CN113842857B - System and method for preparing acylation liquid - Google Patents

System and method for preparing acylation liquid Download PDF

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Publication number
CN113842857B
CN113842857B CN202111075055.5A CN202111075055A CN113842857B CN 113842857 B CN113842857 B CN 113842857B CN 202111075055 A CN202111075055 A CN 202111075055A CN 113842857 B CN113842857 B CN 113842857B
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liquid
port
outlet
inlet
heat exchange
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CN113842857A (en
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毛学锋
张笑然
李恒
李振涛
郭玉辉
胡发亭
赵鹏
陈贵锋
李军芳
钟金龙
王�琦
王吉坤
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CCTEG China Coal Research Institute
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CCTEG China Coal Research Institute
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Priority to CN202111075055.5A priority Critical patent/CN113842857B/en
Publication of CN113842857A publication Critical patent/CN113842857A/en
Priority to PCT/CN2022/115478 priority patent/WO2023040641A1/en
Priority to JP2022573236A priority patent/JP2023546762A/en
Priority to US18/057,394 priority patent/US20230095165A1/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18—Stationary reactors having moving elements inside
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006—Controlling or regulating processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006—Controlling or regulating processes
    • B01J19/0013—Controlling the temperature of the process
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053—Details of the reactor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00—Feed or outlet devices; Feed or outlet control devices
    • B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00—Feed or outlet devices; Feed or outlet control devices
    • B01J4/008—Feed or outlet control devices
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
    • C07C45/45—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by condensation
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
    • C07C45/45—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by condensation
    • C07C45/46—Friedel-Crafts reactions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2204/00—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices
    • B01J2204/002—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices the feeding side being of particular interest
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2204/00—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices
    • B01J2204/005—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices the outlet side being of particular interest
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00054—Controlling or regulating the heat exchange system
    • B01J2219/00056—Controlling or regulating the heat exchange system involving measured parameters
    • B01J2219/00058—Temperature measurement
    • B01J2219/00063—Temperature measurement of the reactants
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
    • B01J2219/00094—Jackets
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/141—Feedstock

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses a system and a method for preparing an acylation liquid, wherein the method for preparing the acylation liquid comprises the following steps: a. weighing the Lewis catalyst under the protection of inert gas; b. adding the Lewis catalyst weighed in the step a into a solvent for dissolution to obtain a mixed solution; c. and c, adding a Lewis acylating agent into the mixed solution obtained in the step b to obtain an acylating liquid. The acylation liquid prepared by the method for preparing the acylation liquid has high stability, can be used for a microchannel reactor, has higher yield and selectivity, does not need cooling treatment in the preparation process, saves energy consumption and improves the preparation efficiency.

Description

System and method for preparing acylation liquid
Technical Field
The invention belongs to the technical field of preparation of acylation liquid, and particularly relates to a system and a method for preparing the acylation liquid.
Background
2, 6-naphthalene dicarboxylic acid is an important monomer of special high-end polyester polyethylene naphthalate (PEN), and is a high-performance material with excellent heat resistance, gas barrier property, chemical stability and the like because of high symmetry of the monomer.
The synthetic method of 2, 6-naphthalene dicarboxylic acid is to take 2-methylnaphthalene as raw material, to generate 2-methyl-6 acyl naphthalene through acylation reaction, and then to oxidize to obtain 2, 6-naphthalene dicarboxylic acid.
In the acylation reaction using 2-methylnaphthalene as a raw material, it is very critical how to prepare an acylation solution with high stability and high uniformity. The acylation reaction adopts Lewis acid as a catalyst, and has the technical advantages of high yield and high product purity. The acylating agent reacts with the Lewis catalyst to form an electrophilic complex, which is easy to enter the para position of the acylated product, so that the selectivity of the reaction is higher. However, the catalyst and the acylating agent have higher activity, are easy to react with water and deteriorate, can generate a large amount of white acid mist when contacting with air with higher humidity, and can generate precipitation after the catalyst reacts, so that the acylating liquid is unstable in the air. In addition, the reaction needs to be carried out in a homogeneous phase, and undissolved catalyst in the solution and particles generated by deterioration can influence the reaction efficiency of the acylation liquid and influence the yield and purity of the final product. Therefore, there is a need to develop a method for preparing an acylating solution with high stability so that the reaction can be efficiently performed.
Most of the existing preparation methods are carried out in a traditional batch reactor type. In recent years, the microreactor is superior to a conventional kettle reactor in heat exchange efficiency, reaction speed, yield, safety, stability and the like, and can perform more refined production control. However, microchannel reactors require reactions in a completely homogeneous phase and no solid particles are present. It is desirable to formulate a uniform and stable acylation solution for use in a microchannel acylation reaction device. Therefore, developing a continuous acylation solution preparation method with low energy consumption, high process efficiency and safety for the acylation reaction process of the microchannel reactor is a key problem to be solved by the technicians in the field.
