JPH01249131A - Gas feeder - Google Patents

Abstract

PURPOSE:To ease the handling of a corrosive gas by injecting an inert liq. from an ejector to suck the gas, separating the inert liq. discharged from the ejector and the gas, and supplying the separated inert liq. to the ejector. CONSTITUTION:The inert liq. such as perfluorotrihexylamine is injected from the ejector 1 to suck the gas such as gaseous fluorine. The inert liq. discharged from the ejector 1 and the gas are separated by a gas-liquid separator 2. The inert liq. separated in the separator 2 is supplied to the ejector 1 by a feeder 3. The ejector 1, separator 2, and feeder 3 are connected to one another to form a closed circuit. Thus gas feeder has no movable parts at the contact part with the gas. As a result, such trouble as the device corrosion and leakage of gas due to corrosion is hardly caused even when a corrosive gas is handled, and the maintenance of the feeder is also facilitated.

Description

DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention relates to a gas supply device particularly suitable for supplying hazardous gases having toxic, corrosive, or flammable properties.

(Prior art and problems to be solved by the invention) Gases such as phosgene, fluorine, hydrogen heptadide, chlorine, and sulfur dioxide gas are compounds useful as raw materials for chemical reactions and as etching gases in semiconductor manufacturing processes. It is. However, these gases have the disadvantage that they are difficult to handle because they are toxic or corrosive.

As devices for supplying gas into a reactor, devices such as blowers and compressors are known. When supplying the above-mentioned gases with these devices, special consideration must be given to preventing gas leakage when selecting devices. Furthermore, daily operation and maintenance must be done with great care. Therefore, there has been a desire for a device to safely supply the above-mentioned hazardous gases.

(Means for Solving the Problem) The present inventors have developed a device for safely and durablely supplying the above-mentioned hazardous gas that is difficult to handle. As a result, they succeeded in developing a gas supply device that satisfies the above objectives by using an ejector, a pump, and a gas-liquid separator, and completed the present invention. an ejector that injects and sucks gas; a gas-liquid separator that separates the gas from the inert liquid discharged from the nitrogen and lid; and a gas-liquid separator that separates the inert liquid separated by the gas-liquid separator. This is a gas supply device in which supply machines that supply the lid are connected to each other to form a closed circuit.

The present invention will be described below with reference to the accompanying drawings.

FIG. 1 schematically shows the gas supply device of the present invention. The ejector 1, the gas-liquid separator 2, and the inert liquid supply device 3 are connected to each other to form a closed circuit.

Niji. A gas suction pipe 4 is connected to the lid 1.
A gas discharge pipe 5 is connected to the gas-liquid separator 2 . The inert liquid supplied to the lid 1 by the feeder 3 is injected into the lid 1, thereby causing suction I.
Gas is sucked from i#4. The inert liquid and gas mixed in the ejector 1 are separated in the gas-liquid separator 2,
Gas is exhausted from the exhaust pipe 5. The above gas-liquid separator 2 may have a reflux condenser as required. On the other hand, the inert liquid is sent to the supply machine 3 and then supplied to the ejector 1 again. In this way, the inert liquid circulates within the closed circuit, while the gas sucked into the ejector 1 is discharged from the gas-liquid separator 2. The gas supply amount and supply pressure can be determined by selecting the ejector and supply device.

Since the humidity of the inert liquid that is circulated within the closed circuit generally increases, it is preferable to provide an inert liquid cooler 6 at any position within the closed circuit as shown in FIG.

The inert liquid used in the present invention may be any liquid that does not decompose or react on contact with gas and has a sufficiently low viscosity at the operating temperature. Also,
It is difficult to completely prevent the inert liquid from being discharged together with the gas discharged from the gas supply device of the present invention. Therefore, when the gas supplied by the gas supply device of the present invention is used for the reaction, it is preferable that the inert liquid is inert during the reaction process as well.

In order to increase the effect of gas suction through the lid, lid, and lid, it is preferable that the liquid has a somewhat high boiling point and a low vapor pressure at the operating temperature. For example, when used near room temperature, it is usually preferable to have a boiling point of 50° C. or higher. Such liquids vary depending on the type of gas to be supplied, but silicon compounds such as various silicone oils and fluorosilicone oils; compounds such as hydrocarbons, amines, ethers, and polyethers with hydrogen atoms of 7
Fluorine compounds substituted by only one atom or by a fluorine atom and a chlorine atom are preferred. Particularly suitable are fluorine compounds in which all hydrogen atoms in the molecule are replaced by only fluorine atoms or by fluorine atoms and chlorine atoms. Inert liquids that can be suitably used in the present invention include tetrachlorodifluoroethane (trade name: 70n 112);
)! Examples include low polymers of J fluorochloroethylene, perfluoroperhydro-7 enantrene, perfluorotributylamine, perfluorotripentylamine, perfluoroalkyl sulfur compounds, various perfluoro-oligoethers, and the like.

Furthermore, although the device of the present invention can be used for supplying any gas, it is particularly suitable for supplying hazardous gases that are toxic, corrosive, flammable, and the like. For example, phosgene, chlorine, 7
Tsunium, sulfur dioxide gas, hydrogen sulfide, hydrogen chloride, hydrogen fluoride,
ozone, oxygen, nitrogen dioxide, phosphine, hydrazine,
It is used for silane, cibotane, germane, arsine, nitrogen trifluoride, trichlorosilane, phosphorus penta7tside, arsenic pentathide, uranium hexafluoride, tungsten hexafluoride, etc.

The gas supply device of the present invention is particularly suitable as a supply device for fluorine gas, which is particularly corrosive and has high reactivity to various substances. In this case, it is preferable to use a perfluoro compound containing no hydrogen atoms as the inert liquid. In addition, as for the materials of the ejector, piping, etc., those having sufficient corrosion resistance such as stainless steel, iron, diylene, monel, and fluororesin are used.

