CN108191105B - Resin purification treatment method for leaching wastewater from chlorinated tail gas - Google Patents
Resin purification treatment method for leaching wastewater from chlorinated tail gas Download PDFInfo
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- CN108191105B CN108191105B CN201711463123.9A CN201711463123A CN108191105B CN 108191105 B CN108191105 B CN 108191105B CN 201711463123 A CN201711463123 A CN 201711463123A CN 108191105 B CN108191105 B CN 108191105B
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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
Abstract
The invention belongs to the technical field of industrial wastewater treatment, and particularly relates to a resin purification treatment method for leaching wastewater by using chlorinated tail gas. The invention solves the technical problem of providing a resin purification treatment method for leaching waste water by using chlorinated tail gas, which comprises the following steps: a. adding hydrochloric acid into the wastewater, adjusting and controlling the pH of the system to be 1-2, and stirring to remove free chlorine; b. b, adsorbing and removing amphoteric metal and acidic metal impurities from the wastewater treated in the step a by using anion exchange resin; c. b, adding liquid alkali into the wastewater treated in the step b, and adjusting and controlling the pH of the system to be 9-11; d. and c, adsorbing and removing residual metal impurities in the wastewater treated in the step c by using cation exchange resin. The waste water treated by the method has extremely low content of other impurities except a large amount of NaCl, can be directly recycled by chlor-alkali industry, and can reduce or even eliminate TiCl supplied by the waste water4The environmental protection pressure brought by relevant manufacturers of the production can also reduce the production cost of the chlor-alkali industry.
Description
Technical Field
The invention belongs to the technical field of industrial wastewater treatment, and particularly relates to a resin purification treatment method for leaching wastewater by using chlorinated tail gas.
Background
TiCl4Is a main intermediate raw material of titanium industries such as titanium sponge and the like. At present, TiCl is industrially produced4Generally carried out by boiling chlorination and molten salt chlorination, and tail gas generated by a plurality of reasons such as side reaction of raw material impurities, low main reaction efficiency, insufficient subsequent condensation and the like in the production process generally contains HCl and Cl2、CO、CO2、SiCl4、TiCl4And a large amount of solid particles are mixed, so that in order to purify the tail gas to reach the discharge standard, a large amount of alkaline wastewater is generated after the tail gas is leached by liquid alkali, the wastewater is also the main wastewater of the chlorination procedure, and the wastewater amount is increased along with the increase of the yield. The wastewater contains NaClO and NaClO in addition to unreacted NaOH3、Na2CO3、TiO2Hydrates, and various metal hydroxides. At present, the wastewater is generally treated by a process of dechlorination → neutralization → filtration → discharge or slag spraying, and the wastewater cannot be comprehensively utilized. Because the components in the wastewater are complex and the types of impurities are more, most of the impurities in the wastewater cannot be removed by directly neutralizing. The NaCl content in the wastewater after dechlorination and neutralization treatment is more than 15 percent, so the method is used for slag sprayingThe sprinkling treatment affects the operation and also brings in impurities. With the annual increase of the environmental protection requirement, the leaching wastewater needs to be harmlessly recycled by a new method.
The chlorination process is generally carried out by supplying chlorine gas from a nearby chloralkali plant which produces liquid alkali by electrolysis of NaCl solution and simultaneously converts H produced by electrolysis2And part of Cl2The rest is sold for synthesis into hydrochloric acid, and a large amount of water brought out by the liquid caustic soda needs to be supplemented in the production process, and meanwhile, NaCl is purchased as a raw material.
The invention has the significance that different impurities in the wastewater are respectively adsorbed and separated by two kinds of resin, the treated wastewater has extremely low content of other impurities except a large amount of NaCl, is close to the drinking water standard (except pH value and NaCl), can be directly recycled by the chlor-alkali industry, can reduce or even eliminate the environmental protection pressure of the wastewater on related manufacturers, and can reduce the production cost of the chlor-alkali industry. The resin adsorption method is a common purification and impurity removal means in industry, wherein the resin can be repeatedly used in the life span, which is beneficial to reducing the production cost and is convenient for automatic control. The metal impurities adsorbed by the resin can be desorbed into high-concentration metal chloride waste liquid to be discharged when the resin is regenerated, and can be recovered as a raw material.
