Treatment process of waste catalyst in pentafluoroethane production

Abstract

The invention belongs to the technical field of waste catalyst treatment, particularly relates to a treatment process for a waste catalyst in pentafluoroethane production, and provides the following scheme aiming at the problems that in an existing treatment process for the waste catalyst in the pentafluoroethane production, the waste catalyst cannot be sufficiently treated conveniently, the treatment effect is limited, and the recovery rate is reduced. The method comprises the following steps: S1, collecting the waste catalyst, and standing for a certain time; s2, adding part of the waste catalyst into the reaction solution, and mixing; s3, the treated reaction liquid is subjected to electrolysis, and pentafluoroethane is prepared; s4, adding the residual waste catalyst into the reaction solution, and stirring and mixing; and S5, standing the treated reaction liquid, and in the treatment process of the waste catalyst in pentafluoroethane production, the waste catalyst is subjected to electrolysis and reaction with the KOH aqueous solution at the same time, so that the treatment efficiency and the recovery rate can be effectively improved.

Description

Technical Field

[0001] This invention relates to the field of waste catalyst treatment technology, and in particular to a treatment process for waste catalysts in pentafluoroethane production. Background Technology

[0002] In the production of pentafluoroethane, waste catalyst is generated. This waste catalyst may contain unreacted raw materials, catalyst residues, etc. The general treatment methods include stirring the waste catalyst, fully reacting it with alkali, and distilling it in the bottom of a distillation column to obtain a high-purity refined solvent product.

[0003] In the existing technology, the treatment process for waste catalysts in pentafluoroethane production is not convenient for fully treating the waste catalysts, the treatment effect is limited, and the recovery rate is reduced. Therefore, we propose a treatment process for waste catalysts in pentafluoroethane production to solve the above problems. Summary of the Invention

[0004] The purpose of this invention is to address the shortcomings of existing technologies in the treatment of waste catalysts in pentafluoroethane production, which are inconvenient to fully treat the waste catalysts, have limited treatment effects, and have reduced recovery rates. Therefore, this invention proposes a treatment process for waste catalysts in pentafluoroethane production.

[0005] The technical solution provided in this application for treating spent catalysts in pentafluoroethane production is as follows:

[0006] A process for treating spent catalysts in pentafluoroethane production includes the following steps:

[0007] S1: Collect the waste catalyst and let it stand for a certain period of time;

[0008] S2: Add some of the spent catalyst to the reaction solution and mix.

[0009] S3: Electrolyze the treated reaction solution to produce pentafluoroethane;

[0010] S4: Add the remaining waste catalyst to the reaction solution and stir to mix;

[0011] S5: Allow the treated reaction solution to stand and separate the two phases to obtain an organic phase and an inorganic phase;

[0012] S6: Filter the organic phase to obtain an aqueous solution of KF;

[0013] S7: The inorganic phase is subjected to vacuum distillation to obtain high-purity organic amines.

[0014] Furthermore, in step S1, the waste catalyst is collected by a collection mechanism and transported to a storage tank by a conveying mechanism, where it is left to stand for 20-25 hours.

[0015] Furthermore, in step S2, 50% of the upper part of the static waste catalyst is extracted by the extraction mechanism and transported to the first reaction vessel by the conveying mechanism. Alkali solution is added to the reaction vessel by the adding mechanism, and the waste catalyst and alkali solution are stirred and mixed by the stirring mechanism. The mixing reaction time is 1-6 hours, and the temperature of the first reaction vessel is 100-220℃.

[0016] Furthermore, in step S3, the conveying mechanism transports the waste liquid after the reaction to an electrolytic cell, where the waste liquid after the reaction is electrolyzed to obtain pentafluoroethane.

[0017] Furthermore, in step S4, the remaining 50% of the waste catalyst in the storage tank is transported to the second reactor via a conveying mechanism, and a KOH aqueous solution is added to the second reactor via an adding mechanism.

[0018] Furthermore, in step S4, the KOH aqueous solution and the waste catalyst in the second reactor are stirred and mixed by a stirring mechanism for 2-7 hours.

