CN113842857A - System and method for preparing acylation liquid - Google Patents

System and method for preparing acylation liquid Download PDF

Info

Publication number
CN113842857A
CN113842857A CN202111075055.5A CN202111075055A CN113842857A CN 113842857 A CN113842857 A CN 113842857A CN 202111075055 A CN202111075055 A CN 202111075055A CN 113842857 A CN113842857 A CN 113842857A
Authority
CN
China
Prior art keywords
liquid
acylation
port
outlet
heat exchange
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN202111075055.5A
Other languages
Chinese (zh)
Other versions
CN113842857B (en
Inventor
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
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
CCTEG China Coal Research Institute
Original Assignee
CCTEG China Coal Research Institute
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by CCTEG China Coal Research Institute filed Critical CCTEG China Coal Research Institute
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
Application granted granted Critical
Publication of CN113842857B publication Critical patent/CN113842857B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • 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

Landscapes

  • 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 method for preparing an acylation liquid, which is used for preparing the acylation liquid and comprises the following steps: a. weighing a Lewis catalyst under the protection of inert gas; b. adding the Lewis catalyst weighed in the step a into a solvent for dissolving 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 acylated solution. The acylation liquid prepared by the method for preparing the acylation liquid has high stability, can be used for a micro-channel reactor, has high 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 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 due to high symmetry of the monomer.
The synthesis method of 2, 6-naphthalene dicarboxylic acid is characterized by that it uses 2-methylnaphthalene as raw material, and adopts the acylation reaction to produce 2-methyl-6-acylnaphthalene, then makes the 2-methyl-6-acylnaphthalene undergo the process of oxidation treatment to obtain 2, 6-naphthalene dicarboxylic acid, and said synthesis method is rich in raw material source, less in side reaction and easy to refine product, and compared with the synthesis route of adopting 2, 6-dialkyl naphthalene to make 2, 6-naphthalene dicarboxylic acid by means of oxidation treatment, it is easy 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 liquid with high stability and high uniformity. Lewis acid is adopted as a catalyst in the acylation reaction, and the method has the technical advantages of high yield and high product purity. The acylating agent reacts with Lewis catalyst to generate electrophilic complex which is easy to enter the para position of acylated compound, so the reaction selectivity is high. However, the catalyst and the acylating agent have high activity, are easy to react with water and deteriorate, generate a large amount of white acid mist when contacting air with high humidity, and generate precipitate after the reaction of the catalyst, so that the acylated liquid is unstable in the air. In addition, the reaction needs to be carried out in a homogeneous phase, and both the undissolved catalyst and the particles generated by deterioration in the solution affect the efficiency of the reaction of the acylation liquid and the yield and purity of the final product. Therefore, it is necessary to develop a method for preparing an acylation liquid with high stability so that the reaction can be efficiently carried out.
Most of the existing preparation methods are carried out in a traditional batch reaction kettle type. In recent years, the micro-reactor is superior to a conventional kettle-type reactor in the aspects of heat exchange efficiency, reaction speed, yield, safety, stability and the like, and can carry out more refined production control. However, microchannel reactors require reaction in a completely homogeneous phase and no solid particles are present. Therefore, it is necessary to prepare a uniform and stable acylation liquid for the microchannel acylation reaction apparatus. Therefore, the development of a continuous acylation liquid 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 technical personnel in the field.
Disclosure of Invention
The present invention is based on the discovery and recognition by the inventors of the following facts and problems: the high-stability acylation liquid can be used for a microchannel acylation reaction device. The preparation method of the acylation liquid commonly used at present is kettle type preparation. A three-neck flask is taken as a container, and an acylating agent, a Lewis catalyst and a solvent are added into the container. Firstly mixing a Lewis catalyst and a solvent, slowly dripping an acylating agent after the temperature of a thermostatic bath is reduced to-5 ℃, and continuously stirring to obtain a uniform and transparent solution. In the existing preparation method, the prepared acylation liquid is exposed to the air, and particularly under the condition of high air humidity, a Lewis catalyst and an acylating agent are extremely easy to inactivate and form a large amount of highly corrosive white acid mist. And the acylation liquid contacts with air and reacts to generate aluminum hydroxide solid particles, which not only can cause insufficient reaction, but also can block the microchannel reactor due to the existence of the solid particles to influence the continuity of the acylation reaction. Secondly, in the existing preparation method, acylating agents are added into the Lewis catalyst solution at low temperature, but in actual operation, the Lewis catalyst solution can be slurried or a large amount of Lewis catalyst crystals can be precipitated under the low temperature condition, and the temperature reduction not only consumes a large amount of energy, but also increases the preparation time of the acylating solution.
The application publication number is CN107879909A, which is named as a patent application of a method for synthesizing acylnaphthalene by using a microchannel reactor, the reactor is put into a low-temperature tank, nitrobenzene, aluminum trichloride and propionyl chloride are added in sequence, and the temperature is controlled to be 0-3 ℃. But does not relate to dissolving aluminum trichloride, how to avoid the generation or existence of particles, and ensure the high uniform stability of the acylation liquid to enter the reaction.
The application publication number is CN110105191A, which is named as a patent application of a method for preparing high-purity naphthalenedicarboxylic acid by taking beta-methylnaphthalene as a raw material, the preparation of the acylation liquid uses a reactor with the tail end connected with anhydrous CaCl2, nitrobenzene, aluminum trichloride and propionyl chloride are added in sequence, and the temperature is controlled to be 0-5 ℃. However, there is no mention of a method in which the mixed solution is completely dissolved to be homogeneous.
The patent application with the application publication number of CN112876359A and the name of a preparation method of dimethyl 2, 6-naphthalene dicarboxylate relates to the mixture ratio of each compound of acylation liquid. However, there is no mention of a method of preventing the deterioration of the acylation liquid and ensuring the homogeneity and stability of the mixed liquid.