Disclosure of Invention
Aiming at the prior treatment of TiCl4The invention provides a novel resin purification treatment method for leaching waste water from chlorinated tail gas. The wastewater is TiCl production4The alkaline waste water containing free chlorine generated by leaching the tail gas of the chlorination procedure. The method of the invention firstly adds hydrochloric acid into the wastewater to reduce the pH value of the wastewater and converts the free chlorine in the wastewater into Cl2And stirring to remove free chlorine, then removing partial impurities by adopting anion resin, adjusting the pH of the system to be alkaline, and removing residual impurities by adopting cation resin, wherein the treated wastewater has extremely low content of other impurities except a large amount of NaCl, is close to the drinking water standard (except the pH value and the NaCl), can be directly recycled by the chlor-alkali industry, can reduce or even eliminate the environmental protection pressure brought by the wastewater to related manufacturers, and can reduce the production cost of the chlor-alkali industry.
The invention aims to solve the technical problem of providing a resin purification treatment method for leaching waste water by using chlorinated tail gas. The method comprises the following steps:
a. adding hydrochloric acid into the wastewater, adjusting and controlling the pH of the system to be 1-2, and stirring to remove free chlorine;
b. b, passing the wastewater treated in the step a through anion exchange resin;
c. b, adding liquid alkali into the wastewater treated in the step b, and adjusting and controlling the pH of the system to be 9-11;
d. and c, passing the wastewater treated in the step c through cation exchange resin to obtain a purified solution.
Preferably, in step a of the resin purification treatment method for leaching wastewater from chlorinated tail gas, the pH is 1.3.
Specifically, in step b of the resin purification treatment method for leaching wastewater from chlorinated tail gas, the anion exchange resin is a weakly basic primary amine, secondary amine or tertiary amine resin. D301 macroporous weakly basic tertiary amine anion exchange resin is preferred.
Preferably, in the step b of the resin purification treatment method for leaching wastewater from chlorinated tail gas, the operation temperature is controlled to be 35-45 ℃ and the flow rate is controlled to be 1-20 BV/h during adsorption.
Preferably, in step c of the resin purification treatment method for leaching wastewater from chlorinated tail gas, the pH is 9.7.
Specifically, in the step d of the resin purification treatment method for leaching wastewater from chlorinated tail gas, the cation exchange resin is an amine carboxyl chelating resin. The D403 type macroporous imine diacid chelating type cation exchange resin is preferable.
Preferably, in the step d of the resin purification treatment method for leaching wastewater from chlorinated tail gas, the operation temperature is controlled to be 60-70 ℃ and the flow rate is controlled to be 1-15 BV/h during adsorption.
Preferably, in step b or d of the resin purification treatment method for leaching wastewater from chlorinated tail gas, a plurality of adsorption towers are designed to alternately adsorb in turn, and the number of adsorption towers is more than 2.
Specifically, in step b or d of the resin purification treatment method for leaching wastewater from chlorinated tail gas, the desorption liquid of the exchange resin is hydrochloric acid, and the regeneration liquid is liquid alkali.
The method has the following beneficial effects:
1. the resin adsorption purification treatment process is mature, widely used, convenient for obtaining equipment and instruments, and easy for continuous production and automatic control.
2. The resin can be used repeatedly in the life cycle, and the rest of the needed raw materials, namely hydrochloric acid and liquid alkali, have low price and low cost.
3. The purification effect is good, and besides a large amount of NaCl and the pH value of 9-11, the content of other metal and nonmetal impurities is extremely low and is close to the drinking water standard (except the pH value and the NaCl).
4. The treated waste water can be directly used as production raw materials and supplementary water for production of chlorine raw material factories (chlor-alkali factories), the pH value does not need to be adjusted again, and the waste recycling rate is improved.
Detailed Description
The invention provides a resin purification treatment method for leaching waste water from chlorinated tail gas, and the waste water treated by the method contains a large amount of NaCl, has extremely low content of other impurities, is close to the drinking water standard (except pH value and NaCl), and can be directly recycled by the chlor-alkali industry.
