CN220238517U - Raney nickel catalyst recovery device for preparing amine from aliphatic nitrile - Google Patents
Raney nickel catalyst recovery device for preparing amine from aliphatic nitrile Download PDFInfo
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- CN220238517U CN220238517U CN202321515052.3U CN202321515052U CN220238517U CN 220238517 U CN220238517 U CN 220238517U CN 202321515052 U CN202321515052 U CN 202321515052U CN 220238517 U CN220238517 U CN 220238517U
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- NPXOKRUENSOPAO-UHFFFAOYSA-N Raney nickel Chemical compound [Al].[Ni] NPXOKRUENSOPAO-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 238000011084 recovery Methods 0.000 title claims abstract description 37
- 229910000564 Raney nickel Inorganic materials 0.000 title claims abstract description 36
- 150000001412 amines Chemical class 0.000 title claims abstract description 27
- -1 aliphatic nitrile Chemical class 0.000 title claims abstract description 26
- 238000000605 extraction Methods 0.000 claims abstract description 77
- 238000011069 regeneration method Methods 0.000 claims abstract description 73
- 230000008929 regeneration Effects 0.000 claims abstract description 71
- 238000006243 chemical reaction Methods 0.000 claims abstract description 65
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000002904 solvent Substances 0.000 claims abstract description 35
- 239000006228 supernatant Substances 0.000 claims abstract description 21
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 20
- 238000011049 filling Methods 0.000 claims abstract description 19
- 239000001257 hydrogen Substances 0.000 claims abstract description 19
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 19
- 239000007788 liquid Substances 0.000 claims description 2
- 238000005984 hydrogenation reaction Methods 0.000 description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 11
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- 239000000463 material Substances 0.000 description 9
- 239000003880 polar aprotic solvent Substances 0.000 description 8
- 239000000047 product Substances 0.000 description 8
- 238000005086 pumping Methods 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 7
- 239000012046 mixed solvent Substances 0.000 description 7
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- CYSGHNMQYZDMIA-UHFFFAOYSA-N 1,3-Dimethyl-2-imidazolidinon Chemical group CN1CCN(C)C1=O CYSGHNMQYZDMIA-UHFFFAOYSA-N 0.000 description 5
- RWNUSVWFHDHRCJ-UHFFFAOYSA-N 1-butoxypropan-2-ol Chemical compound CCCCOCC(C)O RWNUSVWFHDHRCJ-UHFFFAOYSA-N 0.000 description 5
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical compound CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 239000003586 protic polar solvent Substances 0.000 description 5
- 230000001172 regenerating effect Effects 0.000 description 5
- 239000007868 Raney catalyst Substances 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- GLDOVTGHNKAZLK-UHFFFAOYSA-N octadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 description 4
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000009849 deactivation Effects 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 150000002825 nitriles Chemical class 0.000 description 2
- 238000000638 solvent extraction Methods 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000000010 aprotic solvent Substances 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 239000002638 heterogeneous catalyst Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Landscapes
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
The utility model discloses a Raney nickel catalyst recovery device for preparing amine from aliphatic nitrile, which comprises the following components: the device comprises a reaction kettle, an extraction regeneration kettle, a rectifying kettle, a solvent filling pipeline, a hydrogen recovery pipeline, a nitrogen pipeline and a vacuum pipeline; the reaction kettle is connected with a feed inlet of the extraction regeneration kettle through a pipeline, a discharge outlet of the extraction regeneration kettle is connected with the feed inlet of the reaction kettle through a pipeline, the extraction regeneration kettle is connected with a feed inlet of the rectification kettle through a supernatant extraction pipe, a solvent filling pipeline is connected with the reaction kettle and the extraction regeneration kettle, a hydrogen recovery pipeline is connected with the reaction kettle, a nitrogen pipeline is connected with the reaction kettle, and a vacuum pipeline is connected with the reaction kettle, the extraction regeneration kettle and the rectification kettle.
Description
Technical Field
The utility model relates to the technical field of catalyst recovery, in particular to a Raney nickel catalyst recovery device for preparing amine from aliphatic nitrile.