The present invention also provides an inert liquid manufacturing apparatus having the above-described gas supply device.

That is, a reaction system that includes an ejector that injects an inert liquid and sucks a gas, and a reaction that separates the inert liquid and gas discharged from the tube and lid, and produces an inert liquid using the gas as a raw material. This is an inert liquid manufacturing apparatus in which a reactor and a supply device that supplies the inert liquid separated or produced in the reactor to the ejector are connected to each other to form a closed circuit.

FIG. 2 shows a schematic diagram of an inert liquid manufacturing apparatus. The inert liquid production device uses a reactor for producing an inert liquid in place of the gas-liquid separator of the gas supply device described above. The reactor 7 has a function of separating the inert liquid and gas discharged from the ejector 1.

Further, in the reactor 7, an inert liquid is produced by a reaction between the separated gas and an organic compound that is separately supplied. The inert liquid separated or produced in the reactor is supplied to the ejector 1 again by the supply device 3. The inert liquid circulating within the closed circuit is appropriately taken out of the system.

Preferably, the outlet 8 to the outside of the system is provided between the reactor 7, the feeder 3, and the nitrogen lid 1.

(Effects) The gas supply device of the present invention has a simple structure and has no movable parts in the portion that comes into contact with gas. Therefore, even when corrosive gases are handled, problems such as equipment corrosion and gas leakage due to corrosion are less likely to occur. Furthermore, maintenance of the device is easy.

In addition, in an inert liquid manufacturing device in which the above gas supply device is applied to inert liquid manufacturing, the inert liquid to be manufactured is
It is used to supply gases that are raw materials for inert liquids, and can safely and stably supply hazardous gases over long periods of time.
Inert liquids can also be produced stably.

(Examples) Examples are given below to explain the present invention in more detail, but the present invention is not limited to these Examples.

Example 1 Perfluorotrihexylamine was used as the inert liquid, and fluorine gas was supplied using the gas supply apparatus shown in FIG.

By circulating approximately 3001 perfluorotrihexylane at a rate of 2.5 mJ/hour between an ejector, a gas-liquid separator, and a feeder, fluorine gas at room temperature and pressure is sucked into the gas. Fluorine gas is discharged from the discharge pipe at a pressure of 3
by/c! G could be supplied at a rate of 0.751v/hour.

Note that the temperature of perfluorotrihexylamine in the ejector was 40°C. At this time, the discharge pressure of the feeder was 7 to 8 kg/cJ G, and the pressure on the gas inlet side of the ejector was -0.15 kg/c+yfG.

After two months of operation, we were able to stably supply fluorine gas and no damage was observed to the equipment. In addition, perfluorotrihexylamine was analyzed, but no decomposition or alteration was observed.
For the purpose of blowing kg/crd G into the chlorination reactor, the gas supply apparatus of the present invention shown in FIG. 1 was used with perfluorotrihexylamine as the working liquid.

By circulating approximately 3001 perfluorotrihexylamine between the ejector, gas-liquid separator, and feeder at a rate of 2♂/hour, 15N+x of chlorine gas was produced.
could be fed at a rate of J/hour. Note that the temperature of perfluorotrihexylamine in a part of the ejector was 45°C. At this time, the discharge pressure of the feeder is 3
~4 to 9/cda, the pressure on the suction side of the lid is -
It was 0.9 kg/crl G.

After two months of operation, we were able to stably supply chlorine gas and no damage was observed to the equipment. In addition, an analysis of perfluorotrihecylyazine was conducted, but no decomposition or alteration was found.

Example 3 Fluorine gas was supplied using the apparatus shown in FIG. 2 to fluorinate a partially fluorinated product obtained by electrolytic fluorination of tributylamine.

The same rainbow, lid, feeder, and cooler as in Example 1 were used. As a reactor, a packed tower made of Niranal, which had a reflux condenser at the top and was filled with a nickel Raschig ring, was used.

A ram with a capacity of 25 C) Il is directly connected to the bottom of this column, and the perfluorotributylamine that accumulates there is circulated through a cooler and an ejector under the conditions shown in Example 1. was suctioned and fed from the bottom of the reaction tower, and the electrolytic fluorinated product was fed quantitatively from the top. Note that the reaction mixture was diluted by blowing fluorine gas into the center of the reaction tower. The temperature of the reaction tower was adjusted to -140°C by heating from the outside. As a result, the target product Bar 7A/otributylamine could be obtained from the tank. Also, it could be operated stably for a long time.

[Brief explanation of the drawing]

FIG. 1 is a schematic diagram of the gas supply device of the present invention, and FIG.
The figure is a schematic diagram of an inert liquid manufacturing apparatus of the present invention. In the figure, l is an ejector, 2 is a gas-liquid separator, 3 is a feeder, 4 is a gas g&pipe, 5 is a gas discharge pipe, 6 is a cooler, 7 is a reactor, and 8 is an inert liquid Each outlet is shown.

Claims (2)

[Claims] (1) An ejector that injects an inert liquid and sucks gas, a gas-liquid separator that separates the inert liquid and gas discharged from the ejector, and an inert liquid separated by the gas-liquid separator. A gas supply device comprising supply machines that supply gas to the ejector and are connected to each other to form a closed circuit. (2) An ejector that injects an inert liquid and sucks a gas, a reactor that separates the inert liquid and gas discharged from the ejector, and produces an inert liquid using the gas as a raw material, and the reaction An apparatus for producing an inert liquid, wherein supply machines for supplying the inert liquid separated or produced by the ejector to the ejector are connected to each other to form a closed circuit.