CN216946815U - Device for separating caprolactam from caprolactam sulfate and co-producing compound fertilizer - Google Patents
Device for separating caprolactam from caprolactam sulfate and co-producing compound fertilizer Download PDFInfo
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- CN216946815U CN216946815U CN202220688878.9U CN202220688878U CN216946815U CN 216946815 U CN216946815 U CN 216946815U CN 202220688878 U CN202220688878 U CN 202220688878U CN 216946815 U CN216946815 U CN 216946815U
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Abstract
The utility model provides a device for separating caprolactam from caprolactam sulfate and co-producing a compound fertilizer, which comprises a reaction kettle and an extraction tower, wherein the reaction kettle is provided with a first feed inlet and a second feed inlet, the first feed inlet is connected with a caprolactam sulfate pipeline, and the second feed inlet is connected with a batching pipeline; the device also comprises a batching tank, wherein the batching tank is provided with a batching feeding port and a solvent feeding port, and a liquid outlet of the batching tank is connected with a batching pipeline; the discharge port of the reaction kettle is connected to the feed port of the extraction tower through a pipeline and a pump, the upper extraction phase outlet of the extraction tower is connected to the caprolactam refining process through a pipeline, the lower extraction phase outlet is arranged at the lower part of the extraction tower, and the extraction phase outlet is connected to the compound fertilizer production system. The utility model has simple structure and low investment cost, avoids using high-risk gas ammonia and can greatly reduce the production cost of caprolactam.
Description
Technical Field
The utility model belongs to the field of chemical industry, relates to production of caprolactam, and particularly relates to a device for separating caprolactam from caprolactam sulfate and co-producing a compound fertilizer.
Background
The Beckmann rearrangement reaction is a key reaction for industrially producing caprolactam, i.e. free caprolactam is not generated in the production of caprolactam, but cyclohexanone oxime and SO3Generating cyclohexanone oxime sulfate and further generating caprolactam sulfate by transposition. Caprolactam and ammonium sulfate are produced commercially by a process in which caprolactam sulfate is neutralized with ammonia. The process is continuously used in caprolactam production, has the advantages of mature process, generation of salt by acid-base neutralization and convenient separation of caprolactam, and has the main disadvantages of large consumption of ammonia and fuming sulfuric acid with higher economic value, byproduct of ammonium sulfate with lower economic value and increase of production cost. How to improve the production process and reduce the consumption of ammonia becomes the direction of reducing the production cost in the production of caprolactam.
Meanwhile, the ammonium sulfate is unfavorable to soil as a nitrogenous fertilizer with low efficiency and obvious acidity, and acidification and hardening are easy to occur after long-term use of the ammonium sulfate, so that the ammonium sulfate is not welcomed by farmers all the time, is low in price, produces too much ammonium sulfate as a byproduct, and has the problem of difficult sale.
The company has three industrial chains of coal chemical industry, phosphorus chemical industry and petrochemical industry, and how to give full play to the advantages of the industrial chains and reduce the ammonium sulfate as a byproduct of caprolactam is always the research and development direction of the company.
Disclosure of Invention
The utility model provides a device for separating caprolactam from caprolactam sulfate and co-producing a compound fertilizer, which has the advantages of simple process flow, low equipment investment cost, capability of reducing the consumption of raw material ammonia and reduction of the production cost of caprolactam.
The technical scheme of the utility model is that the device for separating caprolactam from caprolactam sulfate and co-producing compound fertilizer comprises a reaction kettle and an extraction tower, wherein the reaction kettle is provided with a first feed inlet and a second feed inlet, the first feed inlet is connected with a caprolactam sulfate pipeline, and the second feed inlet is connected with a batching pipeline; the device also comprises a batching tank, wherein the batching tank is provided with a batching feeding port and a solvent feeding port, and a liquid outlet of the batching tank is connected with a batching pipeline; the discharge port of the reaction kettle is connected to the feed port of the extraction tower through a pipeline and a pump, the upper extraction phase outlet of the extraction tower is connected to the caprolactam refining process through a pipeline, the lower extraction phase outlet is arranged at the lower part of the extraction tower, and the extraction phase outlet is connected to the compound fertilizer production system.
Further, the device also comprises a rearrangement reactor, wherein a discharge port of the rearrangement reactor is connected to the first feed inlet of the reaction kettle.
Furthermore, a rearrangement circulating pump and a rearrangement cooler are arranged outside the rearrangement reactor to form a circulating pipeline, a fuming sulfuric acid pipeline is arranged between a rearrangement reactor circulating discharge port and the rearrangement circulating pump, and a cyclohexanone oxime feeding pipe is also arranged between the rearrangement cooler and the rearrangement reactor.
