JP2002095956A - Method for introducing hygroscopic or solidifiable powdery raw material into reaction tank - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a method for introducing a hygroscopic or solidifiable powdery raw material into a reaction tank, in which operability is good. SOLUTION: In the method for introducing the hygroscopic or solidifiable powdery raw material, in the case of collectively or dividedly introducing the powdery raw material which absorbs moisture or is easily solidified by vapor existing in the gas phase of a reaction tank, into the same from a hopper provided in the upper part of the reaction tank, the inside of the hopper is made to a pressurized state by dry gas.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for introducing a powdery raw material into a reaction vessel, and more particularly, to a powdery raw material (hereinafter referred to as "powder material") which is easily absorbed or solidified by steam present in a gas phase portion of the reaction vessel.
(Referred to as a moisture-absorbing or solidifying powder raw material) into a reaction tank.

[0002]

2. Description of the Related Art Conventionally, when a moisture-absorbing or solidifying powdery raw material is introduced into a reaction tank from a hopper above the reaction tank, nitrogen gas or the like is conventionally introduced into the gas phase of the hopper. (See FIG. 2). However, when the vapor pressure of a reaction solvent such as water or an organic solvent is high, the powder raw material present at the lower part of the hopper becomes wet with the vapor of the reaction solvent, and the fluidity of the powder decreases, which is the worst case. In such a case, there has been a problem that the raw material agglomerated by consolidation causes a bridging phenomenon, and the operability is significantly deteriorated.

[0003]

Means for Solving the Problems The inventors of the present invention have conducted intensive studies to provide a method of collectively or dividedly introducing a moisture-absorbing or caking powder material into a reaction tank with good operability. It has been found that the above-mentioned problems can be solved by setting the pressure to a value, and the present invention has been completed. That is, the present invention provides a method for introducing a powder material which is easily absorbed or solidified by the vapor present in the gas phase part of the reaction tank into the reaction tank collectively or separately from a hopper installed above the reaction tank. Another object of the present invention is to provide a method for introducing a hygroscopic or solidified powdery raw material, wherein the inside of the hopper is pressurized by a dry gas.
Hereinafter, the present invention will be described in detail.

[0004]

BEST MODE FOR CARRYING OUT THE INVENTION The method of the present invention can be suitably carried out using, for example, a powder introducing apparatus shown in FIG. The powder introduction device, a hopper (1) installed above the reactor, a control valve (2) attached with a pressure gauge (5), and,
It consists of a powder material introduction valve (3) at the bottom of the hopper. First, a powder raw material (7) is supplied to a hopper from a pipe (not shown) via a supply valve (4). At this time, a dry gas such as an inert gas such as nitrogen or argon or a dehumidified air is supplied through the control valve with a pressure gauge, and the inside of the hopper (1) is always pressurized by the dry gas. When the moisture-absorbing or solidifying powdery raw material is introduced in batch or dividedly, the introduction valve (3) is opened, but also in this case, the dry gas is supplied through the control valve with a pressure gauge, and the pressure in the gas phase of the hopper reacts. Since the pressure is maintained higher than the gas phase of the tank, the vapor of the gas phase of the reaction tank is prevented from entering the upper hopper. At this time, the difference between the pressure of the gas phase of the hopper and the pressure of the gas phase of the reaction tank is preferably in the range of 0.1 to 0.3 atm. Further, even when the pressure in the reaction tank is higher than the atmospheric pressure, the pressure in the hopper can be set higher than the pressure in the reaction tank. Furthermore, even for powders that have relatively poor fluidity and a low rate of introduction into the reaction tank,
The introduction speed can be increased by pressurizing the inside of the hopper. The method of the present invention is suitably used when dividing and introducing a powder raw material into a reaction tank.

[0005] The moisture-absorbing or solidifying powdery raw material is not particularly limited as long as it is used as a raw material for a chemical reaction. For example, a reaction reagent such as an inorganic compound or an organic compound, a catalyst, or the like may be used. , Salting-out agents, neutralizing agents and the like. The method of the present invention is suitably used particularly when a catalyst whose fluidity is deteriorated due to moisture absorption, for example, ferric chloride, anhydrous aluminum chloride or the like is introduced into a reaction tank.

[0006]

According to the method of the present invention, a moisture-absorbing or caking powder material can be introduced into a reaction tank from a hopper with good operability.

[0007]

DESCRIPTION OF THE PREFERRED EMBODIMENTS Using the apparatus shown in FIG.
The reaction described in Reference Example 2 of JP-A No. 4 was carried out. In the reaction tank,
2810 parts by weight of tribromoacetaldehyde and 1500 parts by weight of petroleum ether were charged and mixed. 1680 parts by weight of isobutene were gradually introduced into the resulting mixture at about -5 ° C. At about -5 ° C, anhydrous aluminum chloride powder 13
0 parts by weight was added in several portions, and the mixture was stirred at about -5 ° C for 5 hours. Since crystals were precipitated with the progress of the reaction, diethyl ether was added at the latter stage of the reaction, and the mixture was stirred in a solution state at room temperature for 30 minutes. 2000 parts by weight of water was added to the obtained reaction solution,
The organic layer was separated, concentrated by a conventional method, and distilled under reduced pressure to obtain 2
870 parts by weight of 1,1,1-tribromo-4-methyl-
4-penten-2-ol was obtained. The anhydrous aluminum chloride powder did not deteriorate in fluidity due to moisture absorption by the vapor of the reaction solvent during the above-mentioned divisional addition.

[Brief description of the drawings]

FIG. 1 shows an apparatus used in an embodiment of the present invention.

FIG. 2 shows a conventional device.

[Explanation of symbols]

1. hopper, 2. control valve with pressure gauge, 3. powder introduction valve, 4. powder supply valve, 6. reaction tank, 7. powder,
2 '・ ・ On-off valve

Claims (3)

[Claims] (1) When a powder material which is easily absorbed or solidified by steam present in a gas phase portion of a reaction tank is introduced into the reaction tank collectively or separately from a hopper installed above the reaction tank,
A method for introducing a hygroscopic or solidified powdery raw material, wherein the inside of a hopper is pressurized by a dry gas. 2. The method according to claim 1, wherein the pressure difference between the gas phase of the hopper and the gas phase of the reaction tank is in the range of 0.1 to 0.3 atm. 3. The powdery raw material is a hygroscopic catalyst.
Or the method of 2.