Disclosure of Invention
The present invention has been made based on the findings and knowledge of the inventors regarding the following facts and problems: the high-stability acylating liquid can be used in the microchannel acylation reaction device. The preparation method of the conventional acylating liquid is kettle type preparation. A three-neck flask is selected as a container, and an acylating agent, a Lewis catalyst and a solvent are added into the container. Firstly mixing Lewis catalyst and solvent, slowly dripping acylating agent after the temperature of the constant temperature tank is reduced to minus 5 ℃, and continuously stirring to obtain uniform and transparent solution. In the existing preparation method, the prepared acylating liquid is exposed to air, particularly under the condition of high air humidity, the Lewis catalyst and the acylating agent are easy to deactivate, and a large amount of more corrosive white acid mist is formed. And the acylating liquid contacts with air to react to generate aluminum hydroxide solid particles, which not only can lead to insufficient reaction, but also can block the microchannel reactor due to the existence of solid particles, thereby influencing the continuity of the acylation reaction. Secondly, in the existing preparation method, the acylating agent is added into the Lewis catalyst solution at low temperature, but in actual operation, the Lewis catalyst solution pulps or a great amount of Lewis catalyst crystals are separated out under the low temperature condition, and the cooling not only consumes a great amount of energy, but also increases the preparation time of the acylating solution.
In the patent application with the application publication number of CN107879909A and named as a method for synthesizing acyl naphthalene by using a microchannel reactor, the reactor is placed in a low-temperature tank, nitrobenzene, aluminum trichloride and propionyl chloride are sequentially added, and the temperature is controlled to be 0-3 ℃. However, there is no concern about dissolving aluminum trichloride and how to avoid the formation or presence of particulate matter, ensuring a high uniform stability of the acylating solution, and entering the reaction.
The application publication number is CN110105191A, the name is a patent application of a method for preparing high-purity naphthalene dicarboxylic acid by taking beta-methylnaphthalene as a raw material, the preparation of an acylation liquid is carried out by connecting the tail end of the acylation liquid into a reactor of anhydrous CaCl2, adding nitrobenzene, aluminum trichloride and propionyl chloride in sequence, and controlling the temperature to be 0-5 ℃. However, no mention is made of a method in which the mixture is completely dissolved as homogeneous.
The application publication number is CN112876359A, the name is a patent application of a preparation method of 2, 6-dimethyl naphthalene dicarboxylate, and the patent application relates to the proportion of each compound in an acylation liquid. However, no mention is made of a method for preventing deterioration of the acylating liquid and ensuring uniformity and stability of the mixed liquid.
The present invention aims to solve at least one of the technical problems in the related art to some extent.
To this end, embodiments of the present invention provide a system for preparing an acylating solution to improve stability and uniformity of the prepared acylating solution.
The embodiment of the invention provides a method for preparing an acylation liquid, which is implemented by using the system for preparing the acylation liquid, wherein the prepared acylation liquid has high stability, can be used for a micro-channel reactor, has higher yield and selectivity compared with a batch reaction kettle, does not need cooling treatment in the preparation process, saves energy consumption and improves the preparation efficiency.
The system for preparing the acylation liquid comprises:
the kettle body is provided with a first charging hole, a second charging hole, a stirring hole and a liquid outlet, wherein the first charging hole, the second charging hole, the stirring hole and the liquid outlet are communicated with the first chamber;
a charging port cover, wherein the charging port cover is detachably sealed and arranged on the first charging port;
a feed pump sealingly connected to the second feed port for adding an acylating agent to the second feed port; and
the stirrer is inserted in the stirring port in a sealing way, the stirrer comprises a stirring shaft and stirring blades, the stirring blades are arranged on the stirring shaft, and at least one part of the stirring shaft and each of the stirring blades are arranged in the first cavity.
The system for preparing the acylation liquid has the advantages of good stability and uniformity of the prepared acylation liquid and the like.
In some embodiments, the tank comprises:
the liquid outlet is formed in the first shell, and the upper end of the first shell is open;
an upper cover sealing the cover on the first housing, the first housing and the upper cover defining the first chamber, each of the first feed inlet, the second feed inlet, and the agitation port being provided on the upper cover; and
the jacket is sleeved on the first shell and is provided with a heat exchange medium first inlet for the heat exchange medium to enter and a heat exchange medium first outlet for the heat exchange medium to flow out.
In some embodiments, further comprising:
the heating device is provided with a heat exchange medium second inlet and a heat exchange medium second outlet, the heat exchange medium first outlet is connected with the heat exchange medium second inlet, and the heat exchange medium first inlet is connected with the heat exchange medium second outlet;
the kettle body is provided with a temperature measuring port communicated with the first cavity, a part of the temperature sensor is inserted in the temperature measuring port in a sealing way, and the detection end of the temperature sensor is arranged in the first cavity; and
and a controller connected to each of the heating device and the temperature sensor so that the controller controls the heating device according to the temperature detected by the temperature sensor.
In some embodiments, further comprising a suction filtration device comprising:
the filtering device comprises a second shell and a filtering membrane, the second shell defines a second cavity, the filtering membrane is arranged in the second cavity, the filtering membrane divides the second cavity into a first part and a second part, a filtering device inlet and a filtering device outlet which are communicated with the second cavity are formed in the second shell, the filtering device inlet is arranged corresponding to the first part, the filtering device outlet is arranged corresponding to the second part, and the filtering device inlet is connected with the liquid outlet;
the liquid storage tank comprises a third shell, a third cavity is defined by the third shell, a liquid storage tank inlet and a liquid storage tank outlet are formed in the third shell, and the liquid storage tank inlet is communicated with the filtering device outlet; and
the vacuum pump is provided with a first vacuum-pumping port, a second vacuum-pumping port communicated with the third cavity is arranged on the third shell, and the first vacuum-pumping port is communicated with the second vacuum-pumping port.
