CN218710089U - Device for producing tetramethyl piperidone through continuous catalytic synthesis - Google Patents
Device for producing tetramethyl piperidone through continuous catalytic synthesis Download PDFInfo
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- CN218710089U CN218710089U CN202222906420.9U CN202222906420U CN218710089U CN 218710089 U CN218710089 U CN 218710089U CN 202222906420 U CN202222906420 U CN 202222906420U CN 218710089 U CN218710089 U CN 218710089U
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Abstract
The utility model discloses a device for producing tetramethylpiperidone by continuous catalytic synthesis, which comprises a premixing kettle, a reaction kettle group, a synthesis kettle group and a rotary settling separator which are sequentially communicated, wherein the reaction kettle group comprises at least two stages of reaction kettles, and the synthesis kettle group comprises at least two stages of curing kettles; liquid level differences are arranged between the adjacent two-stage reaction kettles, between the last-stage reaction kettle of the reaction kettle group and the first-stage curing kettle of the synthesis kettle group, between the adjacent two-stage curing kettles, and between the discharge port of the last-stage curing kettle of the synthesis kettle group and the material tangential inlet of the rotary sedimentation separator; a catalyst replenishing port is arranged at the top of the first-stage curing kettle of the synthesis kettle group; and the rotary sedimentation separator is also connected with a caustic soda inlet pipe, and a centrifugal pump is arranged on the caustic soda inlet pipe. The utility model discloses can realize the serialization production of technology, reduce the use amount of catalyst by a wide margin, improve catalysis efficiency, reduce the time of reaction, improve the product yield.
Description
Technical Field
The utility model relates to a device of synthetic production tetramethyl piperidone of continuous catalysis belongs to hindered amine light stabilizer midbody synthesis technical field.
Background
The chemical name of the tetramethylpiperidone is 2, 6-tetramethylpiperidone, namely triacetonamine, and the triacetonamine is an important synthesis intermediate, and the main synthesis methods are an indirect method and a direct method.
The indirect method is to synthesize intermediates such as diacetone alcohol, acetonine and phorone by taking acetone and ammonia as raw materials, and then synthesize triacetonamine by taking the intermediates, acetone and ammonia as raw materials, for example, patent US3943139 and patent US3960875 respectively disclose a method for synthesizing triacetonamine by taking acetonine, phorone and diacetone alcohol as raw materials and synthesizing triacetonamine with good yield. However, the synthesis and separation of acetonine, phorone and diacetone alcohol are very difficult, the steps are long, the cost is high, and the industrialization is difficult to realize. Therefore, the current methods at home and abroad are mainly direct methods.
The direct method is a method for directly synthesizing triacetonamine by taking acetone and ammonia as raw materials under the action of a catalyst. Compared with an indirect method, the method can avoid the step of separating and purifying the intermediate product, can save manpower and material resources to a great extent, and reduces the production cost, but although the yield of the method is still good, strong base such as sodium hydroxide is required to be added in the post-treatment process to neutralize the ammonium nitrate used as the catalyst, a large amount of waste water is generated, difficulty is brought to the post-treatment, and meanwhile, potential safety hazards can also exist due to improper treatment.
In view of the foregoing, it is apparent that the prior art has inconvenience and disadvantages in practical use, and thus, needs to be improved.
SUMMERY OF THE UTILITY MODEL
The utility model discloses to not enough in the background art, provide a device of continuous catalytic synthesis production tetramethyl piperidone, can realize the serialization production of technology, reduce the use amount of catalyst by a wide margin, improve catalytic efficiency, reduce the time of reaction, improve the product yield.
For solving the technical problem, the utility model adopts the following technical scheme:
a device for producing tetramethylpiperidone through continuous catalytic synthesis comprises a premixing kettle, a reaction kettle group, a synthesis kettle group and a rotary settling separator which are sequentially communicated, wherein the reaction kettle group comprises at least two stages of reaction kettles, and the synthesis kettle group comprises at least two stages of curing kettles;
liquid level differences are arranged between the adjacent two-stage reaction kettles, between the last-stage reaction kettle of the reaction kettle group and the first-stage curing kettle of the synthesis kettle group, between the adjacent two-stage curing kettles, and between the discharge port of the last-stage curing kettle of the synthesis kettle group and the material tangential inlet of the rotary sedimentation separator;
a catalyst replenishing port is arranged at the top of the first-stage curing kettle of the synthesis kettle group;
and the rotary sedimentation separator is also connected with a caustic soda inlet pipe, and a centrifugal pump is installed on the caustic soda inlet pipe.
According to an optimized scheme, heat exchange jackets are arranged outside the premixing kettle, the reaction kettle and the curing kettle.
Further, stirring devices are arranged inside the premixing kettle, the reaction kettle and the curing kettle.
Furthermore, the top of the premixing kettle is provided with a catalyst inlet and a material inlet, and the bottom of the premixing kettle is provided with a material outlet.
Further, the feed inlets of the premixing kettle and the first-stage reaction kettle are communicated through a pipeline; the top of the reaction kettle is provided with a feed inlet and a discharge outlet, the bottom of the reaction kettle is provided with a liquid ammonia inlet, and the top of the reaction kettle is provided with a liquid ammonia outlet; and the liquid ammonia inlet is respectively communicated with the delivery pump A.