[0019] Furthermore, in step S5, the reaction liquid after the reaction is transported to a storage tank for settling by a conveying mechanism. After settling, the two phases separate, with the lower layer being an inorganic phase containing potassium fluoride and the upper layer being an organic phase containing organic amines.

[0020] Furthermore, in step S6, the inorganic phase is conveyed by a conveying mechanism and filtered by a filtration mechanism to obtain a KF aqueous solution.

[0021] Furthermore, in step S7, the organic phase is conveyed to a distillation column via a conveying mechanism. The distillation column performs vacuum distillation on the inorganic phase to obtain high-purity organic amines. The temperature of the distillation column is 140-220℃, and the pressure of the distillation column is 0.2-0.8 MPa.

[0022] Furthermore, in step S7, the obtained high-purity organic amine is tested by a testing mechanism, and the organic amine with the required purity is transported to a storage tank for storage by a conveying mechanism, so that it can be used as a catalyst solvent for pentafluoroethane production.

[0023] In summary, this application includes at least one of the following beneficial technical effects:

[0024] 1. This method involves adding alkaline solution to the upper part of the static waste catalyst, stirring and mixing the waste catalyst and alkaline solution to react, and then electrolyzing the waste liquid after the reaction in an electrolytic cell to obtain pentafluoroethane;

[0025] 2. In this scheme, the remaining waste catalyst is transported to the second reactor and reacted by adding KOH aqueous solution. The inorganic phase generated by the reaction is filtered to obtain KF aqueous solution, and the organic phase is distilled under reduced pressure to obtain high-purity organic amine, which can be used as a catalyst solvent for pentafluoroethane production.

[0026] This invention can effectively improve the treatment efficiency and recovery rate of waste catalysts in the production of pentafluoroethane by simultaneously treating the waste catalysts through electrolysis and reaction with KOH aqueous solution. Attached Figure Description

[0027] Figure 1 This is a flowchart of a process for treating waste catalysts in the production of pentafluoroethane, as proposed in this invention. Detailed Implementation

[0028] The technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings of the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments.

[0029] Example 1

[0030] Reference Figure 1 A process for treating spent catalysts in pentafluoroethane production includes the following steps:

[0031] S1: Collect the waste catalyst and let it stand for a certain period of time;

[0032] S2: Add some of the spent catalyst to the reaction solution and mix.

[0033] S3: Electrolyze the treated reaction solution to produce pentafluoroethane;

[0034] S4: Add the remaining waste catalyst to the reaction solution and stir to mix;

[0035] S5: Allow the treated reaction solution to stand and separate the two phases to obtain an organic phase and an inorganic phase;

[0036] S6: Filter the organic phase to obtain a KF aqueous solution;

[0037] S7: The inorganic phase is subjected to vacuum distillation to obtain high-purity organic amines.

[0038] In this embodiment, in S1, the waste catalyst is collected by a collection mechanism and transported to a storage tank by a conveying mechanism, where it is left to stand for 20 hours.

[0039] In this embodiment, in step S2, 50% of the upper part of the static waste catalyst is extracted by the extraction mechanism and transported to the first reaction vessel by the conveying mechanism. Alkali solution is added to the reaction vessel by the adding mechanism, and the waste catalyst and alkali solution are stirred and mixed by the stirring mechanism. The mixing reaction time is 1 hour, and the temperature of the first reaction vessel is 100°C.

[0040] In this embodiment, in step S3, the conveying mechanism transports the waste liquid after the reaction to the electrolytic cell, and the waste liquid after the reaction is electrolyzed in the electrolytic cell to obtain pentafluoroethane.

[0041] In this embodiment, in step S4, the remaining 50% of the waste catalyst in the storage tank is transported to the second reactor by the conveying mechanism, and KOH aqueous solution is added to the second reactor by the adding mechanism. The KOH aqueous solution and waste catalyst in the second reactor are stirred and mixed by the stirring mechanism for 2 hours.

