CN104556522A - Method for treating waste water containing vanadium and chromium - Google Patents
Method for treating waste water containing vanadium and chromium Download PDFInfo
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- CN104556522A CN104556522A CN201510004197.0A CN201510004197A CN104556522A CN 104556522 A CN104556522 A CN 104556522A CN 201510004197 A CN201510004197 A CN 201510004197A CN 104556522 A CN104556522 A CN 104556522A
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Abstract
The invention relates to a method for treating waste water containing vanadium and chromium. The method comprises the following steps of: (1) adsorption: adopting an adsorbing medium to adsorb vanadium and chromium ions in the waste water containing vanadium and chromium; (2) desorption: adding a desorption agent into the adsorbing medium containing vanadium and chromium ions obtained in the step (1) to carry out desorption; (3) vanadium precipitation: adding alkaline substances into desorption solution, stirring to be uniform, and then filtering to obtain a calcium-vanadate product and vanadium-precipitated supernant; (4) chromium crystallization: carrying out evaporating concentration and cooling crystallization on the vanadium-precipitated supernant to obtain a sodium-chromate crude product and crystallizing mother liquor; (5) recrystallization: heating and dissolving the sodium-chromate crude product, and carrying out cooling crystallization to obtain a sodium-chromate product and cooling-crystallizing mother liquor; and (6) returning of the crystallizing mother liquor: returning the crystallizing mother liquor to the step (2) as the ingredient of the analysis solution to be repeatedly utilized. The method has the advantages that the recovery rate for the vanadium and chromium elements in the waste water reaches 99.9% or higher, simultaneously high-purity calcium vanadate and sodium chromate are obtained, and no waste water and waste residue are generated in the whole process.
Description
Technical field
The present invention relates to the method for process trade effluent, be specifically related to the method for a kind of process containing vanadium, chrome waste water.
Background technology
Vanadium, chrome waste water are the trade effluents that vanadium slag produces in the explained hereafter barium oxide processes such as sodium roasting-leaching filtration-acid ammonium salt precipitation, its pentavalent vanadium content about 50ppm-100ppm, content of 6-valence Cr ions especially up between 500ppm-1000ppm, considerably beyond discharging standards.High price vanadium, chromium cpd are as serious pollution thing, and as outer row or leakage, can cause very big pollution to water body, edatope, farm crop do great damage, and seriously jeopardize HUMAN HEALTH, meanwhile, cause the waste of metals resources.
At present, process this kind of waste water more efficiently method have: (1) reduction moderate water-cut stage, number of patent application 201010591828.0 discloses and add reductive agent (as Sodium Pyrosulfite, sodium bisulfite etc.) in vanadium wastewater, make pentavalent vanadium, hexavalent chromium Restore All is trivalent, in the waste water solution after reduction, add alkali lye again, neutralized wastewater solution makes chromium, vanadium ion formation hydrate be precipitated out from waste water solution simultaneously.The method equipment is simple, treatment capacity is comparatively large, but have that vanadium chromium recovery ratio is low, precipitation waste residue directly cannot reclaim vanadium chromium valuable element, medicament add-on needs accurately to control that manipulation difficulty is large, reagent consumption amount is large, the more high defect of long processing period, processing cost.(2) conventional ion exchange process, even if spent ion exchange resin reclaims the anionic group in vanadium extracting waste water, reclaims the novel process of the vanadium in vanadium extracting waste water, chromium.The method operational path is simple, vanadium chromium adsorption rate is higher, but still there is many defects being difficult to avoid.Desorbed solution pregnant solution containing vanadium, chromium adopts traditional ammonium to sink technique: i.e. ammonium salt precipitation, filtration, filter cake calcining can obtain the V that purity is 99.8%
2o
5product.Precipitation supernatant liquor through reduction, neutralization heavy chromium, filtration, process, this process not only brings ammonia nitrogen waste water again, and can not realize the recycling of chromium.
Summary of the invention
The present invention is directed to the existing defect containing vanadium, chrome waste water treatment process, provide a kind of process containing the method for vanadium, chrome waste water, the method fast, efficient, cost is low, meanwhile, can truly realize vanadium, the recycling of chromium valuable element.
