CN105731525A - Preparation method of gallium trichloride granules - Google Patents
Preparation method of gallium trichloride granules Download PDFInfo
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- CN105731525A CN105731525A CN201410773154.4A CN201410773154A CN105731525A CN 105731525 A CN105731525 A CN 105731525A CN 201410773154 A CN201410773154 A CN 201410773154A CN 105731525 A CN105731525 A CN 105731525A
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- gallium trichloride
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- trichloride
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Abstract
The invention relates to the technical field of gallium trichloride synthesis and discloses a preparation method of gallium trichloride granules. The preparation method includes the steps of: 1) moving gallium trichloride in a glove box, controlling the contents of water and oxygen in the glove box to be lower than 5 ppm, and increasing the temperature to melt the gallium trichloride; 2) adding the molten gallium trichloride dropwisely in liquid nitrogen in the glove box; 3) solidifying the molten gallium trichloride to obtain spherical or spherical-like gallium trichloride granules. The preparation method is simple in process steps, employs low-cost and easy-to-obtain raw materials, is free of introduction of impurities and can prepare regular spherical granules. These regular spherical granules have strong flowability, are not adhered on wall of a container, are very easy to move and apply, and are very easy to control in addition amount.
Description
Technical field
The present invention relates to gallium trichloride synthesis technical field, the preparation method being specifically related to a kind of gallium trichloride granule.
Background technology
Class water gallium trichloride molecular formula: GaCl3, character: colorless needle crystals, density: 2.47g/cm3(25 DEG C), fusing point: 78 DEG C, boiling point: 201.3 DEG C, easy deliquescence, oxidizable, soluble in water, benzene, carbon tetrachloride and Carbon bisulfide can be dissolved in.Gallium trichloride is produced typically via gallium and chlorine direct reaction, or is produced by hydrogen chloride and Digallium trioxide reaction at 200 DEG C.Gallium trichloride is the catalyst for spectrum analysis and organic reaction, for synthesizing the important source material of Organogallium reagent.
When gallium trichloride prepares, it is colorless needle crystals, and its preparation and post processing need to operate when anhydrous and oxygen-free, and it has very strong corrosivity, and most macromolecular material, stainless steel material, Organic substance are had very strong corrosivity.Owing to the mobility of needle-like or pulverous gallium trichloride is very poor, it is easy to adhere on the wall, operate very inconvenient in transfer, application process；And needs are applied after being heated, and so will also result in the problems such as temperature height, bad control addition.Therefore, gallium trichloride being granulated, the application making gallium trichloride is convenient, is that this area is needed badly and solved the technical problem that.
Summary of the invention
For above-mentioned Problems existing, the invention provides a kind of spherical or class is spherical, the preparation method of the gallium trichloride granule of good fluidity, this preparation method is simple to operate, save energy, industrialized production is easily achieved, can make gallium trichloride on application operating convenient effectively.
The present invention for achieving the above object, takes techniques below scheme to be achieved:
The preparation method of a kind of gallium trichloride granule, comprises the following steps:
(1) gallium trichloride moving into glove box, in control glove box, water, oxygen content are respectively less than 5ppm, heat up and make gallium trichloride melt；
(2) in described glove box, melted gallium trichloride liquid is added drop-wise in liquid nitrogen；
(3) after described melted gallium trichloride droplet solidification, spherical or that class is spherical gallium trichloride granule is obtained.
Preferably, the described glove the temperature inside the box of step (1) is 90～150 DEG C.
Preferably, step (1) described intensification makes gallium trichloride melted particularly as follows: gallium trichloride moves in constant pressure funnel, adds heat fusing by heating and temperature controlling device；
Being maintained in the dropping liquid process of step (2) gallium trichloride liquid does not solidify.
Preferably, the described melted gallium trichloride liquid of step (2) is added drop-wise in liquid nitrogen by constant pressure funnel.
Melted gallium trichloride liquid is slowly added drop-wise in liquid nitrogen by constant pressure funnel by this step equably, average speed be 1～2 per second, so can give the cooled and solidified time that the gallium trichloride drop oozed is enough.
Preferably, described liquid nitrogen is contained in Dewar tank.
Preferably, step (3), particularly as follows: described melted gallium trichloride droplet settling 5 to 15 minutes, is poured out upper strata liquid nitrogen, after the volatilization completely of remaining liquid nitrogen, is obtained spherical or that class is spherical gallium trichloride granule after solidification.
Preferably, in described glove box, the gallium trichloride granule obtained is sieved, obtain particle diameter gallium trichloride granule between 1～6mm.
Preferably, sieving described in screen cloth is polytetrafluoro screen cloth.
