CN109173340B - Method for removing chlorine from strong acidic solution by adsorption - Google Patents
Method for removing chlorine from strong acidic solution by adsorption Download PDFInfo
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- CN109173340B CN109173340B CN201811321882.6A CN201811321882A CN109173340B CN 109173340 B CN109173340 B CN 109173340B CN 201811321882 A CN201811321882 A CN 201811321882A CN 109173340 B CN109173340 B CN 109173340B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/345—Regenerating or reactivating using a particular desorbing compound or mixture
- B01J20/3475—Regenerating or reactivating using a particular desorbing compound or mixture in the liquid phase
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/04—Chlorides
Abstract
A process for adsorbing and removing chlorine from strong acidic solution includes such steps as contacting the solution containing chlorine with the oxide or hydrate of trivalent antimony, adsorbing for removing chlorine, and filtering to obtain the dechlorinated liquid and dechlorinated filter residue. And then adding substances containing pentavalent antimony oxide and hydrate thereof into the primary dechlorinated liquid for secondary dechlorination, converting residual antimony and chlorine into pentavalent antimony or tetravalent antimony oxide and oxychloride thereof for precipitation and precipitation, and filtering to obtain secondary dechlorinated liquid and secondary dechlorinated filter residues, wherein the Cl content of the secondary dechlorinated liquid is less than 0.25g/L, and the Sb content is less than 0.03 g/L. Regenerating the primary dechlorination filter residue with alkali liquor, and regenerating the secondary dechlorination filter residue with alkali liquor containing oxidant for recycling. The invention has the advantages of good dechlorination effect, cleanness, environmental protection, economy, high efficiency and the like, and is suitable for the industrial application of dechlorination of strong acid solution.
Description
Technical Field
The invention relates to a method for adsorbing and removing chlorine from a strong acid solution, belonging to the field of metallurgy and chemical industry.
Background
Chlorine is a nonmetallic chemical element, is active in chemical property, can be combined with most metallic elements to form a compound, and most chlorides have good solubility in water. The chlorine-containing acidic solution is corrosive to metal equipment, and the chlorine is generated by the electrolysis of the acidic chlorine-containing solution, so that the environment is polluted. In addition, high concentration chlorine-containing waste liquid is a serious environmental hazard. Therefore, it is necessary to remove chlorine from the wastewater during the wastewater purification process. Common methods for removing chlorine from aqueous solutions are: chemical precipitation, solvent extraction, ion exchange, adsorption, and the like.
The chemical precipitation method is divided into a chloride precipitation method and an oxychloride precipitation method. Chloride precipitation, e.g. by addition of Ag to the solution+The chloride ions are precipitated in the form of AgCl, or the reducing agent is added after the copper sulfate is added to precipitate the chloride ions in the form of CuCl. The chlorine oxide precipitation method is to add metal oxide and its hydrate to a chlorine-containing solution and convert the solution into chlorine oxide under appropriate pH conditions, for example, adding bismuth hydroxide to a chlorine-containing solution to convert the solution into bismuth oxychloride, and removing chlorine from the solution. Dechlorinating the obtained chloride or chlorine-oxygen compound with sodium hydroxide or sodium carbonate solution, recycling, and evaporating the dechlorinated solution to crystallize sodium chloride. The chemical precipitation method has the disadvantages that the dechlorination reagent is large in loss in the using process, such as high solubility of cuprous ions, trivalent bismuth and the like in an acid solution, and the energy consumption of evaporating, concentrating and crystallizing sodium chloride from dechlorinated liquid is high, so that the industrial production is not acceptable.
The solvent extraction method is to adjust the pH value of a chlorine-containing solution to 6-8, then extract the chlorine in the solution to an organic phase through solvent extraction, and change the pH value of the solution, which is not allowable for most chemical and metallurgical technological processes.
The ion exchange method is to use anion exchange resin to adsorb chloride ions in a solution with the pH value of 2-7, the exchange capacity of the used resin is only 3-5mg/L, the ion exchange process comprises the working procedures of adsorption, desorption, regeneration and the like, the process is complicated, and finally the generated chlorine-containing wastewater needs to be treated by evaporation, concentration, crystallization and dechlorination.