The present invention is directed to solving, at least to some extent, one of the technical problems in the related art.
To this end, embodiments of the present invention propose a system for preparing an acylation liquid to improve stability and uniformity of the prepared acylation liquid.
The embodiment of the invention provides a method for preparing the acylation liquid, which is implemented by utilizing the system for preparing the acylation liquid, the prepared acylation liquid has high stability, can be used for a microchannel reactor, has higher yield and selectivity compared with an intermittent reaction kettle, and does not need cooling treatment in the preparation process, thereby not only saving energy consumption, but also improving the preparation efficiency.
The system for preparing the acylation liquid of the embodiment of the invention comprises:
the kettle body is provided with a first feeding port, a second feeding port, a stirring port and a liquid outlet, wherein the first feeding port, the second feeding port, the stirring port and the liquid outlet are communicated with the first chamber;
the charging port cover is detachably sealed and arranged on the first charging port in a sealing way;
the feeding pump is hermetically connected with the second feeding port so as to add an acylating agent into the second feeding port; and
the stirrer comprises a stirring shaft and stirring blades, wherein a part of the stirrer is inserted in the stirring port in a sealing manner, the stirring blades are arranged on the stirring shaft, and each of at least one part of the stirring shaft and the stirring blades is arranged in the first cavity.
The system for preparing the acylation liquid provided by the embodiment of the invention has the advantages of good stability and uniformity of the prepared acylation liquid and the like.
In some embodiments, the kettle body comprises:
the liquid outlet is arranged on the first shell, and the upper end of the first shell is open;
an upper cover hermetically mounted on the first housing, the first housing and the upper cover defining the first chamber, each of the first feed opening, the second feed opening, and the agitation opening being disposed on the upper cover; and
the jacket is sleeved on the first shell and is provided with a first heat exchange medium inlet for the heat exchange medium to enter and a first heat exchange medium outlet for the heat exchange medium to flow out.
In some embodiments, further comprising:
the heating device is provided with a second heat exchange medium inlet and a second heat exchange medium outlet, the first heat exchange medium outlet is connected with the second heat exchange medium inlet, and the first heat exchange medium inlet is connected with the second heat exchange medium outlet;
the kettle body is provided with a temperature measuring port communicated with the first cavity, one part of the temperature sensor is inserted in the temperature measuring port in a sealing manner, 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.
In some embodiments, further comprising a suction filtration device, the suction filtration device comprising:
the filtering device comprises a second shell and a filtering membrane, the second shell defines a second chamber, the filtering membrane is arranged in the second chamber, the filtering membrane divides the second chamber into a first part and a second part, the second shell is provided with a filtering device inlet and a filtering device outlet which are communicated with the second chamber, 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, the third shell limits a third chamber, the third shell is provided with a liquid storage tank inlet and a liquid storage tank outlet, and the liquid storage tank inlet is communicated with the filtering device outlet; and
and the vacuum pumping pump is provided with a first vacuum pumping port, a second vacuum pumping port communicated with the third chamber 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 casing, the second casing and the third casing are of an integrated structure, wherein the liquid outlet is disposed at the bottom of the first casing, the inlet of the filtering device is disposed at the top of the second casing, the filtering device is disposed at the bottom of the kettle body, the outlet of the filtering device is disposed at the bottom of the second casing, the inlet of the liquid storage tank is disposed at the top of the third casing, and the liquid storage tank is disposed at the bottom of the filtering device.
The method for preparing the acylation liquid of the embodiment of the invention comprises the following steps:
a. weighing a Lewis catalyst under the protection of inert gas;
b. adding a solvent and the Lewis catalyst weighed in the step a into the first chamber through the first feeding port, and stirring by using the stirrer so as to dissolve the Lewis catalyst weighed in the step a 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 to obtain an acylated liquid.
The method for preparing the acylation liquid of the embodiment of the invention brings advantages and technical effects, 1, in the method for preparing the acylation liquid of the embodiment of the invention, when the Lewis catalyst is weighed, the Lewis catalyst is weighed under the protection of inert gas, so that the activity of the Lewis catalyst is effectively ensured, the Lewis catalyst is not influenced by weather environment, and the formation of acid mist when the air humidity is high is avoided; 2. according to the method for preparing the acylation liquid, the Lewis catalyst is weighed in an inert environment and then added into the solvent, so that the contact time of the Lewis catalyst and air is reduced in a liquid seal mode; 3. in the method for preparing the acylation liquid, the solvent added into the kettle body and the Lewis catalyst weighed in the step a are stirred by a stirrer in the step b, and the acylating agent and the mixed solution obtained in the step b are stirred by the stirrer in the step c, 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, adding nitrobenzene into the first chamber through the first feeding 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 simultaneously stirring by using the stirrer at 200-400 rpm so as to dissolve the Lewis catalyst weighed in the step a to obtain a mixed solution.
In some embodiments, the method further comprises a step d of performing suction filtration treatment on the acylation liquid obtained in the step c by using a suction filtration device under an inert gas atmosphere so as to obtain a 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 at a stirring speed of 200 to 400 rpm.
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 acylate solution according to an embodiment of the present invention.
FIG. 2 is a schematic view of the internal structure of the kettle, the filtering device and the liquid storage tank in FIG. 1.
Fig. 3 is a schematic diagram of the structure of the pH meter in fig. 2.
Reference numerals:
a system 100 for formulating an acylation solution;
a kettle body 1; a first feed port 101; a second feed port 102; a stirring port 103; a liquid outlet 104; a first control valve 1041; a temperature measuring port 105; a pH meter port 106; a first housing 107; an upper cover 108; a jacket 109; a first heat exchange medium inlet 1091; a first heat exchange medium 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; filter inlet 7011; a filter device 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 vacuum port 8013;
a vacuum pump 9; a second hose 900; a first vacuum port 901;