[0042] In this embodiment, in step S5, the reaction liquid after the reaction is transported to a storage tank for settling by a conveying mechanism. After settling, the two phases separate, with the lower layer being an inorganic phase containing potassium fluoride and the upper layer being an organic phase containing organic amines.

[0043] In this embodiment, in step S6, the inorganic phase is conveyed by a conveying mechanism and filtered by a filtration mechanism to obtain a KF aqueous solution.

[0044] In this embodiment, in step S7, the organic phase is conveyed to a distillation column via a conveying mechanism. The distillation column performs vacuum distillation on the inorganic phase to obtain a high-purity organic amine. The temperature of the distillation column is 140°C and the pressure of the distillation column is 0.2 MPa. The obtained high-purity organic amine is tested by a detection mechanism. The organic amine with the required purity is then conveyed to a storage tank via a conveying mechanism for storage. It can be used as a catalyst solvent for the production of pentafluoroethane.

[0045] Example 2

[0046] Reference Figure 1 A process for treating spent catalysts in pentafluoroethane production includes the following steps:

[0047] S1: Collect the waste catalyst and let it stand for a certain period of time;

[0048] S2: Add some of the spent catalyst to the reaction solution and mix.

[0049] S3: Electrolyze the treated reaction solution to produce pentafluoroethane;

[0050] S4: Add the remaining waste catalyst to the reaction solution and stir to mix;

[0051] S5: Allow the treated reaction solution to stand and separate the two phases to obtain an organic phase and an inorganic phase;

[0052] S6: Filter the organic phase to obtain a KF aqueous solution;

[0053] S7: The inorganic phase is subjected to vacuum distillation to obtain high-purity organic amines.

[0054] In this embodiment, in S1, the waste catalyst is collected by a collection mechanism and transported to a storage tank by a conveying mechanism, where it is left to stand for 21 hours.

[0055] In this embodiment, in step S2, 50% of the upper part of the static waste catalyst is extracted by the extraction mechanism and transported to the first reaction vessel by the conveying mechanism. Alkali solution is added to the reaction vessel by the adding mechanism, and the waste catalyst and alkali solution are stirred and mixed by the stirring mechanism. The mixing reaction time is 2 hours, and the temperature of the first reaction vessel is 150°C.

[0056] In this embodiment, in step S3, the conveying mechanism transports the waste liquid after the reaction to the electrolytic cell, and the waste liquid after the reaction is electrolyzed in the electrolytic cell to obtain pentafluoroethane.

[0057] In this embodiment, in step S4, the remaining 50% of the waste catalyst in the storage tank is transported to the second reactor by the conveying mechanism, and KOH aqueous solution is added to the second reactor by the adding mechanism. The KOH aqueous solution and waste catalyst in the second reactor are stirred and mixed by the stirring mechanism for 3 hours.

[0058] In this embodiment, in step S5, the reaction liquid after the reaction is transported to a storage tank for settling by a conveying mechanism. After settling, the two phases separate, with the lower layer being an inorganic phase containing potassium fluoride and the upper layer being an organic phase containing organic amines.

[0059] In this embodiment, in step S6, the inorganic phase is conveyed by a conveying mechanism and filtered by a filtration mechanism to obtain a KF aqueous solution.

[0060] In this embodiment, in step S7, the organic phase is conveyed to a distillation column via a conveying mechanism. The distillation column performs vacuum distillation on the inorganic phase to obtain a high-purity organic amine. The temperature of the distillation column is 150°C and the pressure of the distillation column is 0.3 MPa. The obtained high-purity organic amine is tested by a detection mechanism. The organic amine with the required purity is then conveyed to a storage tank via a conveying mechanism for storage. It can be used as a catalyst solvent for the production of pentafluoroethane.

[0061] Example 3

[0062] Reference Figure 1 A process for treating spent catalysts in pentafluoroethane production includes the following steps:

[0063] S1: Collect the waste catalyst and let it stand for a certain period of time;

[0064] S2: Add some of the spent catalyst to the reaction solution and mix.

