CN214233991U - Preparation facilities of 1-methoxy-4-oxygen-cyclohexanecarboxylic acid methyl ester - Google Patents
Preparation facilities of 1-methoxy-4-oxygen-cyclohexanecarboxylic acid methyl ester Download PDFInfo
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- CN214233991U CN214233991U CN202023267769.XU CN202023267769U CN214233991U CN 214233991 U CN214233991 U CN 214233991U CN 202023267769 U CN202023267769 U CN 202023267769U CN 214233991 U CN214233991 U CN 214233991U
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Abstract
The utility model relates to a preparation facilities of 1-methoxy-4-oxygen-cyclohexyl methyl formate, including reation kettle, reation kettle connects 1, 4-cyclohexanedione monoethylene ketal storage tank through the solenoid valve, reation kettle still connects the diaphragm pump, reation kettle's import is connected through the flowmeter and is located the high-order dropwise add jar of reation kettle top, still be equipped with the balance tube between reation kettle and the high-order dropwise add jar, the export of reation kettle connects gradually aftertreatment unit, takes off ketal reation kettle; and a pH sensor is arranged in the reaction kettle. The 1-methoxy-4-oxygen-methyl cyclohexanecarboxylate prepared by the preparation device of the 1-methoxy-4-oxygen-methyl cyclohexanecarboxylate of the utility model has high content and high yield, and avoids generating the impurity 8, 8-dimethoxy-1, 4-dioxaspiro [4.5] decane.
Description
Technical Field
The utility model belongs to the technical field of the meticulous chemical industry of medicine, concretely relates to preparation facilities of 1-methoxy-4-oxygen-methyl cyclohexanecarboxylate.
Background
1-methoxy-4-oxygen-cyclohexyl methyl formate (structural formula 1) is an important medical intermediate in chemical industry, and the prior process for producing the 1-methoxy-4-oxygen-cyclohexyl methyl formate compound comprises the following steps: adding methanol, tribromomethane and 1, 4-cyclohexanedione monoethylene ketal (structural formula 2) into a reaction kettle, heating to 40-45 ℃, dropwise adding a methanol solution of an organic base, reacting to obtain an intermediate, and performing a ketal removal reaction to obtain a product, wherein the tribromomethane serving as a raw material is easy to decompose in the standing process, a small amount of acid is generated, the 1, 4-cyclohexanedione monoethylene ketal can react with the methanol under the catalysis of a small amount of acid to generate an impurity 8, 8-dimethoxy-1, 4-dioxaspiro [4.5] decane (structural formula 3), and the impurity can be subjected to the ketal removal reaction to obtain an impurity 4, 4-dimethoxycyclohexanone (structural formula 4), and the two impurities of the structural formula 3 and the structural formula 4 are difficult to remove in the production process, so that the product quality is seriously affected.
Disclosure of Invention
The utility model aims at providing a preparation facilities of 1-methoxy-4-oxygen-cyclohexanecarboxylic acid methyl ester, the 1-methoxy-4-oxygen-cyclohexanecarboxylic acid methyl ester content of preparing is high, and the yield is high, avoids producing impurity 8, 8-dimethoxy-1, 4-dioxaspiro [4.5] decane.
The utility model provides a technical scheme that above-mentioned problem adopted does: a preparation device of 1-methoxy-4-oxygen-methyl cyclohexanecarboxylate comprises a reaction kettle, wherein the reaction kettle is connected with a 1, 4-cyclohexanedione monoethylene ketal storage tank through an electromagnetic valve, the reaction kettle is also connected with a diaphragm pump, an inlet of the reaction kettle is connected with a high-position dropwise adding tank positioned above the reaction kettle through a flow meter, a balance pipe is further arranged between the reaction kettle and the high-position dropwise adding tank, and an outlet of the reaction kettle is sequentially connected with a post-treatment unit and a ketal removal reaction kettle; and a pH sensor is arranged in the reaction kettle.
Preferably, a first regulating valve is arranged on a pipeline for communicating the reaction kettle with the diaphragm pump.
Preferably, the reaction kettle is provided with a heater and a stirring mechanism, and the stirring mechanism comprises a stirring shaft and an airfoil-shaped axial-flow type stirring paddle.
Preferably, the inlet of the reaction kettle is connected with the high-level dripping tank through a feed valve, the flowmeter and a second regulating valve in sequence.
Preferably, the high-level dripping tank is also provided with a liquid level meter.
Preferably, the reaction kettle and the high-position dropwise adding tank are both connected with a nitrogen storage tank through a nitrogen pipe.
Compared with the prior art, the utility model has the advantages of:
compare in adding into reation kettle with methyl alcohol, tribromomethane and 1, 4-cyclohexanedione monoethylene glycol ketal among the prior art, heat up 40~45 ℃, the methanol solution of dropwise add organic base again, the utility model discloses a preparation facilities of 1-methoxy-4-oxygen-cyclohexanecarboxylate avoids acid that raw materials tribromomethane decomposes production to react with another raw materials 1, 4-cyclohexanedione monoethylene glycol ketal and generates impurity 8, 8-dimethoxy-1, 4-dioxa spiro [4.5] decane that is difficult to get rid of, improves the yield, practices thrift the cost, and has promoted product quality and productivity.
Drawings
FIG. 1 is a schematic structural diagram of a device for preparing 1-methoxy-4-oxo-methyl cyclohexanecarboxylate in the embodiment of the present invention.
Wherein: 1 is the reation kettle, 2 is the solenoid valve, 3 is 1, 4-cyclohexanedione monoethylene ketal storage tank, 4 is the diaphragm pump, 5 is the flowmeter, 6 is the high-order dropwise add jar, 6.1 is the level gauge, 7 is the balance tube, 8 is the aftertreatment unit, 9 is the ketal reation kettle that takes off, 10.1 is first governing valve, 10.2 is the second governing valve, 11 is the feed valve.