a glass cover 10; a mating surface 1001.
Detailed Description
The following detailed description of embodiments of the invention is intended to be illustrative, and not to be construed as limiting the invention.
As shown in fig. 1 to 3, a system 100 for preparing an acylation liquid according to an embodiment of the present invention includes a tank 1, a lid 2, a feed 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 hole 101, a second feeding hole 102, a stirring hole 103 and a liquid outlet 104 which are communicated with the first chamber 110.
Optionally, each of first addition port 101, second addition port 102, and stirring port 103 is disposed above liquid outlet 104.
Thus, a solvent and a Lewis catalyst for preparing an acylation liquid may be introduced into the first chamber 110 through the first feed port 101, and an acylation agent may be introduced into the first chamber 110 through the second feed port 102.
The filler cap 2 is detachably sealed and attached to the first filler port 101. When the (solvent and Lewis catalyst) needs to be fed into the kettle body 1, the feeding port cover 2 is taken down from the first feeding port 101, and after the feeding is completed, the feeding port cover 2 is tightly sealed and arranged on the first 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 in the external environment through the first feeding port 101 is reduced.
The addition pump 6 is hermetically connected to the second addition port 102 to add an acylating agent into the second addition port 102. Therefore, during and after the charging process of the charging pump 6 into the first chamber 110 is completed, the contact of the acylating agent with the external environment can be effectively avoided, and the exposure of the first chamber 110 to the external environment through the second charging opening 102 can be avoided.
A part of the agitator 3 is hermetically inserted into the agitating port 103, the agitator 3 includes an agitating shaft 301 and agitating blades 302, the agitating blades 302 are provided on the agitating shaft 301, and at least a part of the agitating shaft 301 and each of the agitating 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 in the stirring port 103 in a sealing manner, so that the stirring port 103 is always sealed in 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 the acylation liquid, which is implemented by the system 100 for preparing the acylation liquid of the embodiment of the present invention, comprises the following steps:
a. weighing a Lewis catalyst under the protection of inert gas;
b. adding a solvent and the Lewis catalyst weighed in the step a into a first chamber 110 through a first feeding port 101, and stirring by using a 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 means of a feed pump 6 and stirred by means of a stirrer 3 to obtain an acylated liquid.
According to the method for preparing the acylation liquid, the Lewis catalyst is weighed under the protection of the inert gas when being weighed, so that the activity of the Lewis catalyst is effectively ensured, the Lewis catalyst is not influenced by the weather environment, and the formation of acid mist when the humidity is high in summer is avoided; according to the method for preparing the acylation liquid, the Lewis catalyst is weighed in an inert environment and then added into the solvent, the feeding port cover 2 is covered, the contact time of the Lewis catalyst and the air is reduced in a liquid sealing mode, so that the contact of the Lewis catalyst and the acylation agent with water and the like can be effectively reduced in the process of preparing the acylation liquid, and the prepared acylation liquid has good stability and uniformity; in the method for preparing the acylation liquid of the embodiment of the invention, due to the stirring effect of the stirrer 3, the Lewis catalyst can be fully and quickly dissolved in the solvent, which is beneficial to shortening the preparation time of the acylation liquid and improving the preparation efficiency of the acylation liquid; 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.
Optionally, in step a, the Lewis catalyst is selected from AlCl3、BF3、ZnCl2Or FeCl3At least one of (1). There is no particular limitation on the Lewis catalyst in the examples of the present invention, and any Lewis catalyst that can be used for synthesizing 2-methyl-6-acylnaphthalene can be used for preparing the acylation liquid by the method for preparing the acylation liquid in the examples of the present 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 ground port, the second feeding port 102 is connected with a pagoda joint in a sealing manner, and the discharge pipe of the peristaltic pump is connected with the pagoda joint in a sealing manner.
Optionally, the charge 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 the uniformity of the prepared acylating solution can be further improved.
Optionally, the charge pump 6 is connected to the second charge port 102 via a first hose 600. The first hose 600 may be a polytetrafluoroethylene tube.
In some embodiments, the material of the stirring shaft 301 and the stirring blade 302 is metal, and the stirrer 33 includes a shaft anti-corrosion layer and a blade anti-corrosion layer, wherein the shaft anti-corrosion layer is coated on a part of the stirring shaft 301, and the blade anti-corrosion layer is coated on the stirring blade 302.
Optionally, the stirring shaft 301 and the stirring blade 302 are made of stainless steel, and the shaft anti-corrosion layer and the blade anti-corrosion layer are made of polytetrafluoroethylene.
The stirring shaft 301 and the stirring blades 302 are made of metal materials, so that the stirring shaft 301 and the stirring blades 302 can be effectively guaranteed 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 material parts of the stirring shaft 301 and the stirring blade 302 can be prevented from contacting with a solvent, a Lewis catalyst and an acylating agent, the corrosion of the stirring shaft 301 and the stirring blade 302 can be avoided, and the corrosion product can be prevented from entering the acylating solution to influence the quality of the prepared acylating solution.
Alternatively, 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 3 is 200 to 400 rpm.
In some embodiments, as shown in fig. 2, the kettle body 1 comprises a first shell 107, an upper cover 108 and a jacket 109, the liquid outlet 104 is arranged on the first shell 107, and the upper end of the first shell 107 is open. The upper cover 108 is hermetically fitted on the first housing 107, the first housing 107 and the upper cover 108 define a first chamber 110, and each of the first material addition port 101, the second material addition port 102, and the agitating port 103 is provided on the upper cover 108. The jacket 109 is sleeved on the first shell 107, and the jacket 109 has a first heat exchange medium inlet 1091 for the heat exchange medium to enter and a first heat exchange medium outlet 1092 for the heat exchange medium to flow out.
Therefore, when the kettle body 1 is processed, the first shell 107 and the upper cover 108 can be separately processed, so that the kettle body 1 can be conveniently processed. In the case of the Lewis catalyst dissolution operation, the heat exchange medium may flow into the jacket 109 through the first heat exchange medium inlet 1091 and exchange heat with the material in the first chamber 110 through the first shell 107, and then the heat exchange medium may flow out of the jacket 109 through the first heat exchange medium outlet 1092. Therefore, the materials in the first chamber 110 are heated, the temperature in the first chamber 110 is kept at the preset temperature suitable for the solvent of the Lewis catalyst, and the Lewis catalyst is quickly dissolved in the solvent, so that the preparation time of the acylation liquid is greatly shortened, and the preparation efficiency of the acylation liquid is improved.
