JP2002079078A - Microwave chemical reactor - Google Patents

Abstract

PROBLEM TO BE SOLVED: To enable a correct temperature measurement and the control of a reaction temperature by measuring directly the temperature of a reaction vessel and simultaneously during reaction in a microwaves chemical reactor, and to provide a technology which enables the direct, simultaneous measurement of the change in optical properties during the reaction by optical analysis equipment, etc. SOLUTION: In the chemical reaction apparatus by microwave-heating, in order to control a reaction temperature, etc., a metallic device such as a thermocouple is inserted into the reactor to be approximately perpendicular to the TE mode microwave electric field of a microwave electromagnetic field.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

The present invention relates to a method and an apparatus for managing and controlling the temperature of a chemical reaction in a microwave electromagnetic field. The present invention also relates to a method and an apparatus for confirming a state of a chemical reaction in a microwave electromagnetic field by optical characteristics and managing and controlling the reaction.

[0002]

2. Description of the Related Art When it is desired to know the temperature inside a reaction vessel in a microwave heating chemical reaction apparatus, a non-contact type thermometer such as an infrared radiation thermometer or an optical fiber thermometer or a non-metallic device is used from outside the reaction vessel. Temperature measurement method has been performed.
However, according to such a method, there are almost no cases where a non-contact type thermometer cannot be used at all depending on the type of the reaction tank, or where accurate temperature measurement cannot be performed due to an atmosphere such as steam or gas generated from the reaction tank. It is. As a method of measuring the temperature in the reaction system, a method of externally measuring the temperature while avoiding the microwave irradiation part is generally known.However, since the temperature measurement point is not in the reaction part, it can be said that it is appropriate for control. Not something. On the other hand, when a metal device such as a thermocouple was inserted into the microwave electromagnetic field, abnormal heating occurred, the cable portion was discharged, and satisfactory measurement could not be performed.

[0003] In addition, it has been considered that visual observation and measurement by an optical device cannot be performed in the vicinity of a microwave irradiation part due to a problem of microwave shielding.

[0004]

SUMMARY OF THE INVENTION The object of the present invention is to solve such problems because the temperature and optical characteristics of a reaction vessel cannot be directly and continuously measured in a microwave heating chemical reactor. I have.

[0005]

SUMMARY OF THE INVENTION The present invention relates to the installation of a metallic device such as a thermocouple for measuring the temperature or the like of a reaction vessel in a microwave heating chemical reaction apparatus. Surprisingly, accurate temperature measurement can be performed without abnormal heating or electric discharge of metallic equipment such as thermocouples by inserting it so as to be almost orthogonal to the electric field of the microwave electromagnetic field TE mode microwave. I understood. The present invention relates to a method and an apparatus that can easily manage and control the temperature of a chemical reaction in a microwave electromagnetic field.

According to the present invention, in order to confirm the state of a chemical reaction, a window having a size such that microwaves do not leak is formed in a part of the waveguide, and the reaction vessel is made to pass through a reaction vessel made of a light-transmitting material. The present invention relates to a method and apparatus for managing and controlling a reaction by simultaneously measuring optical characteristics during an internal reaction step visually or by an optical analyzer such as visible light, infrared spectroscopy, and ultraviolet light.

[0007]

The present invention will be described in detail below with reference to embodiments. The parts in the examples are shown on a weight basis.

Embodiment 1 As shown in FIG. 1, an apparatus comprising a magnetron 1 and a waveguide 2 and a non-reflection terminator 3 is further provided. After the reaction tank 5 is inserted into the reflection tank installation hole and set in the waveguide 2, a stirring blade 6 connected to a stirrer 7 and a thermometer 8 such as a thermocouple can be inserted. A thermometer 8 such as a thermocouple is connected to an electromagnetic wave control measuring device and an electromagnetic wave control device 9 from which the output of the magnetron 1 is controlled. As shown in the side view of FIG. 2, the waveguide 2 is provided with a window 11 on one side or both sides for measuring optical characteristics during reaction.
As shown in FIG. 3, a metal material such as a thermocouple is inserted so as to be substantially orthogonal to the electric field 12 of the microwave of the TE mode single mode.

A test tube was used as a reaction vessel, and 256 parts of phthalidinitrile and 80 parts of copper sulfate were added to ethylene glycol 10
In addition to 000 parts, set at the reaction tank installation position shown in FIG. 1.6 mm diameter covered with stirring blades and metal
1 is inserted as shown in FIG. The thermocouple is connected to a measuring device for electromagnetic wave control, so that the output of the magnetron can be controlled according to the temperature instruction in the reaction condition setting condition. As reaction conditions, the temperature was raised from room temperature to 130 ° C. in 2 minutes, further raised to 160 ° C. in 2 minutes, then raised to 170 ° C. in 2 minutes,
The temperature condition for holding for 5 minutes was set in the control device.

After the stirring is started, 2.45 GHz, 50
Irradiation with a 0 W TE-wave single-mode microwave gave no abnormal heating of the thermometer or discharge of the cable. When the temperature inside the reaction tank was measured with an installed thermometer, the temperature could be controlled according to the set conditions, and the crude copper phthalocyanine (CI Pigment Blue 1) was used.
5: 3) was obtained. In addition, the state in which the reaction solution changes from colorless to blue is set in the optical property confirmation window 1 opened in the waveguide.
It was possible to confirm visually from 1.

