CN111333504A - Method for synthesizing 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate by adopting micro-channel reactor - Google Patents
Method for synthesizing 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate by adopting micro-channel reactor Download PDFInfo
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Abstract
The invention discloses a method for synthesizing 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate by adopting a microchannel reactor, which belongs to the technical field of organic synthesis application and comprises four procedures of preparation of composite catalyst solution, setting of reaction conditions of the microchannel reactor, and synthesis and post-treatment of 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate, wherein isobutyraldehyde is used as a raw material, alkali metal hydroxide and tetrabutylammonium bromide are used as composite catalysts, and the 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate is synthesized in the microchannel reactor in a continuous flow mode. And the conversion rate of isobutyraldehyde reaches more than 95%, reaction byproducts are few, the selectivity reaches 80-95%, and the yield of target products reaches 76-85%.
Description
Technical Field
The invention belongs to the technical field of organic synthesis application, and particularly relates to a method for synthesizing 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate by using a microchannel reactor.
Background
The 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate is a water-insoluble dihydric alcohol ester with high boiling point and low freezing point, has very good compatibility with various solvents, is nontoxic, is a commonly accepted green solvent, and is widely used in the fields of paint film-forming aids, synthetic lubricants, plasticizers and the like.
In the prior art, the 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate adopts an intermittent or continuous production process, and the problems of too high or too low local catalyst concentration and the like are easily caused due to uneven mixing of reaction materials, so that the defects of increased side reactions, low product yield, low product purity and the like are caused. The microchannel reactor has the characteristics of large specific surface area, laminar flow mass transfer and the like, so that the microchannel reactor has the characteristics of mass transfer, heat transfer and mixing which are incomparable with the conventional reactor, has the advantages of mild reaction conditions, high product selectivity, high yield and the like, has small environmental pollution, effectively reduces the consumption of expensive, toxic and harmful reactants, and is a novel environment-friendly and safe organic synthesis platform.
The Chinese invention patents 201610932350.0, 201610931483.6 and 201610965286.6 disclose several microchannel reactors designed by Shandong Haimai chemical engineering Co., Ltd, wherein the structures, sizes, channel arrangements and the like of the several microchannel reactors are described in detail, and it is pointed out that the reactor enhances the reaction process by means of high specific surface area, the liquid holdup and the treatment capacity are further increased, the product conversion rate and the yield can be effectively improved, and the heat conduction coefficient and the heat exchange effect are remarkably improved, thereby being beneficial to the precise control of the reaction and the reduction of energy consumption.
To date, no study has been made on a method for synthesizing 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate by reacting isobutyraldehyde in the presence of a composite catalyst (alkali metal hydroxide and tetrabutylammonium bromide) in a microchannel continuous flow manner. The invention provides a process route for synthesizing 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate by taking isobutyraldehyde and a composite catalyst solution as reactants in a continuous flow mode in a luxury microchannel reactor, which has the following reaction formula:
the route has the advantages that the reaction conditions, the addition amount of raw materials, the reaction residence time and the like are accurately controlled, and the target product 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate is obtained in a high yield within a period of several minutes to more than ten minutes.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a method for synthesizing 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate by adopting a micro-channel reactor, the method takes isobutyraldehyde as a raw material and takes alkali metal hydroxide and tetrabutylammonium bromide as a composite catalyst, synthesizing 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate product in a microchannel reactor in a continuous flow mode, compared with the prior art, the method has the characteristics of accurate and controllable reaction conditions, continuous production mode, high safety and short reaction time, and the conversion rate of the isobutyraldehyde reaction raw material is more than 95%, the reaction byproducts are few, the product selectivity is 80-95%, and the yield of 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate is 76-85%.
