D301 type macroporous type alkalescent tertiary amine groups anion exchange resin.
Preferably, in the above method, control parameter ranging from 35~45 DEG C of running temperature, the flow velocity of the step (2)
For 1~20BV/h.
Preferably, in the above method, the pH controls 9.7 of the step (3).
Specifically, in the above method, the cation exchange resin of the step (4) is amine carboxyl chelating resin.It is preferred that
D403 type macroporous type imines diacyloxy chelating type cation exchange resins.
Preferably, in the above method, control parameter ranging from 60~70 DEG C of running temperature, the flow velocity of the step (4)
For 1~15BV/h.
Specifically, in the above method, the step (2), (4) resin tower, handled for ease of continuous production and guarantee
Effect, should separately design standby for dual-purpose one, i.e. each 3 of 2 kinds of resin towers switch in turn.
Specifically, in the above method, the step (2), (4) resin tower, stripping liquid is hydrochloric acid, and regenerated liquid is liquid
The anion exchange resin tower regeneration solution concentration requirement of alkali, wherein step (2) is relatively low, and the cation of step (4) can be used directly
Regenerated liquid raffinate after exchange resin tower use, to reduce liquid caustic soda consumption, reduce cost.
Specifically, in the above method, the step (2), (4) resin tower, the raffinate discharged after desorption be enriched by
The metal impurities of resin adsorption, therefore the metal component containing high concentration can be used as raw materials recovery.
The specific embodiment of the present invention is further described with reference to embodiment, is not therefore limited the present invention
System is among the embodiment described range.
Embodiment 1 handles chlorinated exhaust wastewater eluting using the method for the present invention
Certain titanium sponge factory chlorination workshop TiCl4Chlorination production technology generate alkaline tail gas wastewater eluting contain a large amount of Ca,
The nonmetallic inclusions such as the metal impurities such as Mg, Al, Fe, Co, Cu, V, Ti, Cr, Ni and Si, its impurity content of before processing use inductance
The detections such as coupling plasma emission spectrometer, the results are shown in Table 1：
Table 1
| Impurity | Ca | Mg | Si | Al | Fe | Co |
| Content (mg/L) | 6.26 | 6.174 | 0.7898 | 0.2741 | 0.3942 | 0.3392 |
| Impurity | Cu | V | Ti | Cr | Ni | Free chlorine |
| Content (mg/L) | 0.4151 | 2.4294 | 325.36 | 0.0223 | 0.0155 | 24400 |
Above-mentioned waste water is handled by the chlorinated exhaust wastewater eluting Shu Zhi Jing Hua processing method of the present invention, process
For：
1st, since processed waste water will be recycled by chlorine industry, to avoid bringing into impurity, acid used for total acidity >=
31% standard industry synthetic hydrochloric acid.Hydrochloric acid is rapidly joined into waste water first, begins with Cl as pH is continuously decreased in the process2
Bubble is emerged, and as hydrochloric acid is continuously added into, waste water is because of Cl2Bubbles volume quickly increases and is in boiling-like.Work as Cl2Bubble gradually subtracts
As little as waste water calmness when, wastewater pH is close to target zone 1~2.Continue to be slowly added to hydrochloric acid, final pH stabilization is 1.37.This
When waste water in still have the Cl of dissolving2, therefore use N210min is stirred to waste water, free chlorine is down to after testing after the completion of stirring
75mg/L。
2nd, by dechlorination, treated that waste water is added in anion exchange resin tower, and selected resin is weak for D301 type macroporous types
Basic tertiary amine base anion exchange resin, resin tower process control parameter ranging from 35~45 DEG C of running temperature, flow velocity 1~
20BV/h。
3rd, detection is through anion exchange resin tower treated pH value of waste water, and is slowly added to liquid caustic soda thereto, slightly carries
High wastewater pH is slowly stirred in the process to target zone 9~11 so as to react more abundant.Since processed waste water will be by chlor-alkali work
Industry recycles, and brings impurity into avoid, alkali used is the standard industry liquid sodium hydroxide (liquid of mass fraction >=30%
Alkali).
4th, the waste water for improving pH is added in cation exchange resin tower, selected resin is D403 type macroporous type imines
Diacyloxy chelating type cation exchange resin, resin tower process control parameter ranging from 60~70 DEG C of running temperature, flow velocity for 1~
15BV/h is purification waste water after the processing of cation exchange resin tower.