The heat exchange medium can adopt liquid such as water, oil and the like.
In some embodiments, the solvent is nitrobenzene and step b above is:
nitrobenzene is first fed into the first chamber 110 through the first feed port 101;
adding the Lewis catalyst weighed in the step a into nitrobenzene;
thereafter, nitrobenzene and the Lewis catalyst were heated to 50 ℃ to 60 ℃ by the heat transfer medium in the jacket 109 while being stirred by the stirrer 3 at 200rpm to 400rpm, so that the Lewis catalyst weighed in step a was dissolved to obtain a mixed solution.
Therefore, the temperature in the first chamber 110 is kept at the preset temperature suitable for dissolving the Lewis catalyst, the stirring speed of the stirrer 3 is also kept at the stirring speed suitable for dissolving the Lewis catalyst, and the Lewis catalyst is quickly dissolved in the nitrobenzene, so that the preparation time of the acylation liquid is greatly shortened, and the preparation efficiency of the acylation liquid is improved.
In some embodiments, the acylate dispensing system further comprises a heating device, a temperature sensor 5, and a controller. The heating device is provided with a second heat exchange medium inlet and a second heat exchange medium outlet, the first heat exchange medium outlet 1092 is connected with the second heat exchange medium inlet, and the first heat exchange medium inlet 1091 is connected with the second heat exchange medium outlet.
The kettle body 1 is provided with a temperature measuring port 105 communicated with the first cavity 110, one part of the temperature sensor 5 is hermetically inserted in the temperature measuring port 105, and the detection end of the temperature sensor 5 is arranged in the first cavity 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.
Therefore, the heat exchange medium heated by the heating device flows to the first heat exchange medium inlet 1091 through the second heat exchange medium outlet, flows to the jacket 109 through the first heat exchange medium inlet 1091, and is used for heating the material in the first chamber 110; then 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 heat exchange medium can circularly flow between the heating device and the kettle body 1.
The temperature of the material in the first chamber 110 can be detected in real time by the temperature sensor 5, and the temperature of the material in the first chamber 110 detected by the temperature sensor 5 is transmitted to the controller, so that the heating device is controlled 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. In the dissolving process of the Lewis catalyst, the temperature in the first chamber 110 is kept at the preset temperature suitable for dissolving the Lewis catalyst, which is beneficial to improving the dissolving speed of the Lewis catalyst and improving the preparation efficiency of the acylation liquid.
Optionally, the controller is model DSC 350.
In the step c, the temperature of the mixed solution obtained in the step b is not higher than 60 ℃, and preferably is 25-60 ℃.
In the method for preparing the acylation liquid, the Lewis catalyst is dissolved in the solvent in the step b, and the acylation agent is directly added to prepare the acylation liquid 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 cooling of the mixed solution can also be achieved by introducing a heat exchange medium (e.g., cooling water or coolant) into the jacket 109 through the first inlet 1091 of the heat exchange medium while adding the acylating agent into the first chamber 110 by the addition pump 6.
As shown in fig. 1 and 2, the system 100 for preparing an acylation liquid further comprises a pH meter 4, the kettle body 1 is provided with a pH meter 4 port 106 communicated with the first chamber 110, a part of the pH meter 4 is hermetically inserted into the pH meter 4 port 106, and a detection end of the pH meter 4 is arranged in the first chamber 110.
Therefore, the pH meter 4 can be used for detecting the pH value of the material in the first chamber 110 in real time, so that the preparation efficiency of the acylation liquid is improved, and the quality of the prepared acylation liquid is improved.
Optionally, the pH meter 4 port 106 is a mill port. Thus, the sealing of the port 106 of the pH meter 4 is conveniently realized.
For example, as shown in fig. 3, a glass cover 10 is provided outside the pH meter 4, 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.
Optionally, the pH meter 4 is SIN-PH 6.3-5022-AL/Y.
In some embodiments, the device further comprises a suction filtration device, wherein the suction filtration device comprises a filtering device 7, a liquid storage tank 8 and a vacuum pump 9.
The filter unit 7 comprises a second housing 701 and a filter membrane 702, the second housing 701 defining a second chamber, the filter membrane 702 being disposed within the second chamber, the filter membrane 702 dividing the second chamber into a first portion 7013 and a second portion 7014, the second housing 701 being provided with a filter unit inlet 7011 and a filter unit outlet 7012 in communication with the second chamber, the first portion 7013 being disposed adjacent the filter unit inlet 7011, the second portion 7014 being disposed adjacent the filter unit outlet 7012, the filter unit inlet 7011 being connected to the liquid outlet 104.
The liquid storage tank 8 comprises a third shell 801, the third shell 801 defines a third chamber, a liquid storage tank inlet 8011 and a liquid storage tank outlet 8012 are arranged on the third shell 801, and the liquid storage tank inlet 8011 is communicated with the filtering device outlet 7012. The vacuum pump 9 has a first vacuum port 901, a second vacuum port 8013 connected to the third chamber is provided in the third housing 801, and the first vacuum port 901 is connected to the second vacuum port 8013.
Optionally, the method for preparing the acylation liquid further comprises a step d of performing suction filtration treatment on the acylation liquid obtained in the step c under an inert gas atmosphere to remove solid particles. The method is used for preparing the acylation liquid, the prepared acylation liquid is subjected to suction filtration 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 forms negative pressure in the filtering device 7, so that the acylation liquid prepared by the kettle body 1 rapidly passes through the filtering membrane 702 of the filtering 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 acylation 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, when the suction filtration operation is performed, the first feeding port 101 may be connected to an inert gas source, and the inert gas is fed into the acylation liquid preparation system through the first feeding port 101, so that the prepared acylation liquid is subjected to suction filtration in an inert atmosphere. Alternatively, before the solvent is added to the first supply port 101, an inert gas is introduced into the first housing 107, the second housing 701 and the third housing 801 through the first supply port 101, so that the entire preparation process of the acylate solution 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 1. The filter outlet 7012 is disposed at the bottom of the second housing 701, the reservoir inlet 8011 is disposed at the top of the third housing 801, and the reservoir 8 is disposed at the lower portion of the filter 7.
