JPH05317602A - Method for reaction and concentration of chemical substance and flask for rotary evaporator used therefor - Google Patents

Abstract

PURPOSE:To easily increase the reaction and concentration efficiency, to easily detach a flask after the process and to clean the flask by providing a freely detachable baffle in the flask for a rotary evaporator and rotating the flask. CONSTITUTION:A baffle 11 consists of a support 12 and a blade 13, and the blade 13 is screw-joined to the support 12. The total length of the baffle 11 is made shorter than the inner diameter of a spherical flask, the baffle is inserted into the flask, passed through the center of the flask and horizontally placed, the screw joint of the blade 13 is loosened, the inner surface of the flask is pressed, and a return nut 14 is fastened to fix the flask. The flask is heated and rotated in a thermostatic bath to agitate a material to be treated by the baffle.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for reacting and concentrating chemical substances, and a rotary evaporator flask used therefor.

[0002]

2. Description of the Related Art A rotary evaporator is used for chemical reaction or concentration of a product in the production of chemicals, and the flask is a spherical glass flask in consideration of chemical corrosion resistance. Is used. The rotary evaporator is usually set and operated as shown in FIG. Ie flask 1
The object to be treated is placed inside and set on the constant temperature bath 2, and the drive unit 3
The chemical reaction and concentration are carried out while rotating. It is generally more efficient to carry out the chemical reaction and concentration while stirring the material to be treated. In particular, the effect of stirring is remarkable when a solid substance is contained in the object to be treated.

On the other hand, a spherical glass flask has a smooth inner surface so that the liquid can slide smoothly, and even if the flask is rotated, the object to be treated is hardly stirred. As a method to solve this, it is possible to make the inner surface of the flask uneven, or to install a separate stirrer, but the former has difficulty in manufacturing the flask and the problem of strength, and the latter is airtight. There is a technical problem such as maintenance of.

As a result of various investigations aimed at improving the reaction and concentration efficiency in the rotary evaporator, the inventors of the present invention have found that the desired effect can be obtained by providing a removable baffle plate in the flask. The present invention has been completed. That is, the present invention is a reaction and concentration method of a chemical substance, characterized in that a removable baffle is fixed in the flask of a rotary evaporator, and the object to be treated is agitated by rotating the flask. It is a flask for rotary evaporator, which has a baffle detachably attached inside.

The present invention will be specifically described below. FIG. 1 is a sectional view of an example of a baffle plate according to the present invention, and FIG. 2 is A- of FIG.
A sectional view and FIG. 3 are sectional views of a glass spherical flask to which the baffle plate 1 is attached. The baffle plate 11 is composed of a support portion 12 and a blade portion 13, and the blade portion 13 is screwed to the support portion 12. In FIG. 1, each of the blade portions 13 has four
Although it has a single blade, the number of blades is arbitrary, and any material may be used for the baffle plate as long as it satisfies heat resistance, chemical corrosion resistance and the like.

In order to attach such a baffle plate to the flask, the blade portion 13 is screwed into the support portion 12 so that the total length of the baffle plate is shorter than the inner diameter of the flask, and this is inserted into the flask, and the flask is inserted. The blade 13 is pressed against the inner surface 1 ′ of the flask by loosening the screwing of the vane 13 at the horizontal position passing through the center and the return nut 14 is tightened and fixed. Using such a flask, reaction of chemical substances,
For concentration, there is no difference from the usual method except that the amount of the object to be processed is adjusted so that the tip of the baffle plate comes into contact with the object to be processed in advance.

That is, the flask is set as shown in FIG. 4, and the flask is rotated while being heated to a constant temperature in a constant temperature bath. At this time, when one end of the baffle plate is located at the lowest position, the water level of the object to be treated may be higher than the tip of the baffle plate. By doing so, the workpiece is stirred by the baffle as the flask rotates.

[0008]

According to the present invention, the reaction and concentration efficiency can be improved by a simple means of providing a removable baffle in the flask, and the reaction and concentration steps can be easily removed and washed.

[0009]

[Experimental Example] An experimental example is shown below to clarify the effect of the present invention. Industrial rotary evaporator PRE-100E (made by Shibata Scientific Instruments Co., Ltd.) similar to that shown in FIG.
A polypropylene baffle similar to that shown in Fig. 1 was fixed to a glass spherical flask (100 L capacity), and the
Add 40 L of% saline and rotate at a rotation speed of 3 in a constant temperature bath at 60 ° C.
The solution was concentrated under reduced pressure at 5 rpm and an absolute pressure of 20 mmHg, and the residual liquid amount was measured over time. As a control, vacuum concentration was carried out in the same manner as above except that no baffle plate was attached. The results are shown in Table 1. The numerical value in the table is the residual liquid amount (L).

[0010]

[0011]

[Brief description of drawings]

FIG. 1 is a sectional view of an example of a baffle plate according to the present invention.

FIG. 2 is a sectional view taken along line AA of FIG.

FIG. 3 is a cross-sectional view of a glass spherical flask to which a baffle plate 1 is attached.

FIG. 4 is an explanatory diagram of a rotary evaporator.

[0012]

[Explanation of reference signs] 1 Flask 2 Constant temperature bath 3 Drive part 4 Cooler 11 Baffle plate 12 Support part 13 Blade part 14 Return nut

 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Tadashi Tomikura, 339 Noda, Noda, Chiba Prefecture, Kikkoman Corporation (72) Inventor, Yosumi Furuhashi, 339, Noda, Chiba Prefecture, Kikkoman Corporation

Claims (2)

[Claims] 1. A method for reacting and concentrating chemical substances, characterized in that a removable baffle is fixed in the flask of a rotary evaporator, and the object to be treated is stirred by rotating the flask. 2. A flask for a rotary evaporator in which a baffle is detachably provided in a spherical flask.