The adsorption method mainly uses bismuth oxide to adsorb chlorine in solution and convert the chlorine into bismuth oxychloride, but the pH interval of bismuth oxychloride precipitate is narrow, the pH is 2.0-5.0, the loss of bismuth is serious when the pH is lower than 2.0, and the adsorption rate of chlorine is obviously reduced when the pH is higher than 5.0.
The existing methods can only remove chlorine from neutral or weak acidic solution, and the removal of chlorine from the strong acidic solution cannot be realizedForce. Although trivalent antimony can form antimony oxychloride with chlorine in a strong acid solution, the solubility of antimony oxychloride in the strong acid solution is high, chlorine in the strong acid solution is adsorbed by using antimony trioxide and a hydrate thereof, the chlorine removal effect is poor, the loss of antimony is large, and Cl in the adsorbed solution is high-The ion concentration is usually>1g/L, and wherein the concentration of Sb>0.3g/L, and the practical application process generally requires the residual Cl in the solution-Ion concentration<0.25 g/L. In addition, when the pH of the solution is adjusted>0.1, antimony oxychloride is difficult to form therein. Therefore, it has been almost nobody has been using antimony oxides and hydrates thereof for a long time to remove chlorine from solutions.
Disclosure of Invention
The invention aims to provide a method for adsorbing and removing chlorine from a strong acid solution, which has the advantages of good dechlorination effect, cleanness, environmental protection, economy and high efficiency.
The invention relates to a method for adsorbing and removing chlorine from a strong acid solution, which comprises the following steps:
the method comprises the following steps: dechlorination by primary adsorption
Using trivalent antimony oxide and hydrate thereof as a primary adsorption dechlorinating agent to adsorb chlorine in a strong acid solution, and filtering to obtain a primary dechlorinated liquid and a primary dechlorinated filter residue;
step two: dechlorination by secondary adsorption
And (3) using a substance containing pentavalent antimony oxide and hydrate thereof as a secondary adsorption dechlorinating agent, adding the secondary adsorption dechlorinating agent into the primary dechlorinated liquid, and filtering to obtain a secondary dechlorinated liquid and secondary dechlorinated filter residues.
The substance containing pentavalent antimony oxide and hydrate thereof refers to pentavalent antimony oxide and hydrate thereof or mixture of pentavalent antimony oxide and hydrate thereof and tetravalent antimony oxide and hydrate thereof.
The invention relates to a method for removing chlorine from strong acid solution by adsorption, wherein the solution after secondary dechlorination contains less than 0.25g/L of Cl and less than 0.03g/L of Sb.
The invention relates to a method for removing chlorine from a strong acid solution by adsorption, wherein a primary adsorption dechlorinating agent is added according to the proportion of 1-5 times of the theoretical amount of chlorine in the strong acid solution converted into antimony oxychloride, and the mixture is stirred for 0.5-3.5 hours at the temperature of 0-85 ℃.
The invention relates to a method for removing chlorine from a strong acid solution by adsorption, wherein a secondary adsorption dechlorinating agent is added according to the theoretical amount of antimony converted into tetravalent antimony which is 1-5 times of the theoretical amount of antimony in a solution after primary dechlorination, and the mixture is stirred for 1-10 hours at the temperature of 25-95 ℃ so that residual antimony and chlorine in the solution are converted into tetravalent antimony oxides and oxychlorides thereof.
The invention relates to a method for adsorbing and removing chlorine from a strong acidic solution, which is H+Cl-containing solution with ion concentration of more than or equal to 0.05mol/L-The solution of (1).
The invention relates to a method for adsorbing and removing chlorine from a strong acid solution, which comprises the steps of adding water into primary dechlorination filter residues, adding an alkaline substance containing sodium into the filter residues to adjust the pH value of the solution to 8-14, desorbing chlorine in the filter residues, filtering to obtain a first desorbed solution and a regenerated primary adsorption dechlorinating agent, and returning the regenerated primary adsorption dechlorinating agent to the first step for recycling.
The invention relates to a method for removing chlorine from a strong acid solution by adsorption, which comprises the steps of adding water into primary dechlorination filter residue according to the solid-to-liquid ratio of 1:1-6g/mL, adding an alkaline substance to adjust the pH value of the solution, and stirring at 0-100 ℃ or grinding and stirring for 0.5-5 h.
Adding water into secondary dechlorination filter residue, adding an alkaline substance containing sodium to adjust the pH value of the solution to 8-14, desorbing chlorine in the filter residue, adding an oxidant to oxidize low-valent antimony in the filter residue into pentavalent antimony or tetravalent antimony, filtering to obtain a second desorbed solution and a regenerated secondary adsorption dechlorinating agent, and returning the regenerated secondary adsorption dechlorinating agent to the second step for recycling.
The invention relates to a method for removing chlorine from a strong acid solution by adsorption, which comprises the steps of adding water into secondary dechlorination filter residues according to the solid-to-liquid ratio of 1:1-6g/mL, adding an alkaline substance to adjust the pH value of the solution, and stirring or grinding and stirring for 0.5-5h at the temperature of 0-100 ℃.
The invention relates to a method for removing chlorine from strong acid solution by adsorption, which comprises adding sodium-containing alkaline substance into the first and second desorbed solutions, utilizing the uniionic effect generated by sodium ions to force the chlorine to crystallize and separate out in the form of sodium chloride, filtering to obtain sodium chloride crystal and crystallized solution, and returning the crystallized solution to be used as regeneration solution of primary dechlorination filter residue or secondary dechlorination filter residue.
The invention relates to a method for removing chlorine from a strong acid solution by adsorption, wherein the sodium chloride crystallization refers to adding a sodium-containing alkaline substance into a chlorine-containing solution to enable Na in the solution to be Na+The ion concentration is increased to more than 6.2mol/L, and chlorine in the solution is forced to be crystallized and separated out in the form of sodium chloride by utilizing the same ion effect generated by sodium ions.
The invention relates to a method for removing chlorine from a strong acidic solution by adsorption, wherein a sodium-containing alkaline substance is at least one selected from sodium hydroxide, sodium carbonate and sodium bicarbonate.
The invention relates to a method for removing chlorine from a strong acid solution by adsorption, wherein an oxidant is at least one selected from hydrogen peroxide, chlorine and sodium hypochlorite.
The principle of the method for adsorbing and removing chlorine from a strongly acidic solution according to the present invention can be represented by the following reaction formula:
Sb2O3·xH2O+2Cl-+2H+＝2SbOCl+(x+1)H2O (1)
2Sb2O3·xH2O+2Cl-+2H+＝Sb4O5Cl2+(x+1)H2O (2)
Sb2O5·xH2O+2SbO++(x+1)H2O＝2Sb2O4·xH2O↓+2H+ (3)
Sb2O4·xH2O+4H++4Cl-＝2SbOCl2+(x+2)H2O (4)
2SbOCl+2OH-+(x-1)H2O＝Sb2O3·xH2O+2Cl- (5)
Sb4O5Cl2+2OH-+2(x-1)H2O＝2Sb2O3·xH2O+2Cl- (6)
2SbOCl2+4OH-+(x-2)H2O＝Sb2O4·xH2O+4Cl- (7)
Sb2O4·xH2O+H2O2＝Sb2O5·xH2O+H2O (8)
compared with the prior art, the invention has the following advantages and effects:
the invention uses antimony oxide and its hydrate as adsorbent, skillfully utilizes the adsorption effect of trivalent antimony on chlorine in strong acidic solution and the characteristic of small solubility of tetravalent antimony in the acidic solution, and adopts two-stage adsorption method to remove chlorine in the strong acidic solution, i.e. one stage uses trivalent antimony oxide and its hydrate to adsorb chlorine, and the other stage uses substance containing pentavalent antimony oxide and its hydrate to adsorb residual antimony in the solution, thus not only ensuring Cl in the adsorbed solution-Concentration of<0.25g/L, and can effectively remove arsenic in the solution. The invention can desorb and regenerate the loaded adsorbent for recycling, can separate and recover sodium chloride from the desorbed liquid, has the advantages of good dechlorination effect, cleanness, environmental protection, economy, high efficiency and the like, and is suitable for the industrial application of dechlorination of strong acid solution.
Detailed Description
The invention will now be further described with reference to the following examples, which are intended to illustrate the invention but not to limit it further.
Example 1
Get H+1.5m sulfuric acid leach liquor of 1.5mol/L metallurgical material3Adding hydrated oxide of trivalent antimony according to 4.5 times of theoretical amount of chlorine converted into antimony oxychloride, stirring at room temperature for 2.5h for primary dechlorination, and filtering to obtain primary dechlorinated filter residue and primary dechlorinated liquid. Then adding antimony pentoxide into the solution after the first dechlorination according to the amount 2.5 times of the theoretical amount of antimony converted into tetravalent antimony, stirring for 3.5h at 65 ℃ for second dechlorination, and filtering to obtain second dechlorination filter residue and second dechlorinated solution. The obtained secondary dechlorinated liquid contains 0.23g/L Cl and 0.02g/L Sb, acid in the secondary dechlorinated liquid is separated and recovered by diffusion dialysis, the obtained recovered acid is returned to be used for preparing leachate of metallurgical materials, and trapped liquid is used for extracting valuable metals in the leachate. Adding the obtained primary dechlorination filter residue into water according to the solid-to-liquid ratio of 1:2.5g/mL, and adding sodium hydroxideAdjusting pH of the solution to 9.5, stirring at 80 deg.C for 2.5h for regeneration, filtering to obtain desorbed solution and regenerated first-time adsorption dechlorinating agent, and returning the obtained regenerated first-time adsorption dechlorinating agent to the first-time dechlorinating process for recycling. Adding the obtained secondary dechlorination filter residue into water according to the solid-to-liquid ratio of 1:2g/mL, adding sodium carbonate, adjusting the pH value of the solution to 10, grinding and stirring for 0.5h at 50 ℃, adding a proper amount of hydrogen peroxide to oxidize low-valent antimony in the filter residue into pentavalent antimony, regenerating the pentavalent antimony, filtering to obtain desorbed solution and a regenerated secondary adsorption dechlorinating agent, and returning the obtained regenerated secondary adsorption dechlorinating agent to the secondary dechlorinating process for recycling. The dechlorination experiment result of the leaching solution of the metallurgical material is as follows:
example 2
Taking smelting flue gas to wash waste acid 0.5m3Adding hydrated oxide of trivalent antimony according to the proportion of 1.5 times of the theoretical amount of the chlorine in the chlorine-containing chlorine, stirring at room temperature for 1.5h for primary dechlorination, and filtering to obtain primary dechlorinated filter residue and primary dechlorinated liquid. Adding antimonic acid according to 2 times of theoretical amount of antimony converted into quadrivalent antimony in the dechlorinated liquid, stirring at 95 deg.C for 1.5 hr for secondary dechlorination, and filtering to obtain secondary dechlorinated filter residue and secondary dechlorinated liquid. The obtained secondary dechlorinated liquid contains 0.19g/L Cl and 0.02g/L Sb, and a dilute acid solution is obtained after defluorination. Adding the obtained primary dechlorination filter residue into water according to the solid-to-liquid ratio of 1:4g/mL, adding sodium carbonate to adjust the pH value of the solution to 10.5, stirring for 1.5h at 70 ℃ to regenerate the solution, filtering to obtain desorbed solution and a regenerated primary adsorption dechlorination agent, and returning the obtained regenerated primary adsorption dechlorination agent to the primary dechlorination process for recycling. Adding the obtained secondary dechlorination filter residue into water according to the solid-to-liquid ratio of 1:3.5g/mL, adding sodium hydroxide, adjusting the pH value of the solution to 9.5, adding a proper amount of sodium hypochlorite to oxidize low-valent antimony in the filter residue into pentavalent antimony, stirring at 90 ℃ for 2.5 hours to regenerate the filter residue, filtering to obtain desorbed solution and a regenerated secondary adsorption dechlorinating agent, and returning the obtained regenerated secondary adsorption dechlorinating agent to the secondary dechlorinating process for recycling. The experimental result of the dechlorination of the smelting waste acid is as follows:
| Cl | F | Cu | Zn | As | H2SO4 | |
| g/L of waste acid from smelting | 7.15 | 3.91 | 1.51 | 7.01 | 8.01 | 287.31 |
| Dechlorinated solution, g/L | 0.19 | 3.90 | 1.50 | 7.01 | 0.02 | 267.54 |
Claims (8)
1. A method for removing chlorine from a strongly acidic solution by adsorption, comprising the steps of:
the method comprises the following steps: dechlorination by primary adsorption