Further, a stirrer is arranged in the reaction kettle, and the discharged material at the bottom of the reaction kettle is connected to a circulating feed inlet through a reaction kettle circulating pump and a reaction kettle cooler to form a circulating loop; a branch pipe is arranged on the pipeline between the reaction kettle cooler and the reaction kettle and is connected to the extraction tower.
Furthermore, the feed inlet of the extraction tower is positioned at the upper part, and the lower part is provided with an extractant inlet.
Further, the raffinate phase outlet is positioned at the bottom and is connected to a compound fertilizer production system through a pipeline and a pump.
The utility model has the following beneficial effects:
cyclohexanone oxime and fuming sulfuric acid are mixed according to a certain proportion, rearrangement reaction is carried out in a rearrangement reactor, rearrangement liquid containing caprolactam sulfate enters a reaction kettle to react with ingredients from a proportioning tank, then the reaction liquid is cooled and then sent to an extraction tower to be in contact extraction with an extracting agent, caprolactam is extracted from the mixed solution to the extracting agent, and therefore separation of caprolactam and sulfate phases is achieved. The extracted light phase enters a caprolactam refining device from the upper part of the extraction device to separate high-purity caprolactam, and the sulfate aqueous solution of the extraction device is used as the extracted heavy phase and enters a slurry tank from the lower part of the extraction device to be used as a raw material for producing compound fertilizer and sent to a compound fertilizer production device.
The device has simple structure and low investment cost, uses the inorganic ammonium salt with low raw material price to replace ammonia to neutralize the sulfuric acid in the caprolactam sulfate, does not need to use gas ammonia, avoids the serious safety risks and environmental influences of ammonia leakage, poisoning, explosion and the like, can directly use the obtained raffinate as the raw material for producing the compound fertilizer, has high utilization rate, and can greatly reduce the production cost of the caprolactam.
Drawings
FIG. 1 is a schematic structural diagram of the apparatus of the present invention.
The system comprises a rearrangement reactor 1, a rearrangement cooler 2, a rearrangement circulating pump 3, a reaction kettle 4, a dosing tank 5, a dosing delivery pump 6, a reaction kettle circulating pump 7, a reaction kettle cooler 8, an extraction tower 9, an aqueous solution delivery pump 10, a stirrer 11, a dosing inlet 12 and an extractant inlet 13.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but those skilled in the art will appreciate that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention.
A device for separating caprolactam from caprolactam sulfate and co-producing a compound fertilizer comprises a reaction kettle 4 and an extraction tower 9, wherein the reaction kettle is provided with a first feed inlet and a second feed inlet, the first feed inlet is connected with a caprolactam sulfate pipeline, and the second feed inlet is connected with a batching pipeline; the device also comprises a batching tank 5, wherein the batching tank is provided with a batching feeding port and a solvent feeding port, and a liquid outlet of the batching tank is connected with a batching pipeline; the discharge port of the reaction kettle is connected to the feed port of the extraction tower through a pipeline and a pump, the extraction phase outlet at the upper part of the extraction tower is connected to the caprolactam refining process through a pipeline, the raffinate phase outlet is arranged at the lower part of the extraction tower, and the raffinate phase outlet is connected to a compound fertilizer production system. The ingredients are preferably ammonium chloride or ammonium carbonate or ammonium bicarbonate. The solvent is preferably demineralized water. The batching tank 5 is connected to the reaction vessel by a batching transfer pump 6.
Preferably, the device also comprises a rearrangement reactor 1, wherein a discharge port of the rearrangement reactor is connected to a first feed port of the reaction kettle. And directly feeding the liquid after the rearrangement reaction into a reaction kettle for reaction treatment.
Preferably, a circulation pipeline is formed by a rearrangement circulating pump 3 and a rearrangement cooler 2 outside the rearrangement reactor, a fuming sulfuric acid pipeline is arranged between a rearrangement reactor circulation discharge port and the rearrangement circulating pump, and a cyclohexanone oxime feeding pipe is also arranged between the rearrangement cooler and the rearrangement reactor.
Preferably, a stirrer is further arranged in the reaction kettle, and the discharged material at the bottom of the reaction kettle is connected to a circulating feed inlet through a reaction kettle circulating pump 7 and a reaction kettle cooler 8 to form a circulating loop; a branch pipe is arranged on the pipeline between the reaction kettle cooler and the reaction kettle and is connected to the extraction tower.
