TW201506030A - Producing method of organometallic compound - Google Patents

Abstract

A producing method of an organometallic compound is provided. A reactant is firstly provided and the reactant is performed a synthesis reaction in an inert gas. The reactant is consisting of an alkyl halide compound, magnesium and a III group metal. The alkyl halide compound is methyl iodide, methyl bromide, ethyl iodide or ethyl bromide. The III group metal is gallium, indium or aluminum. Trimethyl gallium, triethyl gallium, trimethyl indium, triethyl indium, trimethyl aluminum or triethyl aluminum is synthesized by controlling reaction temperature and reaction pressure.

Description

Method for producing organometallic compounds

The present invention relates to a method of manufacture, and more particularly to a method of making an organometallic compound.

Metal-organic chemical vapor deposition (MOCVD) is commonly used to form compound semiconductor thin films in photovoltaic elements, which are indium gallium arsenide (InGaAsN), indium gallium arsenide (InGaAs), and indium. Films such as gallium phosphorus (InGaP) are the most common.

The raw material of the compound semiconductor film utilizes an organometallic compound as a raw material for vapor phase deposition. The preparation method of a common common organometallic compound (for example, trimethylgallium, triethylgallium, trimethylindium or triethylindium) is prepared by using an ether solvent, a magnesium metal, and a halogenated alkyl compound. Grignard reagent. Then, a Grenner reagent is used to carry out a synthesis reaction with a metal of the above-mentioned raw material (for example, gallium or magnesium or aluminum), or a reaction is carried out by using a Grignard reagent and a metal halide compound (for example, gallium trichloride) to synthesize a corresponding reaction. An organometallic compound.

However, this method takes more than 24 hours, and the reaction requires the addition of a solvent such as an ether to increase the manufacturing cost of the organometallic compound. Moreover, the cost of the metal halide compound of this method is higher, and the raw material cost of the organometallic compound is increased.

In view of the above, it is not necessary to provide a method for producing an organometallic compound to improve the defects of the conventional method for producing an organometallic compound.

Accordingly, an aspect of the present invention provides a method for producing an organometallic compound which utilizes a halogenated alkyl compound, a magnesium metal, and a Group III metal to synthesize an organometallic compound.

According to the above aspect of the invention, an organometallic compound is proposed. In one embodiment, the process provides the reactants and the synthesis reaction is carried out in the presence of an inert gas. The foregoing reactants are composed of a halogenated alkyl compound, a magnesium metal and a group III metal, wherein the halogenated alkyl compound is methyl iodide, methyl bromide, ethyl iodide or ethyl bromide, and the group III metal is a gallium metal, an indium metal or Aluminum metal. The molar number of the group III metal based on the above is 1 mole, and the molar ratio of the halogenated alkyl compound, the magnesium metal and the group III metal is 3:1.5:1 to 6:3:1.

The pressure of the aforementioned synthesis reaction is from 3 atm to 10 atm, the temperature is from 90 ° C to 180 ° C, and the reaction time is from 6 hours to 10 hours. After the reaction is completed, the liquid phase product is separated to obtain an organometallic compound. The organometallic compound is trimethylgallium, triethylgallium, trimethylindium, triethylindium, trimethylaluminum or triethylaluminum, and the yield of the product of the production method It is 55% to 65%.

According to an embodiment of the invention, the inert gas system described above is nitrogen, helium or argon.

The method for producing an organometallic compound of the present invention is carried out by subjecting a halogenated alkyl compound, a magnesium metal and a Group III metal to a synthesis reaction, whereby an organometallic compound can be obtained quickly.

100‧‧‧ method

110‧‧‧ Providing reactants

120‧‧‧Synthesis reaction

130‧‧‧ Purified organometallic compounds

BRIEF DESCRIPTION OF THE DRAWINGS Figure 1 is a flow chart showing a method of producing an organometallic compound according to an embodiment of the present invention.

The making and using of the embodiments of the invention are discussed in detail below. However, it will be appreciated that the embodiments provide many applicable inventive concepts that can be implemented in a wide variety of specific content. The specific embodiments discussed are illustrative only and are not intended to limit the scope of the invention.

The "reactor" as hereinafter referred to as a "reactor" is a reaction vessel which is resistant to high pressure and has a stirring function, and has a temperature control system and a condensation system for controlling the temperature of the method for producing the organometallic compound of the present invention. The reaction synthesizes an organometallic compound.

Please refer to FIG. 1 , which is a flow chart showing a method of manufacturing an organometallic compound according to an embodiment of the present invention. In one embodiment, the method of making an organometallic compound 100 is followed by a step 110 of providing a reactant. The reactants are from halogenated alkyl compounds, magnesium metals and Group III metals. The composition wherein the halogenated alkyl compound is methyl iodide, methyl bromide, ethyl iodide or ethyl bromide, and the group III metal is a gallium metal, an indium metal or an aluminum metal. Based on the above-mentioned Group III metal, the molar number is 1 mole, and the molar ratio of the halogenated alkyl compound, the magnesium metal and the Group III metal in the reactant is 3:1.5:1 to 6:3:1.

Step 120 of the synthesis reaction is then carried out in the presence of an inert gas. In step 120, the above reactant is placed in a reaction vessel under normal temperature and normal pressure (for example, 25 ° C to 1 atm), and heating is started to start the reaction. The pressure of the synthesis reaction is from 3 atm to 10 atm, the temperature is from 90 ° C to 180 ° C, and the reaction is carried out for 6 hours to 10 hours. In one embodiment, the inert gas is nitrogen, helium, argon or other suitable inert gas. In the present invention, the high or low pressure of the synthesis reaction correspondingly shortens or lengthens the reaction time. If the pressure of the synthesis reaction is less than 3 atm, the reaction time will be more than 10 hours, and the manufacturing cost of the organometallic compound is increased. If the aforementioned pressure is more than 10 atm, an excessive pressure causes the reaction to fail to synthesize an organometallic compound.