In order to achieve the purpose, the technical scheme of the invention is to design a method for synthesizing 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate by using a microchannel reactor, which comprises the following steps:
s1: preparing a composite catalyst solution, namely dissolving alkali metal hydroxide and tetrabutylammonium bromide in deionized water to prepare the composite catalyst solution with a certain concentration;
s2: setting the reaction conditions of the microchannel reactor, connecting a heat exchange sheet integrated with a reaction sheet in the microchannel reactor with an external heating and cooling circulator, wherein a heat exchange medium in the heat exchange sheet is heat conduction oil, and setting the reaction temperature of the microchannel reactor through the heating and cooling circulator;
s3: synthesizing 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate, namely respectively introducing isobutyraldehyde and the composite catalyst solution prepared in the step S1 into a feed inlet of a microchannel reactor at a certain feed flow rate by adopting different flow pumps, wherein the isobutyraldehyde and the composite catalyst solution flow, mix, heat and react in the microchannel reactor to obtain a reaction product mixed solution, wherein the feed volume ratio of the isobutyraldehyde to the composite catalyst solution is adjusted to be 5-20: 1 by the flow pumps, the feed flow rate of the isobutyraldehyde is 2-6 mL/min, the feed flow rate of the composite catalyst solution is 0.1-1.2 mL/min, the reaction residence time of the reaction process in the microchannel reactor is 5-17 min, the reaction temperature is 30-60 ℃, and the pressure is normal pressure;
s4: and (4) post-treatment, namely cooling and rectifying the reaction product mixed solution synthesized in the step S3 to obtain 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate, wherein the total conversion rate of isobutyraldehyde is more than 95%, the selectivity is 80-90%, and the yield of the 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate product is 76-85%.
In the preferable technical scheme, in the step S1, the alkali metal hydroxide is one of potassium hydroxide and sodium hydroxide, the mass concentration of the alkali metal hydroxide in the composite catalyst solution is 10 to 40%, and the mass concentration of tetrabutylammonium bromide is 0.6 to 1%.
In the preferable technical scheme, in the step S3, the feeding volume ratio of isobutyraldehyde to the composite catalyst solution is 5-15: 1.
In the preferable technical scheme, in the step S3, the feeding flow rate of isobutyraldehyde is 3-5 mL/min, and the feeding flow rate of the composite catalyst solution is 0.5-0.8 mL/min.
In the preferable technical scheme, in the step S3, the reaction residence time of the reaction process in the microchannel reactor is 6-12 min, and the reaction temperature is 40-50 ℃.
The invention has the advantages and beneficial effects that:
1. compared with the prior synthesis process, the method has the characteristics of accurate and controllable reaction conditions, continuous production mode, high safety and short reaction time, wherein the reaction time is shortened from the traditional hours to several minutes, and the reaction efficiency is obviously improved.
2. Because the reactant and the composite catalyst solution are mixed in the microchannel with excellent effect and the temperature is accurate and controllable, the conversion rate of the reactant and the selection singleness of the generated target product are obviously improved, wherein the conversion rate of the isobutyraldehyde reaction raw material is over 95 percent, reaction byproducts are few, the product selectivity is 80-95 percent, and the yield of 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate is 76-85 percent.
3. In the microchannel reactor, reactants and a composite catalyst solution are sequentially preheated, flow, mixed and reacted, the whole process is continuous flow reaction, the phenomenon that a device needs to be additionally configured and leakage occurs in transfer in conventional intermittent reaction is avoided, the safety and the environmental protection performance of the whole reaction process are improved, and the high efficiency of production is ensured.
4. The catalyst is a composite solution of alkali metal hydroxide and tetrabutylammonium bromide, and strengthens interphase mass transfer and accelerates the reaction speed in addition to ensuring the alkali catalysis strength of the aldol condensation reaction; the aldol condensation reaction is an exothermic reaction, the reaction is more favorably carried out at low temperature, the composite catalyst can reduce the reaction temperature, improve the conversion rate of raw materials and simultaneously reduce side reactions.
Drawings
FIG. 1 is a flow diagram of the process of the present invention for the synthesis of 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate using a microchannel reactor.
Detailed Description
The following description of the embodiments of the present invention will be made with reference to the accompanying drawings. The following examples are only for illustrating the technical solutions of the present invention more clearly, and the protection scope of the present invention is not limited thereby.
The microchannel reactor used in examples 1 to 4 was a microchannel reactor (model CS1005, liquid holdup 10.4mL) produced by Shandong Haimai chemical engineering Co., Ltd. and was assembled by connecting a plurality of reaction plates in series or in parallel, and the reaction plates and the heat exchanger plates were closely adhered and integrated. The heat exchange plates are provided with temperature sensors which can be used for measuring the temperature of the heat exchange medium in the heat exchange plates in real time. The reaction sheet can be made of metal materials such as 304 stainless steel, Hastelloy, titanium and the like, or non-metal materials such as SiC, quartz and the like, and different materials can be suitable for different reaction conditions, such as metal materials which are more resistant to high pressure and SiC materials which are more resistant to acid and alkali corrosion; the materials and the quantity of the heat exchange sheets and the reaction sheets are consistent; the number of reaction plates is determined by the reaction residence time, and the reagents used in examples 1 to 4 are all commercially available chemical reagents.
Example 1
The method for synthesizing 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate by adopting the microchannel reactor, disclosed by the invention, is used for synthesizing the 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate in the microchannel reactor by taking isobutyraldehyde as a raw material and taking a composite solution prepared from sodium hydroxide and tetrabutylammonium bromide as a composite catalyst solution (see the attached figure 1), and comprises the following steps of:
s1: preparing a composite catalyst solution, namely dissolving sodium hydroxide and tetrabutylammonium bromide in deionized water to prepare the composite catalyst solution with a certain concentration, wherein the mass concentration of the sodium hydroxide is 20% and the mass concentration of the tetrabutylammonium bromide is 0.6%;
s2: setting the reaction conditions of the microchannel reactor, connecting a heat exchange sheet integrated with a reaction sheet in the microchannel reactor with an external heating and cooling circulator, wherein a heat exchange medium in the heat exchange sheet is heat conduction oil, and setting the reaction temperature of the microchannel reactor through the heating and cooling circulator;
s3: synthesizing 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate, namely respectively introducing isobutyraldehyde and the composite catalyst solution prepared in the step S1 into a feed inlet of a microchannel reactor at a certain feed flow rate by adopting different flow pumps, wherein the isobutyraldehyde and the composite catalyst solution flow, mix, heat and react in the microchannel reactor to obtain a reaction product mixed solution, wherein the feed volume ratio of the isobutyraldehyde to the composite catalyst solution is adjusted to be 5: 1 by the flow pumps, the feed flow rate of the isobutyraldehyde is 5mL/min, the feed flow rate of the composite catalyst solution is 1mL/min, the reaction residence time of the reaction process in the microchannel reactor is 6min, the reaction temperature is 40 ℃, and the pressure is normal pressure;
s4: and (4) post-treatment, namely cooling and rectifying the reaction product mixed solution synthesized in the step S3 to obtain 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate, wherein the total conversion rate of isobutyraldehyde is 96%, the selectivity is 81%, and the yield of the 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate product is 78%.
Example 2
The method for synthesizing 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate by adopting the microchannel reactor, disclosed by the invention, is used for synthesizing the 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate in the microchannel reactor by taking isobutyraldehyde as a raw material and taking a composite solution prepared from potassium hydroxide and tetrabutylammonium bromide as a composite catalyst solution, and comprises the following steps of:
s1: preparing a composite catalyst solution, namely dissolving potassium hydroxide and tetrabutylammonium bromide in deionized water to prepare the composite catalyst solution with a certain concentration, wherein the mass concentration of the potassium hydroxide is 30% and the mass concentration of the tetrabutylammonium bromide is 1%;
s2: setting the reaction conditions of the microchannel reactor, connecting a heat exchange sheet integrated with a reaction sheet in the microchannel reactor with an external heating and cooling circulator, wherein a heat exchange medium in the heat exchange sheet is heat conduction oil, and setting the reaction temperature of the microchannel reactor through the heating and cooling circulator;
s3: synthesizing 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate, namely respectively introducing isobutyraldehyde and the composite catalyst solution prepared in the step S1 into a feed inlet of a microchannel reactor at a certain feed flow rate by adopting different flow pumps, wherein the isobutyraldehyde and the composite catalyst solution flow, mix, heat and react in the microchannel reactor to obtain a reaction product mixed solution, wherein the feed volume ratio of the isobutyraldehyde to the composite catalyst solution is adjusted to 10: 1 by the flow pumps, the feed flow rate of the isobutyraldehyde is 3mL/min, the feed flow rate of the composite catalyst solution is 0.3mL/min, the reaction residence time of the reaction process in the microchannel reactor is 10min, the reaction temperature is 60 ℃, and the pressure is normal pressure;
s4: and (4) post-treatment, namely cooling and rectifying the reaction product mixed solution synthesized in the step S3 to obtain 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate, wherein the total conversion rate of isobutyraldehyde is 97%, the selectivity is 88%, and the yield of the 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate product is 85%.
