CN111233015A - Deactivated Fe2O3/Ni2O3/Al2O3Method for recycling catalyst - Google Patents

Deactivated Fe2O3/Ni2O3/Al2O3Method for recycling catalyst Download PDF

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CN111233015A
CN111233015A CN202010223798.1A CN202010223798A CN111233015A CN 111233015 A CN111233015 A CN 111233015A CN 202010223798 A CN202010223798 A CN 202010223798A CN 111233015 A CN111233015 A CN 111233015A
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solution
catalyst
filtering
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邸万山
司颐
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Liaoning Petrochemical Vocational and Technical College
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Liaoning Petrochemical Vocational and Technical College
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00—Compounds of aluminium
    • C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00—Compounds of aluminium
    • C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
    • C01F7/30—Preparation of aluminium oxide or hydroxide by thermal decomposition or by hydrolysis or oxidation of aluminium compounds
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00—Compounds of aluminium
    • C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
    • C01F7/46—Purification of aluminium oxide, aluminium hydroxide or aluminates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00—Compounds of iron
    • C01G49/14—Sulfates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00—Compounds of nickel
    • C01G53/10—Sulfates

Abstract

Deactivated Fe2O3/Ni2O3/Al2O3Method for recycling catalyst, taking deactivated Fe2O3/Ni2O3/Al2O3Adding sodium hydroxide solution into catalyst, heating the solution to boiling, keeping the temperature, and filtering to obtain a filtrate NaAlO2A solution, precipitated as nickel oxide and iron oxide; NaAlO is added2Introducing CO into the solution2Filtering, depositing and firing to obtain aluminum oxide; oxidizing the precipitateAdding sulfuric acid into nickel and ferric oxide, heating to boil, preserving heat, filtering, transferring the filtrate into a container, heating, adjusting pH, preserving heat, filtering, heating the filtrate in the container until a crystal film appears on the liquid surface, stopping heating, cooling for crystallization, and filtering to obtain a nickel sulfate crystal. The advantages are that: the process is simple and easy to operate; the recovery rate of Fe, Ni and Al in the inactivated catalyst is high, three metal elements of Fe, Ni and Al are completely separated and are recycled, no pollutant is generated, and the method is safe and environment-friendly.

Description

Deactivated Fe2O3/Ni2O3/Al2O3Method for recycling catalyst
Technical Field
The invention relates to deactivated Fe2O3/Ni2O3/Al2O3A method for recycling the catalyst.
Background
In industrial waste water treatment, NaClO is commonly used as an oxidant, and Fe is used2O3/Ni2O3/Al2O3The catalyst is used for decoloring the wastewater and eliminating COD. And Fe2O3/Ni2O3/Al2O3Ni in catalyst2O3Deactivation of NiO formation and deactivated Fe2O3/Ni2O3/Al2O3The catalyst contains three metal elements of iron, nickel and aluminum, so that if the catalyst is not recycled, resource waste is caused, and the catalyst can cause environmental pollution after being stacked for a long time.
Disclosure of Invention
The technical problem to be solved by the invention is to provide the inactivated Fe2O3/Ni2O3/Al2O3The method for recycling the catalyst has simple technical process and easy operation; deactivated Fe2O3/Ni2O3/Al2O3The recovery rate of Fe, Ni and Al in the catalyst is high, and the recovered Al2O3Activated Al2O3Can be used for preparing Fe again2O3/Ni2O3/Al2O3Catalyst support, NiSO4The method can be used as a raw material for producing metallic nickel, and the three metallic elements of Fe, Ni and Al are completely separated and recycled, so that no pollutant is generated, and the method is safe and environment-friendly.