A resin purification treatment method for chlorinated tail gas leaching wastewater comprises the following steps:
(1) adding hydrochloric acid into the wastewater to reduce the pH of the wastewater to 1-2, and stirring to remove free chlorine;
(2) adding the wastewater with the pH value reduced to acidity after removing free chlorine into an anion exchange resin tower to adsorb and remove the double metal and acidic metal impurities in the wastewater;
(3) adding liquid alkali into the wastewater treated by the anion exchange resin, and increasing the pH of the wastewater to 9-11;
(4) and adding the wastewater with the pH value increased to be alkaline into a cation exchange resin tower to adsorb and remove residual metal impurities in the wastewater to obtain a purified solution.
Preferably, in the above method, the pH in the step (1) is controlled to 1.3.
Specifically, in the above method, the step (1) of adding hydrochloric acid to the wastewater requires a gas (such as N) which is mechanically or non-reactive with the wastewater components2) Stirring was continued to accelerate chlorine evolution.
Specifically, in the method, a large amount of chlorine gas is emitted in the step (1), and collection and protection measures need to be taken.
Specifically, in the above method, the anion exchange resin in step (2) is a weak basic primary, secondary or tertiary amine-based resin. D301 macroporous weakly basic tertiary amine anion exchange resin is preferred.
Preferably, in the method, the control parameter range of the step (2) is 35-45 ℃ of the operating temperature and 1-20 BV/h of the flow rate.
Preferably, in the above method, the pH in the step (3) is controlled to 9.7.
Specifically, in the above method, the cation exchange resin in the step (4) is an amine carboxyl chelating resin. The D403 type macroporous imine diacid chelating type cation exchange resin is preferable.
Preferably, in the method, the control parameter range of the step (4) is 60-70 ℃ and the flow rate is 1-15 BV/h.
Specifically, in the above method, the resin towers in steps (2) and (4) should be designed as two-purpose towers, i.e. 3 resin towers each, to be switched in turn, in order to facilitate continuous production and ensure treatment effect.
Specifically, in the above method, the desorption liquid of the resin tower in the steps (2) and (4) is hydrochloric acid, and the regeneration liquid is liquid caustic soda, wherein the concentration requirement of the regeneration liquid of the anion exchange resin tower in the step (2) is low, and the regeneration liquid residual liquid after the cation exchange resin tower in the step (4) is used can be directly used, so as to reduce the liquid caustic soda consumption and reduce the cost.
Specifically, in the above method, the residual liquid discharged from the resin column in the steps (2) and (4) after desorption is enriched in the metal impurities adsorbed by the resin, and therefore contains a high concentration of metal components, and can be recovered as a raw material.
The following examples are provided to further illustrate the embodiments of the present invention and are not intended to limit the scope of the present invention.
Example 1 treatment of chlorinated Tail gas elution wastewater by the method of the present invention
TiCl in chlorination workshop of certain titanium sponge factory4Alkaline tail gas leaching wastewater generated by the chlorination production process contains a large amount of metal impurities such as Ca, Mg, Al, Fe, Co, Cu, V, Ti, Cr, Ni and the like and non-metal impurities such as Si and the like, and the impurity content is detected by using an inductively coupled plasma emission spectrometer and the like before treatment, and the results are shown in table 1:
TABLE 1
| Impurities | Ca | Mg | Si | Al | Fe | Co |
| Content (mg/L) | 6.26 | 6.174 | 0.7898 | 0.2741 | 0.3942 | 0.3392 |
| Impurities | Cu | V | Ti | Cr | Ni | Free chlorine |
| Content (mg/L) | 0.4151 | 2.4294 | 325.36 | 0.0223 | 0.0155 | 24400 |
The resin purification treatment method for the chlorinated tail gas leaching wastewater treats the wastewater, and comprises the following steps:
1. because the treated waste water is recycled by chlor-alkali industry, in order to avoid bringing in impurities, the acid is standard industrial synthetic hydrochloric acid with total acidity more than or equal to 31 percent. Firstly, hydrochloric acid is quickly added into the waste water, and Cl begins to exist along with the gradual reduction of pH in the process2Bubbles emerge and the wastewater is caused by Cl along with the continuous addition of the hydrochloric acid2The amount of bubbles rapidly increases and boils. When Cl is present2And gradually reducing the bubbles until the pH of the wastewater is close to the target range of 1-2 when the wastewater is calm. The hydrochloric acid addition was continued slowly and the final pH stabilized at 1.37. At this time, the wastewater still contains dissolved Cl2Thus using N2Stirring the wastewater for 10min, and detecting free chlorine to reduce to 75mg/L after stirring.
