CN105905937A

CN105905937A - Process for removing trace chlorine gas in gallium trichloride

Info

Publication number: CN105905937A
Application number: CN201610256992.3A
Authority: CN
Inventors: 赵毅; 裴凯; 计燕秋; 刘颖
Original assignee: Dalian Kelide Optoelectronic Materials Co Ltd
Current assignee: Dalian Kelide Optoelectronic Materials Co Ltd
Priority date: 2016-04-25
Filing date: 2016-04-25
Publication date: 2016-08-31
Anticipated expiration: 2036-04-25
Also published as: CN105905937B

Abstract

The invention relates to a process for purifying gallium trichloride; in the process, an end point of a reaction is determined by excess chlorine gas, and then the excess chlorine gas is consumed by adding metal gallium back to remove chlorine impurities; the process comprises the process steps: adding 500 g-3000 g of the metal gallium into a reaction kettle, at the reaction temperature of 180 DEG C, introducing chlorine gas, and carrying out a reaction; and when gallium trichloride is reacted to the end point, namely, a reaction solution is pale yellow green, stopping introduction of the chlorine gas, opening nitrogen gas purging, adding 1.0 g-2.0 g of metal gallium to the reaction kettle, and continuing to maintain 180 DEG C until the reaction solution turns from yellow green to colorless. In the process, the end point of the reaction is determined by excess chlorine gas, and then the excess chlorine gas is consumed by adding the metal gallium back to remove the chlorine impurities, so that the content of the chlorine gas impurities in the gallium trichloride is decreased to 1 ppm or less, and the product yield is high.

Description

A kind of remove the technique of trace chlorine in gallium trichloride

Technical field

The present invention relates to the purifying process of a kind of gallium trichloride, a kind of remove the technique of trace chlorine in gallium trichloride, belong to chemical technology field.

Background technology

Owing to gallium trichloride production technology using chlorine react, the reaction mechanism mechanism of reaction generates gallium trichloride after gallium dichloride transition, is changed by color in the judgement of reaction end and judges, when color by colourless become pistac time, i.e. reaction reaches terminal, and now chlorine is the most excessive.So often containing trace chlorine in gallium trichloride product, and the chlorine of trace can cause product colour the most yellow.In the actual application of electronic grade high-purity gallium trichloride, chlorine is a kind of objectionable impurities, and therefore the requirement to chlorine content is typically less than 1ppm.

For the requirement that touches the mark, the most mostly select to use rectifying column to carry out rectification and purification, but owing to chlorine has certain solubility, simple rectification and purification to be extremely difficult to purify requirement in gallium trichloride.

Summary of the invention

The defect existed in view of above-mentioned technology, it is an object of the invention to provide and a kind of remove the technique of trace chlorine in gallium trichloride, make the excessive chlorine contained in gallium trichloride be reduced to 1ppm once so that it is index reaches the requirement of electronic grade high-purity gallium trichloride.

The technical scheme is that and a kind of remove the technique of trace chlorine in gallium trichloride, this technique is to judge reaction end by chlorine excess, consume unnecessary chlorine remove chlora matter by the anti-gallium that adds again, its processing step is: put into 500g-3000 g gallium in reactor, reaction temperature is 180 DEG C, logical chlorine reaction, when gallium trichloride is reacted to terminal, i.e. reactant liquor present pistac time, stop being passed through chlorine, unlatching nitrogen purges, the gallium of 1.0g-2.0g is added in reactor, and continue to keep 180 DEG C until reactant liquor is become colourless by yellow green.The present invention be former by color on the basis of judging terminal, then in reactor, add minimal amount of gallium, make reactant liquor color become again more colourless, consume unnecessary chlorine.Because gallium trichloride differs bigger with the boiling point of its intermediate state monochlor(in)ate gallium and gallium dichloride, just can well be separated by simple decompression distillation, the most both before ensureing, the gallium total overall reaction in reactor generates gallium trichloride, and unnecessary chlorine is consumed.It is possible not only to ensure that product has the highest yield by the method, also ensure that the purity requirement of product.

The beneficial effects of the present invention is: this technique is to judge reaction end by chlorine excess, then consume unnecessary chlorine remove chlora matter by the anti-gallium that adds, make chlorine impurity content in gallium trichloride be reduced to below 1ppm, and have the highest product yield.

Detailed description of the invention

Below in conjunction with specific embodiment, the present invention is described in detail to use the different gallium trichloride purification experiment of chlorine content.

Embodiment 1 :

Put into 500g gallium, 180 DEG C, lead to chlorine reaction.When gallium trichloride is reacted to terminal, i.e. reactant liquor present pistac time, stop being passed through chlorine, open nitrogen purging, in reactor, add the gallium of 1.0g, and continue to keep 180 DEG C until reactant liquor is become colourless by yellow green.

After before purification, chlorine content contrast is as follows:

	Chlorine content (ppm)
		Chlorine excess	15.8
After adding gallium	0.4

Embodiment 2 :

Put into 1000g gallium, 180 DEG C, lead to chlorine reaction.When gallium trichloride is reacted to terminal, i.e. reactant liquor present pistac time, stop being passed through chlorine, open nitrogen purging, in reactor, add the gallium of 1.0g, and continue to keep 180 DEG C until reactant liquor is become colourless by yellow green.

After before purification, chlorine content contrast is as follows:

	Chlorine content (ppm)
		Chlorine excess	20.5
After adding gallium	0.6

Embodiment 3 :

Put into 3000g gallium, 180 DEG C, lead to chlorine reaction.When gallium trichloride is reacted to terminal, i.e. reactant liquor present pistac time, stop being passed through chlorine, open nitrogen purging, in reactor, add the gallium of 2.0g, and continue to keep 180 DEG C until reactant liquor is become colourless by yellow green.

After before purification, chlorine content contrast is as follows:

	Chlorine content (ppm)
		Chlorine excess	18.6
After adding gallium	0.5

Claims

1. remove the technique of trace chlorine in gallium trichloride for one kind, it is characterized in that, this technique is to judge reaction end by chlorine excess, consume unnecessary chlorine remove chlora matter by the anti-gallium that adds again, its processing step is: put into 500g-3000 g gallium in reactor, reaction temperature is 180 DEG C, logical chlorine reaction, when gallium trichloride is reacted to terminal, i.e. reactant liquor present pistac time, stop being passed through chlorine, unlatching nitrogen purges, the gallium of 1.0g-2.0g is added in reactor, and continue to keep 180 DEG C until reactant liquor is become colourless by yellow green.