In some embodiments, the first housing, the second housing, and the third housing are of an integral structure, wherein the liquid outlet is disposed at a bottom of the first housing, the filter inlet is disposed at a top of the second housing, the filter is disposed at a bottom of the tank, the filter outlet is disposed at a bottom of the second housing, the liquid reservoir inlet is disposed at a top of the third housing, and the liquid reservoir is disposed at a bottom of the filter.
The method for preparing the acylation liquid comprises the following steps:
a. weighing the Lewis catalyst under the protection of inert gas;
b. adding a solvent and the Lewis catalyst weighed in the step a into the first cavity through the first feeding port, and stirring by using the stirrer so that the Lewis catalyst weighed in the step a is dissolved to obtain a mixed solution;
c. and c, adding an acylating agent into the mixed solution obtained in the step b by using the feeding pump, and stirring by using the stirrer so as to obtain an acylated liquid.
In the method for preparing the acylation liquid, 1, when the Lewis catalyst is weighed under the protection of inert gas, the activity of the Lewis catalyst is effectively ensured, the influence of weather environment is avoided, and the formation of acid mist when the air humidity is high is avoided; 2. in the method for preparing the acylation liquid, the Lewis catalyst is weighed in an inert environment and then added into the solvent, and the contact time of the Lewis catalyst and air is reduced in a liquid sealing manner; 3. in the method for preparing the acylating solution, in the step b, the solvent added into the kettle body and the Lewis catalyst weighed in the step a are stirred by using a stirrer, and in the step c, the acylating agent and the mixed solution obtained in the step b are stirred by using the stirrer, so that the preparation efficiency is improved; 4. the acylation liquid prepared by the method for preparing the acylation liquid provided by the embodiment of the invention has good solution homogeneity and high stability, can be used for a microchannel reactor, and improves the reaction efficiency.
In some embodiments, the solvent is nitrobenzene, and step b is:
firstly, nitrobenzene is added into the first cavity through the first charging port;
then adding the Lewis catalyst weighed in the step a into nitrobenzene;
and then heating the nitrobenzene and the Lewis catalyst to 50-60 ℃ by using a heat exchange medium, and stirring at 200-400 rpm by using the stirrer so that the Lewis catalyst weighed in the step a is dissolved to obtain a mixed solution.
In some embodiments, the method further comprises a step d, and the acylation liquid obtained in the step c is subjected to suction filtration treatment by a suction filtration device under the inert gas atmosphere, so as to obtain the filtered acylation liquid.
In some embodiments, in step c, the acylating agent is added at a rate of 3 to 10 drops per second and the stirrer is agitated at a rate of 200 to 400rpm.
In some embodiments, the molar mass ratio of the acylating agent to the Lewis catalyst is (1.1-1.5): 1.3-1.7; and/or
The molar mass ratio of the Lewis catalyst to the solvent is (1.3-1.7): 5.
drawings
FIG. 1 is a perspective view of a system for preparing an acylating liquid in accordance with one embodiment of the present invention.
Fig. 2 is a schematic view showing the internal structure of the tank body, the filtering device and the liquid storage tank in fig. 1.
FIG. 3 is a schematic diagram of the structure of the pH meter of FIG. 2.
Reference numerals:
a system 100 for preparing an acylating liquid;
a kettle body 1; a first charging port 101; a second feed inlet 102; a stirring port 103; a liquid outlet 104; a first control valve 1041; a temperature measurement port 105; a pH meter port 106; a first housing 107; an upper cover 108; a jacket 109; a heat exchange medium first inlet 1091; a heat exchange medium first outlet 1092; a first chamber 110;
a charging port cover 2;
a stirrer 3; a stirring shaft 301; a stirring blade 302;
a pH meter 4;
a temperature sensor 5;
a feed pump 6; a first hose 600;
a filtering device 7; a second housing 701; a filter inlet 7011; a filter outlet 7012; a first portion 7013; a second portion 7014; a filter membrane 702;
a liquid storage tank 8; a third housing 801, a reservoir inlet 8011; a reservoir outlet 8012; a second evacuation port 8013;
a vacuum pump 9; a second hose 900; a first vacuum port 901;
a glass cover 10; mating surface 1001.
Detailed Description
The following detailed description of embodiments of the invention is exemplary and intended to be illustrative of the invention and not to be construed as limiting the invention.
As shown in fig. 1 to 3, a system 100 for preparing an acylating liquid according to an embodiment of the present invention includes a tank body 1, a charging port cover 2, a charging pump 6, and a stirrer 3. The kettle body 1 defines a first chamber 110, and the kettle body 1 is provided with a first feeding port 101, a second feeding port 102, a stirring port 103 and a liquid outlet 104 which are communicated with the first chamber 110.
Optionally, each of the first feeding port 101, the second feeding port 102 and the stirring port 103 is provided above the liquid outlet 104.
Thus, the solvent and Lewis catalyst for preparing the acylating liquid may be fed into the first chamber 110 through the first feed port 101, and the acylating agent may be fed into the first chamber 110 through the second feed port 102.
The charging port cover 2 is detachably sealed and attached to the first charging port 101. When the material (solvent and Lewis catalyst) is required to be fed into the kettle body 1, the material feeding port cover 2 is taken down from the first material feeding port 101, and after the material feeding is completed, the material feeding port cover 2 is sealed and covered on the first material feeding port 101 in time, so that the contact time of the solvent and the Lewis catalyst with the external environment is reduced, and the time of exposing the first chamber 110 to the external environment through the first material feeding port 101 is reduced.