Therefore, the acylation liquid prepared in the kettle body 1 can directly flow out of the kettle body 1 through the liquid outlet 104 by means of the self gravity and enter the filtering device 7 through the filtering device inlet 7011, and liquid pumps for pumping the acylation liquid are not required to be additionally arranged between the liquid outlet 104 and the filtering device inlet 7011 and between the filtering device outlet 7012 and the liquid storage tank inlet 8011. It is advantageous to simplify the overall structure of the system 100 for preparing the acylation liquid, and to reduce the manufacturing and operating costs of the system 100 for preparing the acylation liquid. In addition, when the system 100 for preparing an acylation liquid is assembled, the connection of the liquid outlet 104 with the inlet 7011 of the filtering device, the outlet 7012 of the filtering device and the inlet 8011 of the liquid storage tank can be omitted, and the assembly of the system 100 for preparing an acylation liquid can be facilitated.
Optionally, the first housing 107, the jacket 109, the second housing 701, and the third housing 801 are made of borosilicate glass. Therefore, 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 dispensing an acylation liquid further comprises a first control valve 1041, and the first control valve 1041 is disposed on the liquid outlet 104 so as to control the on-off of the liquid outlet 104.
Therefore, when the first control valve 1041 is opened, the prepared acylation liquid flows out of the kettle body 1 through the liquid outlet 104, when the first control valve 1041 is closed, the kettle body 1 is sealed, and the prepared acylation liquid is stored in the kettle body 1.
In some embodiments, the system 100 for dispensing an acylation liquid further comprises a second control valve disposed on the reservoir outlet 8012 to control the on/off of the reservoir outlet 8012.
Therefore, when the second control valve is opened, the filtered acylation liquid flows out of the liquid storage tank 8 through the outlet 8012 of the liquid storage tank, when the second control valve is closed, the liquid storage tank 8 is sealed, and the filtered acylation 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 acylating agent, Lewis catalyst and solvent satisfies: the mol mass ratio of the acylating agent, the Lewis catalyst and the solvent is (1.1-1.5): 1.3-1.7):5, and the mol mass ratio of the Lewis catalyst and the solvent is (1.3-1.7): 5; or the mol mass ratio of the acylating agent, the Lewis catalyst and the solvent is (1.1-1.5) to (1.3-1.7) to 5; or the molar mass ratio of the Lewis catalyst to the 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 formulating the acylate 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, the mixture is stirred by a stirrer 3, a heat exchange medium is used for heating to 60 ℃, the mixture is stirred and dissolved at 300rpm to obtain a mixed solution, 120.13g of propionating agent is dropwise added by a feeding pump 6 at the temperature of 50 ℃, the dropwise adding speed is 1 second and 5 drops are stirred at 300rpm, and the prepared acylation liquid is obtained after the dropwise adding is finished.
The acylation liquid prepared in the embodiment is mixed with the prepared 2-methylnaphthalene raw material liquid, acylation reaction is carried out in a microchannel reactor, the reaction temperature is 35 ℃, the reaction time is 4 hours, hydrolysis, reduced pressure distillation and recrystallization are carried out after the reaction to obtain a 2-methyl-6-acylnaphthalene crude product, and a sampling detection product has the yield of 89.4 percent and the selectivity of 85 percent.
Example 2
The same method as that of example 1, except that the prepared acylation liquid was subjected to suction filtration treatment with a suction filtration apparatus under nitrogen protection to remove solid particles in the acylation liquid, thereby obtaining an acylation liquid.
The acylation liquid prepared in the example and the prepared 2-methylnaphthalene raw material liquid are mixed, the reaction conditions are the same as those in the example 1, and the obtained crude 2-methyl-6-acylnaphthalene product is detected, so that the yield is 91.2%, and the selectivity is 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 propionating agent was added dropwise at a temperature of 30 ℃.
The acylation liquid prepared in the example and the prepared 2-methylnaphthalene raw material liquid are mixed, the reaction conditions are the same as those in the example 1, and the obtained crude 2-methyl-6-acylnaphthalene product is detected, so that the yield is 89.6%, and the selectivity is 85.5%.
Comparative example 1
The same procedure as in example 1 was followed, except that the aluminum chloride was weighed without nitrogen blanket.
Comparative example 1 when aluminum chloride was weighed, white smoke was observed at the bottle mouth, and the color of the aluminum chloride changed from pale yellow to white, indicating the presence of deactivation on the surface of the aluminum chloride.
The acylation liquid prepared in the comparative example 1 and the prepared 2-methylnaphthalene raw material liquid are mixed, the reaction conditions are the same as those of the example 1, and obvious solid residues are left on the wall of the reactor after the reaction. The obtained crude 2-methyl-6-acylnaphthalene product was examined to find that the yield was 83.31% and the selectivity was 70.85%.
Comparative example 2
The same procedure as in example 1 was followed, except that the aluminum chloride was weighed without nitrogen blanket. After the aluminum chloride is dissolved in the nitrobenzene to form a mixed solution, the mixed solution is cooled to 0 ℃, the solution is slurried and is continuously stirred to become a smoothie-like solid, and the phenomenon that the stirrer 3 is blocked occurs. Heating the mixed solution to 10-14 ℃, and then dropwise adding a propionating agent to obtain the prepared acylation solution.
The acylation liquid prepared in the comparative example 2 and the prepared 2-methylnaphthalene raw material liquid were mixed, the reaction conditions were the same as in example 1, and a significant solid residue was left on the reactor wall after the reaction. The obtained crude 2-methyl-6-acylnaphthalene product is detected, the yield is 82.8 percent, and the selectivity is 70.04 percent.
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 propionating agent was added dropwise at a temperature of 5 ℃.
The acylation liquid prepared in the comparative example 3 and the prepared 2-methylnaphthalene raw material liquid are mixed, the reaction conditions are the same as those in the example 1, and the obtained crude 2-methyl-6-acylnaphthalene product is detected, so that the yield is 89.1 percent, and the selectivity is 84.7 percent.
In the present disclosure, the terms "one embodiment," "some embodiments," "an example," "a specific example," or "some examples" and the like mean that a specific feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present disclosure. In this specification, the schematic representations of the terms used above are not necessarily intended to refer 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, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.