Example 2 Using the same apparatus and test tube as in Example 1, 592 parts of phthalic anhydride, 960 parts of urea, 105 parts of cuprous chloride, 80 parts of titanium tetrachloride and 30 parts of 4-sulfophthalic acid To 6000 parts of sulfolane, and set at the reaction tank installation position shown in FIG. A 1.6 mm diameter alumel chromel thermocouple covered with a stirring blade and metal is inserted as shown. The thermocouple is connected to a measuring device for electromagnetic wave control, so that the output of the magnetron can be controlled according to the temperature instruction in the reaction condition setting condition. A non-contact type color manager is set in the optical characteristic confirmation window 11 attached to the waveguide. As the reaction conditions, a temperature condition in which the temperature was raised from room temperature to 190 ° C. in 15 minutes and maintained at 190 ° C. for 20 minutes was set in the control device.

After starting the stirring, 2.45 GHz, 15
Irradiation with a 00W TE-wave single-mode microwave did not cause abnormal heating of the thermometer or discharge of the cable. When the temperature inside the reaction tank was measured with a thermometer installed, the temperature could be controlled according to the set conditions, and crude copper phthalocyanine (CI Pigment Blue 1) was used.
5: 3) was obtained. The change in the color of the reaction solution was measured by a non-contact color controller set in the optical property confirmation window 11, and the state of colorless to blue change could be confirmed as a colorimetric value.

Example 3 Using the same apparatus and test tube as in Example 1, 240 parts of polyphosphoric acid and 40 parts of 2,5-bis (phenylamino) terephthalic acid were added to the reaction tank shown in FIG. set. A 1.6 mm diameter alumel chromel thermocouple covered with a stirring blade and metal is inserted as shown. The thermocouple is connected to a measuring device for electromagnetic wave control, so that the output of the magnetron can be controlled according to the temperature instruction in the reaction condition setting condition. As reaction conditions, the temperature was raised from room temperature to 200 ° C. for 2 minutes, and 200 ° C.
Was set in the control device for 5 minutes.

After the stirring is started, 2.45 GHz, 50
Irradiation with a 0 W TE-wave single-mode microwave gave no abnormal heating of the thermometer or discharge of the cable. When the temperature inside the reaction tank was measured with an installed thermometer, the temperature could be controlled according to the set conditions, and crude quinaclodone (CI Pigment Violet 1) was used.
9) was obtained. Further, a change in the color of the reaction solution could be confirmed from the optical property confirmation window 11 opened in the waveguide.

[0015]

As described above, the present invention enables accurate temperature measurement and control of the reaction temperature by directly and simultaneously measuring the temperature of the reaction tank in the microwave heating chemical reaction apparatus during the reaction. It is made possible. Further, it is possible to directly and simultaneously measure a change in optical characteristics during the reaction using an optical analyzer or the like during the reaction.
Direct simultaneous measurement of not only visible light but also infrared spectroscopy and ultraviolet light becomes possible, and the state at the time of reaction can be analyzed and measured on the spot.

[Brief description of the drawings]

FIG. 1 is a sectional view illustrating a heating chemical reaction temperature measurement control device in a microwave electric field according to the present invention.

FIG. 2 is a side view of a chemical reaction device in a microwave electric field according to the present invention and an explanatory diagram of a window for confirming optical characteristics.

FIG. 3 is a schematic electric field of a TE mode single-mode microwave and a cross-sectional view of a reactor in a waveguide cross section of a chemical reaction apparatus in a microwave electric field according to the present invention.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 1 Magnetron 2 Waveguide 3 Non-reflection terminator 4 Reaction tank installation hole 5 Reaction tank 6 Stirrer blade 7 Stirrer 8 Thermometer 9 Electromagnetic wave control measuring device and control device 10 Data recording measuring device 11 Optical characteristic confirmation window 12 TE Schematic electric field of a single-wave microwave

 ──────────────────────────────────────────────────続 き Continuing on the front page (72) Inventor Kazuchika Ota 1-15-4, Tsukiiri Ueda City (72) Inventor Itsuo Yamaura 1112-1-2 Suwagata, Ueda City (72) Inventor Taizo Oshima Miyagi, Adachi-ku, Tokyo 1-1-25-1 Sumika Color Co., Ltd. Tokyo factory F-term (reference) 2G054 BB13 CB03 CE01 EA10 FA10 FA12 FA16 FA37 GA03 GB01 GB04 3K086 AA07 AA10 BB02 CA02 CB04 FA09 FA10 3K090 LA00 PA00 4G057 AD01 4G075 AA01A CA26 EA01 EB21 FC04 FC20

Claims (2)

[Claims] In a chemical reaction apparatus using microwave heating, a metallic device such as a thermocouple is inserted into a reaction vessel, and a metallic device such as a thermocouple is installed in the microwave to control and control the temperature and the like. A chemical reaction apparatus characterized by being inserted so as to be substantially orthogonal to an electric field of a microwave in a TE mode of an electromagnetic field. 2. A method according to claim 1, wherein a window is opened in a part of the waveguide, and optical characteristics inside the reaction tank are visually or visually confirmed by an optical analyzer through a reaction tank made of a light-transmitting material. Chemical reactor.