Detailed Description
The present invention will be described in further detail with reference to the following embodiments.
As shown in fig. 1, the structure of the apparatus for preparing 1-methoxy-4-oxo-cyclohexanecarboxylic acid methyl ester in this example is schematically illustrated.
A preparation device of 1-methoxy-4-oxygen-methyl cyclohexanecarboxylate comprises a reaction kettle 1, wherein the reaction kettle 1 is provided with a heater and a stirring mechanism, and the stirring mechanism comprises a stirring shaft and an airfoil axial-flow type stirring paddle; a pH sensor is arranged in the reaction kettle 1.
Wherein, the pH sensor and the electromagnetic valve 2 are both connected and controlled by a PLC controller.
The operation of this embodiment is described in detail below with reference to the accompanying drawings:
firstly introducing nitrogen from a nitrogen storage tank into a reaction kettle 1 and a high-level dropwise addition tank 6 through a nitrogen pipe, enabling the reaction kettle 1 and the high-level dropwise addition tank 6 to be in a nitrogen atmosphere, pumping tribromomethane and methanol into the reaction kettle 1 and the high-level dropwise addition tank 6 through a diaphragm pump 4, opening a flow meter 3, a second regulating valve 10.2 and a feeding valve 11, enabling a methanol solution of organic base in the high-level dropwise addition tank to be dropwise added into the reaction kettle 1 at a certain speed, detecting the pH of the reaction kettle 1 in real time by a pH sensor in the reaction kettle 1, transmitting the pH detection result to a PLC (programmable logic controller) until the pH value of a material in the reaction kettle 1 is 7-8, controlling an electromagnetic valve 2 to be opened by the PLC to add 1, 4-cyclohexanedione monoethylene ketal in a 1, 4-monoethylene ketal storage tank 3 (at the moment, the second regulating valve 10.2, the flow meter 3 and the feeding valve 11 are all closed), then heating the reaction kettle to 40-45 ℃, and opening the second regulating valve 10.2, the flow meter 3 and the feed valve 11, continuously dripping the residual methanol solution of the organic base in the high-position dripping tank 2, closing the second regulating valve 10.2, the flow meter 3 and the feed valve 11 after dripping is finished, obtaining an intermediate from the reaction material through a post-treatment unit 8 after the reaction is finished, and obtaining the 1-methoxy-4-oxygen-methyl cyclohexanecarboxylate after the ketal removal reaction of the intermediate in a ketal removal reaction kettle 9.
In addition to the above embodiments, the present invention also includes other embodiments, and all technical solutions formed by equivalent transformation or equivalent replacement should fall within the protection scope of the claims of the present invention.
Claims (6)
1. A preparation facilities of 1-methoxy-4-oxygen-cyclohexanecarboxylic acid methyl ester, its characterized in that: the device comprises a reaction kettle (1), wherein the reaction kettle (1) is connected with a 1, 4-cyclohexanedione monoethylene ketal storage tank (3) through an electromagnetic valve (2), the reaction kettle (1) is further connected with a diaphragm pump (4), an inlet of the reaction kettle (1) is connected with a high-level dropping tank (6) positioned above the reaction kettle (1) through a flowmeter (5), a balance pipe (7) is further arranged between the reaction kettle (1) and the high-level dropping tank (6), and an outlet of the reaction kettle (1) is sequentially connected with a post-treatment unit (8) and a ketal removal reaction kettle (9); and a pH sensor is arranged in the reaction kettle (1).
2. The apparatus for preparing methyl 1-methoxy-4-oxo-cyclohexanecarboxylate according to claim 1, characterized in that: a first adjusting valve (10.1) is arranged on a pipeline for communicating the reaction kettle (1) with the diaphragm pump (4).
3. The apparatus for preparing methyl 1-methoxy-4-oxo-cyclohexanecarboxylate according to claim 1, characterized in that: the reaction kettle (1) is provided with a heater and a stirring mechanism, and the stirring mechanism comprises a stirring shaft and an airfoil-shaped axial-flow type stirring paddle.
4. The apparatus for preparing methyl 1-methoxy-4-oxo-cyclohexanecarboxylate according to claim 1, characterized in that: the inlet of the reaction kettle (1) is connected with the high-level dropwise adding tank (6) through a feed valve (11), the flowmeter (5) and a second regulating valve (10.2) in sequence.
5. The apparatus for preparing methyl 1-methoxy-4-oxo-cyclohexanecarboxylate according to claim 1, characterized in that: the high-level dripping tank (6) is also provided with a liquid level meter (6.1).
6. The apparatus for preparing methyl 1-methoxy-4-oxo-cyclohexanecarboxylate according to claim 1, characterized in that: the reaction kettle (1) and the high-level dropwise adding tank (6) are both connected with a nitrogen storage tank through a nitrogen pipe.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202023267769.XU CN214233991U (en) | 2020-12-30 | 2020-12-30 | Preparation facilities of 1-methoxy-4-oxygen-cyclohexanecarboxylic acid methyl ester |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202023267769.XU CN214233991U (en) | 2020-12-30 | 2020-12-30 | Preparation facilities of 1-methoxy-4-oxygen-cyclohexanecarboxylic acid methyl ester |
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| Publication Number | Publication Date |
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| CN214233991U true CN214233991U (en) | 2021-09-21 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202023267769.XU Active CN214233991U (en) | 2020-12-30 | 2020-12-30 | Preparation facilities of 1-methoxy-4-oxygen-cyclohexanecarboxylic acid methyl ester |
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| CN (1) | CN214233991U (en) |
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