The object of the present invention is to provide a kind of process containing the method for vanadium, chrome waste water, comprise the steps:
1) adsorb: adopt adsorption medium to adsorb containing the vanadium in vanadium, chrome waste water, chromium ion, obtain the adsorption medium containing vanadium, chromium ion;
2) resolve: to step 1) obtain containing vanadium, chromium ion adsorption medium add resolve agent resolve, obtain desorbed solution, resolve after adsorption medium can reuse;
3) precipitation: add in desorbed solution after alkaline matter stirs and filter, obtain calcium vanadate product and precipitation supernatant liquor;
4) chromium crystallization: precipitation supernatant liquor step 3) obtained carries out evaporating, concentrated after, naturally cool to 25-45 DEG C, stirred crystallization 1-4h, obtain Sodium chromate crude product and crystalline mother solution;
5) recrystallization: be added to the water to the Sodium chromate crude product that step 4) obtains, controls Sodium chromate concentration at 300-500g/L, is heated to 60-100 DEG C of dissolving, naturally cools to 25-45 DEG C, crystallization 1-4h, obtain Sodium chromate product and crystalline mother solution;
6) crystalline mother solution returns: to step 4), 5) crystalline mother solution that obtains returns step 2) as the recycling of desorbed solution batching.
In the present invention, the adsorption medium in described step 1) is any one in anionite-exchange resin or anion-exchange fibre; Preferably, adsorption medium is strong basic type anion-exchange resin is D201.
In the present invention, described anion-exchange fibre, the product obtained for grafting season after polypropylene grafted vinylbenzene is amino.
In the present invention, described step 2) in resolution temperature be 20-80 DEG C.
In the present invention, described step 2) in resolve agent be the 1-5mol/L NaOH aqueous solution.
In the present invention, the alkaline matter in described step 3) is any one in calcium oxide, calcium hydroxide powder or calcium hydroxide slurry; Addition is v element amount of substance in desorbed solution: calcium constituent amount of substance=0.8:1-1.2:1 in alkaline matter.
In the present invention, in described step 3), stirring reaction temperature is 40-100 DEG C, and the stirring reaction time is 0.5-4h.
In the present invention, in described step 4), evaporation concentration refers to and precipitation supernatant liquor is evaporated to naoh concentration 40-45 wt %.
In the present invention, in described step 3), calcium vanadate product purity is more than 95%, and in described step 5), Sodium chromate product purity is more than 98%.
The present invention adopts anionite-exchange resin or anion-exchange fibre to adsorb completely or selectivity stepwise adsorption the high price vanadium in vanadium extracting waste water, chromium ion as adsorption medium, and its beneficial effect is:
(1) there is vanadium, chromium adsorption rate is high, the advantages such as rate of adsorption is fast; Realize vanadium, effective separation of chromium component and the recycling of valuable element, and vanadium, chromium element all can obtain GB level product, sell, whole flow process produces without waste water and dregs.
(2) ion-exchange fiber or resin is adopted to have better adsorption selectivity, the adsorptive power extremely strong to high price vanadium chromium ion tool, tail washings vanadium after absorption, chromium content can be made all lower than 0.5mg/L, and vanadium, chromium recovery ratio all reach more than 99.9%, reach discharging standards.
(3) ion-exchange fiber adopted has stronger heat resistance, can ensure life-time service under 100 DEG C of conditions, without swelling Fragmentation Phenomena, therefore, in application process, without the need to waste water is carried out cooling operation, reduces energy consumption.
(4) the present invention is to the method for resolving rear liquid employing calcium vanadate precipitation and Sodium chromate crystallization, and carry out the separation of vanadium, chromium component, be separated the corresponding calcium vanadate product obtained, purity, more than 95%, can be directly used in the raw material as smelting ferrovanadium; Sodium chromate is through recrystallization purity more than 98%.After crystallization, liquid recycles as desorbed solution, has both achieved the comprehensive utilization of valuable element, makes again whole flow process produce without waste water and dregs, meets green cleaner production requirement.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is further detailed explanation.