Owing to stainless steel mesh is had corrosiveness by gallium trichloride itself, but under inert conditions the screen cloth of stainless steel is affected less, therefore the embodiment of the present invention both can be selected the screen cloth of stainless steel, the screen cloth of polytetrafluoro material can also be chosen, preferred polytetrafluoro screen cloth in the present invention.
Preferably, the productivity of described gallium trichloride granule is 90%.
Compared with prior art, beneficial effects of the present invention is as follows:
(1) present invention process step is simple, and cheaper starting materials is easy to get, and obtains more regular spheroidal particle.These are spherical or the spherical gallium trichloride mobility of particle of class strong, will not adhere on the wall, and in transfer, application process, operation is very easy, and addition also controls very well.
(2) present invention will not introduce impurity in operation, it is ensured that the purity of product.
Detailed description of the invention
It is an object of the invention to provide a kind of spherical or class is spherical, the preparation method of the gallium trichloride granule of good fluidity, this preparation method is simple to operate, save energy, industrialized production is easily achieved, can make gallium trichloride on application operating convenient effectively.
The concrete grammar that the present invention prepares gallium trichloride granule is as follows:
(1) gallium trichloride is moved into glove box, control water, oxygen content in glove box and be respectively less than 5ppm, gallium trichloride is moved in constant pressure funnel, by heating and temperature controlling device the gallium trichloride in constant pressure funnel being heated makes it melt, and is maintained in ensuing dropping liquid process gallium trichloride liquid and does not solidify；
(2) being added drop-wise in liquid nitrogen by melted gallium trichloride liquid by constant pressure funnel in glove box, controlling rate of addition is 1 to 2 per second；
(3) after the gallium trichloride droplet solidification melted, spherical or that class is spherical gallium trichloride granule is obtained.
The heating-up temperature in glove box in step (1) is 90～150 DEG C.
In step (2), liquid nitrogen is contained in Dewar tank.
The gallium trichloride droplet settling that step (3) melts five to ten five minutes, pours out upper strata liquid nitrogen, after the volatilization completely of remaining liquid nitrogen, obtains spherical or that class is spherical gallium trichloride granule.
In glove box, the gallium trichloride granule obtained being sieved, controlling screen cloth diameter is 6mm, obtains particle diameter gallium trichloride granule between 1～6mm.Screen cloth can be polytetrafluoro screen cloth or stainless steel mesh.
In the present invention, the productivity of gallium trichloride granule is 90%.
Below in conjunction with specific embodiment, the present invention is further illustrated.
Embodiment 1
Weigh 40g gallium trichloride needle powder crystal and be put in borosilicate glass bottle, borosilicate glass bottle is put in glove box, control water in glove box, oxygen content is respectively less than 5ppm, be adjusted to 150 DEG C make the gallium trichloride in bottle melt borosilicate glass bottle heating by adding hot jacket.The gallium trichloride melted is transferred in constant pressure funnel.Open constant pressure funnel to be dripped to by gallium trichloride drop equipped with, in the degree crock of liquid nitrogen, settling five to ten five minutes, pour out upper strata liquid nitrogen, after waiting the volatilization completely of remaining liquid nitrogen, bottom degree crock, obtain the spherical shape gallium trichloride granule of tens.
Embodiment 2
Weigh 100g gallium trichloride needle powder crystal and be put in borosilicate glass bottle, borosilicate glass bottle is put in glove box, control water, oxygen content in glove box and be respectively less than 5ppm, then the gallium trichloride in bottle is transferred in constant pressure funnel.By heating and temperature controlling device the gallium trichloride in constant pressure funnel being heated makes it melt, and controlling heating-up temperature is 90～150 DEG C, and is maintained in ensuing dropping liquid process gallium trichloride and does not solidify.Open constant pressure funnel and gallium trichloride drop is dripped to equipped with in the degree crock of liquid nitrogen according to the speed of one to two per second, settle about ten minutes, pour out upper strata liquid nitrogen, after waiting the volatilization completely of remaining liquid nitrogen, bottom degree crock, obtain the spherical shape gallium trichloride granule of 90g.
Embodiment 3
Weigh 200g gallium trichloride needle powder crystal and be put in borosilicate glass bottle, borosilicate glass bottle is put in glove box, control water, oxygen content in glove box and be respectively less than 5ppm, then the gallium trichloride in bottle is transferred in constant pressure funnel.By heating and temperature controlling device the gallium trichloride in constant pressure funnel being heated makes it melt, and is maintained in ensuing dropping liquid process gallium trichloride and does not solidify.Open constant pressure funnel to be dripped to by gallium trichloride drop equipped with, in the degree crock of liquid nitrogen, settling about ten minutes, pour out upper strata liquid nitrogen, after waiting the volatilization completely of remaining liquid nitrogen, bottom degree crock, obtain the spherical shape gallium trichloride granule of 180g.The granule obtained is sieved by glove box, chooses the polytetrafluoro screen cloth that sieve diameter is 6mm and screen, obtain 150g particle diameter spherical shape gallium trichloride granule between 1～6mm.