Preferably, the feed inlet of the extraction tower is positioned at the upper part, and the lower part is provided with an extractant inlet.
Preferably, the raffinate phase outlet is located at the bottom and is connected to a compound fertilizer production system through a pipeline and a pump.
During specific production, cyclohexanone oxime and oleum enter a rearrangement reactor according to a certain proportion to carry out Beckmann rearrangement reaction, then rearrangement liquid containing caprolactam sulfate enters a reaction kettle to react with ammonium salt aqueous solution from a batching tank, and the reaction kettle strengthens mass transfer through stirring to ensure that the aqueous solution and the rearrangement liquid can completely react. And then the reaction kettle is sent to a reaction kettle cooler through a reaction kettle circulating pump to exchange heat with circulating water to 50 ℃, and then the reaction product enters the top of the extraction tower and is subjected to countercurrent extraction with the organic solvent from the bottom of the extraction tower. The caprolactam is extracted from the mixed solution into an organic phase by utilizing the solubility of the organic solvent to the caprolactam, thereby realizing the separation of the caprolactam and the sulfate phase. The extracted light phase enters a caprolactam refining device from the upper part of the extraction device to separate high-purity caprolactam, and the sulfate aqueous solution of the raffinate heavy phase enters a slurry tank from the lower part of the extraction device to be used as a raw material for producing compound fertilizer and sent to a compound fertilizer production device.
Claims (6)
1. The device for separating caprolactam from caprolactam sulfate and co-producing compound fertilizer is characterized in that: the extraction device comprises a reaction kettle and an extraction tower, wherein the reaction kettle is provided with a first feed inlet and a second feed inlet, the first feed inlet is connected with a caprolactam sulfate pipeline, and the second feed inlet is connected with a batching pipeline; the device also comprises a batching tank, wherein the batching tank is provided with a batching feeding port and a solvent feeding port, and a liquid outlet of the batching tank is connected with a batching pipeline; the discharge port of the reaction kettle is connected to the feed port of the extraction tower through a pipeline and a pump, the upper extraction phase outlet of the extraction tower is connected to the caprolactam refining process through a pipeline, the lower extraction phase outlet is arranged at the lower part of the extraction tower, and the extraction phase outlet is connected to the compound fertilizer production system.
2. The apparatus of claim 1, wherein: the device also comprises a rearrangement reactor, wherein a discharge port of the rearrangement reactor is connected to the first feed inlet of the reaction kettle.
3. The apparatus of claim 2, wherein: the rearrangement reactor is externally provided with a circulating pipeline consisting of a rearrangement circulating pump and a rearrangement cooler, a fuming sulfuric acid pipeline is arranged between a rearrangement reactor circulating discharge port and the rearrangement circulating pump, and a cyclohexanone oxime feeding pipe is also arranged between the rearrangement cooler and the rearrangement reactor.
4. The apparatus of claim 1, wherein: a stirrer is also arranged in the reaction kettle, and the discharged material at the bottom of the reaction kettle is connected to a circulating feed inlet through a reaction kettle circulating pump and a reaction kettle cooler to form a circulating loop; a branch pipe is arranged on the pipeline between the reaction kettle cooler and the reaction kettle and is connected to the extraction tower.
5. The apparatus of claim 1, wherein: the feed inlet of the extraction tower is positioned at the upper part, and the lower part is provided with an extractant inlet.
6. The apparatus of claim 1, wherein: the raffinate phase outlet is positioned at the bottom and is connected to a compound fertilizer production system through a pipeline and a pump.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202220688878.9U CN216946815U (en) | 2022-03-28 | 2022-03-28 | Device for separating caprolactam from caprolactam sulfate and co-producing compound fertilizer |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202220688878.9U CN216946815U (en) | 2022-03-28 | 2022-03-28 | Device for separating caprolactam from caprolactam sulfate and co-producing compound fertilizer |
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| CN216946815U true CN216946815U (en) | 2022-07-12 |
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| CN202220688878.9U Active CN216946815U (en) | 2022-03-28 | 2022-03-28 | Device for separating caprolactam from caprolactam sulfate and co-producing compound fertilizer |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114605323A (en) * | 2022-03-31 | 2022-06-10 | 湖北三宁化工股份有限公司 | Process for separating caprolactam from caprolactam sulfate |
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- 2022-03-28 CN CN202220688878.9U patent/CN216946815U/en active Active
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114605323A (en) * | 2022-03-31 | 2022-06-10 | 湖北三宁化工股份有限公司 | Process for separating caprolactam from caprolactam sulfate |
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