2. And adding the wastewater after dechlorination treatment into an anion exchange resin tower, wherein the selected resin is D301 type macroporous weak-base tertiary amino anion exchange resin, and the process control parameter range of the resin tower is that the operating temperature is 35-45 ℃ and the flow rate is 1-20 BV/h.
3. And detecting the pH value of the wastewater treated by the anion exchange resin tower, slowly adding liquid caustic soda into the wastewater, slightly increasing the pH value of the wastewater to a target range of 9-11, and slowly stirring the wastewater in the process to ensure that the reaction is more sufficient. Because the treated waste water is recycled by chlor-alkali industry, in order to avoid bringing impurities, the alkali is standard industrial liquid sodium hydroxide (liquid alkali) with the mass fraction of more than or equal to 30 percent.
4. And adding the wastewater with the pH value increased into a cation exchange resin tower, wherein the selected resin is D403 type macroporous imine diacid chelating type cation exchange resin, the process control parameter range of the resin tower is 60-70 ℃, the flow rate is 1-15 BV/h, and the purified wastewater is obtained after the treatment of the cation exchange resin tower.
After four steps of dechlorination, anion exchange resin treatment, pH adjustment and cation exchange resin treatment, the impurity content is detected by an inductively coupled plasma emission spectrometer, and the results are shown in Table 2:
TABLE 2
| Impurities | Ca | Mg | Si | Al | Fe | Co |
| Content (mg/L) | 0.0149 | 0.0011 | 0.5332 | 0.0418 | 0.0007 | 0.0005 |
| Impurities | Cu | V | Ti | Cr | Ni | Free chlorine |
| Content (mg/L) | 0.0005 | 0.0022 | 0.0654 | 0.0144 | 0.0062 | 75 |
In conclusion, the resin purification treatment method for the chlorinated tail gas leaching wastewater has a good purification effect.
Claims (5)
1. The resin purification treatment method of the chlorination tail gas leaching wastewater is characterized by comprising the following steps: the method comprises the following steps:
a. adding hydrochloric acid into the wastewater, adjusting and controlling the pH of the system to be 1-2, and stirring to remove free chlorine;
b. b, passing the wastewater treated in the step a through anion exchange resin; the anion exchange resin is D301 macroporous weak-base tertiary amino anion exchange resin; controlling the operation temperature to be 35-45 ℃ and the flow rate to be 1-20 BV/h during the adsorption;
c. b, adding liquid alkali into the wastewater treated in the step b, and adjusting and controlling the pH of the system to be 9-11;
d. c, passing the wastewater treated in the step c through cation exchange resin to obtain a purified solution; the cation exchange resin is D403 type macroporous imido diacid chelating type cation exchange resin; and during adsorption, the operation temperature is controlled to be 60-70 ℃, and the flow rate is controlled to be 1-15 BV/h.
2. The resin purification treatment method of chlorinated tail gas elution wastewater according to claim 1, which is characterized in that: in step a, the pH is 1.3.
3. The resin purification treatment method of chlorinated tail gas elution wastewater according to claim 1, which is characterized in that: in step c, the pH is 9.7.
4. The resin purification treatment method of chlorinated tail gas elution wastewater according to claim 1, which is characterized in that: in the step b or d, a plurality of resin adsorption towers are designed to alternately adsorb, wherein the number of resin adsorption towers is more than 2.
5. The resin purification treatment method of chlorinated tail gas elution wastewater according to claim 1, which is characterized in that: in the step b or d, the desorption liquid of the anion or cation exchange resin is hydrochloric acid, and the regeneration liquid is liquid alkali.
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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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| US3446719A (en) * | 1965-02-16 | 1969-05-27 | Olin Mathieson | Dechlorination of brine and recovery of chlorine |
| US5073355A (en) * | 1989-07-05 | 1991-12-17 | Kronos (U.S.A.), Inc. | Process for the removal of chlorine from off-gases |
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