Claims (10)

1. A system for dispensing an acylation liquid, comprising:
the kettle body is provided with a first feeding port, a second feeding port, a stirring port and a liquid outlet, wherein the first feeding port, the second feeding port, the stirring port and the liquid outlet are communicated with the first chamber;
the charging port cover is detachably sealed and arranged on the first charging port in a sealing way;
the feeding pump is hermetically connected with the second feeding port so as to add an acylating agent into the second feeding port; and
the stirrer comprises a stirring shaft and stirring blades, wherein a part of the stirrer is inserted in the stirring port in a sealing manner, the stirring blades are arranged on the stirring shaft, and each of at least one part of the stirring shaft and the stirring blades is arranged in the first cavity.
2. The system for formulating an acylation liquid according to claim 1, wherein the tank body comprises:
the liquid outlet is arranged on the first shell, and the upper end of the first shell is open;
an upper cover hermetically mounted on the first housing, the first housing and the upper cover defining the first chamber, each of the first feed opening, the second feed opening, and the agitation opening being disposed on the upper cover; and
the jacket is sleeved on the first shell and is provided with a first heat exchange medium inlet for the heat exchange medium to enter and a first heat exchange medium outlet for the heat exchange medium to flow out.
3. The system for formulating an acylation liquid according to claim 2, further comprising:
the heating device is provided with a second heat exchange medium inlet and a second heat exchange medium outlet, the first heat exchange medium outlet is connected with the second heat exchange medium inlet, and the first heat exchange medium inlet is connected with the second heat exchange medium outlet;
the kettle body is provided with a temperature measuring port communicated with the first cavity, one part of the temperature sensor is inserted in the temperature measuring port in a sealing manner, 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.
4. The system for formulating an acylation liquid according to claim 2, further comprising a suction filtration device, the suction filtration device comprising:
the filtering device comprises a second shell and a filtering membrane, the second shell defines a second chamber, the filtering membrane is arranged in the second chamber, the filtering membrane divides the second chamber into a first part and a second part, the second shell is provided with a filtering device inlet and a filtering device outlet which are communicated with the second chamber, 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, the third shell limits a third chamber, the third shell is provided with a liquid storage tank inlet and a liquid storage tank outlet, and the liquid storage tank inlet is communicated with the filtering device outlet; and
and the vacuum pumping pump is provided with a first vacuum pumping port, a second vacuum pumping port communicated with the third chamber is arranged on the third shell, and the first vacuum pumping port is communicated with the second vacuum pumping port.
5. The system for preparing acylation liquid according to claim 4, wherein the first housing, the second housing and the third housing are of an integrated structure, wherein the liquid outlet is disposed at the bottom of the first housing, the inlet of the filtering device is disposed at the top of the second housing, the filtering device is disposed at the bottom of the kettle, the outlet of the filtering device is disposed at the bottom of the second housing, the inlet of the liquid storage tank is disposed at the top of the third housing, and the liquid storage tank is disposed at the bottom of the filtering device.
6. A method for preparing an acylation liquid, which is carried out using the system for preparing an acylation liquid according to any one of claims 1 to 5, characterized by comprising the steps of:
a. weighing a 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 as to dissolve the Lewis catalyst weighed in the step a 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 to obtain an acylated solution.
7. The method for preparing acylation liquid according to claim 6, wherein the solvent is nitrobenzene, and the step b is:
firstly, adding nitrobenzene into the first chamber through the first feeding 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 simultaneously stirring by using the stirrer at 200-400 rpm so as to dissolve the Lewis catalyst weighed in the step a to obtain a mixed solution.
8. The method for preparing an acylation liquid according to claim 6, further comprising a step d of subjecting the acylation liquid obtained in the step c to suction filtration treatment by a suction filtration device under an inert gas atmosphere so as to obtain a filtered acylation liquid.
9. The method for preparing an acylation liquid according to claim 6, wherein in the step c, the addition speed of the acylation agent is 3 drops to 10 drops per second, and the stirring speed of the stirrer is 200rpm to 400 rpm.
10. The method for preparing an acylation liquid according to claim 6, wherein the molar mass ratio of the acylating agent to the Lewis catalyst is (1.1-1.5) to (1.3-1.7); and/or
The molar mass ratio of the Lewis catalyst to the solvent is (1.3-1.7): 5.
CN202111075055.5A 2021-09-14 2021-09-14 System and method for preparing acylation liquid Active CN113842857B (en)