The feed pump 6 is hermetically connected to the second feed port 102 so as to add the acylating agent into the second feed port 102. Thus, during and after the charging of the first chamber 110 by the charging pump 6, the acylating agent is effectively prevented from contacting the external environment, and the first chamber 110 is prevented from being exposed to the external environment through the second charging port 102.
A part of the stirrer 3 is sealingly inserted in the stirring port 103, the stirrer 3 includes a stirring shaft 301 and stirring blades 302, the stirring blades 302 are provided on the stirring shaft 301, and at least a part of the stirring shaft 301 and each of the stirring blades 302 are provided in the first chamber 110.
Therefore, the stirrer 3 can be used for fully stirring and mixing the materials in the first chamber 110, so that the Lewis catalyst is fully dissolved, and the preparation efficiency of the acylation liquid is improved; and a part of the stirrer 3 is inserted into the stirring port 103 in a sealing way, so that the stirring port 103 is always kept sealed during the working process of the stirrer 3, and the first chamber 110 is prevented from being exposed to the external environment through the stirring port 103.
The method for preparing an acylating liquid implemented with the system 100 for preparing an acylating liquid of an embodiment of the present invention includes the steps of:
a. weighing the Lewis catalyst under the protection of inert gas;
b. adding the solvent and the Lewis catalyst weighed in the step a into the first chamber 110 through the first feeding port 101, and stirring by using the stirrer 3 so that the Lewis catalyst weighed in the step a is dissolved to obtain a mixed solution;
c. the acylating agent is added to the mixed solution obtained in step b by a feed pump 6 and stirred by a stirrer 3 to obtain an acylated liquid.
According to the method for preparing the acylation liquid, disclosed by the embodiment of the invention, when the Lewis catalyst is weighed, the weighing is performed under the protection of inert gas, so that the activity of the Lewis catalyst is effectively ensured, the influence of weather environment is avoided, and the formation of acid mist in the presence of high humidity in summer is avoided; in the method for preparing the acylation liquid, the Lewis catalyst is weighed in an inert environment and then added into the solvent, and the charging port cover 2 is covered, so that the contact time of the Lewis catalyst and air is reduced in a liquid sealing manner, the contact of the Lewis catalyst and the acylation agent with moisture and the like can be effectively reduced and even reduced in the process of preparing the acylation liquid, and the stability and uniformity of the prepared acylation liquid are better; in the method for preparing the acylation liquid, the Lewis catalyst can be fully and rapidly dissolved in the solvent due to the stirring effect of the stirrer 3, so that the preparation time of the acylation liquid is shortened, and the preparation efficiency of the acylation liquid is improved; the acylation liquid prepared by the method for preparing the acylation liquid provided by the embodiment of the invention has good solution homogeneity and high stability, can be used for a microchannel reactor, and improves the reaction efficiency.
Alternatively, in step a, the Lewis catalyst is selected from AlCl 3 、BF 3 、ZnCl 2 Or FeCl 3 At least one of them. The Lewis catalyst in the embodiment of the invention is not particularly limited, and the Lewis catalyst capable of being used for synthesizing 2-methyl-6 acyl naphthalene can be prepared by adopting the method for preparing the acylation liquid in the embodiment of the invention. The acylating agent may be at least one acylating agent selected from an acetylating agent, a propionylating agent or a butyrylating agent.
Optionally, the second feeding port 102 is a grinding port, the second feeding port 102 is connected with the pagoda joint in a sealing way, and the discharging pipe of the peristaltic pump is connected with the pagoda joint in a sealing way.
Optionally, the feed pump 6 is a peristaltic pump.
Therefore, the flow rate of the acylating agent added into the first chamber 110 of the kettle body 11 can be controlled by adjusting the flow rate of the peristaltic pump, so that the amount of the acylating agent added into the first chamber 110 can be conveniently controlled, and the stability and uniformity of the prepared acylating liquid can be further improved.
Optionally, the feed pump 6 is connected to the second feed inlet 102 via a first hose 600. The first hose 600 may be a polytetrafluoroethylene tube.
In some embodiments, stirring shaft 301 and stirring blades 302 are made of metal, and stirrer 33 includes a shaft erosion protection layer and a blade erosion protection layer, the shaft erosion protection layer being coated on a portion of stirring shaft 301, and the blade erosion protection layer being coated on stirring blades 302.
Optionally, the stirring shaft 301 and the stirring blade 302 are made of stainless steel, and the shaft anticorrosive layer and the blade anticorrosive layer are made of polytetrafluoroethylene.
The stirring shaft 301 and the stirring blade 302 are made of metal materials, so that the stirring shaft 301 and the stirring blade 302 can be effectively ensured to have enough structural strength. The stirring shaft 301 is coated with the shaft anti-corrosion layer, and the stirring blade 302 is coated with the blade anti-corrosion layer, so that the metal parts of the stirring shaft 301 and the stirring blade 302 are prevented from contacting with the solvent, the Lewis catalyst and the acylating agent, corrosion of the stirring shaft 301 and the stirring blade 302 is prevented, and corrosion products can be prevented from entering the acylating liquid to influence the quality of the prepared acylating liquid.
Alternatively, in the step c, the acylating agent is added at a rate of 3 to 10 drops per second, and the stirrer 3 is stirring at a rate of 200 to 400rpm.