Background
The higher aliphatic amine (carbon chain length is between C8 and C24) is a chemical raw material with wide application, and is generally prepared by the steps of hydrogenation of higher aliphatic nitrile under the action of nickel catalyst, removal of catalyst by precipitation of hydrogenation product, removal of solvent and the like. Raney nickel is a catalyst commonly used for nitrile hydrogenation by virtue of the advantages of low preparation cost, high activity and the like, and the preparation method is that a nickel-aluminum alloy is adopted to remove aluminum through alkali dissolution to prepare a solid heterogeneous catalyst with a porous structure and composed of fine grains. Therefore, the recovery sleeve of Raney nickel is important in the aspect of controlling the production cost of the higher aliphatic amine.
As is well known, the Raney nickel catalyst is recovered by filtration after hydrogenation, and is washed and regenerated under the action of an alkali solution and a solvent, and the solvent is usually combustible liquid such as methanol, ethanol, toluene, isopropanol, ethyl acetate, tetrahydrofuran and the like, so that the solvents are high in volatility and extremely dangerous when being mixed with the Raney nickel which is extremely easy to self-ignite, so that the Raney nickel recovery process has extremely high potential safety hazard, and the filtering time is quite long, thereby influencing the production efficiency.
On the other hand, higher aliphatic nitrile and higher aliphatic amine products thereof have smaller solubility in solvents such as methanol and ethanol, even slightly soluble, and poor washing and regeneration effects by solvents such as methanol and ethanol, and are easy to cause catalyst particle adhesion due to larger molecular weight compared with lower nitrile and lower amine products.
In view of the foregoing, it is desirable to provide a new Raney nickel catalyst recovery device for the preparation of amines from aliphatic nitriles that overcomes the above-mentioned drawbacks.
Disclosure of Invention
The utility model aims to provide a Raney nickel catalyst recovery device for preparing amine from aliphatic nitrile, which can extract aliphatic amine and regenerate the Raney nickel catalyst, thereby being beneficial to improving the production efficiency.
In order to achieve the above object, the present utility model provides a Raney nickel catalyst recovery device for preparing amine from aliphatic nitrile, comprising: the device comprises a reaction kettle, an extraction regeneration kettle, a rectifying kettle, a solvent filling pipeline, a hydrogen recovery pipeline, a nitrogen pipeline and a vacuum pipeline;
the reaction kettle is connected with a feed inlet of the extraction regeneration kettle through a pipeline, a discharge outlet of the extraction regeneration kettle is connected with the feed inlet of the reaction kettle through a pipeline, the extraction regeneration kettle is connected with a feed inlet of the rectification kettle through a supernatant extraction pipe, a solvent filling pipeline is connected with the reaction kettle and the extraction regeneration kettle, a hydrogen recovery pipeline is connected with the reaction kettle, a nitrogen pipeline is connected with the reaction kettle, and a vacuum pipeline is connected with the reaction kettle, the extraction regeneration kettle and the rectification kettle.
Preferably, the device further comprises a pump, wherein the pump is connected with the top of the reaction kettle and the bottom of the extraction regeneration kettle through a suction pipeline.
Preferably, a first valve is connected between the hydrogen recovery pipeline and the reaction kettle.
Preferably, a second valve is connected between the nitrogen pipeline and the bottom of the reaction kettle.
Preferably, a third valve is arranged at the joint of the solvent filling pipeline and the reaction kettle, and a fourth valve is arranged at the joint of the solvent filling pipeline and the extraction regeneration kettle.
Preferably, a fifth valve is arranged on the supernatant extracting pipe between the extraction regeneration kettle and the rectifying kettle.
A recovery method of Raney nickel catalyst recovery device for preparing amine from aliphatic nitrile comprises the following steps:
transferring a product after the hydrogenation reaction of the aliphatic nitrile in the reaction kettle into an extraction regeneration kettle for sedimentation, and extracting supernatant of a mixture in the extraction regeneration kettle to a rectifying kettle;
adding a non-flammable and low-volatility solvent into an extraction regeneration kettle, extracting, regenerating and settling, extracting the supernatant of the mixture in the extraction regeneration kettle into a rectifying kettle, and repeating the extraction and regeneration for three times;
and after the extraction regeneration is finished, performing reduced pressure distillation to separate the higher aliphatic amine and the non-flammable and low-volatility mixed solvent in the mixture, and transferring the Raney nickel catalyst into a reaction kettle for hydrogenation reaction.