Priority Applications (4)

Application Number Priority Date Filing Date Title
CN202111075055.5A CN113842857B (en) 2021-09-14 2021-09-14 System and method for preparing acylation liquid
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

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202111075055.5A CN113842857B (en) 2021-09-14 2021-09-14 System and method for preparing acylation liquid

Publications (2)

Publication Number Publication Date
CN113842857A true CN113842857A (en) 2021-12-28
CN113842857B CN113842857B (en) 2023-08-29

Family

ID=78974167

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202111075055.5A Active CN113842857B (en) 2021-09-14 2021-09-14 System and method for preparing acylation liquid

Country Status (1)

Country Link
CN (1) CN113842857B (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114230447A (en) * 2021-12-31 2022-03-25 河南豫辰药业股份有限公司 Continuous flow preparation method of 4' -fluoro-2-phenylacetophenone
WO2023040641A1 (en) * 2021-09-14 2023-03-23 煤炭科学技术研究院有限公司 Acylation solution and process method for continuously synthesizing acyl naphthalene using acylation solution

Citations (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1999019288A1 (en) * 1997-10-13 1999-04-22 Quest International B.V. Improvements in or relating to friedel-crafts reactions
CN104096388A (en) * 2014-07-28 2014-10-15 湘潭大学 Method used for directly separating catalyst from solid-liquid phase reacting system
CN104292198A (en) * 2014-09-27 2015-01-21 安徽金禾实业股份有限公司 Grignard hydrolysis two-phase separation synthesis method and device in maltol production
CN205288404U (en) * 2015-12-22 2016-06-08 江西省欧陶科技有限公司 Novel main equipment of water -reducing agent production
CN205965855U (en) * 2016-08-30 2017-02-22 石清元 Thiosemicarbazides class germicide synthesizer
CN107020061A (en) * 2017-06-02 2017-08-08 江苏中天科技股份有限公司 A kind of mini-plant of silicium cathode material strong acid alkali process
CN206661208U (en) * 2017-04-10 2017-11-24 铜仁学院 A kind of heterogeneous catalytic reaction separation coupling device
CN108745252A (en) * 2018-07-09 2018-11-06 北京市计量检测科学研究院 A kind of micro Nano material preparation facilities
CN110947313A (en) * 2018-09-26 2020-04-03 湘潭微动农业发展有限公司 Washing article production facility
CN211462268U (en) * 2019-12-26 2020-09-11 广东也乐新材料制造有限公司 Vacuum suction filtration integrated device
CN211586558U (en) * 2019-10-31 2020-09-29 杭州颖泰生物科技有限公司 Acylation washing cauldron
CN211964172U (en) * 2020-03-26 2020-11-20 浙江新诺高分子材料有限公司 A multi-functional reation kettle for preparation of ageing-resistant polyurethane resin
CN212882440U (en) * 2020-07-23 2021-04-06 新亚强硅化学股份有限公司 High-refractive-index phenyl silicone resin synthesis device