In some embodiments, as shown in fig. 2, the kettle body 1 includes a first housing 107, an upper cover 108, and a jacket 109, and the liquid outlet 104 is disposed on the first housing 107, and an upper end of the first housing 107 is open. An upper cover 108 is hermetically sealed to the first housing 107, the first housing 107 and the upper cover 108 defining a first chamber 110, and each of the first charging port 101, the second charging port 102 and the stirring port 103 is provided on the upper cover 108. The jacket 109 is sleeved on the first shell 107, and the jacket 109 is provided with a heat exchange medium first inlet 1091 for the heat exchange medium to enter and a heat exchange medium first outlet 1092 for the heat exchange medium to flow out.
Thus, when the kettle body 1 is processed, the first housing 107 and the upper cover 108 can be processed separately, thereby facilitating the processing of the kettle body 1. In the case of the Lewis catalyst dissolution operation, the heat exchange medium may flow into the jacket 109 through the heat exchange medium first inlet 1091 and exchange heat with the material in the first chamber 110 through the first housing 107, and then flow out of the jacket 109 through the heat exchange medium first outlet 1092. Thereby realizing the heating of the materials in the first chamber 110, keeping the temperature in the first chamber 110 at the preset temperature suitable for the solvent of the Lewis catalyst, and enabling the Lewis catalyst to be rapidly dissolved in the solvent, thereby greatly shortening the preparation time of the acylation liquid and improving the preparation efficiency of the acylation liquid.
The heat exchange medium can be water, oil or other liquid.
In some embodiments, the solvent is nitrobenzene, and step b above is:
firstly, nitrobenzene is added into a first chamber 110 through a first charging port 101;
then adding the Lewis catalyst weighed in the step a into nitrobenzene;
the nitrobenzene and Lewis catalyst are then heated to 50℃to 60℃by means of a heat exchange medium in a jacket 109, while stirring at 200rpm to 400rpm by means of a stirrer 3, so that the Lewis catalyst weighed in step a is dissolved to give a mixed solution.
Therefore, the temperature in the first chamber 110 is kept at a preset temperature suitable for dissolving the Lewis catalyst, and the stirring speed of the stirrer 3 is also kept at a stirring speed suitable for dissolving the Lewis catalyst, so that the Lewis catalyst is quickly dissolved in nitrobenzene, thereby greatly shortening the preparation time of the acylation liquid and improving the preparation efficiency of the acylation liquid.
In some embodiments, the acylating liquid formulation system further includes a heating device, a temperature sensor 5, and a controller. The heating device is provided with a heat exchange medium second inlet and a heat exchange medium second outlet, the heat exchange medium first outlet 1092 is connected with the heat exchange medium second inlet, and the heat exchange medium first inlet 1091 is connected with the heat exchange medium second outlet.
The kettle body 1 is provided with a temperature measuring port 105 communicated with the first chamber 110, a part of the temperature sensor 5 is inserted into the temperature measuring port 105 in a sealing way, and the detection end of the temperature sensor 5 is arranged in the first chamber 110. The controller is connected to each of the heating device and the temperature sensor 5 so that the controller controls the heating device according to the temperature detected by the temperature sensor 5.
Thus, the heat exchange medium heated by the heating device flows to the heat exchange medium first inlet 1091 through the heat exchange medium second outlet, flows into the jacket 109 through the heat exchange medium first inlet 1091, and heats the material in the first chamber 110 by using the heat exchange medium in the jacket 109; the heat exchange medium in the jacket 109 flows out of the jacket 109 through the first outlet 1092 of the heat exchange medium and flows back to the heating device through the second inlet of the heat exchange medium to be heated by the heating device, so that the circulation flow of the heat exchange medium between the heating device and the kettle body 1 is realized.
The temperature sensor 5 can be used for detecting the temperature of the material in the first chamber 110 in real time, and the temperature of the material in the first chamber 110 detected by the temperature sensor 5 is transmitted to the controller so as to control the heating device by the controller. For example, when the temperature detected by the temperature sensor 5 is higher than the preset temperature, the controller controls the heating device to stop heating so as to prevent the material in the first chamber 110 from being higher than the preset temperature; when the temperature detected by the temperature sensor 5 is lower than the preset temperature, the controller controls the heating device to start heating so as to prevent the material in the first chamber 110 from being lower than the preset temperature. The temperature in the first chamber 110 is kept at the preset temperature suitable for dissolving the Lewis catalyst in the Lewis catalyst dissolving process, which is favorable for improving the dissolving speed of the Lewis catalyst and the preparation efficiency of the acylation liquid.
Optionally, the controller is model number DSC350.
In the step c, the temperature of the mixed solution obtained in the step b is not higher than 60 ℃, preferably 25 ℃ to 60 ℃.
In the method for preparing the acylation liquid, after the Lewis catalyst is dissolved in the solvent in the step b, the acylation liquid can be directly prepared by adding the acylation agent without cooling the mixed solution, so that the energy consumption is reduced, the preparation time of the acylation liquid is shortened, and the preparation efficiency is improved.
Of course, after the Lewis catalyst is dissolved in the solvent in step b, the acylating agent may be added to the first chamber 110 by the feed pump 6, and a heat exchange medium (e.g., cooling water or coolant) may be introduced into the jacket 109 through the heat exchange medium first inlet 1091 to cool the mixed solution.
As shown in fig. 1 and 2, the system 100 for preparing an acylating solution further includes a pH meter 4, the tank 1 has a pH meter 4 port 106 communicating with the first chamber 110, a part of the pH meter 4 is sealingly inserted into the pH meter 4 port 106, and a detection end of the pH meter 4 is disposed in the first chamber 110.