[0065] S3: Electrolyze the treated reaction solution to produce pentafluoroethane;

[0066] S4: Add the remaining waste catalyst to the reaction solution and stir to mix;

[0067] S5: Allow the treated reaction solution to stand and separate the two phases to obtain an organic phase and an inorganic phase;

[0068] S6: Filter the organic phase to obtain a KF aqueous solution;

[0069] S7: The inorganic phase is subjected to vacuum distillation to obtain high-purity organic amines.

[0070] In this embodiment, in S1, the waste catalyst is collected by a collection mechanism and transported to a storage tank by a conveying mechanism, where it is left to stand for 22 hours.

[0071] In this embodiment, in step S2, 50% of the upper part of the static waste catalyst is extracted by the extraction mechanism and transported to the first reaction vessel by the conveying mechanism. Alkali solution is added to the reaction vessel by the adding mechanism, and the waste catalyst and alkali solution are stirred and mixed by the stirring mechanism. The mixing reaction time is 3 hours, and the temperature of the first reaction vessel is 180°C.

[0072] In this embodiment, in step S3, the conveying mechanism transports the waste liquid after the reaction to the electrolytic cell, and the waste liquid after the reaction is electrolyzed in the electrolytic cell to obtain pentafluoroethane.

[0073] In this embodiment, in step S4, the remaining 50% of the waste catalyst in the storage tank is transported to the second reactor by the conveying mechanism, and KOH aqueous solution is added to the second reactor by the adding mechanism. The KOH aqueous solution and waste catalyst in the second reactor are stirred and mixed by the stirring mechanism for 4 hours.

[0074] In this embodiment, in step S5, the reaction liquid after the reaction is transported to a storage tank for settling by a conveying mechanism. After settling, the two phases separate, with the lower layer being an inorganic phase containing potassium fluoride and the upper layer being an organic phase containing organic amines.

[0075] In this embodiment, in step S6, the inorganic phase is conveyed by a conveying mechanism and filtered by a filtration mechanism to obtain a KF aqueous solution.

[0076] In this embodiment, in step S7, the organic phase is conveyed to a distillation column via a conveying mechanism. The distillation column performs vacuum distillation on the inorganic phase to obtain a high-purity organic amine. The temperature of the distillation column is 180°C and the pressure of the distillation column is 0.4 MPa. The obtained high-purity organic amine is tested by a detection mechanism. The organic amine with the required purity is then conveyed to a storage tank via a conveying mechanism for storage. It can be used as a catalyst solvent for the production of pentafluoroethane.

[0077] Example 4

[0078] Reference Figure 1 A process for treating spent catalysts in pentafluoroethane production includes the following steps:

[0079] S1: Collect the waste catalyst and let it stand for a certain period of time;

[0080] S2: Add some of the spent catalyst to the reaction solution and mix.

[0081] S3: Electrolyze the treated reaction solution to produce pentafluoroethane;

[0082] S4: Add the remaining waste catalyst to the reaction solution and stir to mix;

[0083] S5: Allow the treated reaction solution to stand and separate the two phases to obtain an organic phase and an inorganic phase;

[0084] S6: Filter the organic phase to obtain an aqueous solution of KF;

[0085] S7: The inorganic phase is subjected to vacuum distillation to obtain high-purity organic amines.

[0086] In this embodiment, in S1, the waste catalyst is collected by a collection mechanism and transported to a storage tank by a conveying mechanism, where it is left to stand for 23 hours.

[0087] In this embodiment, in step S2, 50% of the upper part of the static waste catalyst is extracted by the extraction mechanism and transported to the first reaction vessel by the conveying mechanism. Alkali solution is added to the reaction vessel by the adding mechanism, and the waste catalyst and alkali solution are stirred and mixed by the stirring mechanism. The mixing reaction time is 4 hours, and the temperature of the first reaction vessel is 200°C.

[0088] In this embodiment, in step S3, the conveying mechanism transports the waste liquid after the reaction to the electrolytic cell, and the waste liquid after the reaction is electrolyzed in the electrolytic cell to obtain pentafluoroethane.