After dechlorinated-anion exchange resin process-tune pH- cation exchange resins handle four steps, impurity contains
Amount is through detections such as Inductively coupled plasma optical emission spectrometers, and the results are shown in Table 2：
Table 2
| Impurity | Ca | Mg | Si | Al | Fe | Co |
| Content (mg/L) | 0.0149 | 0.0011 | 0.5332 | 0.0418 | 0.0007 | 0.0005 |
| Impurity | Cu | V | Ti | Cr | Ni | Free chlorine |
| Content (mg/L) | 0.0005 | 0.0022 | 0.0654 | 0.0144 | 0.0062 | 75 |
It in summary it can be seen, there is the Shu Zhi Jing Hua processing method of chlorinated exhaust wastewater eluting of the present invention good purification to imitate
Fruit.
Claims (9)
1. the Shu Zhi Jing Hua processing method of chlorinated exhaust wastewater eluting, it is characterised in that：Include the following steps：
A, hydrochloric acid is added in into waste water, adjustment control system pH is 1~2, stirring removing free chlorine；
B, pass through anion exchange resin through step a treated waste water；
C, liquid caustic soda is added in the waste water of step b processing, adjustment control system pH is 9~11；
D, through step c treated waste water solution after cation exchange resin is to get purification.
2. the Shu Zhi Jing Hua processing method of chlorinated exhaust wastewater eluting according to claim 1, it is characterised in that：Step a
In, the pH is 1.3.
3. the Shu Zhi Jing Hua processing method of chlorinated exhaust wastewater eluting according to claim 1, it is characterised in that：Step b
In, the anion exchange resin is alkalescent primary amine, secondary amine or tertiary amine based resin；It is preferred that D301 type macroporous type alkalescent tertiary amines
Base anion exchange resin.
4. according to the Shu Zhi Jing Hua processing method of claims 1 to 3 any one of them chlorinated exhaust wastewater eluting, feature exists
In：In step b, control running temperature is 35~45 DEG C during the absorption, flow velocity is 1~20BV/h.
5. the Shu Zhi Jing Hua processing method of chlorinated exhaust wastewater eluting according to claim 1, it is characterised in that：Step c
In, the pH is 9.7.
6. the Shu Zhi Jing Hua processing method of chlorinated exhaust wastewater eluting according to claim 1, it is characterised in that：Step d
In, the cation exchange resin is amine carboxyl chelating resin；It is preferred that D403 type macroporous type imines diacyloxies chelating type is cationic
Exchanger resin.
7. according to the Shu Zhi Jing Hua processing method of claim 1~6 any one of them chlorinated exhaust wastewater eluting, feature exists
In：In step d, control running temperature is 60~70 DEG C during the absorption, flow velocity is 1~15BV/h.
8. the Shu Zhi Jing Hua processing method of chlorinated exhaust wastewater eluting according to claim 1, it is characterised in that：Step b
Or in d, design multiple resin adsorption towers and carry out alternate turns absorption, it is described it is multiple be 2 or more.
9. the Shu Zhi Jing Hua processing method of chlorinated exhaust wastewater eluting according to claim 1, it is characterised in that：Step b
Or in d, the stripping liquid of anion or cation exchange resin is hydrochloric acid, and regenerated liquid is liquid caustic soda.
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Cited By (3)
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| CN110606471A (en) * | 2019-09-18 | 2019-12-24 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for comprehensively utilizing low-temperature chlorination tail gas |
| CN113546446A (en) * | 2021-07-28 | 2021-10-26 | 江西东江环保技术有限公司 | Method for recovering copper in BCC synthetic mother liquor by using cationic resin |
| CN114956489A (en) * | 2022-07-07 | 2022-08-30 | 嘉兴启欣生态科技有限公司 | High-concentration salt-containing industrial wastewater treatment process |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110606471A (en) * | 2019-09-18 | 2019-12-24 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for comprehensively utilizing low-temperature chlorination tail gas |
| CN113546446A (en) * | 2021-07-28 | 2021-10-26 | 江西东江环保技术有限公司 | Method for recovering copper in BCC synthetic mother liquor by using cationic resin |
| CN114956489A (en) * | 2022-07-07 | 2022-08-30 | 嘉兴启欣生态科技有限公司 | High-concentration salt-containing industrial wastewater treatment process |
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| CN108191105B (en) | 2021-08-13 |
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