Compared with prior art, beneficial effects of the present invention is as follows:
(1) present invention process step is simple, and cheaper starting materials is easy to get, and obtains more regular spheroidal particle.These are spherical or the spherical gallium trichloride mobility of particle of class strong, will not adhere on the wall, and in transfer, application process, operation is very easy, and addition also controls very well.
(2) present invention will not introduce impurity in operation, it is ensured that the purity of product.
The technical scheme above embodiment of the present invention provided is described in detail, principle and the embodiment of the embodiment of the present invention are set forth by specific case used herein, and the explanation of above example is only applicable to help to understand the principle of the embodiment of the present invention；Simultaneously for one of ordinary skill in the art, according to the embodiment of the present invention, all will change in detailed description of the invention and range of application, in sum, this specification content should not be construed as limitation of the present invention.
Claims (9)
1. the preparation method of a gallium trichloride granule, it is characterised in that comprise the following steps:
(1) gallium trichloride moving into glove box, in control glove box, water, oxygen content are respectively less than 5ppm, heat up and make gallium trichloride melt；
(2) in described glove box, melted gallium trichloride liquid is added drop-wise in liquid nitrogen；
(3) after described melted gallium trichloride droplet solidification, spherical or that class is spherical gallium trichloride granule is obtained.
2. the preparation method of a kind of gallium trichloride granule according to claim 1, it is characterised in that the described glove the temperature inside the box of step (1) is 90～150 DEG C.
3. the preparation method of a kind of gallium trichloride granule according to claim 1, it is characterised in that step (1) described intensification makes gallium trichloride melted particularly as follows: gallium trichloride moves in constant pressure funnel, adds heat fusing by heating and temperature controlling device；
Being maintained in the dropping liquid process of step (2) gallium trichloride liquid does not solidify.
4. the preparation method of a kind of gallium trichloride granule according to claim 1, it is characterised in that the described melted gallium trichloride liquid of step (2) is added drop-wise in liquid nitrogen by constant pressure funnel.
5. the preparation method of a kind of gallium trichloride granule according to claim 1, it is characterised in that described liquid nitrogen is contained in Dewar tank.
6. the preparation method of a kind of gallium trichloride granule according to claim 1, it is characterized in that, step (3) is particularly as follows: described melted gallium trichloride droplet settling 5 to 15 minutes, upper strata liquid nitrogen is poured out after solidification, after the volatilization completely of remaining liquid nitrogen, obtain spherical or that class is spherical gallium trichloride granule.
7. the preparation method of a kind of gallium trichloride granule according to claim 1, it is characterised in that in described glove box, the gallium trichloride granule obtained is sieved, obtains particle diameter gallium trichloride granule between 1～6mm.
8. the preparation method of a kind of gallium trichloride granule according to claim 7, it is characterised in that described in sieve with screen cloth be polytetrafluoro screen cloth.
9. the preparation method of a kind of gallium trichloride granule according to claim 1, it is characterised in that the productivity of described gallium trichloride granule is 90%.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410773154.4A CN105731525A (en) | 2014-12-12 | 2014-12-12 | Preparation method of gallium trichloride granules |
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| CN201410773154.4A CN105731525A (en) | 2014-12-12 | 2014-12-12 | Preparation method of gallium trichloride granules |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114210259A (en) * | 2021-11-15 | 2022-03-22 | 广东先导微电子科技有限公司 | Gallium trichloride granulation packaging device and method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004075507A (en) * | 2002-08-09 | 2004-03-11 | Yamanaka Hutech Corp | Method of manufacturing granular gallium trichloride |
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- 2014-12-12 CN CN201410773154.4A patent/CN105731525A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004075507A (en) * | 2002-08-09 | 2004-03-11 | Yamanaka Hutech Corp | Method of manufacturing granular gallium trichloride |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114210259A (en) * | 2021-11-15 | 2022-03-22 | 广东先导微电子科技有限公司 | Gallium trichloride granulation packaging device and method |
| CN114210259B (en) * | 2021-11-15 | 2023-10-24 | 广东先导微电子科技有限公司 | Gallium trichloride granulating and packaging device and method |
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Application publication date: 20160706 |