The technical scheme of the invention is as follows:
deactivated Fe2O3/Ni2O3/Al2O3The method for recycling the catalyst comprises the following specific steps:
(1) recovery of Al2O3
① preparation of NaAlO2
100g of washed deactivated Fe was taken2O3/Ni2O3/Al2O3Catalyst, adding sodium hydroxide solution with the mass concentration of 15 percent, and inactivating Fe2O3/Ni2O3/Al2O3The molar weight of the alumina in the catalyst and the molar ratio of the sodium hydroxide are 1:2.02-1:2.1, stirring and heating the solution to boiling, keeping the temperature for 30min-35min, filtering, wherein the filtrate is NaAlO2A solution, precipitated as nickel oxide and iron oxide;
② preparation of Al2O3
The obtained filtrate NaAlO2Placing the solution in a container, and adding CO2Introducing into a container until no white precipitate is generated, filtering, retaining the precipitate, and burning the precipitate at 950-1000 ℃ for 60-70 min to obtain aluminum oxide;
(2) recovery of NiO
① preparation of Fe2(SO4)3、NiSO4
Putting the obtained precipitated nickel oxide and ferric oxide into a container, adding a sulfuric acid solution with the mass concentration of 20%, and inactivating Fe2O3/Ni2O3/Al2O3The reaction of nickel oxide and iron oxide in the catalyst is 1.01-1.05 times of the metering relation of the reaction of sulfuric acid, stirring and heating the solution to boiling, keeping the temperature for 40-50 min, filtering, and retaining the filtrate, wherein the filtrate is Fe2(SO4)3And NiSO4；
② separation of Fe2(SO4)3
Mixing Fe2(SO4)3、NiSO4Transferring into a container, stirring and heating to 85-95 deg.C, adjusting pH to 1.5-2.5 with 10% ammonia water, maintaining the temperature for 30-40 min, filtering and separating to obtain NiSO4A solution;
③ preparation of NiSO4
Mixing NiSO4Placing the solution in a container, and heating NiSO4Evaporating solvent from the solution to boiling, stopping heating when crystal film appears on the liquid surface, stirring the solution to disperse the crystal film into the solution as crystal nucleus, and cooling the solution to room temperatureAnd crystallizing the nickel sulfate from the solution, and filtering to obtain nickel sulfate crystals.
Further, the deactivated Fe2O3/Ni2O3/Al2O3The molar ratio of the molar amount of alumina to the molar amount of sodium hydroxide in the catalyst was 1: 2.02.
Further, the deactivated Fe2O3/Ni2O3/Al2O3The nickel oxide and iron oxide in the catalyst were 1.01 times the stoichiometric relationship for the reaction with sulfuric acid.
Further, NaAlO is added in the filtrate2Introducing CO into the solution2Before that, 10mL of phenolphthalein indicator solution with the mass concentration of 2% is added, and the solution is pink, and CO is added2Introducing into the solution in the container until the pink color of the solution just disappears, and introducing NaAlO2All conversion to Al (OH)3White precipitate.
The invention has the beneficial effects that:
the process is simple and easy to operate; deactivated Fe2O3/Ni2O3/Al2O3The recovery rate of Fe, Ni and Al in the catalyst is high, and the recovered Al2O3Activated Al2O3Can be used for preparing Fe again2O3/Ni2O3/Al2O3Catalyst support, NiSO4The method can be used as a raw material for producing metallic nickel, and the three metallic elements of Fe, Ni and Al are completely separated and recycled, so that no pollutant is generated, and the method is safe and environment-friendly.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
Example 1
(1) Recovery of Al2O3
① preparation of NaAlO2
As shown in FIG. 1, first, the deactivated Fe2O3/Ni2O3/Al2O3Washing the catalyst with sodium carbonate solution to remove the surface residue, and collecting 100g of the washed deactivated Fe2O3/Ni2O3/Al2O3Putting catalyst (alumina content is 78.5%, ferric oxide content is 12.9%, nickel oxide content is 8.6%) in a container, adding 15% sodium hydroxide solution 414.8g, stirring and heating the solution to boiling, keeping the temperature for 30min, filtering, and obtaining NaAlO filtrate2A solution, precipitated as nickel oxide and iron oxide;
② preparation of Al2O3
The obtained filtrate NaAlO2Placing the solution in a container, and adding CO2Introducing into a container until no white precipitate is generated (10 mL phenolphthalein indicator solution with mass concentration of 2% can be added for auxiliary judgment, and the phenolphthalein indicator solution is added to make the solution pink, CO2Introducing into the solution in the container until the pink color of the solution just disappears, and introducing NaAlO2All conversion to Al (OH)3White precipitate), filtering, retaining the precipitate, and burning the precipitate at 950-1000 ℃ for 60min to obtain aluminum oxide; weighing the mass of the alumina, and calculating the recovery rate of the alumina to be 98.6%;
the chemical reaction equation is as follows:
NaAlO2+CO2+2H2O＝Al(OH)3↓+NaHCO3
2Al(OH)3＝Al2O3+3H2O
(2) recovery of NiO
① preparation of Fe2(SO4)3、NiSO4
Placing the obtained precipitated nickel oxide and ferric oxide in a container, adding 176.8g of sulfuric acid solution with mass concentration of 20%, stirring and heating the solution to boiling, keeping the temperature for 40min, filtering, and retaining filtrate, wherein the filtrate is Fe2(SO4)3、NiSO4；
The chemical reaction equation is as follows:
Fe2O3+3H2SO4＝Fe2(SO4)3+3H2O
NiO+H2SO4＝NiSO4+H2O
② separation of Fe2(SO4)3
Mixing Fe2(SO4)3、NiSO4Transferring into container, stirring and heating to 90 deg.C, adjusting pH to 2.5 with 10% ammonia water, maintaining the temperature for 30min, filtering to obtain precipitate (NH)4)2Fe6(SO4)4(OH)12The filtrate is NiSO4A solution; the chemical reaction equation is as follows:
2NH3+3Fe2(SO4)3+12H2O＝(NH4)2Fe6(SO4)4(OH)12↓+5H2SO4；
③ preparation of NiSO4
Mixing NiSO4And (3) placing the solution in a container, heating the solution to boiling to evaporate the solvent, stopping heating when a crystal film appears on the liquid surface, stirring the solution to disperse the crystal film into the solution to be used as a crystal nucleus, cooling the solution to room temperature, crystallizing nickel sulfate out of the solution, filtering to obtain nickel sulfate crystals, converting the nickel sulfate crystals into the mass of nickel oxide, and calculating the recovery rate to be 98.9%.
Example 2
(1) Recovery of Al2O3
① preparation of NaAlO2
100g of washed deactivated Fe was taken2O3/Ni2O3/Al2O3Putting catalyst (alumina content is 78.5%, iron oxide content is 12.9%, nickel oxide content is 8.6%) in container, adding sodium hydroxide solution 431.2g with mass concentration of 15%, stirring and heating the solution to boiling, keeping temperature for 30min, filtering, the filtrate is NaAlO2A solution, precipitated as nickel oxide and iron oxide;
② preparation of Al2O3
The obtained filtrate NaAlO2Placing the solution in a container, and adding CO2Introducing into a container until no white precipitate is generated, filtering, retaining the precipitate, and burning the precipitate at 950-1000 ℃ for 60min to obtain aluminum oxide;weighing the mass of the alumina, and calculating the recovery rate of the alumina to be 98.8%;
(2) recovery of NiO
① preparation of Fe2(SO4)3、NiSO4
Placing the obtained precipitated nickel oxide and ferric oxide in a container, adding 183.8g of sulfuric acid solution with mass concentration of 20%, stirring and heating the solution to boiling, keeping the temperature for 40min, filtering, and retaining filtrate, wherein the filtrate is Fe2(SO4)3、NiSO4；
② separation of Fe2(SO4)3
Mixing Fe2(SO4)3、NiSO4Transferring into container, stirring and heating to 90 deg.C, adjusting pH to 2.5 with 10% ammonia water, maintaining the temperature for 30min, filtering to obtain precipitate (NH)4)2Fe6(SO4)4(OH)12The filtrate is NiSO4A solution;
③ preparation of NiSO4
Mixing NiSO4And putting the solution in a container, heating the solution until the solution is boiled to evaporate the solvent, stopping heating when a crystal film appears on the liquid surface, stirring the solution to disperse the crystal film into the solution to be used as crystal nuclei, cooling the solution to room temperature, crystallizing nickel sulfate from the solution, and filtering to obtain nickel sulfate crystals.
Different sodium hydroxide addition amounts for Al2O3Influence of recovery
① preparation of NaAlO2
100g of washed deactivated Fe was taken2O3/Ni2O3/Al2O3Placing catalyst (alumina content is 78.5%, iron oxide content is 12.9%, nickel oxide content is 8.6%) in a container, adding 15% sodium hydroxide solution, stirring and heating the solution to boiling, keeping the temperature for 30min, filtering, and obtaining NaAlO filtrate2A solution, precipitated as nickel oxide and iron oxide;
② preparation of Al2O3
The obtained filtrate NaAlO2Placing the solution in a container, and adding CO2Introducing into a container until no white precipitate is generated, filtering, retaining the precipitate, and burning the precipitate at 950-1000 ℃ for 60min to obtain aluminum oxide; weighing the mass of alumina, and calculating the recovery rate of alumina, as shown in table 1;
TABLE 1 sodium hydroxide addition vs. Al2O3Influence of recovery
Mass of sodium hydroxide, g 30.8 48.5 55 61.6 62.2 64.6
15% by weight of sodium hydroxide solution, g 205.3 323.3 366.7 410.7 414.8 431.2
Al2O3Percent recovery rate% 50.0 78.8 89.3 97.5 98.6 98.8
As shown in Table 1, the recovery of alumina was 98.6% when the excess of sodium hydroxide was 1%, and the recovery of alumina was 98.8% when the excess of sodium hydroxide was 5%, and the recovery varied little, and the amount of sodium hydroxide added was 62.2g in consideration of the cost of the reagent and the problem of introduction of other substances.
Example 3
(1) Recovery of Al2O3
① preparation of NaAlO2
100g of washed deactivated Fe was taken2O3/Ni2O3/Al2O3Putting catalyst (alumina content is 78.5%, ferric oxide content is 12.9%, nickel oxide content is 8.6%) in a container, adding 15% sodium hydroxide solution 414.8g, stirring and heating the solution to boiling, keeping the temperature for 30min, filtering, and obtaining NaAlO filtrate2A solution, precipitated as nickel oxide and iron oxide;
② preparation of Al2O3
The obtained filtrate NaAlO2Placing the solution in a container, and adding CO2Introducing into a container until no white precipitate is generated, filtering, retaining the precipitate, and burning the precipitate at 950-1000 ℃ for 60min to obtain aluminum oxide; weighing the mass of the alumina, and calculating the recovery rate of the alumina to be 98.6%;
(2) recovery of NiO
① preparation of Fe2(SO4)3、NiSO4
Placing the obtained precipitated nickel oxide and ferric oxide in a container, adding 183.8g of sulfuric acid solution with mass concentration of 20%, stirring and heating the solution to boiling, keeping the temperature for 40min, filtering, and retaining filtrate, wherein the filtrate is Fe2(SO4)3、NiSO4；
② separation of Fe2(SO4)3
Mixing Fe2(SO4)3、NiSO4Transferring into container, stirring and heating to 90 deg.C, adjusting pH to 2.5 with 10% ammonia water, maintaining the temperature for 30min, filtering to obtain precipitate (NH)4)2Fe6(SO4)4(OH)12The filtrate is NiSO4A solution;
③ preparation of NiSO4
Mixing NiSO4And (3) placing the solution in a container, heating the solution to boiling to evaporate the solvent, stopping heating when a crystal film appears on the liquid surface, stirring the solution to disperse the crystal film into the solution to be used as a crystal nucleus, cooling the solution to room temperature, crystallizing nickel sulfate out of the solution, filtering to obtain nickel sulfate crystals, converting the nickel sulfate crystals into the mass of nickel oxide, and calculating the recovery rate to be 99.1%.
The influence of different sulfuric acid addition amounts on the NiO recovery rate is the same
Deactivated Fe2O3/Ni2O3/Al2O3Catalyst recovery of Al2O3In the same manner as in example 3, sulfuric acid was added in different amounts during NiO recovery, the amount of sulfuric acid added was as shown in Table 2, and the NiO recovery rate was calculated and the results are shown in Table 2.
TABLE 2 influence of sulfuric acid dosage on NiO recovery
Mass of sulfuric acid, g 24.5 28.0 31.4 33.2 35.0 35.4 36.8
20% by weight of sulfuric acid, g 122.5 140 157 166 175 176.8 183.8
NiO recovery rate% 23.1 42.7 67.4 85.1 96.5 98.9 99.1
From Table 2, it is found that the recovery rate of alumina is 98.9% when the sulfuric acid is excessive by 1%, and the recovery rate of alumina is 99.1% when the sulfuric acid is excessive by 5%, and the change in the recovery rate is small, and it is preferable that the amount of sulfuric acid added is 35.3g in consideration of the cost of the reagent and the problem of introduction of other substances.
Example 4
(1) Recovery of Al2O3
① preparation of NaAlO2
100g of washed deactivated Fe was taken2O3/Ni2O3/Al2O3Putting catalyst (alumina content is 78.5%, iron oxide content is 12.9%, nickel oxide content is 8.6%) in a container, adding 15% sodium hydroxide solution 414.8g, stirring and heating the solution to boiling, keeping the temperature for 33min, filtering, and obtaining NaAlO filtrate2A solution, precipitated as nickel oxide and iron oxide;
② preparation of Al2O3
The obtained filtrate NaAlO2Placing the solution in a container, and adding CO2Introducing into a container until no white precipitate is generated, filtering, retaining the precipitate, and burning the precipitate at 950-1000 ℃ for 65min to obtain aluminum oxide; weighing the mass of the alumina, and calculating the recovery rate of the alumina to be 98.5%;
(2) recovery of NiO
① preparation of Fe2(SO4)3、NiSO4
Placing the obtained precipitated nickel oxide and ferric oxide in a container, adding 176.8g of sulfuric acid solution with mass concentration of 20%, stirring and heating the solution to boiling, keeping the temperature for 45min, filtering, and retaining filtrate, wherein the filtrate is Fe2(SO4)3、NiSO4；
② separation of Fe2(SO4)3
Mixing Fe2(SO4)3、NiSO4Transferring into container, stirring, heating to 85 deg.C, adjusting pH to 2.5 with 10% ammonia water, maintaining the temperature for 30min, filtering to obtain precipitate (NH)4)2Fe6(SO4)4(OH)12The filtrate is NiSO4A solution;
③ preparation of NiSO4
Mixing NiSO4And (3) placing the solution in a container, heating the solution to boiling to evaporate the solvent, stopping heating when a crystal film appears on the liquid surface, stirring the solution to disperse the crystal film into the solution to be used as a crystal nucleus, cooling the solution to room temperature, crystallizing nickel sulfate out of the solution, filtering to obtain nickel sulfate crystals, converting the nickel sulfate crystals into the mass of nickel oxide, and calculating the recovery rate to be 99.0%.
Example 5
(1) Recovery of Al2O3
① preparation of NaAlO2
100g of washed deactivated Fe was taken2O3/Ni2O3/Al2O3Putting catalyst (alumina content is 78.5%, ferric oxide content is 12.9%, nickel oxide content is 8.6%) in container, adding 15% sodium hydroxide solution 414.8g, stirring and heating the solution to boiling, keeping temperature for 35min, filtering, the filtrate is NaAlO2A solution, precipitated as nickel oxide and iron oxide;
② preparation of Al2O3
The obtained filtrate NaAlO2Placing the solution in a container, and adding CO2Introducing into a container until no white precipitate is generated, filtering, retaining the precipitate, and burning the precipitate at 950-1000 ℃ for 70min to obtain aluminum oxide; weighing the mass of the alumina, and calculating the recovery rate of the alumina to be 98.5%;
the chemical reaction equation is as follows:
NaAlO2+CO2+2H2O＝Al(OH)3↓+NaHCO3
2Al(OH)3＝Al2O3+3H2O
(2) recovery of NiO
① preparation of Fe2(SO4)3、NiSO4
Placing the obtained precipitated nickel oxide and ferric oxide in a container, adding 176.8g of sulfuric acid solution with mass concentration of 20%, stirring and heating the solution to boiling, keeping the temperature for 50min, filtering, and retaining filtrate, wherein the filtrate is Fe2(SO4)3、NiSO4；
The chemical reaction equation is as follows:
Fe2O3+3H2SO4＝Fe2(SO4)3+3H2O
NiO+H2SO4＝NiSO4+H2O
② separation of Fe2(SO4)3
Mixing Fe2(SO4)3、NiSO4Transferring into a container, stirring and heating to 95 deg.C, adjusting pH to 2.5 with 10% ammonia water, maintaining the temperature for 30min, filtering to obtain precipitate (NH)4)2Fe6(SO4)4(OH)12The filtrate is NiSO4A solution; the chemical reaction equation is as follows:
2NH3+3Fe2(SO4)3+12H2O＝(NH4)2Fe6(SO4)4(OH)12↓+5H2SO4；
③ preparation of NiSO4
Mixing NiSO4And (3) placing the solution in a container, heating the solution to boiling to evaporate the solvent, stopping heating when a crystal film appears on the liquid surface, stirring the solution to disperse the crystal film into the solution to be used as a crystal nucleus, cooling the solution to room temperature, crystallizing nickel sulfate out of the solution, filtering to obtain nickel sulfate crystals, converting the nickel sulfate crystals into the mass of nickel oxide, and calculating the recovery rate to be 98.9%.
