CN111302937A - Method for preparing p-tert-butyl methyl benzoate - Google Patents

Method for preparing p-tert-butyl methyl benzoate Download PDF

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CN111302937A
CN111302937A CN202010269651.6A CN202010269651A CN111302937A CN 111302937 A CN111302937 A CN 111302937A CN 202010269651 A CN202010269651 A CN 202010269651A CN 111302937 A CN111302937 A CN 111302937A
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tert
reaction
channel
rectifying column
benzoic acid
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吴芹
欧阳梦洁
黎汉生
史大昕
矫庆泽
陈琪
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Beijing Institute of Technology BIT
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Beijing Institute of Technology BIT
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00Preparation of carboxylic acid esters
    • C07C67/08Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0093Microreactors, e.g. miniaturised or microfabricated reactors
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00Preparation of carboxylic acid esters
    • C07C67/48Separation; Purification; Stabilisation; Use of additives
    • C07C67/52Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
    • C07C67/54Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation

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  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)

Abstract

The invention provides a method for preparing p-tert-butyl methyl benzoate, which comprises the steps of taking methanol and p-tert-butyl benzoic acid as reactants, and carrying out esterification reaction through a multichannel microflow reactor to synthesize the p-tert-butyl methyl benzoate. The method for preparing the p-tert-butyl methyl benzoate can realize continuous production, is simple to operate, can quickly and fully mix reaction materials, and has the advantages of high reaction rate, controllable residence time, quick heat transfer, controllable temperature, small amount of reaction reagent, easy optimization of reaction, high temperature and high pressure resistance, easy amplification of a multi-channel microflow reactor and realization of mass production of products.