Further, a material tangential inlet of the rotary sedimentation separator is communicated with a discharge hole of a final-stage curing kettle of the synthesis kettle group through a pipeline, and a delivery pump B is installed on the pipeline.
Furthermore, an organic phase crude material outlet is formed in the top of the rotary settling separator and communicated with a product crude product storage tank, a water phase outlet is formed in the bottom of the rotary settling separator and communicated with a byproduct crude product storage tank.
The utility model adopts the above technical scheme after, compare with prior art, have following advantage:
the utility model adopts the continuous synthesis design, realizes the continuous production of the process, greatly reduces the usage amount of the catalyst, and improves the catalytic efficiency; the curing stage adopts the composite catalyst, so that the reaction time is reduced, and the product yield is improved; the side reaction is small, the rectification and purification are easy, and the product purity is high; the reaction can be carried out by using a recyclable solid catalyst, and the production amount of byproduct salt is greatly reduced.
The present invention will be described in detail with reference to the accompanying drawings and examples.
Drawings
Fig. 1 is a schematic structural diagram of the present invention.
In the figure, 1-a premixing kettle, 11-a catalyst inlet, 2-a reaction kettle group, 21-a liquid ammonia inlet, 22-a liquid ammonia outlet, 23-a delivery pump A, 3-a synthesis kettle group, 31-a catalyst replenishing port, 4-a rotary settling separator, 41-a delivery pump B, 42-a caustic soda inlet pipe, 43-a centrifugal pump, 44-an organic phase coarse material outlet and 45-a water phase outlet.
Detailed Description
In order to clearly understand the technical features, objects and effects of the present invention, the embodiments of the present invention will be described with reference to the accompanying drawings.
As shown in figure 1, the utility model provides a device of synthetic production tetramethyl piperidone of catalysis in succession, including intercommunication in proper order set up mix cauldron 1 in advance, reation kettle group 2, synthetic cauldron group 3 and rotatory sedimentation separator 4, reation kettle group 2 includes at least two-stage reation kettle, and synthetic cauldron group 3 includes at least two-stage curing kettle.
Liquid level differences are arranged between the adjacent two-stage reaction kettles, between the last-stage reaction kettle of the reaction kettle group 2 and the first-stage curing kettle of the synthesis kettle group 3, between the adjacent two-stage curing kettles, and between the discharge port of the last-stage curing kettle of the synthesis kettle group 3 and the material tangential inlet of the rotary sedimentation separator 4.
The outside of premixing cauldron 1, reation kettle and curing cauldron all is equipped with the heat transfer and presss from both sides the cover, and the heat transfer presss from both sides the cover and is used for realizing the heating and the cooling of cauldron internal material.
And stirring devices are arranged in the premixing kettle 1, the reaction kettle and the curing kettle.
The top of the premixing kettle 1 is provided with a catalyst inlet 11 and a material inlet, and the bottom of the premixing kettle 1 is provided with a material outlet.
The feed inlets of the premixing kettle 1 and the first-stage reaction kettle are communicated through a pipeline; the top of the reaction kettle is provided with a feed inlet and a discharge outlet, the bottom of the reaction kettle is provided with a liquid ammonia inlet 21, and the top of the reaction kettle is provided with a liquid ammonia outlet 22; the liquid ammonia inlets 21 are respectively communicated with a delivery pump A23.
The top of the first-stage curing kettle of the synthesis kettle group 3 is provided with a catalyst replenishing port 31; the material inlet and the material outlet of the two adjacent stages of curing kettles are connected end to end.
The material tangential inlet of the rotary sedimentation separator 4 is communicated with the discharge hole of the final-stage curing kettle of the synthesis kettle group 3 through a pipeline, and a delivery pump B41 is arranged on the pipeline.
The rotary sedimentation separator 4 is also connected with a caustic soda inlet pipe 42, and a centrifugal pump 43 is arranged on the caustic soda inlet pipe 42; the top of the rotary settling separator 4 is provided with an organic phase crude material outlet 44, the organic phase crude material outlet 44 is communicated with a product crude product storage tank, the bottom of the rotary settling separator 4 is provided with a water phase outlet 45, and the water phase outlet 45 is communicated with a byproduct crude product storage tank.