Embodiment 1:
Get the vanadium extracting waste water 1L of Chengde iron and steel enterprise, process as follows:
1) adsorb: adopt strong basic type anion-exchange resin D201 to adsorb the vanadium in waste water, chromium ion, obtain the strong basic type anion-exchange resin containing vanadium, chromium ion;
2) resolve: under 20 DEG C of conditions, to the strong basic type anion-exchange resin containing vanadium, chromium ion that step 1) obtains, add the 3mol/L NaOH aqueous solution and resolve, obtain desorbed solution, after resolving, adsorption medium can reuse;
3) precipitation: add alkaline matter in desorbed solution, this alkaline matter is calcium hydroxide slurry, addition is v element amount of substance in desorbed solution: calcium constituent amount of substance=0.8:1 in alkaline matter, stirring reaction, temperature is 80 DEG C, reaction times is 1h, filters, obtain calcium vanadate product and precipitation supernatant liquor evenly; Calcium vanadate product purity is 95.0%;
4) chromium crystallization: it is 40wt% that precipitation supernatant liquor step 3) obtained carries out evaporation concentration to naoh concentration, naturally cools to 36 DEG C, stirred crystallization 1h, and crystallisation by cooling obtains Sodium chromate crude product and crystalline mother solution;
5) recrystallization: the Sodium chromate crude product that step 4) obtains is added to the water, control Sodium chromate concentration at 300g/L, be heated to 100 DEG C of dissolvings, naturally cool to 45 DEG C, crystallization 4h, obtain Sodium chromate product, purity is 98.3%; Crystallisation by cooling mother liquor;
6) crystalline mother solution returns: to step 4), 5) crystalline mother solution that obtains returns step 2) as the recycling of desorbed solution batching.
In vanadium extracting waste water process post crystallization mother liquor, vanadium, chromium content reach discharging standards completely, and vanadium, chromium recovery ratio all reach more than 99.9%, and in waste water, before and after process, vanadium, chromium content are in table 1, and in desorbed solution, main chemical compositions is in table 2.
Before and after the process of table 1 vanadium extracting waste water, main chemical compositions compares
| V 5+(mg/l) | Cr 6+(mg/l) | pH | |
| Before process | 57 | 660 | 1.9 |
| After process | 0.2 | 0.3 | 2.1 |
Table 2 desorbed solution main chemical compositions
| V 5+(mg/l) | Cr 6+(mg/l) | pH |
| 533 | 16500 | 14 |
Embodiment 2:
Get the vanadium extraction tail washings 2L of Chengde iron and steel enterprise, process as follows:
1) adsorb: adopt strong basic type anion-exchange resin to adsorb the vanadium in waste water, chromium ion, obtain the strong basic type anion-exchange resin containing vanadium, chromium ion;
2) resolve: under 40 DEG C of conditions, to the strong basic type anion-exchange resin containing vanadium, chromium ion that step 1) obtains, add the 5mol/L NaOH aqueous solution and resolve, obtain desorbed solution, after resolving, adsorption medium can reuse;
3) precipitation: add alkaline matter in desorbed solution, this alkaline matter is calcium hydroxide powder, addition is v element amount of substance in desorbed solution: calcium constituent amount of substance=1:1 in alkaline matter, stirring reaction, temperature is 90 DEG C, reaction times is 2h, filters, obtain calcium vanadate product and precipitation supernatant liquor evenly; Calcium vanadate product purity is 95.9%;
4) chromium crystallization: it is 43wt% that precipitation supernatant liquor step 3) obtained carries out evaporation concentration to naoh concentration, naturally cools to 45 DEG C, stirred crystallization 4h, and crystallisation by cooling obtains Sodium chromate crude product and crystalline mother solution;
5) recrystallization: the Sodium chromate crude product that step 4) obtains is added to the water, control Sodium chromate concentration at 350g/L, be heated to 80 DEG C of dissolvings, naturally cool to 40 DEG C, crystallization 2h, obtain Sodium chromate product, purity is 98.6%, crystallisation by cooling mother liquor;
6) crystalline mother solution returns: to step 4), 5) crystalline mother solution that obtains returns step 2) as the recycling of desorbed solution batching.
In vanadium extracting waste water process post crystallization mother liquor, vanadium, chromium content reach discharging standards completely, and vanadium, chromium recovery ratio all reach more than 99.9%, and in waste water, before and after process, vanadium, chromium content are in table 3, and in desorbed solution, main chemical compositions is in table 4.
Before and after the process of table 3 vanadium extracting waste water, main chemical compositions compares
| V 5+(mg/l) | Cr 6+(mg/l) | pH | |
| Before process | 50 | 653 | 1.9 |
| After process | 0.3 | 0.2 | 2.1 |
Table 4 desorbed solution main chemical compositions
| V 5+(mg/l) | Cr 6+(mg/l) | pH |
| 628 | 15500 | 14 |
Embodiment 3:
Get the vanadium extraction tail washings 2L of Chengde iron and steel enterprise, process as follows:
1) adsorb: adopt strong base anion exchange fiber to adsorb the vanadium in waste water, chromium ion, obtain the anion-exchange fibre containing vanadium, chromium ion, this anion-exchange fibre be after polypropylene grafted vinylbenzene grafting season the amino product obtained;
2) resolve: under 80 DEG C of conditions, to the strong basic type anion-exchange resin containing vanadium, chromium ion that step 1) obtains, add the 4mol/L NaOH aqueous solution and resolve, obtain desorbed solution, after resolving, adsorption medium can reuse;
3) precipitation: add alkaline matter in desorbed solution, this alkaline matter is calcium oxide, addition is v element amount of substance in desorbed solution: calcium constituent amount of substance=1.1:1 in alkaline matter, stirring reaction, temperature is 60 DEG C, reaction times is 1h, filters, obtain calcium vanadate product and precipitation supernatant liquor evenly; Calcium vanadate product purity is 96.0%;
4) chromium crystallization: it is 45wt% that precipitation supernatant liquor step 3) obtained carries out evaporation concentration to naoh concentration, naturally cools to 28 DEG C, stirred crystallization 2h, and crystallisation by cooling obtains Sodium chromate crude product and crystalline mother solution;
5) recrystallization: the Sodium chromate crude product that step 4) obtains is added to the water, control Sodium chromate concentration at 450g/L, be heated to 60 DEG C of dissolvings, naturally cool to 28 DEG C, crystallization 1h, obtain Sodium chromate product, purity is 98.8%, crystallisation by cooling mother liquor;
6) crystalline mother solution returns: to step 4), 5) crystalline mother solution that obtains returns step 2) as the recycling of desorbed solution batching.
In vanadium extracting waste water process post crystallization mother liquor, vanadium, chromium content reach discharging standards completely, and vanadium, chromium recovery ratio all reach more than 99.9%, and in waste water, before and after process, vanadium, chromium content are in table 5, and in desorbed solution, main chemical compositions is in table 6.
Before and after the process of table 5 vanadium extracting waste water, main chemical compositions compares
| V 5+(mg/l) | Cr 6+(mg/l) | pH | |
| Before process | 50 | 703 | 1.9 |
| After process | 0.1 | ≤0.001 | 2.1 |
Table 6 desorbed solution main chemical compositions
| V 5+(mg/l) | Cr 6+(mg/l) | pH |
| 650 | 18500 | 14 |
Embodiment 4:
Get the vanadium extraction tail washings 2L of Chengde iron and steel enterprise, process as follows:
1) adsorb: adopt strong base anion exchange fiber to adsorb the vanadium in waste water, chromium ion, obtain the anion-exchange fibre containing vanadium, chromium ion, this anion-exchange fibre be after polypropylene grafted vinylbenzene grafting season the amino product obtained;
2) resolve: under 25 DEG C of conditions, to the strong basic type anion-exchange resin containing vanadium, chromium ion that step 1) obtains, add the 1mol/L NaOH aqueous solution and resolve, obtain desorbed solution, after resolving, adsorption medium can reuse;
3) precipitation: add alkaline matter in desorbed solution, this alkaline matter is calcium hydroxide slurry, addition is v element amount of substance in desorbed solution: calcium constituent amount of substance=1.2:1 in alkaline matter, stirring reaction, temperature is 40 DEG C, reaction times is 4h, filters, obtain calcium vanadate product and precipitation supernatant liquor evenly; Calcium vanadate product purity is 96.3%;
4) chromium crystallization: it is 42wt% that precipitation supernatant liquor step 3) obtained carries out evaporation concentration to naoh concentration, naturally cools to 25 DEG C, stirred crystallization 4h, and crystallisation by cooling obtains Sodium chromate crude product and crystalline mother solution;
5) recrystallization: the Sodium chromate crude product that step 4) obtains is added to the water, control Sodium chromate concentration at 500g/L, be heated to 76 DEG C of dissolvings, naturally cool to 28 DEG C, crystallization 2h, obtain Sodium chromate product, purity is 98.9%, crystallisation by cooling mother liquor;
6) crystalline mother solution returns: to step 4), 5) crystalline mother solution that obtains returns step 2) as the recycling of desorbed solution batching.
In vanadium extracting waste water process post crystallization mother liquor, vanadium, chromium content reach discharging standards completely, and vanadium, chromium recovery ratio all reach more than 99.9%, and in waste water, before and after process, vanadium, chromium content are in table 7, and in desorbed solution, main chemical compositions is in table 8.
Before and after the process of table 7 vanadium extracting waste water, main chemical compositions compares
| V 5+(mg/l) | Cr 6+(mg/l) | pH | |
| Before process | 50 | 703 | 1.9 |
| After process | 0.1 | 0.2 | 2.1 |
Table 8 desorbed solution main chemical compositions
| V 5+(mg/l) | Cr 6+(mg/l) | pH |
| 642 | 17500 | 14 |
Embodiment 5:
Get the vanadium extraction tail washings 2L of Chengde iron and steel enterprise, process as follows:
1) adsorb: adopt strong basic type anion-exchange resin D201 to adsorb the vanadium in waste water, chromium ion, obtain the strong basic type anion-exchange resin containing vanadium, chromium ion;
2) resolve: under 32 DEG C of conditions, to the strong basic type anion-exchange resin containing vanadium, chromium ion that step 1) obtains, add the 2mol/L NaOH aqueous solution and resolve, obtain desorbed solution, after resolving, adsorption medium can reuse;
3) precipitation: add alkaline matter in desorbed solution, this alkaline matter is calcium hydroxide slurry, addition is v element amount of substance in desorbed solution: calcium constituent amount of substance=0.9:1 in alkaline matter, stirring reaction, temperature is 100 DEG C, reaction times is 0.5h, filters, obtain calcium vanadate product and precipitation supernatant liquor evenly; Calcium vanadate product purity is 96.1%;
4) chromium crystallization: it is 41wt% that precipitation supernatant liquor step 3) obtained carries out evaporation concentration to naoh concentration, naturally cools to 40 DEG C, stirred crystallization 3h, and crystallisation by cooling obtains Sodium chromate crude product and crystalline mother solution;
5) recrystallization: the Sodium chromate crude product that step 4) obtains is added to the water, control Sodium chromate concentration at 400g/L, be heated to 60-100 DEG C of dissolving, naturally cool to 25-45 DEG C, crystallization 1-4h, obtain Sodium chromate product, purity is 98.7%, crystallisation by cooling mother liquor;
6) crystalline mother solution returns: to step 4), 5) crystalline mother solution that obtains returns step 2) as the recycling of desorbed solution batching.
In vanadium extracting waste water process post crystallization mother liquor, vanadium, chromium content reach discharging standards completely, and vanadium, chromium recovery ratio all reach more than 99.9%, and in waste water, before and after process, vanadium, chromium content are in table 9, and in desorbed solution, main chemical compositions is in table 10.
Before and after the process of table 9 vanadium extracting waste water, main chemical compositions compares
| V 5+(mg/l) | Cr 6+(mg/l) | pH | |
| Before process | 50 | 653 | 1.9 |
| After process | 0.3 | 0.2 | 2.1 |
Table 10 desorbed solution main chemical compositions
| V 5+(mg/l) | Cr 6+(mg/l) | pH |
| 638 | 16800 | 14 |
Above by embodiment to invention has been detailed description; but described content is only preferred embodiment of the present invention; utilize technical solutions according to the invention; or those skilled in the art is under the inspiration of technical solution of the present invention; design similar technical scheme; and reach above-mentioned technique effect, be all fall into protection scope of the present invention.