Description

Method for preparing p-tert-butyl methyl benzoate
Technical Field
The invention belongs to the field of preparation of p-tert-butyl methyl benzoate, and particularly relates to a method for preparing p-tert-butyl methyl benzoate.
Background
The p-tert-butyl methyl benzoate is used as an important organic synthesis intermediate and a medical intermediate, and is widely applied to the industries of chemical synthesis, cosmetics, medicines, essences, spices and the like. The annual demand of the market is very large, so that the research on the synthesis of p-tert-butyl methyl benzoate has important value.
The production process of methyl p-tert-butyl benzoate is mainly characterized by that the esterification reaction of p-tert-butyl benzoic acid and methyl alcohol is implemented under the catalytic action of acid catalyst to obtain the invented product. The existing industrial synthesis method of p-tert-butyl methyl benzoate adopts a batch reactor, firstly, the raw materials of p-tert-butyl benzoic acid, methanol and catalyst concentrated sulfuric acid are added at one time to carry out esterification reaction, and the method has the problems of low mass transfer efficiency of raw materials, slow reaction rate, discontinuous production process, long reaction time, large equipment volume, low equipment production capacity, high production cost and the like, and the power required by a stirrer is increased rapidly. Therefore, the problem to be solved at present is to find a novel reaction process with fast reaction rate, continuous production, safe operation, strong production capacity and low production cost for the synthesis of p-tert-butyl methyl benzoate.
Disclosure of Invention
In view of the above, the invention aims to provide a method for preparing p-tert-butyl methyl benzoate, which can realize continuous production, is simple to operate, has the advantages of rapid and sufficient mixing of reaction materials, rapid reaction rate, controllable residence time, rapid heat transfer, controllable temperature, small amount of reaction reagents, easy optimization of reaction, high temperature and high pressure resistance, easy amplification of a multi-channel microflow reactor and realization of mass production of products.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
the utility model provides a system for be used for preparing methyl p-tert-butylbenzoate, is including stirred tank, multichannel microflow reactor, first rectifying column, the liquid-liquid separation ware that connects gradually, and liquid-liquid separation ware's bottom is connected with the second rectifying column, and liquid-liquid separation ware's upper portion is connected with the third rectifying column, the top of first rectifying column, second rectifying column, third rectifying column all is connected with the reflux drum, multichannel microflow reactor includes from last feed channel, multichannel miniflow reaction subassembly, the discharging channel who communicates down in proper order, and the outside of multichannel miniflow reaction subassembly is equipped with the heat transfer room.
The system and the method can realize continuous production, simple operation, rapid and sufficient mixing of reaction materials, rapid reaction rate, controllable residence time, rapid heat transfer, controllable temperature, small amount of reaction reagent, easy optimization of reaction, high temperature and high pressure resistance, easy amplification of the multi-channel microflow reactor, and realization of mass production of products
The multi-channel microflow reactor has the advantages of high heat transfer area, rapid heat transfer, accurate reaction temperature control and capability of realizing isothermal operation.
The multi-channel microflow reactor has small pipe diameter, less consumption of reaction reagents, easy optimization of reaction, high temperature and high pressure resistance and low production cost.
The multichannel microflow reactor is easy to realize amplification and realizes mass production of products.
Furthermore, a plurality of partition plates are arranged in the heat exchange chamber, and the partition plates divide the heat exchange chamber into a plurality of heat exchange sub-chambers.
Furthermore, the direction of the baffle plate is vertical to the direction of the one-way straight pipe and the multi-stage bent pipe.
The arrangement of the partition plate can increase the contact area between the outer walls of the single-pass straight pipe and the multistage bent pipe and the heat exchange chamber, and improve the heat transfer efficiency.
Further, the upper part of the stirring kettle is connected with a methanol feeding channel, a p-tert butyl benzoic acid feeding hole and a catalyst feeding channel, the bottom of the stirring kettle is communicated with the feeding hole of the multi-channel micro-flow reactor, a discharging hole of the multi-channel micro-flow reactor is connected with a first rectifying tower, the bottom of the first rectifying tower is connected with a liquid-liquid separator, the upper part of the liquid-liquid separator is connected with a third rectifying tower, the upper part of the third rectifying tower is connected with a third reflux tank, and the bottom of the third reflux tank is connected with a p-tert butyl benzoic acid methyl ester outlet.
Further, the bottom of the first reflux tank is respectively connected with the methanol feeding channel and the upper part of the first rectifying tower.
Furthermore, the bottom of the third reflux tank is respectively connected with a p-tert-butyl methyl benzoate outlet and the upper part of a third rectifying tower, and the bottom of the third rectifying tower is connected with a p-tert-butyl benzoic acid feeding channel.
Furthermore, the bottom of the second reflux tank is respectively connected with the wastewater outlet and the upper part of the second rectifying tower, and the bottom of the second rectifying tower is respectively connected with the catalyst feeding channel and the waste sulfuric acid outlet.
Reactants and catalysts which are not completely reacted in the reaction system can be recycled, so that the energy is saved, the environment is protected, and the resources are saved.
Furthermore, the multichannel microflow reaction component is a plurality of single-pass straight pipes arranged in parallel, the top of the single-pass straight pipe is communicated with the feeding channel, and the bottom of the single-pass straight pipe is communicated with the discharging channel.
Furthermore, the multi-channel micro-flow reaction component is a multi-stage bent pipe, a feed inlet of the multi-stage bent pipe is communicated with the feed channel, and a discharge outlet of the multi-stage bent pipe is communicated with the discharge channel.
A process for preparing methyl p-tert-butylbenzoate includes the esterification reaction of methanol and p-tert-butylbenzoic acid as reactants in a multi-channel microflow reactor.
Further, methanol and p-tert-butyl benzoic acid are used as raw materials, acid is used as a catalyst, and esterification reaction is carried out through a multi-channel microflow reactor to synthesize the p-tert-butyl methyl benzoate.
Further, the catalyst is one of sulfuric acid, acidic ionic liquid and sulfonic acid resin.
Further, if the catalyst is a sulfonic acid resin catalyst. The catalyst may be immobilized directly in the multi-channel microflow reactor.
Further, when acid is added as a catalyst for reaction, the reaction temperature is 60-200 ℃.
Further, when the reaction is carried out by adding an acid as a catalyst, the reaction temperature is preferably 100 ℃ to 160 ℃.
Further, when the reaction was carried out without adding a catalyst, the reaction temperature was 100 ℃ and 200 ℃.
Further, when the reaction is carried out without adding a catalyst, the reaction temperature is preferably 150 ℃ to 200 ℃.
Further, the reaction pressure is 0.1 to 5 MPa.
Further, the residence time of the reactants in the multi-channel microflow reactor is 0.5 to 8 hours
Further, the residence time of the reactants in the multi-channel microflow reactor is preferably 0.5 to 5 hours.
Further, the molar ratio of the p-tert-butyl benzoic acid to the methanol is 1:1-1: 15.
Further, the molar ratio of p-tert-butylbenzoic acid to methanol is preferably 1:5 to 1: 10.
Furthermore, the number of single-pass straight tubes or multi-stage bent tubes in the multi-channel microfluidic reaction component is 1-800.
Furthermore, the inner diameter of the single-pass straight pipe or the multi-stage bent pipe is 10-3000 micrometers.
The single-pass straight pipe or the multi-stage bent pipe can strengthen the reaction by adjusting the scale effect of the reactor, and can realize the accurate control of the retention time by changing the length or the flow speed of the single-pass straight pipe or the multi-stage bent pipe, control the occurrence of side reaction and improve the yield of the product.
Further, the weight of the catalyst is 1-20% of the total weight of the reactants.
Further, the weight of the catalyst is preferably 6-15% of the total weight of the reactants.
When the reaction is carried out, methanol is fed into the stirred tank from the methanol feed channel, p-tert-butyl benzoic acid is poured into the stirred tank from the p-tert-butyl benzoic acid feed port, and a catalyst (concentrated sulfuric acid is taken as an example) is fed into the stirred tank from the catalyst feed channel (if the catalyst is not added, the step is omitted). The reactants and the catalyst are fully stirred and dissolved in the stirring kettle, and then are fed from a feed inlet of the multi-channel micro-flow reactor. The reactant flows into a single-pass straight pipe or a multi-stage bent pipe from the feeding channel and then is discharged from the discharge hole. And (3) allowing the crude product discharged from the discharge hole to flow into a first rectifying tower, layering in the first rectifying tower, allowing the methanol at the top to flow into a first reflux tank, allowing part of the methanol in the first reflux tank to return to a methanol feeding channel for recycling, and allowing the other part of the methanol to flow back to the first rectifying tower. And the mixture at the lower part of the first rectifying tower enters a liquid-liquid separator for separation, the mixture at the upper part of the liquid-liquid separator flows into a third rectifying tower, part of the p-tert-butyl methyl benzoate at the upper part of the third rectifying tower flows out from a p-tert-butyl methyl benzoate outlet after passing through a third reflux tank, the other part of the p-tert-butyl methyl benzoate flows back to the third rectifying tower, and the p-tert-butyl benzoic acid at the lower part of the third rectifying tower is recycled. And the sulfuric acid solution at the lower part of the liquid-liquid separator enters a second rectifying tower for concentration, and the wastewater is discharged from a wastewater outlet. Concentrated sulfuric acid suitable for recycling at the bottom of the second rectifying tower is recycled to the catalyst feeding channel for use, and sulfuric acid unsuitable for recycling flows out from a waste sulfuric acid outlet.
Compared with the prior art, the method and the system for preparing the p-tert-butyl methyl benzoate have the following advantages:
(1) the method for preparing the p-tert-butyl methyl benzoate can realize continuous production, is simple to operate, can quickly and fully mix reaction materials, has the advantages of high reaction rate, controllable residence time, quick heat transfer, controllable temperature, small amount of reaction reagent, easy optimization of reaction, high temperature and high pressure resistance, easy amplification of a multi-channel microflow reactor, and realization of mass production of products.
(2) The method for preparing the p-tert-butyl methyl benzoate provided by the invention has the advantages that the adopted multi-channel microflow reactor can realize the continuous production of the p-tert-butyl methyl benzoate, the operation is simple, the reaction materials are quickly and fully mixed, and the reaction rate is high.
(3) According to the method for preparing the p-tert-butyl methyl benzoate, a single-pass straight pipe or a multi-stage bent pipe can be used for strengthening the reaction by adjusting the scale effect of a reactor, the accurate control of the retention time can be realized by changing the length or the flow rate of the single-pass straight pipe or the multi-stage bent pipe, the occurrence of side reactions is controlled, and the product yield is improved.
(4) The method for preparing the p-tert-butyl methyl benzoate has the advantages that the multi-channel microflow reactor has high heat transfer area, rapid heat transfer and accurate reaction temperature control, and can realize isothermal operation.
(5) The method for preparing p-tert-butyl methyl benzoate has the advantages of small pipe diameter of the multi-channel microflow reactor, small using amount of reaction reagents, easy optimization of reaction, high temperature and high pressure resistance and low production cost.
(6) The method for preparing the p-tert-butyl methyl benzoate has the advantages that the multichannel microflow reactor is easy to realize amplification, and the mass production of products is realized.
(7) The method for preparing the p-tert-butyl methyl benzoate avoids the problems of low mass transfer efficiency of raw materials, low reaction rate, discontinuous production process and the like of the traditional batch kettle type reactor.
(8) According to the method for preparing the p-tert-butyl methyl benzoate, reactants and catalysts which are not completely reacted in a reaction system can be recycled, so that the method is energy-saving and environment-friendly, and saves resources.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and, together with the description, serve to explain the invention without limitation. In the drawings:
FIG. 1 is a schematic diagram of a system for preparing methyl p-tert-butylbenzoate according to the inventive example;
FIG. 2 is a schematic view of a multi-channel microflow reactor according to an embodiment of the present invention;
fig. 3 is a schematic view of a plurality of parallel and connected multi-stage elbows according to an embodiment of the present invention.
Description of reference numerals:
a 1-methanol feed channel; a feed inlet for 2-p-tert-butylbenzoic acid; 3-a catalyst feed channel; 4-stirring the mixture in a kettle; 5-a multi-channel microflow reactor; 51-a feed channel; 52-a heat exchange chamber; 521-a partition plate; 53-a discharge channel; 54-single pass straight pipe; 55-multi-stage bent pipe; 6-a first reflux drum; 7-a first rectification column; 8-liquid separator; 9-a second rectification column; 10-a second reflux drum; 11-a third rectification column; 12-a third reflux drum;
an outlet of methyl A-p-tert-butylbenzoate; b-a waste water outlet; c-a waste sulfuric acid outlet; d-a feed port; an E-heat exchange medium inlet; an F-heat exchange medium outlet; g-a discharge hole.
Detailed Description
It should be noted that the embodiments and features of the embodiments of the present invention may be combined with each other without conflict.
In the description of the present invention, it is to be understood that the terms "central," "longitudinal," "lateral," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like are used in the orientation or positional relationship indicated in the drawings, which are merely for convenience in describing the invention and to simplify the description, and are not intended to indicate or imply that the referenced device or element must have a particular orientation, be constructed and operated in a particular orientation, and are therefore not to be construed as limiting the invention. Furthermore, the terms "first", "second", etc. are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first," "second," etc. may explicitly or implicitly include one or more of that feature. In the description of the invention, the meaning of "a plurality" is two or more unless otherwise specified.
In the description of the invention, it is to be noted that, unless otherwise explicitly specified or limited, the terms "mounted", "connected" and "connected" are to be construed broadly, e.g. as being fixed or detachable or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meaning of the above terms in the creation of the present invention can be understood by those of ordinary skill in the art through specific situations.
The invention will be described in detail with reference to the following embodiments with reference to the attached drawings.
Example 1
Continuously feeding methanol with a molar ratio of 10:1, p-tert-butyl benzoic acid and a sulfuric acid catalyst accounting for 10 percent of the weight of the raw materials into a multi-channel microflow reactor 5, carrying out esterification reaction at a reaction temperature of 120 ℃ and a reaction pressure of 1Mpa, keeping reactants for 1.5h, and sequentially separating methanol, a sulfuric acid aqueous solution and p-tert-butyl benzoic acid from a product mixture obtained at the outlet of the reactor to obtain the p-tert-butyl methyl benzoate, wherein the yield is 93 percent, and the purity is more than or equal to 99.99 percent. Wherein unreacted p-tert-butyl benzoic acid and methanol are recycled, and the catalyst is recycled.
Example 2
Continuously feeding methanol with a molar ratio of 10:1, p-tert-butyl benzoic acid and a sulfuric acid catalyst accounting for 10 percent of the weight of the raw materials into a multi-channel microflow reactor 5, carrying out esterification reaction at a reaction temperature of 140 ℃ and a reaction pressure of 1.5Mpa, keeping the reactant for 1h, and sequentially separating the methanol, a sulfuric acid aqueous solution and the p-tert-butyl benzoic acid from a product mixture obtained at the outlet of the reactor to obtain the methyl p-tert-butyl benzoate, wherein the yield is 96 percent, and the purity is more than or equal to 99.99 percent. Wherein unreacted p-tert-butyl benzoic acid and methanol are recycled, and the catalyst is recycled.
Example 3
Continuously feeding methanol with a molar ratio of 10:1, p-tert-butyl benzoic acid and a sulfuric acid catalyst accounting for 15% of the weight of the raw materials into a multi-channel microflow reactor 5, carrying out esterification reaction at a reaction temperature of 120 ℃ and a reaction pressure of 1.5Mpa, keeping the reaction for 1h, and sequentially separating methanol, a sulfuric acid aqueous solution and p-tert-butyl benzoic acid from a product mixture obtained at the outlet of the reactor to obtain the p-tert-butyl methyl benzoate, wherein the yield is 93%, and the purity is more than or equal to 99.99%. Wherein unreacted p-tert-butyl benzoic acid and methanol are recycled, and the catalyst is recycled.
Example 4
Continuously feeding methanol with a molar ratio of 8:1, p-tert-butyl benzoic acid and a sulfuric acid catalyst accounting for 10 percent of the weight of the raw materials into a multi-channel microflow reactor 5, carrying out esterification reaction at a reaction temperature of 140 ℃ and a reaction pressure of 2Mpa, keeping the reactant for 1.5h, and sequentially separating the methanol, a sulfuric acid aqueous solution and the p-tert-butyl benzoic acid from a product mixture obtained at the outlet of the reactor to obtain the methyl p-tert-butyl benzoate, wherein the yield is 96 percent, and the purity is more than or equal to 99.99 percent. Wherein unreacted p-tert-butyl benzoic acid and methanol are recycled, and the catalyst is recycled.
Example 5
Continuously feeding methanol with a molar ratio of 10:1, p-tert-butyl benzoic acid and a sulfonic acid resin catalyst accounting for 8 percent of the weight of the raw materials into a multi-channel microflow reactor 5, carrying out esterification reaction at a reaction temperature of 120 ℃ and a reaction pressure of 1.5Mpa, keeping the reactant for 2.5h, and sequentially separating methanol, a sulfuric acid aqueous solution and the p-tert-butyl benzoic acid from a product mixture obtained at the outlet of the reactor to obtain the methyl p-tert-butyl benzoate, wherein the yield is 96 percent, and the purity is more than or equal to 99.99 percent. Wherein unreacted p-tert-butyl benzoic acid and methanol are recycled, and the catalyst is recycled.
Example 6
Continuously feeding methanol with a molar ratio of 10:1, p-tert-butyl benzoic acid and a sulfonic acid resin catalyst accounting for 10 percent of the weight of the raw materials into a multi-channel microflow reactor 5, carrying out esterification reaction at a reaction temperature of 120 ℃ and a reaction pressure of 1.5Mpa, keeping the reaction for 2 hours, and sequentially separating methanol, a sulfuric acid aqueous solution and p-tert-butyl benzoic acid from a product mixture obtained at the outlet of the reactor to obtain the methyl p-tert-butyl benzoate, wherein the yield is 96 percent, and the purity is more than or equal to 99.99 percent. Wherein unreacted p-tert-butyl benzoic acid and methanol are recycled, and the catalyst is recycled.
Example 7
Continuously feeding methanol with a molar ratio of 8:1, p-tert-butyl benzoic acid and a sulfonic acid resin catalyst accounting for 10 percent of the weight of the raw materials into a multi-channel microflow reactor 5, carrying out esterification reaction at a reaction temperature of 100 ℃ and a reaction pressure of 0.9Mpa, keeping the reactant for 5.5h, and sequentially separating methanol, a sulfuric acid aqueous solution and the p-tert-butyl benzoic acid from a product mixture obtained at the outlet of the reactor to obtain the methyl p-tert-butyl benzoate, wherein the yield is 95 percent, and the purity is more than or equal to 99.99 percent. Wherein unreacted p-tert-butyl benzoic acid and methanol are recycled, and the catalyst is recycled.
Example 8
Continuously feeding methanol and p-tert-butyl benzoic acid with a molar ratio of 10:1 into a multi-channel microflow reactor 5, performing esterification reaction at a reaction temperature of 160 ℃ and a reaction pressure of 3.0Mpa for 5.5h, respectively separating methanol and water from a product mixture obtained at the outlet of the reactor in sequence, and then performing rotary evaporation treatment on a crude product to obtain the p-tert-butyl methyl benzoate, wherein the yield is 94% and the purity is more than or equal to 99.99%. Wherein unreacted p-tert-butyl benzoic acid and methanol are recycled, and the catalyst is recycled.
Example 9
Continuously feeding methanol with a molar ratio of 10:1, p-tert-butyl benzoic acid and an ionic liquid catalyst accounting for 10% of the weight of the raw materials into a multi-channel microflow reactor 5, carrying out esterification reaction at a reaction temperature of 120 ℃ and a reaction pressure of 1Mpa, keeping reactants for 2h, and sequentially separating methanol, a sulfuric acid aqueous solution and p-tert-butyl benzoic acid from a product mixture obtained at the outlet of the reactor to obtain the methyl p-tert-butyl benzoate, wherein the yield is 94% and the purity is more than or equal to 99.99%. Wherein unreacted p-tert-butyl benzoic acid and methanol are recycled, and the catalyst is recycled.
From the above examples, it can be seen that the method for synthesizing methyl p-tert-butylbenzoate according to the present invention comprises the steps of continuously reacting methanol, p-tert-butylbenzoic acid and methanol in a multi-channel micro-flow reactor under the action of an acidic catalyst to synthesize methyl p-tert-butylbenzoate. The method can realize continuous production, is simple to operate, can quickly and fully mix reaction materials, has the advantages of high reaction speed, controllable residence time, quick heat transfer, controllable temperature, small amount of reaction reagent, easy optimization of reaction, high-temperature and high-pressure resistance of reaction, easy amplification of the multi-channel microflow reactor, and industrial mass production.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and should not be taken as limiting the invention, so that any modifications, equivalents, improvements and the like, which are within the spirit and principle of the present invention, should be included in the scope of the present invention.

Claims (9)

1. A system for the production of methyl p-tert-butylbenzoate characterized by: including stirred tank (4), multichannel microflow reactor (5), first rectifying column (7), liquid-liquid separator (8) that connect gradually, the bottom and second rectifying column (9) of liquid-liquid separator (8) are connected, and the upper portion and third rectifying column (11) of liquid-liquid separator (8) are connected, the top of first rectifying column (7), second rectifying column (9), third rectifying column (11) all is connected with the reflux drum, multichannel microflow reactor (5) include from last feed channel (51), multichannel microflow reaction unit, discharge channel (53) to intercommunication in proper order down, and multichannel microflow reaction unit's outside is equipped with the heat transfer room.
2. The system for preparing methyl p-tert-butylbenzoate according to claim 1, wherein: the upper portion of stirred tank (4) all is connected with methyl alcohol feedstock channel (1), p-tert butyl benzoic acid feed inlet (2), catalyst feedstock channel (3), the bottom of stirred tank (4) with feed inlet (D) intercommunication of multichannel microflow reactor (5), discharge gate (G) and first rectifying column (7) of multichannel microflow reactor (5) are connected, the bottom and the liquid-liquid separator (8) of first rectifying column (7) are connected, the upper portion and third rectifying column (11) of liquid-liquid separator (8) are connected, the upper portion and the third reflux drum (12) of third rectifying column (11) are connected, third reflux drum (12) bottom is connected with p-tert butyl benzoic acid methyl ester export (A).
3. The system for preparing methyl p-tert-butylbenzoate according to claim 1, wherein: the multi-channel microfluidic reaction component is formed by a plurality of one-way straight pipes (54) which are arranged in parallel, the top parts of the one-way straight pipes (54) are communicated with the feeding channel (51), and the bottom parts of the one-way straight pipes (54) are communicated with the discharging channel (53).
4. The system for preparing methyl p-tert-butylbenzoate according to claim 1, wherein: the multi-channel microfluidic reaction component is a multi-stage bent pipe (55), a feed inlet of the multi-stage bent pipe (55) is communicated with the feed channel (51), and a discharge outlet of the multi-stage bent pipe (55) is communicated with the discharge channel (53).
5. A process for producing methyl p-t-butylbenzoate using the system for producing methyl p-t-butylbenzoate according to any one of claims 1 to 4, wherein: comprises the step of synthesizing the p-tert-butyl methyl benzoate by taking methanol and p-tert-butyl benzoic acid as reactants and carrying out esterification reaction through a multi-channel microflow reactor (5).
6. The process according to claim 5, wherein the reaction mixture comprises: comprises the steps of taking methanol and p-tert-butyl benzoic acid as raw materials and acid as a catalyst, and carrying out esterification reaction through a multi-channel microflow reactor (5) to synthesize the p-tert-butyl methyl benzoate.
7. The process according to claim 5, wherein the reaction mixture comprises: the reaction temperature is 60-200 deg.C, and the reaction pressure is 0.1-5 Mpa.
8. The process according to claim 5, wherein the reaction mixture comprises: the molar ratio of the p-tert-butyl benzoic acid to the methanol is 1:1-1: 15.
9. The process according to claim 6, wherein the reaction mixture comprises: the weight of the catalyst is 1-20% of the total weight of the reactants.
CN202010269651.6A 2020-04-08 2020-04-08 Method for preparing p-tert-butyl methyl benzoate Pending CN111302937A (en)

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Cited By (1)

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CN114409927A (en) * 2022-01-24 2022-04-29 安徽省纳胜生物科技有限公司 Ten-thousand-ton-grade high-viscosity instant ultrahigh molecular weight sodium polyacrylate and preparation method and application thereof

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Application publication date: 20200619