Therefore, the pH value of the material in the first chamber 110 can be detected in real time by utilizing the pH meter 4, which is beneficial to improving the preparation efficiency of the acylation liquid and improving the quality of the prepared acylation liquid.
Optionally, the pH meter 4 port 106 is a mill port. Thereby, sealing of the pH meter 4 port 106 is facilitated.
For example, as shown in fig. 3, the outer part of the pH meter 4 is provided with a glass cover 10, and the glass cover 10 has a tapered mating surface 1001, and the mating surface 1001 is in sealing engagement with the port 106 of the pH meter 4.
Alternatively, pH meter 4 is model SIN-PH6.3-5022-AL/Y.
In some embodiments, further comprising a suction filtration device comprising a filtration device 7, a reservoir 8 and a vacuum pump 9.
The filter device 7 comprises a second housing 701 and a filter membrane 702, the second housing 701 defines a second chamber, the filter membrane 702 is arranged in the second chamber, the filter membrane 702 divides the second chamber into a first portion 7013 and a second portion 7014, a filter device inlet 7011 and a filter device outlet 7012 are arranged on the second housing 701 and are communicated with the second chamber, the first portion 7013 is arranged adjacent to the filter device inlet 7011, the second portion 7014 is arranged adjacent to the filter device outlet 7012, and the filter device inlet 7011 is connected with the liquid outlet 104.
The liquid storage tank 8 includes a third housing 801, the third housing 801 defining a third chamber, the third housing 801 being provided with a liquid storage tank inlet 8011 and a liquid storage tank outlet 8012, the liquid storage tank inlet 8011 being in communication with the filter device outlet 7012. The vacuum pump 9 has a first vacuum port 901, a second vacuum port 8013 communicating with the third chamber is provided on the third housing 801, and the first vacuum port 901 communicates with the second vacuum port 8013.
Optionally, the method for preparing the acylation liquid further comprises a step d of carrying out suction filtration treatment on the acylation liquid obtained in the step c under the inert gas atmosphere to remove solid particles. In the method for preparing the acylation liquid, the prepared acylation liquid is subjected to suction filtration treatment in an inert atmosphere, undissolved solid particles in the solution are completely removed, and the homogeneity of the solution is further improved. And the vacuum pump 9 makes the inside of the filter device 7 form negative pressure, so that the acylated liquid prepared by the kettle body 1 rapidly passes through the filter membrane 702 of the filter device 7 and flows into the liquid storage tank 8 for storage under the action of the negative pressure, and the overall preparation efficiency of the acylated liquid can be further improved.
Alternatively, as shown in fig. 1, the first vacuum port 901 and the second vacuum port 8013 are connected by a second hose 900.
Specifically, during the suction filtration operation, the first feed inlet 101 may be connected to an inert gas source, and inert gas may be filled into the acylation liquid preparation system through the first feed inlet 101, so that the prepared acylation liquid is subjected to suction filtration treatment under an inert atmosphere. Alternatively, before the solvent is added to the first feed port 101, inert gas is introduced into the first housing 107, the second housing 701, and the third housing 801 through the first feed port 101 so that the entire preparation process of the acylating agent is performed under an inert atmosphere.
In some embodiments, the first housing 107, the second housing 701, and the third housing 801 are a unitary structure. Wherein, the liquid outlet 104 is arranged at the bottom of the first shell 107, the filter inlet 7011 is arranged at the top of the second shell 701, and the filter 7 is arranged at the lower part of the kettle body 1. The filter outlet 7012 is provided at the bottom of the second housing 701, the tank inlet 8011 is provided at the top of the third housing 801, and the tank 8 is provided at the lower portion of the filter 7.
Therefore, the prepared acylated liquid in the kettle body 1 can directly flow out of the kettle body 1 through the liquid outlet 104 by self gravity and enter the filter device 7 through the filter device inlet 7011, and a liquid pump for pumping the acylated liquid is not required to be additionally arranged between the liquid outlet 104 and the filter device inlet 7011 and between the filter device outlet 7012 and the liquid storage tank inlet 8011. It is advantageous to simplify the overall structure of the system 100 for preparing an acylating liquid and to reduce the manufacturing and operating costs of the system 100 for preparing an acylating liquid. In addition, in performing the assembly of the system 100 for preparing an acylating liquid, the connection of the liquid outlet 104 to the filter inlet 7011 and the filter outlet 7012 to the reservoir inlet 8011 may be omitted, facilitating the assembly of the system 100 for preparing an acylating liquid.
Optionally, the materials of the first housing 107, the jacket 109, the second housing 701 and the third housing 801 are borosilicate glass. Thereby, the conditions in the kettle body 1, the filtering device 7 and the liquid storage tank 8 are convenient to observe.
In some embodiments, the system 100 for preparing an acylating solution further includes a first control valve 1041, where the first control valve 1041 is disposed on the liquid outlet 104 to control the on-off of the liquid outlet 104.
Thus, when the first control valve 1041 is opened, the prepared acylation liquid flows out of the tank body 1 through the liquid outlet 104, and when the first control valve 1041 is closed, the tank body 1 is sealed, and the prepared acylation liquid is stored in the tank body 1.
In some embodiments, the system 100 for preparing an acylating solution further includes a second control valve disposed on the reservoir outlet 8012 to control the on-off of the reservoir outlet 8012.