Further, the synthesis reaction of the present invention is an exothermic reaction, so that the above reaction vessel should pay attention to the heating temperature to avoid uncontrolled reaction, and it is impossible to synthesize an organometallic compound. However, if the reaction temperature is less than 90 ° C, too low a reaction temperature will prolong the reaction time, and increase the time cost of the synthesis reaction, thereby lowering the yield of the reaction. When the reaction temperature is more than 180 ° C, the above-mentioned synthesis reaction tends to cause a side reaction, and a large amount of a gas having a low boiling point is generated, so that an organometallic compound cannot be synthesized.

After the reaction is completed, the liquid phase product in the reaction vessel is separated and subjected to step 130 to purify the organometallic compound and calculate the yield. In an embodiment The organometallic compound is prepared by the above-described production method 100, and the yield of the product is 55% to 65%. Further, an organometallic compound such as trimethylgallium, triethylgallium, trimethylindium, triethylindium, trimethylaluminum or triethylaluminum can be synthesized by the method for producing an organometallic compound of the present invention.

The following examples are used to illustrate the application of the present invention, and are not intended to limit the present invention, and various modifications and refinements can be made without departing from the spirit and scope of the invention.

Example 1

150 ml of methyl iodide, 30 g of magnesium metal and 50 g of gallium metal were placed in a reaction vessel filled with an inert gas to carry out a synthesis reaction, and the temperature of the reaction vessel was controlled not to exceed 120 ° C, and the pressure was not higher than 6 kg. After reacting for 10 hours, the liquid phase product in the reaction vessel was separated, and the above liquid phase product was purified by chemical distillation to obtain trimethylgallium (48.74 g, yield: about 58.96%).

Example 2

225 ml of methyl iodide, 45 g of magnesium metal and 75 g of gallium metal were placed in a reaction vessel filled with an inert gas to carry out a synthesis reaction, and the temperature of the reaction vessel was controlled not to exceed 127 ° C, and the pressure was not higher than 8.5 kg. After reacting for 10 hours, the liquid phase product in the reaction vessel was separated, and the above liquid phase product was purified by chemical distillation to obtain trimethylgallium (68.99 g, yield: about 55.64%).

Example 3

150 ml of methyl iodide, 30 g of magnesium metal and 50 g of gallium metal were placed in a reaction vessel filled with an inert gas to carry out a synthesis reaction, and the temperature of the reaction vessel was controlled not to exceed 122 ° C, and the pressure was not higher than 8.2 kg. After 10 hours of reaction, The liquid phase product in the autoclave was separated and the above liquid phase product was purified by chemical distillation to obtain trimethylgallium (42.62 g, yield: about 51.56%).

Example 4

150 ml of methyl iodide, 30 g of magnesium metal and 50 g of gallium metal were placed in a reaction vessel filled with an inert gas to carry out a synthesis reaction, and the temperature of the reaction vessel was controlled not to exceed 112 ° C, and the pressure was not higher than 6.5 kg. After 12 hours of reaction, the liquid phase product in the reaction vessel was separated, and the above liquid phase product was purified by chemical distillation to obtain trimethylgallium (40.76 g, yield: about 49.31%).

It can be seen from the above embodiments of the present invention that the method for producing the organometallic compound of the present invention has the advantages of using a halogenated alkyl compound, a magnesium metal and a group III metal as a reactant of an organometallic compound, and utilizing high pressure and high temperature reaction conditions and magnesium metal and The high activity of the halide is used for the synthesis reaction of the organometallic compound, and the organometallic compound can be rapidly synthesized.

The present invention has been disclosed in the above embodiments, and is not intended to limit the present invention. Any one of ordinary skill in the art to which the present invention pertains can make various changes without departing from the spirit and scope of the invention. The scope of protection of the present invention is therefore defined by the scope of the appended claims.

100‧‧‧ method

110‧‧‧ Providing reactants

120‧‧‧Synthesis reaction

130‧‧‧ Purified organometallic compounds

Claims (2)

A method for producing an organometallic compound, comprising: providing a reactant, wherein the reactant is composed of a halogenated alkyl compound, wherein the halogenated alkyl compound is methyl iodide, methyl bromide, ethyl iodide or ethyl bromide. a magnesium metal; and a group III metal, wherein the group III metal is a gallium metal, an indium metal or an aluminum metal, and wherein the halogenated alkyl compound, the magnesium metal is based on the molar amount of the group III metal of 1 mole And the molar ratio of the group III metal is from 3:1.5:1 to 6:3:1; in a presence of an inert gas, a synthesis reaction is carried out, wherein the pressure of the synthesis reaction is from 3 atm to 10 atm, a temperature of 90 ° C to 180 ° C, and a reaction time of 6 hours to 10 hours; and separation of a liquid phase product to obtain the organometallic compound, wherein the organometallic compound is trimethylgallium, triethylgallium, trimethylindium And triethylindium, trimethylaluminum or triethylaluminum, and wherein the yield of the product of one of the methods for producing the organometallic compound is from 55% to 65%. The method for producing an organometallic compound according to claim 1, wherein the inert gas system is nitrogen, helium or argon.