Preferably, the non-flammable and low-volatility mixed solvent comprises a strong polar aprotic solvent and a low polar protic solvent, and the material ratio of the strong polar aprotic solvent to the low polar protic solvent is 5-30:70-95.
Preferably, the strongly polar aprotic solvent is 1,3 dimethyl-2-imidazolidone; the low-polarity proton solvent is one or two of ethylene glycol butyl ether and propylene glycol butyl ether.
Compared with the prior art, the beneficial effects are that: the Raney nickel catalyst is prevented from being contacted with air in the whole process of nitrogen protection, is prevented from being absorbed into human body in the air, and is harmful to human health, so that the safety production coefficient is greatly improved, and compared with a filtering method, the solvent extraction regeneration method shortens the extraction regeneration time and improves the production efficiency.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present utility model, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present utility model and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of a Raney nickel catalyst recovery device for preparing amine from aliphatic nitrile.
Reference numerals: 1. a reaction kettle; 2. extracting and regenerating the kettle; 3. a rectifying still; 4. a solvent filling line; 5. a hydrogen recovery line; 6. a nitrogen pipeline; 7. a vacuum pipeline; 8. a pump; 9. a first valve; 10. a second valve; 11. a third valve; 12. a fourth valve; 13. a fifth valve; 14. a suction line; 15. and a suction pump.
Detailed Description
In order to make the objects, technical solutions and advantageous technical effects of the present utility model more apparent, the present utility model will be further described in detail with reference to the accompanying drawings and detailed description. It should be understood that the detailed description is intended to illustrate the utility model, and not to limit the utility model.
It is to be understood that the terms "upper," "lower," "front," "rear," "left," "right," "top," "bottom," "inner," "outer," and the like indicate or are based on the orientation or positional relationship shown in the drawings, merely to facilitate describing the present utility model and simplify the description, and do not indicate or imply that the devices or elements being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus should not be construed as limiting the present utility model.
It should also be noted that unless explicitly stated or limited otherwise, terms such as "mounted," "connected," "secured," "disposed," and the like are to be construed broadly and may be, for example, fixedly connected, detachably connected, or integrally formed; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communicated with the inside of two elements or the interaction relationship of the two elements. It will be apparent to those skilled in the art that the terms described above have the particular meaning in the present utility model, as the case may be.
Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature. Furthermore, the meaning of "a plurality of", "a number" means two or more, unless specifically defined otherwise.
Referring to fig. 1, the present utility model provides a raney nickel catalyst recovery apparatus for preparing amine from aliphatic nitrile, comprising: a reaction kettle 1, an extraction regeneration kettle 2, a rectifying kettle 3, a solvent filling pipeline 4, a hydrogen recovery pipeline 5, a nitrogen pipeline 6 and a vacuum pipeline 7;
the reaction kettle 1 is internally provided with a product (containing Raney nickel catalyst) after the hydrogenation reaction of the aliphatic nitrile, a discharge hole at the bottom of the reaction kettle 1 is connected with a feed inlet at the top of an extraction regeneration kettle 2 through a pipeline, a discharge hole at the bottom of the extraction regeneration kettle 2 is connected with a feed inlet at the top of the reaction kettle 1 through a pipeline, the extraction regeneration kettle 2 is connected with a feed inlet at the bottom of a rectifying kettle 3 through a supernatant extraction pipe, a solvent filling pipeline 4 is connected with the reaction kettle 1 and the extraction regeneration kettle 2, a hydrogen recovery pipeline 5 is connected with the top of the reaction kettle 1, a nitrogen pipeline 6 is connected with the bottom of the reaction kettle 1, and a vacuum pipeline 7 is connected with the reaction kettle 1, the extraction regeneration kettle 2 and the rectifying kettle 3.