Thus, when the second control valve is opened, the filtered acylated liquid flows out of the liquid storage tank 8 through the liquid storage tank outlet 8012, and when the second control valve is closed, the liquid storage tank 8 is sealed, and the filtered acylated liquid is stored in the liquid storage tank 8.
In some embodiments, the molar mass ratio of acylating agent, lewis catalyst to solvent is (1.1-1.5): 1.3-1.7): 5; and/or the molar mass ratio of the Lewis catalyst to the solvent is (1.3-1.7): 5. in other words, the molar mass of the acylating agent, lewis catalyst and solvent satisfies: the molar mass ratio of the acylating agent, the Lewis catalyst and the solvent is (1.1-1.5): (1.3-1.7): 5, and the molar mass ratio of the Lewis catalyst and the solvent is (1.3-1.7): 5, a step of; alternatively, the molar mass ratio of the acylating agent, lewis catalyst to solvent is (1.1-1.5): 1.3-1.7): 5; alternatively, the molar mass ratio of Lewis catalyst to solvent is (1.3-1.7): 5.
in the method for preparing the acylation liquid, the proportion of each substance is optimized, so that the raw materials can be fully utilized, and the production cost is reduced.
The method for preparing an acylating liquid according to the embodiment of the present invention is described in detail below with reference to examples.
Example 1
600.4g of nitrobenzene is added into a three-neck flask, 200.41g of aluminum chloride is weighed under the protection of nitrogen, the mixture is added into nitrobenzene in a first chamber 110, stirred by a stirrer 3, heated to 60 ℃ by a heat exchange medium, stirred and dissolved at 300rpm to obtain a mixed solution, 120.13g of propionylating agent is dropwise added by a feed pump 6 under the condition that the temperature of the mixed solution is 50 ℃, the dropwise adding speed is 5 drops in 1 second, the stirring is carried out at 300rpm, and the prepared acylation liquid is obtained after the dropwise adding is completed.
The acylation solution prepared in this example was mixed with the prepared 2-methylnaphthalene raw material solution, an acylation reaction was performed in a microchannel reactor at 35℃for 4 hours, and after the reaction, hydrolysis, distillation under reduced pressure and recrystallization were performed to obtain a crude 2-methyl-6-acylnaphthalene product, which was sampled and examined to obtain a product with a yield of 89.4% and a selectivity of 85%.
Example 2
The same procedure as in example 1 was repeated except that the prepared acylation liquid was subjected to suction filtration treatment with a suction filtration device under nitrogen protection to remove solid particles in the acylation liquid, thereby obtaining an acylation liquid.
The acylation solution prepared in this example was mixed with the prepared 2-methylnaphthalene feed solution under the same reaction conditions as in example 1, and the obtained crude 2-methyl-6-acylnaphthalene was detected in a yield of 91.2% and a selectivity of 86.5%.
Example 3
The same procedure as in example 1 was repeated except that, after aluminum chloride was dissolved in nitrobenzene to form a mixed solution, a propionylating agent was added dropwise at a temperature of 30 ℃.
The acylation solution prepared in this example was mixed with the prepared 2-methylnaphthalene feed solution under the same reaction conditions as in example 1, and the obtained crude 2-methyl-6-acylnaphthalene was detected in 89.6% yield with a selectivity of 85.5%.
Comparative example 1
The same procedure as in example 1 was followed except that nitrogen protection was not employed in weighing aluminum chloride.
Comparative example 1 when weighing aluminum chloride, white smoke was observed at the mouth of the bottle, and the color of aluminum chloride was changed from pale yellow to white, indicating that the surface of aluminum chloride had been deactivated.
The acylation solution prepared in comparative example 1 was mixed with the prepared 2-methylnaphthalene feed solution under the same reaction conditions as in example 1, and after the reaction, there was a significant solid residue on the reactor wall. The obtained crude 2-methyl-6-acyl naphthalene was detected in a yield of 83.31% and a selectivity of 70.85%.
Comparative example 2
The same procedure as in example 1 was followed except that nitrogen protection was not employed in weighing aluminum chloride. After aluminum chloride is dissolved in nitrobenzene to form a mixed solution, the mixed solution is cooled to 0 ℃, the solution becomes pasty, stirring is continued to become smoothie solid, and the phenomenon that the stirrer 3 is blocked occurs. And heating the mixed solution to 10-14 ℃, and then dropwise adding a propionylating agent to obtain the prepared acylated liquid.
The acylation solution prepared in comparative example 2 was mixed with the prepared 2-methylnaphthalene feed solution under the same reaction conditions as in example 1, and after the reaction, there was a significant solid residue on the reactor wall. The obtained crude 2-methyl-6-acyl naphthalene was detected with a yield of 82.8% and a selectivity of 70.04%.
Comparative example 3
The same procedure as in example 1 was repeated except that, after aluminum chloride was dissolved in nitrobenzene to form a mixed solution, a propionylating agent was added dropwise at a temperature of 5 ℃.
The acylation solution prepared in comparative example 3 was mixed with the prepared 2-methylnaphthalene starting material solution under the same reaction conditions as in example 1, and the obtained crude 2-methyl-6-acylnaphthalene was detected in a yield of 89.1% and a selectivity of 84.7%.
For purposes of this disclosure, the terms "one embodiment," "some embodiments," "example," "a particular example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, schematic representations of the above terms are not necessarily directed to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, the different embodiments or examples described in this specification and the features of the different embodiments or examples may be combined and combined by those skilled in the art without contradiction.