The method for continuously catalytically synthesizing the tetramethyl piperidone by using the device comprises the following steps:
preheating, namely adding acetone and a catalyst a into a premixing kettle 1 according to a mass ratio of 500;
secondly, synthesizing, namely continuously feeding the mixed acetone material into a first-stage reaction kettle from the top, pumping liquid ammonia into the reaction kettle from a liquid ammonia inlet 21, carrying out mixed reaction in the reaction kettle, controlling the reaction pressure to be 0.10MPa and the reaction temperature to be 60 ℃, overflowing the reaction liquid to a second-stage reaction kettle through the top of the reaction kettle, wherein the operation conditions of the second-stage reaction kettle are the same as those of the first-stage reaction kettle;
thirdly, curing, namely, overflowing the reaction solution after the reaction to a first-stage curing kettle through the top of a second-stage reaction kettle, adding a catalyst b through a catalyst replenishing port 31, regulating the temperature in the kettle to 63 ℃ by controlling the flow rate of cooling water of a jacket outside the kettle, communicating the top of the curing kettle with the top of the reaction kettle, keeping the pressure consistent, and setting the pressure in the kettle to be 0.10MPa; the curing liquid overflows to a second-stage curing kettle through the top of the first-stage curing kettle, and the operating conditions of the second-stage curing kettle are the same as those of the first-stage curing kettle;
the fourth part is continuously neutralized and separated, and the synthesized crude product continuously enters a rotary settling separator 4 from a second-stage curing kettle through a conveying pump B41; caustic soda with the concentration of 80% is pumped into the rotary sedimentation separator 4 through a centrifugal pump 43, the flow control adopts flow linkage control, the neutralization temperature is controlled to be 55 ℃, and the pH value of a neutralization solution is controlled to be 14; through the centrifugal action, the organic phase coarse material continuously flows out from the top of the rotary sedimentation separator 4, and the water phase is discharged after being reduced to the cone bottom in a rotational flow mode.
And step five, refining, namely rectifying, crystallizing and separating the obtained organic phase crude material to obtain a tetramethylpiperidone product with the content of 99 percent.
The foregoing is illustrative of the best mode of the invention, and details not described herein are within the common general knowledge of a person of ordinary skill in the art. The protection scope of the present invention is subject to the content of the claims, and any equivalent transformation based on the technical teaching of the present invention is also within the protection scope of the present invention.
Claims (7)
1. A device for producing tetramethyl piperidone through continuous catalytic synthesis is characterized in that: the device comprises a premixing kettle (1), a reaction kettle group (2), a synthesis kettle group (3) and a rotary sedimentation separator (4) which are sequentially communicated, wherein the reaction kettle group (2) comprises at least two stages of reaction kettles, and the synthesis kettle group (3) comprises at least two stages of curing kettles;
liquid level differences are arranged between two adjacent stages of reaction kettles, between the last stage reaction kettle of the reaction kettle group (2) and the first stage curing kettle of the synthesis kettle group (3), between two adjacent stages of curing kettles, and between the discharge port of the last stage curing kettle of the synthesis kettle group (3) and the material tangential inlet of the rotary sedimentation separator (4);
a catalyst replenishing port (31) is arranged at the top of the first-stage curing kettle of the synthesis kettle group (3);
and the rotary sedimentation separator (4) is also connected with a caustic soda inlet pipe (42), and a centrifugal pump (43) is arranged on the caustic soda inlet pipe (42).
2. The apparatus for continuous catalytic synthesis of tetramethylpiperidone according to claim 1, comprising: and heat exchange jackets are arranged outside the premixing kettle (1), the reaction kettle and the curing kettle.
3. The apparatus for continuous catalytic synthesis of tetramethylpiperidone according to claim 1, comprising: and stirring devices are arranged in the premixing kettle (1), the reaction kettle and the curing kettle.
4. The apparatus for continuous catalytic synthesis of tetramethylpiperidone as described in claim 1, comprising: the top of the premixing kettle (1) is provided with a catalyst inlet (11) and a material inlet, and the bottom of the premixing kettle (1) is provided with a material outlet.
5. The apparatus for continuous catalytic synthesis of tetramethylpiperidone according to claim 1, comprising: the premixing kettle (1) is communicated with a feed inlet of the first-stage reaction kettle through a pipeline; the top of the reaction kettle is provided with a feed inlet and a discharge outlet, the bottom of the reaction kettle is provided with a liquid ammonia inlet (21), and the top of the reaction kettle is provided with a liquid ammonia outlet (22); and the liquid ammonia inlet (21) is respectively communicated with a delivery pump A (23).
6. The apparatus for continuous catalytic synthesis of tetramethylpiperidone according to claim 1, comprising: the material tangential inlet of the rotary sedimentation separator (4) is communicated with the discharge hole of the final-stage curing kettle of the synthesis kettle group (3) through a pipeline, and a delivery pump B (41) is arranged on the pipeline.
7. The apparatus for continuous catalytic synthesis of tetramethylpiperidone according to claim 1, comprising: the top of the rotary settling separator (4) is provided with an organic phase coarse material outlet (44), the organic phase coarse material outlet (44) is communicated with a product coarse product storage tank, the bottom of the rotary settling separator (4) is provided with a water phase outlet (45), and the water phase outlet (45) is communicated with a byproduct coarse product storage tank.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202222906420.9U CN218710089U (en) | 2022-11-02 | 2022-11-02 | Device for producing tetramethyl piperidone through continuous catalytic synthesis |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202222906420.9U CN218710089U (en) | 2022-11-02 | 2022-11-02 | Device for producing tetramethyl piperidone through continuous catalytic synthesis |
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| CN218710089U true CN218710089U (en) | 2023-03-24 |
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| CN202222906420.9U Active CN218710089U (en) | 2022-11-02 | 2022-11-02 | Device for producing tetramethyl piperidone through continuous catalytic synthesis |
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