In this way, the non-inflammable and low-volatility compound solvent can be added into the reaction kettle 1 and the extraction regeneration kettle 2 through the solvent filling pipeline 4, and the nitrogen gas can be provided into the reaction kettle 1 through the nitrogen gas pipeline 6 to replace the air and the hydrogen gas in the reaction kettle 1.
It should be noted that the non-flammable and low-volatility composite solvent is composed of a strong polar aprotic solvent and a low polar protic solvent; the strong polar aprotic solvent is 1,3 dimethyl-2-imidazolidone; the low-polarity proton solvent is one or two of ethylene glycol butyl ether and propylene glycol butyl ether, and the material ratio of the strong-polarity aprotic solvent to the low-polarity proton solvent is 5-30: 70-95).
In one embodiment, the Raney nickel catalyst recovery device for preparing amine from aliphatic nitrile further comprises a pump 8, wherein the pump 8 is connected with the top of the reaction kettle 1 and the bottom of the extraction regeneration kettle 2 through a suction pipeline 14. Thus, when the pump is started, the materials in the extraction regeneration kettle 2 can be pumped into the reaction kettle 1 so as to react in the reaction kettle 1 again.
In one embodiment, a first valve 9 is connected between the hydrogen recovery pipeline 5 and the reaction kettle 1, and when the first valve 9 is opened, hydrogen generated after the reaction of the materials in the reaction kettle 1 is recovered to the hydrogen recovery pipeline 5.
In one embodiment, a second valve 10 is connected between the nitrogen pipeline 6 and the bottom of the reaction kettle 1, and when the second valve 10 is opened, nitrogen gradually enters from the bottom of the reaction kettle 1, and residual air and hydrogen in the reaction kettle 1 are slowly extruded, so that the air and hydrogen in the reaction kettle 1 are completely replaced.
In one embodiment, a third valve 11 is arranged at the connection position of the solvent filling pipe 4 and the reaction kettle 1, and a fourth valve 12 is arranged at the connection position of the solvent filling pipe 4 and the extraction regeneration kettle 2. When the third valve 11 is opened, the non-flammable and low-volatility compound solvent in the solvent filling pipeline 4 flows into the reaction kettle 1, and when the fourth valve 12 is opened, the non-flammable and low-volatility compound solvent in the solvent filling pipeline 4 flows into the extraction regeneration kettle 2.
In one embodiment, a fifth valve 13 is arranged on the supernatant extracting pipe between the extraction and regeneration kettle 2 and the rectifying kettle 3, and when the fifth valve 13 is opened, a suction pump 15 on the rectifying kettle 3 is started to pump the supernatant of the extraction and regeneration kettle 2 into the rectifying kettle 3 through the supernatant extracting pipe.
When the hydrogenation reaction of the aliphatic nitrile is finished, the first valve 9 is opened to release the hydrogen in the reaction kettle 1 to the hydrogen recovery system, the second valve 10 is opened, the nitrogen pipeline 6 supplies nitrogen to the reaction kettle 1 to replace the residual air and hydrogen in the reaction kettle 1, positive pressure is maintained, the materials in the reaction kettle 1 enter the extraction regeneration kettle 2 along with nitrogen flow by utilizing the pressure difference between the reaction kettle 1 and the extraction regeneration kettle 2,
the fourth valve 12 is opened, the non-inflammable and low-volatility mixed solvent in the solvent filling pipeline 4 enters the extraction regeneration kettle 2 to extract the higher fatty amine, the fifth valve 13 is opened, the supernatant of the extraction regeneration kettle 2 is pumped into the rectifying kettle 3 through the supernatant pumping pipe, the non-inflammable and low-volatility mixed solvent is added to the extraction regeneration kettle 2 to extract the higher fatty amine, and the supernatant of the extraction regeneration kettle 2 is pumped into the rectifying kettle 3 through the supernatant pumping pipe again.