The above description is only exemplary of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (4)

1. Deactivated Fe2O3/Ni2O3/Al2O3The method for recycling the catalyst is characterized by comprising the following steps:
the method comprises the following specific steps:
(1) recovery of Al2O3
① preparation of NaAlO2
100g of washed deactivated Fe was taken2O3/Ni2O3/Al2O3Catalyst, adding sodium hydroxide solution with the mass concentration of 15 percent, and inactivating Fe2O3/Ni2O3/Al2O3The molar weight of the alumina in the catalyst and the molar ratio of the sodium hydroxide are 1:2.02-1:2.1, stirring and heating the solution to boiling, keeping the temperature for 30min-35min, filtering, wherein the filtrate is NaAlO2A solution, precipitated as nickel oxide and iron oxide;
② preparation of Al2O3
The obtained filtrate NaAlO2Placing the solution in a container, and adding CO2Introducing into a container until no white precipitate is generated, filtering, retaining the precipitate, and burning the precipitate at 950-1000 deg.C for 60-70 min to obtain aluminum oxide;
(2) recovery of NiO
① preparation of Fe2(SO4)3、NiSO4
Putting the obtained precipitated nickel oxide and ferric oxide into a container, adding a sulfuric acid solution with the mass concentration of 20%, and inactivating Fe2O3/Ni2O3/Al2O3The reaction of nickel oxide and iron oxide in the catalyst is 1.01-1.05 times of the metering relation of the reaction of sulfuric acid, stirring and heating the solution to boiling, keeping the temperature for 40-50 min, filtering, and retaining the filtrate, wherein the filtrate is Fe2(SO4)3And NiSO4；
② separation of Fe2(SO4)3
Mixing Fe2(SO4)3、NiSO4Transferring into a container, stirring and heating to 85-95 deg.C, adjusting pH to 1.5-2.5 with 10% ammonia water, maintaining the temperature for 30-40 min, filtering and separating to obtain NiSO4A solution;
③ preparation of NiSO4
Mixing NiSO4Placing the solution in a container, and heating NiSO4Evaporating the solvent when the solution is boiling, stopping heating when a crystal film appears on the liquid surface, stirring the solution to disperse the crystal film into the solution to be used as crystal nucleus, cooling the solution to room temperature, crystallizing nickel sulfate out of the solution, and filtering to obtain nickel sulfate crystals.
2. Deactivated Fe according to claim 12O3/Ni2O3/Al2O3The method for recycling the catalyst is characterized by comprising the following steps: said deactivated Fe2O3/Ni2O3/Al2O3The molar ratio of the molar amount of alumina to the molar amount of sodium hydroxide in the catalyst was 1: 2.02.
3. Deactivated Fe according to claim 12O3/Ni2O3/Al2O3The method for recycling the catalyst is characterized by comprising the following steps: said deactivated Fe2O3/Ni2O3/Al2O3The nickel oxide and iron oxide in the catalyst were 1.01 times the stoichiometric relationship for the reaction with sulfuric acid.
4. Deactivated Fe according to claim 12O3/Ni2O3/Al2O3The method for recycling the catalyst is characterized by comprising the following steps: in the filtrate NaAlO2Introducing CO into the solution2Before that, 10mL of phenolphthalein indicator solution with the mass concentration of 2% is added, and the solution is pink, and CO is added2Introducing into the solution in the container until the pink color of the solution just disappears, and introducing NaAlO2All conversion to Al (OH)3White precipitate.
CN202010223798.1A 2020-03-26 2020-03-26 Deactivated Fe2O3/Ni2O3/Al2O3Method for recycling catalyst Pending CN111233015A (en)

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Cited By (1)

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CN116726919A (en) * 2023-05-22 2023-09-12 大连瑞克科技股份有限公司 Modified carrier of catalyst for synthesizing ethylene oxide by oxidizing ethylene and preparation method thereof

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