Example 3
The method for synthesizing 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate by adopting the microchannel reactor, disclosed by the invention, is used for synthesizing the 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate in the microchannel reactor by taking isobutyraldehyde as a raw material and taking a composite solution prepared from potassium hydroxide and tetrabutylammonium bromide as a composite catalyst solution, and comprises the following steps of:
s1: preparing a composite catalyst solution, namely dissolving potassium hydroxide and tetrabutylammonium bromide in deionized water to prepare the composite catalyst solution with a certain concentration, wherein the mass concentration of the potassium hydroxide is 10% and the mass concentration of the tetrabutylammonium bromide is 0.8%;
s2: setting the reaction conditions of the microchannel reactor, connecting a heat exchange sheet integrated with a reaction sheet in the microchannel reactor with an external heating and cooling circulator, wherein a heat exchange medium in the heat exchange sheet is heat conduction oil, and setting the reaction temperature of the microchannel reactor through the heating and cooling circulator;
s3: synthesizing 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate, namely respectively introducing isobutyraldehyde and the composite catalyst solution prepared in the step S1 into a feed inlet of a microchannel reactor at a certain feed flow rate by adopting different flow pumps, wherein the isobutyraldehyde and the composite catalyst solution flow, mix, heat and react in the microchannel reactor to obtain a reaction product mixed solution, wherein the feed volume ratio of the isobutyraldehyde to the composite catalyst solution is adjusted to 15: 1 by the flow pumps, the feed flow rate of the isobutyraldehyde is 4mL/min, the feed flow rate of the composite catalyst solution is 0.27mL/min, the reaction residence time of the reaction process in the microchannel reactor is 17min, the reaction temperature is 30 ℃, and the pressure is normal pressure;
s4: and (4) post-treatment, namely cooling and rectifying the reaction product mixed solution synthesized in the step S3 to obtain 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate, wherein the total conversion rate of isobutyraldehyde is 95%, the selectivity is 85%, and the yield of the 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate product is 81%.
Example 4
The method for synthesizing 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate by adopting the microchannel reactor, disclosed by the invention, is used for synthesizing the 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate in the microchannel reactor by taking isobutyraldehyde as a raw material and taking a composite solution prepared from sodium hydroxide and tetrabutylammonium bromide as a composite catalyst solution, and comprises the following steps of:
s1: preparing a composite catalyst solution, namely dissolving sodium hydroxide and tetrabutylammonium bromide in deionized water to prepare the composite catalyst solution with a certain concentration, wherein the mass concentration of the sodium hydroxide is 40% and the mass concentration of the tetrabutylammonium bromide is 0.9%;
s2: setting the reaction conditions of the microchannel reactor, connecting a heat exchange sheet integrated with a reaction sheet in the microchannel reactor with an external heating and cooling circulator, wherein a heat exchange medium in the heat exchange sheet is heat conduction oil, and setting the reaction temperature of the microchannel reactor through the heating and cooling circulator;
s3: synthesizing 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate, namely respectively introducing isobutyraldehyde and the composite catalyst solution prepared in the step S1 into a feed inlet of a microchannel reactor at a certain feed flow rate by adopting different flow pumps, wherein the isobutyraldehyde and the composite catalyst solution flow, mix, heat and react in the microchannel reactor to obtain a reaction product mixed solution, wherein the feed volume ratio of the isobutyraldehyde to the composite catalyst solution is adjusted to be 20: 1 by the flow pumps, the feed flow rate of the isobutyraldehyde is 6mL/min, the feed flow rate of the composite catalyst solution is 0.3mL/min, the reaction residence time of the reaction process in the microchannel reactor is 14min, the reaction temperature is 50 ℃, and the pressure is normal pressure;
s4: and (4) post-treatment, namely cooling and rectifying the reaction product mixed solution synthesized in the step S3 to obtain 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate, wherein the total conversion rate of isobutyraldehyde is 97%, the selectivity is 86%, and the yield of the 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate product is 83%.