The utility model also provides a method for recovering the Raney nickel catalyst for preparing amine from the aliphatic nitrile, which comprises the following steps:
transferring Raney nickel catalyst into a reaction kettle 1, carrying out hydrogenation reaction under the condition of 100 ℃ and 2MPa, transferring the product after the hydrogenation reaction of the aliphatic nitrile in the reaction kettle 1 into an extraction regeneration kettle 2, settling for 30-45min, and extracting the supernatant of the mixture in the extraction regeneration kettle 2 into a rectifying kettle 3;
adding non-inflammable and low-volatility solvent into the extraction regeneration kettle 2, extracting and regenerating for 30-45min, wherein the extraction temperature is 30-60 ℃,
settling for 30min, extracting supernatant of the mixture in the extraction regeneration kettle 2 to a rectification kettle 3, and repeating extraction and regeneration for three times;
and after the extraction regeneration is finished, the materials in the rectifying still 3 are subjected to reduced pressure distillation, and the higher fatty amine and the non-flammable and low-volatility mixed solvent in the mixture are separated.
Specifically, the consumption of the non-inflammable and low-volatility mixed solvent for each extraction is 3-10 times of the amount of the Raney nickel catalyst.
Specifically, the non-flammable and low-volatility mixed solvent comprises a strong polar aprotic solvent and a low polar protic solvent, wherein the material ratio of the strong polar aprotic solvent to the low polar protic solvent is 5-30:70-95.
Specifically, the strong polar aprotic solvent is 1,3 dimethyl-2-imidazolidone; the low-polarity proton solvent is one or two of ethylene glycol butyl ether and propylene glycol butyl ether.
Examples:
1) Transferring 3000Kg of a product (containing 100Kg of Raney nickel catalyst) after the hydrogenation reaction of the aliphatic nitrile into an extraction regeneration kettle 2, settling for 30min at 40 ℃, and extracting 2850Kg of supernatant to a rectifying kettle 3;
2) Pumping 50Kg of 1,3 dimethyl-2-imidazolidone and 450kg of propylene glycol butyl ether into the extraction and regeneration kettle 2 through a suction pump on the extraction and regeneration kettle 2, controlling the temperature to 40 ℃, extracting and regenerating for 30min, settling for 30min, pumping supernatant of the extraction and regeneration kettle 2 into a rectifying kettle 3, and repeating the extraction and regeneration for three times;
3) After the extraction regeneration is finished, the materials in the rectifying still 3 are distilled under reduced pressure, and the collected octadecylamine (higher fatty amine) is marked as a sample I;
transferring 100Kg of Raney nickel catalyst into a reaction kettle 1, pumping 50Kg of 1,3 dimethyl-2-imidazolidone, 450Kg of propylene glycol butyl ether and 2400Kg of octadecanol into the reaction kettle 1 by a suction pump, replacing with nitrogen for three times, heating to 100 ℃, and carrying out hydrogenation reaction for 4 hours under the condition of 2 MPa;
after the hydrogenation reaction was completed, the steps 1), 2) and 3) in the above examples were repeated, and the collected octadecylamine (higher aliphatic amine) was designated as sample two.
Comparative example:
1) Transferring 3000Kg of a product (containing 100Kg of Raney nickel catalyst) after the hydrogenation reaction of the aliphatic nitrile into an extraction regeneration kettle 2, settling for 30min at 40 ℃, and extracting 2850Kg of supernatant to a rectifying kettle 3;
2) Pumping 500kg of absolute ethyl alcohol into the extraction and regeneration kettle 2 through a suction pump on the extraction and regeneration kettle 2, extracting and regenerating for 30min at 40 ℃, settling for 30min, pumping supernatant of the extraction and regeneration kettle 2 into a rectifying kettle 3, and repeating the extraction and regeneration for three times;
3) After the extraction regeneration is finished, the materials in the rectifying still 3 are distilled under reduced pressure, and the collected octadecylamine (higher fatty amine) is marked as a sample III;
4) After extraction regeneration is finished, transferring 100Kg of the obtained Raney nickel catalyst into a hydrogenation kettle, pumping 500Kg of absolute ethyl alcohol, 2400Kg of octadecanol, replacing nitrogen for three times, heating to 100-130 ℃, and carrying out hydrogenation reaction for 4 hours under the condition of 2-3 MPa;
5) After the hydrogenation reaction, repeating the steps 1), 2) and 3) in the comparative example, and recording the collected octadecylamine (higher fatty amine) as a sample IV;
the total amine number of the octadecylamine samples was determined and the test results are shown in Table 1:
in the table 1 of the description,
| sequence number | Project | Total amine value (mgKOH/g) |
| 1 | Sample one | 208.5 |
| 2 | Sample two | 206.3 |
| 3 | Sample three | 188.4 |
| 4 | Sample four | 160.8 |
As can be seen from Table 1, the Raney nickel catalyst recovered in the examples of the present utility model showed little sign of deactivation after two cycles of reaction (sample two compared to sample one) and significant deactivation in the comparative example (sample four compared to sample three).
According to the recovery device provided by the utility model, the whole recovery process of the Raney nickel catalyst is under the protection of nitrogen, so that the Raney nickel catalyst is prevented from contacting with air, being absorbed into human body and being harmful to human health, the safety production coefficient is greatly improved, and compared with a filtering method, the solvent extraction regeneration method is adopted, so that the extraction regeneration time is shortened, and the production efficiency is improved.
The present utility model is not limited to the details and embodiments described herein, and thus additional advantages and modifications may readily be made by those skilled in the art, without departing from the spirit and scope of the general concepts defined in the claims and the equivalents thereof, and the utility model is not limited to the specific details, representative apparatus and examples shown and described herein.
Claims (6)
1. A Raney nickel catalyst recovery device for preparing amine from aliphatic nitrile is characterized by comprising: the device comprises a reaction kettle (1), an extraction regeneration kettle (2), a rectifying kettle (3), a solvent filling pipeline (4), a hydrogen recovery pipeline (5), a nitrogen pipeline (6) and a vacuum pipeline (7);
the reaction kettle (1) is connected with a feed inlet of the extraction regeneration kettle (2) through a pipeline, a discharge outlet of the extraction regeneration kettle (2) is connected with the feed inlet of the reaction kettle (1) through a pipeline, the extraction regeneration kettle (2) is connected with a feed inlet of the rectification kettle (3) through a supernatant extraction pipe, a solvent filling pipeline (4) is connected with the reaction kettle (1) and the extraction regeneration kettle (2), a hydrogen recovery pipeline (5) is connected with the reaction kettle (1), a nitrogen pipeline (6) is connected with the reaction kettle (1), and a vacuum pipeline (7) is connected with the reaction kettle (1), the extraction regeneration kettle (2) and the rectification kettle (3).
2. The Raney nickel catalyst recovery device for producing amine from aliphatic nitrile according to claim 1, further comprising a pump (8), wherein the pump (8) is connected with the top of the reaction kettle (1) and the bottom of the extraction regeneration kettle (2) through a suction pipeline (14).
3. The Raney nickel catalyst recovery device for preparing amine from aliphatic nitrile according to claim 1, wherein a first valve (9) is connected between the hydrogen recovery pipeline (5) and the reaction kettle (1).
4. The Raney nickel catalyst recovery device for preparing amine from aliphatic nitrile according to claim 1, wherein a second valve (10) is connected between the nitrogen pipeline (6) and the bottom of the reaction kettle (1).
5. The Raney nickel catalyst recovery device for preparing amine from aliphatic nitrile according to claim 1, wherein a third valve (11) is arranged at the joint of the solvent filling pipeline (4) and the reaction kettle (1), and a fourth valve (12) is arranged at the joint of the solvent filling pipeline (4) and the extraction regeneration kettle (2).
6. The Raney nickel catalyst recovery device for preparing amine from aliphatic nitrile according to claim 1, wherein a fifth valve (13) is arranged on a supernatant liquid extraction pipe between the extraction regeneration kettle (2) and the rectification kettle (3).
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| CN202321515052.3U CN220238517U (en) | 2023-06-14 | 2023-06-14 | Raney nickel catalyst recovery device for preparing amine from aliphatic nitrile |
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| CN202321515052.3U CN220238517U (en) | 2023-06-14 | 2023-06-14 | Raney nickel catalyst recovery device for preparing amine from aliphatic nitrile |
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| Country | Link |
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