[0089] In this embodiment, in step S4, the remaining 50% of the waste catalyst in the storage tank is transported to the second reactor by the conveying mechanism, and KOH aqueous solution is added to the second reactor by the adding mechanism. The KOH aqueous solution and waste catalyst in the second reactor are stirred and mixed by the stirring mechanism for 5 hours.

[0090] In this embodiment, in step S5, the reaction liquid after the reaction is transported to a storage tank for settling by a conveying mechanism. After settling, the two phases separate, with the lower layer being an inorganic phase containing potassium fluoride and the upper layer being an organic phase containing organic amines.

[0091] In this embodiment, in step S6, the inorganic phase is conveyed by a conveying mechanism and filtered by a filtration mechanism to obtain a KF aqueous solution.

[0092] In this embodiment, in step S7, the organic phase is conveyed to a distillation column via a conveying mechanism. The distillation column performs vacuum distillation on the inorganic phase to obtain a high-purity organic amine. The temperature of the distillation column is 200°C and the pressure of the distillation column is 0.6 MPa. The obtained high-purity organic amine is tested by a detection mechanism. The organic amine with the required purity is then conveyed to a storage tank via a conveying mechanism for storage. It can be used as a catalyst solvent for the production of pentafluoroethane.

[0093] Example 5

[0094] Reference Figure 1 A process for treating spent catalysts in pentafluoroethane production includes the following steps:

[0095] S1: Collect the waste catalyst and let it stand for a certain period of time;

[0096] S2: Add some of the spent catalyst to the reaction solution and mix.

[0097] S3: Electrolyze the treated reaction solution to produce pentafluoroethane;

[0098] S4: Add the remaining waste catalyst to the reaction solution and stir to mix;

[0099] S5: Allow the treated reaction solution to stand and separate the two phases to obtain an organic phase and an inorganic phase;

[0100] S6: Filter the organic phase to obtain a KF aqueous solution;

[0101] S7: The inorganic phase is subjected to vacuum distillation to obtain high-purity organic amines.

[0102] In this embodiment, in S1, the waste catalyst is collected by a collection mechanism and transported to a storage tank by a conveying mechanism, where it is left to stand for 26 hours.

[0103] In this embodiment, in step S2, 50% of the upper part of the static waste catalyst is extracted by the extraction mechanism and transported to the first reaction vessel by the conveying mechanism. Alkali solution is added to the reaction vessel by the adding mechanism, and the waste catalyst and alkali solution are stirred and mixed by the stirring mechanism. The mixing reaction time is 6 hours, and the temperature of the first reaction vessel is 220°C.

[0104] In this embodiment, in step S3, the conveying mechanism transports the waste liquid after the reaction to the electrolytic cell, and the waste liquid after the reaction is electrolyzed in the electrolytic cell to obtain pentafluoroethane.

[0105] In this embodiment, in step S4, the remaining 50% of the waste catalyst in the storage tank is transported to the second reactor by the conveying mechanism, and KOH aqueous solution is added to the second reactor by the adding mechanism. The KOH aqueous solution and waste catalyst in the second reactor are stirred and mixed by the stirring mechanism for 7 hours.

[0106] In this embodiment, in step S5, the reaction liquid after the reaction is transported to a storage tank for settling by a conveying mechanism. After settling, the two phases separate, with the lower layer being an inorganic phase containing potassium fluoride and the upper layer being an organic phase containing organic amines.

[0107] In this embodiment, in step S6, the inorganic phase is conveyed by a conveying mechanism and filtered by a filtration mechanism to obtain a KF aqueous solution.

[0108] In this embodiment, in step S7, the organic phase is conveyed to a distillation column via a conveying mechanism. The distillation column performs vacuum distillation on the inorganic phase to obtain a high-purity organic amine. The temperature of the distillation column is 220°C and the pressure of the distillation column is 0.8 MPa. The obtained high-purity organic amine is tested by a detection mechanism. The organic amine with the required purity is then conveyed to a storage tank via a conveying mechanism for storage. It can be used as a catalyst solvent for the production of pentafluoroethane.

[0109] Experimental Example

[0110] The experimental data from the waste catalyst treatment schemes proposed in Examples 1 to 5 for pentafluoroethane production are compared with conventional waste catalyst treatment schemes. The results are shown in the table below.

[0111] Example 1 Example 1 Example 1 Example 1 Example 1 Improved recovery rate Improved recovery rate Improved recovery rate Improved recovery rate Improved recovery rate 6% 8% 10% 12% 15%

[0112] The above description is only a preferred embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any equivalent substitutions or modifications made by those skilled in the art within the scope of the technology disclosed in the present invention, based on the technical solution and inventive concept of the present invention, should be covered within the scope of protection of the present invention.

Claims

1. A process for treating spent catalysts in pentafluoroethane production, characterized in that: Includes the following steps: S1: Collect the waste catalyst and let it stand for a certain period of time; S2: Add some of the spent catalyst to the reaction solution and mix. S3: Electrolyze the treated reaction solution to produce pentafluoroethane; S4: Add the remaining waste catalyst to the reaction solution and stir to mix; S5: Allow the treated reaction solution to stand and separate the two phases to obtain an organic phase and an inorganic phase; S6: Filter the organic phase to obtain a KF aqueous solution; S7: The inorganic phase is subjected to vacuum distillation to obtain high-purity organic amines.

2. The process for treating spent catalyst in pentafluoroethane production according to claim 1, characterized in that: In step S1, the waste catalyst is collected by a collection mechanism and transported to a storage tank by a conveying mechanism, where it is left to stand for 20-25 hours.

3. The process for treating spent catalyst in pentafluoroethane production according to claim 2, characterized in that: In step S2, 50% of the upper part of the static waste catalyst is extracted by the extraction mechanism and transported to the first reaction vessel by the conveying mechanism. Alkali solution is added to the reaction vessel by the adding mechanism, and the waste catalyst and alkali solution are stirred and mixed by the stirring mechanism. The mixing reaction time is 1-6 hours, and the temperature of the first reaction vessel is 100-220℃.

4. The process for treating spent catalyst in pentafluoroethane production according to claim 3, characterized in that: In step S3, the conveying mechanism transports the waste liquid after the reaction to the electrolytic cell, and the waste liquid after the reaction is electrolyzed in the electrolytic cell to obtain pentafluoroethane.

5. The process for treating spent catalyst in pentafluoroethane production according to claim 4, characterized in that: In step S4, the remaining 50% of the waste catalyst in the storage tank is transported to the second reactor by a conveying mechanism, and KOH aqueous solution is added to the second reactor by an adding mechanism.

6. The process for treating spent catalyst in pentafluoroethane production according to claim 5, characterized in that: In step S4, the KOH aqueous solution and the waste catalyst in the second reactor are stirred and mixed by a stirring mechanism for 2-7 hours.

7. The process for treating spent catalyst in pentafluoroethane production according to claim 6, characterized in that: In step S5, the reaction liquid after the reaction is transported to a storage tank for settling through a conveying mechanism. After settling, the two phases separate, with the lower layer being an inorganic phase containing potassium fluoride and the upper layer being an organic phase containing organic amines.

8. The process for treating spent catalyst in pentafluoroethane production according to claim 7, characterized in that: In step S6, the inorganic phase is conveyed by a conveying mechanism and filtered by a filtration mechanism to obtain a KF aqueous solution.

9. The process for treating spent catalyst in pentafluoroethane production according to claim 8, characterized in that: In step S7, the organic phase is conveyed to the distillation column by a conveying mechanism. The distillation column performs vacuum distillation on the inorganic phase to obtain high-purity organic amine. The temperature of the distillation column is 140-220℃ and the pressure of the distillation column is 0.2-0.8 MPa.

10. The process for treating spent catalyst in pentafluoroethane production according to claim 9, characterized in that: In step S7, the obtained high-purity organic amine is tested by a testing agency, and the organic amine with the required purity is transported to a storage tank for storage by a conveying agency, which can be used as a catalyst solvent for pentafluoroethane production.

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