TABLE 1 Experimental data in examples 1-4
The data of the examples 1 to 4 show that the total conversion rate of isobutyraldehyde is more than 95%, the selectivity is 80 to 90%, and the yield of 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate is 76 to 85%, which indicates that all experimental indexes of the method for synthesizing 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate by adopting the microchannel reactor meet the requirements, and the purpose of the invention is achieved.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the technical principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (5)
1. A method for synthesizing 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate by using a microchannel reactor is characterized by comprising the following steps:
s1: preparing a composite catalyst solution, namely dissolving alkali metal hydroxide and tetrabutylammonium bromide in deionized water to prepare the composite catalyst solution with a certain concentration;
s2: setting the reaction conditions of the microchannel reactor, connecting a heat exchange sheet integrated with a reaction sheet in the microchannel reactor with an external heating and cooling circulator, wherein a heat exchange medium in the heat exchange sheet is heat conduction oil, and setting the reaction temperature of the microchannel reactor through the heating and cooling circulator;
s3: synthesizing 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate, namely respectively introducing isobutyraldehyde and the composite catalyst solution prepared in the step S1 into a feed inlet of a microchannel reactor at a certain feed flow rate by adopting different flow pumps, wherein the isobutyraldehyde and the composite catalyst solution flow, mix, heat and react in the microchannel reactor to obtain a reaction product mixed solution, wherein the feed volume ratio of the isobutyraldehyde to the composite catalyst solution is adjusted to be 5-20: 1 by the flow pumps, the feed flow rate of the isobutyraldehyde is 2-6 mL/min, the feed flow rate of the composite catalyst solution is 0.1-1.2 mL/min, the reaction residence time of the reaction process in the microchannel reactor is 5-17 min, the reaction temperature is 30-60 ℃, and the pressure is normal pressure;
s4: and (4) post-treatment, namely cooling and rectifying the reaction product mixed solution synthesized in the step S3 to obtain 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate, wherein the total conversion rate of isobutyraldehyde is more than 95%, the selectivity is 80-90%, and the yield of the 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate product is 76-85%.
2. The method for synthesizing 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate using a microchannel reactor as claimed in claim 1, wherein in step S1, the alkali metal hydroxide is one of potassium hydroxide and sodium hydroxide, the mass concentration of the alkali metal hydroxide in the composite catalyst solution is 10 to 40%, and the mass concentration of tetrabutylammonium bromide is 0.6 to 1%.
3. The method for synthesizing 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate using a microchannel reactor as set forth in claim 1, wherein in step S3, the feeding volume ratio of isobutyraldehyde and the composite catalyst solution is 5 to 15: 1.
4. The method for synthesizing 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate using a microchannel reactor according to claim 1, wherein in step S3, the feed flow rate of isobutyraldehyde is 3 to 5mL/min and the feed flow rate of the composite catalyst solution is 0.5 to 0.8 mL/min.
5. The method for synthesizing 2,2, 4-trimethyl-1, 3-pentanediol monoisobutyrate using a microchannel reactor as claimed in claim 1, wherein in step S3, the reaction process is carried out in the microchannel reactor for a reaction residence time of 6 to 12min and a reaction temperature of 40 to 50 ℃.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113045514A (en) * | 2021-03-31 | 2021-06-29 | 福州大学 | Method for preparing limonene epoxidation product |
| CN113956132A (en) * | 2021-11-19 | 2022-01-21 | 吉林化工学院 | Preparation method of trimethylpentanediol |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113045514A (en) * | 2021-03-31 | 2021-06-29 | 福州大学 | Method for preparing limonene epoxidation product |
| CN113956132A (en) * | 2021-11-19 | 2022-01-21 | 吉林化工学院 | Preparation method of trimethylpentanediol |
| CN113956132B (en) * | 2021-11-19 | 2024-03-19 | 吉林化工学院 | Preparation method of trimethylpentanediol |
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