Using trivalent antimony oxide and hydrate thereof as a primary adsorption dechlorinating agent to adsorb chlorine in a strong acid solution, and filtering to obtain a primary dechlorinated liquid and a primary dechlorinated filter residue; the strongly acidic solution is H+Cl-containing solution with ion concentration of more than or equal to 0.05mol/L-The solution of (1);
step two: dechlorination by secondary adsorption
Using substance containing pentavalent antimony oxide and hydrate thereof as secondary adsorption dechlorinating agent, adding the secondary adsorption dechlorinating agent into the primary dechlorinated liquid, and filtering to obtain secondary dechlorinated liquid and secondary dechlorinated filter residue;
adding a primary adsorption dechlorinating agent according to the theoretical amount of 1-5 times of the chlorine in the strong acid solution converted into antimony oxychloride, and stirring at 0-85 ℃ for 0.5-3.5 h; adding a secondary adsorption dechlorinating agent according to the theoretical amount of antimony converted into tetravalent antimony which is 1-5 times of the theoretical amount of antimony in the liquid after primary dechlorination, and stirring for 1-10 h at 25-95 ℃; converting the residual antimony and chlorine therein into oxides of tetravalent antimony and oxychlorides thereof; the solution after the secondary dechlorination contains 0.25g/L of Cl and 0.03g/L of Sb.
2. The process according to claim 1, wherein the chlorine is removed from the strongly acidic solution by adsorption, and the process comprises the following steps: adding water into the primary dechlorination filter residue, adding an alkaline substance containing sodium to adjust the pH value of the solution to 8-14, desorbing chlorine in the filter residue, filtering to obtain a first desorbed solution and a regenerated primary adsorption dechlorinating agent, and returning the regenerated primary adsorption dechlorinating agent to the first step for recycling.
3. The process according to claim 2, wherein the chlorine is removed from the strongly acidic solution by adsorption, and the process comprises the following steps: adding water into the primary dechlorination filter residue according to the solid-to-liquid ratio of 1:1-6g/mL, and stirring or grinding and stirring at 0-100 ℃ for 0.5-5 h.
4. The process according to claim 2, wherein the chlorine is removed from the strongly acidic solution by adsorption, and the process comprises the following steps: adding water into the secondary dechlorination filter residue, adding an alkaline substance containing sodium to adjust the pH value of the solution to 8-14, desorbing chlorine in the filter residue, adding an oxidant to oxidize low-valent antimony in the filter residue into pentavalent antimony, filtering to obtain a second desorbed solution and a regenerated secondary adsorption dechlorinating agent, and returning the regenerated secondary adsorption dechlorinating agent to the second step for recycling.
5. The process according to claim 4, wherein the chlorine is removed from the strongly acidic solution by adsorption, and the process comprises the following steps: adding water into the secondary dechlorination filter residue according to the solid-to-liquid ratio of 1:1-6g/mL, and stirring or grinding and stirring for 0.5-5h at the temperature of 0-100 ℃.
6. The process according to claim 4, wherein the chlorine is removed from the strongly acidic solution by adsorption, and the process comprises the following steps: adding sodium-containing alkaline substances into the first desorbed solution and the second desorbed solution, using the same ion effect generated by sodium ions to force chlorine in the solutions to crystallize and separate out in the form of sodium chloride, filtering to obtain sodium chloride crystal and crystallized solution thereof, and returning the crystallized solution to be used as regeneration solution of primary dechlorination filter residue or secondary dechlorination filter residue.
7. The process for adsorptive removal of chlorine from strongly acidic solutions according to claim 6, wherein said crystallization of sodium chloride is carried out by adding an alkaline substance containing sodium to a chlorine-containing solution to make Na contained therein+The ion concentration is increased to more than 6.2mol/L, and chlorine in the solution is forced to be crystallized and separated out in the form of sodium chloride by utilizing the same ion effect generated by sodium ions.
8. The process for adsorptive removal of chlorine from strongly acidic solutions according to claim 4, wherein said sodium-containing basic substance is at least one selected from the group consisting of sodium hydroxide, sodium carbonate, sodium bicarbonate; the oxidant is at least one selected from hydrogen peroxide, chlorine and sodium hypochlorite.
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