CN111393343A - Improved method for carrying out liquid-liquid two-phase reaction and continuous reaction equipment for method - Google Patents
Improved method for carrying out liquid-liquid two-phase reaction and continuous reaction equipment for method Download PDFInfo
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- CN111393343A CN111393343A CN202010189528.3A CN202010189528A CN111393343A CN 111393343 A CN111393343 A CN 111393343A CN 202010189528 A CN202010189528 A CN 202010189528A CN 111393343 A CN111393343 A CN 111393343A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C319/00—Preparation of thiols, sulfides, hydropolysulfides or polysulfides
- C07C319/14—Preparation of thiols, sulfides, hydropolysulfides or polysulfides of sulfides
- C07C319/20—Preparation of thiols, sulfides, hydropolysulfides or polysulfides of sulfides by reactions not involving the formation of sulfide groups
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2601/00—Systems containing only non-condensed rings
- C07C2601/12—Systems containing only non-condensed rings with a six-membered ring
- C07C2601/16—Systems containing only non-condensed rings with a six-membered ring the ring being unsaturated
Abstract
The present application relates to an improved process for carrying out the reaction, characterized in that the reaction is carried out in two steps and that after step one a separation of the organic and aqueous phases is carried out, followed by step two. The application also relates to continuous reaction equipment for implementing the method, which comprises a tank reactor, a clarifying tank and a tower reactor which are connected in series in sequence.
Description
Technical Field
The present application relates to an improved method for carrying out a liquid-liquid two-phase reaction and a continuous reaction apparatus for carrying out the method.
Background
In the following reaction, since the raw material compound of formula (1) is insoluble in water and NaOH is soluble in water, the reaction is a liquid-liquid two-phase reaction carried out in a two-phase system composed of an organic phase and an aqueous phase, and the reaction time is long, and it takes 4 to 5 hours.
In the formula, SEt represents an ethylthio group.
In the current industrial production, the equipment for implementing the reaction consists of a 3-stage continuous kettle type reactor and 1 clarifying tank which are connected in series, the equipment scale is large, and the 3-stage continuous kettle has the problems of unstable continuity, unstable production and unstable product quality and productivity due to uneven overflow among kettle kettles.
In addition, in the conventional reaction, the whole reaction process in the 3-stage continuous kettle is a liquid-liquid two-phase reaction in which an organic phase and an aqueous phase coexist, and the separation of the organic phase and the aqueous phase is not carried out in a clarifying tank until the reaction is finished.
Disclosure of Invention
In order to solve the above problems, the present inventors tried to optimize the operation of the above reaction.
The inventors of the present application found that the reaction was actually carried out in two steps:
the method comprises the following steps:
in the first step, the raw material compound of the formula (1) reacts with sodium hydroxide to form sodium salt of the formula (3) because hydroxyl has certain acidity, and is instantly and rapidly completed because of acid-base neutralization reaction.
Step two is hydrolysis of ester group, which requires a long reaction time.
Since the sodium salt produced in the first step is a water-soluble substance, the second step is carried out in an aqueous phase.
Based on the above findings, the present inventors tried to adjust the operation of the above reaction, and performed separation of organic and aqueous phases after step one, and then performed step two.
Corresponding to the step adjustment, the prior equipment with 3 continuous kettle reactors and 1 clarifying tank connected in series is not suitable any more, and the inventor of the application further designs novel continuous reaction equipment.
Specifically, the present invention relates to:
(1) the following improved method for carrying out liquid-liquid two-phase reaction,
in the formula, SEt represents an ethylthio group;
characterized in that it is carried out in two steps, and that after step one a separation of the organic and aqueous phases is carried out, followed by step two,
the method comprises the following steps:
(2) in the method of (1), the organic solvent used in the reaction is one or more of toluene, xylene and trimethylbenzene.
(3) The continuous reaction equipment comprises a kettle type reactor, a clarifying tank and a tower type reactor which are sequentially connected in series.
(4) The continuous reaction apparatus according to the above (3), wherein the column reactor is a packed column reactor.
(5) The continuous reaction apparatus as described in (3) or (4) above for carrying out the process as described in (1) or (2) above.
(6) The continuous reaction equipment in (5) above, wherein the tank reactor is used for performing the liquid-liquid two-phase reaction in the first step, the clarifying tank is used for separating the organic phase and the aqueous phase after the liquid-liquid two-phase reaction in the first step, and the tower reactor is used for performing the single aqueous phase reaction in the second step.
Drawings
FIG. 1 is a schematic structural view of a preferred embodiment of the continuous reaction apparatus of the present application.
Description of reference numerals:
1: a kettle reactor; 2: a clarifying tank; 3: a tower reactor.
Detailed Description
Unlike the conventional liquid-liquid two-phase reaction in which an organic phase and an aqueous phase coexist in the whole reaction process in 3 continuous tank reactors, in the present invention, the above-described reaction is continuously performed step by step, only the first step is a two-phase reaction of an organic phase and an aqueous phase, after the first step is completed, the phase separation is performed, the organic phase is discarded, the aqueous phase containing the target product enters the second step, which is a homogeneous reaction of only an aqueous phase.