While embodiments of the present invention have been shown and described above, it will be understood that the above embodiments are illustrative and not to be construed as limiting the invention, and that variations, modifications, alternatives and variations may be made to the above embodiments by one of ordinary skill in the art within the scope of the invention.

Claims (5)

1. A method for preparing an acylating liquid implemented by a system for preparing an acylating liquid, characterized in that,
a system for preparing an acylating solution comprising:
the kettle body is provided with a first charging hole, a second charging hole, a stirring hole and a liquid outlet, wherein the first charging hole, the second charging hole, the stirring hole and the liquid outlet are communicated with the first chamber;
a charging port cover, wherein the charging port cover is detachably sealed and arranged on the first charging port;
a feed pump sealingly connected to the second feed port for adding an acylating agent to the second feed port; and
a stirrer, a part of which is inserted in the stirring port in a sealing way, wherein the stirrer comprises a stirring shaft and stirring blades, the stirring blades are arranged on the stirring shaft, and at least a part of the stirring shaft and each of the stirring blades are arranged in the first cavity;
the kettle body comprises:
the liquid outlet is formed in the first shell, and the upper end of the first shell is open;
an upper cover sealing the cover on the first housing, the first housing and the upper cover defining the first chamber, each of the first feed inlet, the second feed inlet, and the agitation port being provided on the upper cover; and
the jacket is sleeved on the first shell and is provided with a heat exchange medium first inlet for the heat exchange medium to enter and a heat exchange medium first outlet for the heat exchange medium to flow out;
further comprises:
the heating device is provided with a heat exchange medium second inlet and a heat exchange medium second outlet, the heat exchange medium first outlet is connected with the heat exchange medium second inlet, and the heat exchange medium first inlet is connected with the heat exchange medium second outlet;
the kettle body is provided with a temperature measuring port communicated with the first cavity, a part of the temperature sensor is inserted in the temperature measuring port in a sealing way, and the detection end of the temperature sensor is arranged in the first cavity; and
a controller connected to each of the heating device and the temperature sensor so that the controller controls the heating device according to the temperature detected by the temperature sensor;
further including suction filtration device, suction filtration device includes:
the filtering device comprises a second shell and a filtering membrane, the second shell defines a second cavity, the filtering membrane is arranged in the second cavity, the filtering membrane divides the second cavity into a first part and a second part, a filtering device inlet and a filtering device outlet which are communicated with the second cavity are formed in the second shell, the filtering device inlet is arranged corresponding to the first part, the filtering device outlet is arranged corresponding to the second part, and the filtering device inlet is connected with the liquid outlet;
the liquid storage tank comprises a third shell, a third cavity is defined by the third shell, a liquid storage tank inlet and a liquid storage tank outlet are formed in the third shell, and the liquid storage tank inlet is communicated with the filtering device outlet; and
the vacuum pump is provided with a first vacuum port, a second vacuum port communicated with the third cavity is arranged on the third shell, and the first vacuum port is communicated with the second vacuum port;
the method comprises the following steps:
a. weighing the Lewis catalyst under the protection of inert gas;
b. adding a solvent and the Lewis catalyst weighed in the step a into the first cavity through the first feeding port, and stirring by using the stirrer so that the Lewis catalyst weighed in the step a is dissolved to obtain a mixed solution, wherein the temperature of the mixed solution is 25-60 ℃;
c. c, adding an acylating agent into the mixed solution obtained in the step b by using the feeding pump to obtain an acylated liquid;
d. and c, carrying out suction filtration treatment on the acylation liquid obtained in the step c by using a suction filtration device in an inert gas atmosphere so as to obtain the filtered acylation liquid.
2. The method for preparing an acylating solution according to claim 1, wherein the first housing, the second housing, and the third housing are of an integrated structure, wherein the liquid outlet is provided at a bottom of the first housing, the filter inlet is provided at a top of the second housing, the filter is provided at a bottom of the tank, the filter outlet is provided at a bottom of the second housing, the liquid reservoir inlet is provided at a top of the third housing, and the liquid reservoir is provided at a bottom of the filter.
3. The method for preparing an acylating liquid according to claim 1, wherein the solvent is nitrobenzene, and the step b is:
firstly, nitrobenzene is added into the first cavity through the first charging port;
then adding the Lewis catalyst weighed in the step a into nitrobenzene;
and then heating the nitrobenzene and the Lewis catalyst to 50-60 ℃ by using a heat exchange medium, and stirring at 200-400 rpm by using the stirrer so that the Lewis catalyst weighed in the step a is dissolved to obtain a mixed solution.
4. The method for preparing an acylating liquid according to claim 1, wherein in the step c, the acylating agent is added at a rate of 3 to 10 drops per second, and the stirring speed of the stirrer is 200 to 400rpm.
5. The method for preparing an acylating solution of claim 1 wherein the molar mass ratio of said acylating agent to said Lewis catalyst is (1.1-1.5): 1.3-1.7; and/or
The molar mass ratio of the Lewis catalyst to the solvent is (1.3-1.7): 5.
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PCT/CN2022/115478 WO2023040641A1 (en) 2021-09-14 2022-08-29 Acylation solution and process method for continuously synthesizing acyl naphthalene using acylation solution
JP2022573236A JP2023546762A (en) 2021-09-14 2022-08-29 Acylation liquid and process method for continuous synthesis of acylnaphthalene using acylation liquid
US18/057,394 US20230095165A1 (en) 2021-09-14 2022-11-21 Method for continuous synthesis of acylnaphthalene with acylation liquid

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