Claims (10)
1. process is containing a method for vanadium, chrome waste water, it is characterized in that, comprises the steps:
1) adsorb: adopt adsorption medium to adsorb containing the vanadium in vanadium, chrome waste water, chromium ion, obtain the adsorption medium containing vanadium, chromium ion;
2) resolve: to step 1) obtain containing vanadium, chromium ion adsorption medium add resolve agent resolve, obtain desorbed solution, resolve after adsorption medium can reuse;
3) precipitation: add in desorbed solution after alkaline matter stirs and filter, obtain calcium vanadate product and precipitation supernatant liquor;
4) chromium crystallization: precipitation supernatant liquor step 3) obtained carries out evaporating, concentrated after, naturally cool to 25-45 DEG C, stirred crystallization 1-4h, obtain Sodium chromate crude product and crystalline mother solution;
5) recrystallization: be added to the water to the Sodium chromate crude product that step 4) obtains, controls Sodium chromate concentration at 300-500g/L, is heated to 60-100 DEG C of dissolving, naturally cools to 25-45 DEG C, crystallization 1-4h, obtain Sodium chromate product and crystalline mother solution;
6) crystalline mother solution returns: to step 4), 5) crystalline mother solution that obtains returns step 2) as the recycling of desorbed solution batching.
2. a kind of process according to claim 1 is containing the method for vanadium, chrome waste water, and its feature exists, and the adsorption medium in described step 1) is any one in anionite-exchange resin or anion-exchange fibre.
3. a kind of process according to claim 2 is containing the method for vanadium, chrome waste water, it is characterized in that, described anion-exchange fibre, the product obtained for grafting season after polypropylene grafted vinylbenzene is amino.
4. according to claim 1-3 any one a kind of process containing vanadium, chrome waste water method, it is characterized in that, described step 2) in resolution temperature be 20-80 DEG C.
5. according to claim 1-3 any one a kind of process containing vanadium, chrome waste water method, it is characterized in that, described step 2) in resolve agent be the 1-5mol/L NaOH aqueous solution.
6. a kind of process according to claim 1-3 any one is containing the method for vanadium, chrome waste water, and it is characterized in that, the alkaline matter in described step 3) is any one in calcium oxide, calcium hydroxide powder or calcium hydroxide slurry; Addition is v element amount of substance in desorbed solution: calcium constituent amount of substance=0.8:1-1.2:1 in alkaline matter.
7. a kind of process according to claim 1-3 any one is containing the method for vanadium, chrome waste water, and it is characterized in that, in described step 3), stirring reaction temperature is 40-100 DEG C, and the stirring reaction time is 0.5-4h.
8. a kind of process according to claim 1-3 any one is containing the method for vanadium, chrome waste water, and its feature exists, and in described step 4), evaporation concentration refers to and precipitation supernatant liquor is evaporated to naoh concentration 40-45wt%.
9. a kind of process according to claim 8 is containing the method for vanadium, chrome waste water, and its feature exists, and in described step 3), calcium vanadate product purity is more than 95%, and in described step 5), Sodium chromate product purity is more than 98%.
10. a kind of process according to claim 9 is containing the method for vanadium, chrome waste water, and its feature exists, and refers to containing pentavalent vanadium element, the waste water of sexavalent chrome element in described step 1) containing vanadium, chrome waste water.
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| CN108728649A (en) * | 2018-05-25 | 2018-11-02 | 中国科学院过程工程研究所 | A kind of method of bone coal acid waste water recycling |
| CN109650406A (en) * | 2018-12-29 | 2019-04-19 | 江苏南大环保科技有限公司 | A kind of processing method of the high-salt wastewater containing chrome alum and the processing method of precipitation waste residue |
| CN109665548A (en) * | 2018-12-29 | 2019-04-23 | 江苏南大环保科技有限公司 | A kind of processing method of vanadium wastewater and the processing method of precipitation waste residue |
| CN111453770A (en) * | 2020-03-31 | 2020-07-28 | 有研工程技术研究院有限公司 | Size-controllable high-purity alkali metal chromate crystal powder and preparation method thereof |
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| CN111453770A (en) * | 2020-03-31 | 2020-07-28 | 有研工程技术研究院有限公司 | Size-controllable high-purity alkali metal chromate crystal powder and preparation method thereof |
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