Because the phase separation is carried out after the first step and the organic phase is discarded, the reaction materials in the second step are greatly reduced, and the two-phase reaction is changed into the homogeneous reaction, so that the equipment scale can be reduced, dynamic reaction equipment such as a stirred tank reactor can be changed into static reaction equipment such as a tower reactor, the production stability and efficiency are improved, the product quality is stable, and the stable productivity can be ensured.
When the method of the present invention is carried out using the continuous reaction apparatus shown in FIG. 1, the reaction raw material is introduced into the tank reactor 1, the liquid-liquid two-phase reaction in the first step is carried out in the tank, the material is introduced into the settling tank 2 to separate the organic phase and the aqueous phase, the organic phase is discarded, and the aqueous phase containing the target product is introduced into the column reactor 3 to carry out the reaction. The column reactor 3 is preferably a packed column reactor.
The structures of the tank reactor 1, the clarifier 2, and the column reactor 3 themselves are not particularly limited, and any known apparatus may be used.
The inventor of the present invention used toluene as organic solvent to carry out the above reaction, the conventional 3-stage continuous tank reactor and a clarification tank equipment, required 3 10000L continuous dynamic tank reactor for reaction, and year produce formula (2) compounds 5000 tons, through the improvement method and equipment of the present invention, with the height of 15m, tower diameter 800mm 1 static tower reactor instead of two 10000L continuous dynamic tank reactor, also achieve the same productivity.
The improved method of the present invention is not limited to the continuous reaction apparatus described above, and may be carried out in other ways.
The continuous reaction equipment of the invention is not limited to be used in the improved implementation method of the invention, and can also be used in other similar liquid-liquid two-phase reactions.
The present application is not limited to the above specific embodiments, and any modifications and variations within the scope not departing from the gist of the present application fall within the scope of the present application.
Industrial applicability
The improved implementation method and the continuous reaction equipment of the invention reduce the equipment scale required by the implementation of the liquid-liquid two-phase reaction, and replace part of dynamic continuous kettle type reactors with static tower type reactors, thus improving the production stability and further improving the product quality and the stability of the productivity.
Claims (6)
1. The following improved method for carrying out liquid-liquid two-phase reaction,
in the formula, SEt represents an ethylthio group;
characterized in that it is carried out in two steps, and that after step one a separation of the organic and aqueous phases is carried out, followed by step two,
the method comprises the following steps:
step two:
2. the process according to claim 1, wherein the organic solvent used for the reaction is one or more selected from the group consisting of toluene, xylene and trimethylbenzene.
3. The method of claim 1 or 2, which is carried out by a continuous reaction apparatus comprising a tank reactor, a clarifier and a tower reactor connected in series in this order, wherein the tank reactor is used for carrying out the liquid-liquid two-phase reaction of the first step, the clarifier is used for separating the organic phase and the aqueous phase after the liquid-liquid two-phase reaction of the first step, and the tower reactor is used for carrying out the single aqueous phase reaction of the second step.
4. The process of claim 3, wherein the column reactor is a packed column reactor.
5. A continuous reaction device for implementing the method of any one of claims 1 to 4, comprising a tank reactor, a clarifying tank and a tower reactor which are connected in series in sequence, wherein the tank reactor is used for carrying out the liquid-liquid two-phase reaction of the step one, the clarifying tank is used for separating an organic phase and an aqueous phase after the liquid-liquid two-phase reaction of the step one, and the tower reactor is used for carrying out the single aqueous phase reaction of the step two.
6. The continuous reaction apparatus according to claim 5, wherein the column reactor is a packed column reactor.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010189528.3A CN111393343A (en) | 2020-03-18 | 2020-03-18 | Improved method for carrying out liquid-liquid two-phase reaction and continuous reaction equipment for method |
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| CN202010189528.3A CN111393343A (en) | 2020-03-18 | 2020-03-18 | Improved method for carrying out liquid-liquid two-phase reaction and continuous reaction equipment for method |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0082694A2 (en) * | 1981-12-23 | 1983-06-29 | Ici Australia Limited | Herbicidal cyclohexane-1,3-dione derivatives |
| CN106518740A (en) * | 2016-11-02 | 2017-03-22 | 河北兰升生物科技有限公司 | Improved method for synthesizing clethodim |
| CN212076904U (en) * | 2020-03-18 | 2020-12-04 | 内蒙古兰格生物科技有限公司 | Continuous reaction equipment for liquid-liquid two-phase reaction |
-
2020
- 2020-03-18 CN CN202010189528.3A patent/CN111393343A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0082694A2 (en) * | 1981-12-23 | 1983-06-29 | Ici Australia Limited | Herbicidal cyclohexane-1,3-dione derivatives |
| CN106518740A (en) * | 2016-11-02 | 2017-03-22 | 河北兰升生物科技有限公司 | Improved method for synthesizing clethodim |
| CN212076904U (en) * | 2020-03-18 | 2020-12-04 | 内蒙古兰格生物科技有限公司 | Continuous reaction equipment for liquid-liquid two-phase reaction |
Non-Patent Citations (2)
| Title |
|---|
| PRZEMYSLAW SZCZECINSKI ET AL.: "1H NMR,13C NMR, and Computational DFT Studies of the Structure of 2-Acylcyclohexane-1,3-diones and Their Alkali Metal Salts in Solution", 《J. ORG. CHEM.》 * |
| 欧阳卉等: "《药物分析（第3版）》", 31 January 2017, 中国医药科技出版社 * |
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