Distillation process of metal organic source

A metal-organic source and rectification technology, applied in the fields of organic chemistry, fractionation, distillation and separation, etc., can solve the problems of long time consumption and low single yield, and achieve the goal of reducing workload, reducing required amount and reducing enterprise cost. Effect

Inactive Publication Date: 2017-09-01
安徽亚格盛电子新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The whole process route takes a long time and the single yield is low

Method used

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  • Distillation process of metal organic source

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Effect test

Embodiment 1

[0020] Such as figure 1 As shown, this embodiment provides a rectification process of metal-organic sources. PLC controls the rectification of trimethylgallium in intermittent heat-tracing pulse exhaust exhaust gas. The specific steps are as follows:

[0021] Gradient heating: After the start-up inspection is completed, 125kg of crude trimethylgallium is fed, and heating is started under the protection of high-purity nitrogen. , at 5°C / h, the temperature was raised to 70°C, and then at a temperature gradient of 2°C / h until the system achieved reflux.

[0022] Intermittent heat tracing total reflux removal of impurities: the first time the pressure difference between the top and bottom of the rectification column reaches 0.04bar as the total reflux mark, start to calculate the starting point of total reflux; the setting of PLC intermittent heat tracing is: the pressure difference between the top and bottom of the rectification column reaches 0.04bar, Stop the heat conduction o...

Embodiment 2

[0027] Such as figure 1 As shown, this embodiment provides a rectification process for metal-organic sources. PLC controls the rectification of triethylgallium in intermittent heat-tracing pulse discharge tail gas. The specific steps are as follows:

[0028] Gradient heating: After the start-up inspection is completed, 80kg of crude triethylgallium is fed, and the system pressure is controlled to 250torr under the condition of high-purity nitrogen protection, and heating is started. After reaching the set temperature, raise the temperature to 95°C at 5°C / h, and then use a temperature gradient of 2°C / h until the system achieves reflux (105-110°C).

[0029] Intermittent heat tracing total reflux removal of impurities: the first time the pressure difference between the top and bottom of the rectification column reaches 14Torr as the total reflux mark, start to calculate the starting point of total reflux; Heat conduction oil; when the differential pressure drops to 10bar, PLC co...

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Abstract

The invention provides a rectification process of metal-organic sources. Controlled by PLC, the rectification process of gradient temperature rise, intermittent heat-following total reflux, impurity removal, front fraction collection and product collection is completed. It has wide applicability and most metal-organic sources Compound purification, as long as the crude product contains impurity components with a lower boiling point than the product, it is applicable to this process condition; the invention effectively improves the separation efficiency of impurities in the rectification process, reduces the required amount of the fraction before containing impurities, and improves the efficiency of single rectification. The yield is 3-15%; the degree of automation is high, which greatly reduces the required workload, which is helpful to reduce the cost of the enterprise and control the process stability.

Description

technical field [0001] The invention relates to the field of metal-organic source manufacturing, in particular to a rectification process for metal-organic sources. Background technique [0002] Metal-organic sources (such as: trimethylgallium (TMG), triethylgallium (TEG), trimethylindium (TMIn) and trimethylaluminum (TMAl)) are widely used as the main raw materials in the MOCVD epitaxy industry Solid-state lighting LEDs, semiconductor lasers, high-performance transistors and high-efficiency solar cells. Since the product purity requires high electronic grade 6N (99.9999%), the purification process of the production enterprise generally adopts complex purification and rectification tower distillation. For the purification of complexes, amines, ethers, and high-boiling organic compounds are generally used as ligands, and the relatively volatile impurities in the crude product are removed through a vacuum system. The rectification in the rectification column separates the pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/00B01D3/14B01D3/32B01D3/42
CPCC07F5/00B01D3/14B01D3/32B01D3/4205
Inventor 王伟俞冬雷宣宗亮刘喜
Owner 安徽亚格盛电子新材料有限公司
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