Patent Citations (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1999019288A1 (en) * 1997-10-13 1999-04-22 Quest International B.V. Improvements in or relating to friedel-crafts reactions
CN104096388A (en) * 2014-07-28 2014-10-15 湘潭大学 Method used for directly separating catalyst from solid-liquid phase reacting system
CN104292198A (en) * 2014-09-27 2015-01-21 安徽金禾实业股份有限公司 Grignard hydrolysis two-phase separation synthesis method and device in maltol production
CN205288404U (en) * 2015-12-22 2016-06-08 江西省欧陶科技有限公司 Novel main equipment of water -reducing agent production
CN205965855U (en) * 2016-08-30 2017-02-22 石清元 Thiosemicarbazides class germicide synthesizer
CN206661208U (en) * 2017-04-10 2017-11-24 铜仁学院 A kind of heterogeneous catalytic reaction separation coupling device
CN107020061A (en) * 2017-06-02 2017-08-08 江苏中天科技股份有限公司 A kind of mini-plant of silicium cathode material strong acid alkali process
CN108745252A (en) * 2018-07-09 2018-11-06 北京市计量检测科学研究院 A kind of micro Nano material preparation facilities
CN110947313A (en) * 2018-09-26 2020-04-03 湘潭微动农业发展有限公司 Washing article production facility
CN211586558U (en) * 2019-10-31 2020-09-29 杭州颖泰生物科技有限公司 Acylation washing cauldron
CN211462268U (en) * 2019-12-26 2020-09-11 广东也乐新材料制造有限公司 Vacuum suction filtration integrated device
CN211964172U (en) * 2020-03-26 2020-11-20 浙江新诺高分子材料有限公司 A multi-functional reation kettle for preparation of ageing-resistant polyurethane resin
CN212882440U (en) * 2020-07-23 2021-04-06 新亚强硅化学股份有限公司 High-refractive-index phenyl silicone resin synthesis device

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
刘亮等: "2-甲基萘酰基化反应研究", 《化学工业与工程》 *
李文鹏: "微通道反应器中2-甲基萘酰基化反应制备2-甲基-6-酰基萘的研究", 《中国优秀硕士学位论文库 工程科技Ⅰ辑》 *
王沛等: "2-甲基6-酰基萘的合成", 《大连海事大学学报》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2023040641A1 (en) * 2021-09-14 2023-03-23 煤炭科学技术研究院有限公司 Acylation solution and process method for continuously synthesizing acyl naphthalene using acylation solution
CN114230447A (en) * 2021-12-31 2022-03-25 河南豫辰药业股份有限公司 Continuous flow preparation method of 4' -fluoro-2-phenylacetophenone

Also Published As

Publication number Publication date
CN113842857B (en) 2023-08-29

Similar Documents

Publication Publication Date Title
CN113842857A (en) System and method for preparing acylation liquid
CN106237966B (en) The reactor of production aromatic aldehyde is aoxidized for toluene substance
CN105597651B (en) A kind of nitromethane flow reactor
CN107021889B (en) A kind of preparation method and device of aromatic chlorinated object
KR20020003867A (en) Device and method for producing molten salts and use thereof
CN215610889U (en) System for preparing acylation liquid
CN106423027A (en) Production device and production method for sodium dimethyl dithiocarbamate
CN111018907A (en) Continuous kettle type industrial production method and system for crude acetal product
CN206701265U (en) A kind of ammoniacal liquor storage device for ammonium chloride crystals device
CN201693180U (en) Modified device for stirring sodium for reduction to prepare tantalum powder with potassium fluotantalate
CN208526585U (en) A kind of glassed steel reaction vessels
CN211329360U (en) 1, 4-dihydroxy anthraquinone production is with concentrated extraction device
CN211078479U (en) Lithium hexafluorophosphate reactor
CN109081772A (en) A kind of technique and device effectively improving the chloro- 3,5- xylenol chlorination reaction production efficiency of 4-
CN215654853U (en) Device for preparing acylation liquid
CN201693181U (en) Device for preparing tantalum powder from potassium fluotantalate by sodium reduction in stirring manner
CN208394791U (en) Electrocatalytic oxidation impurity removing equipment
CN216630821U (en) Reation kettle is used in glycerin chlorohydrin production
CN110180480A (en) The reaction unit of water nano macromolecular automobile coating
CN214346377U (en) Reation kettle ejection of compact cooling device
CN211358530U (en) Automobile-used urea agitating unit
CN100432082C (en) Synthesis method of chloro diisopropyl phosphine
CN210620664U (en) Continuous production equipment for 5-nitro salicylic acid
CN213172612U (en) Production device for medicine methyl cyanocarbamate
CN214131627U (en) Luteolin purification reaction kettle

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant