Safe production technique for manufacturing high-purity phosphine on large scale

A technology for phosphine trihydrogen and safe production, applied in the direction of sustainable manufacturing/processing, chemical industry, phosphine, etc., to achieve the effect of reducing the entry of impurities

Inactive Publication Date: 2014-09-24
李达刚 +3
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008]Technical problem to be solved by the present invention: the purpose of the present invention is to provide a kind of safe method for large-scale production of high-purity phosphine trihydrogen in order to overcome the above deficiencies in the prior art The production process can not only produce high-purity phosphine trihydro

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  • Safe production technique for manufacturing high-purity phosphine on large scale

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] The processing steps of adopting above device to produce phosphine trihydride are as follows:

[0032] (1) Preparation for driving:

[0033] a) The low-temperature and low-pressure trapping purifier 8 is put into liquid nitrogen to keep its dehydration tank at -60°C and its storage tank at -150°C.

[0034] b) Put 6000 grams of aluminum phosphide powder into hopper 1, and use high-purity N 2 Replace to oxygen content <3PPM.

[0035] c) Inject deionized water into the first-stage reactor 3 and the second-stage reactor 4 to the overflow port, and start stirring.

[0036] (2) The reaction to produce phosphine trihydride:

[0037] a) Raise the temperature of the first-stage reactor 3 and the second-stage reactor 4 to 50°C, and start the vacuum pump 10 to control the first-stage reactor 3, the second-stage reactor 4 and the third-stage reactor 5 to 500-550mmHg.

[0038] b) Start the screw solid feeder 2, and feed aluminum phosphide with a purity greater than 85% into the ...

Embodiment 2

[0076] Adopt the safe production process device of large-scale preparation of phosphine trihydrogen of embodiment 1 to prepare phosphine trihydrogen, control the vacuum degree of the three-stage series reactor to be 500-600mmHg, wherein the first-stage reactor 3, the second-stage reactor 4 The temperature is 45-55°C, the temperature of the third-stage reactor 5 is 25°C, and the operating condition of the low-temperature and low-pressure trapping purifier 8 is an operating pressure of 500-600mmHg; operating temperature: purifier: -55°C; receiver: - 100°C; trap: -155°C, other control conditions are the same as in Example 1. The yield of the solid-state phosphorus trihydride trapped by the cryogenic trap is calculated by the same method as in Example 1: between 88-91% (weight).

Embodiment 3

[0078] The safety production process device of the large-scale preparation of high-purity phosphine trihydrogen in Example 1 is used to prepare phosphine trihydrogen,

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Abstract

The invention discloses a safe production technique for manufacturing high-purity phosphine on large scale. Aluminum phosphide and deionized water or zinc phosphide and acetic acid used as raw materials are subjected to sealed solid feeding, negative-pressure three-stage cascade reactor reaction, low-temperature low-pressure trapping purification, tail gas oxidation trivalent phosphorus removal, and absorption of phosphorus pentoxide by alkali liquor and activated charcoal under closed reaction conditions. The technique can simultaneously satisfy the four requirements of capability of large-scale industrial manufacturing from laboratories to industrialization, control on the virulent phosphine in air in the production workshop and surrounding environment to be lower than allowable concentration, no intricate corrosion problem in equipment, and high product purity, and provides a safe and reliable production technique for industrial production.

Description

technical field [0001] The present invention relates to a safe and reliable process for industrially manufacturing high-purity trihydrogen phosphine, in particular to provide a large-scale manufacturing of high-purity trihydrogen phosphine that can completely eliminate the potential safety hazards of the operation site and surrounding space for large-scale continuous manufacturing of phosphonane. Safe production process of phosphine hydride. Background technique [0002] Phosphonane, scientific name phosphorus trihydrogen, molecular formula: PH 3 Low boiling point (-132.5°C). Highly toxic, the specific gravity of the gaseous state is close to that of air, it is very easy to cause neurotoxicity in humans, and it is spontaneously combustible and explosive. This is the main ingredient of the will-o'-the-wisps that are common in cemeteries. The allowable concentration in the air is 0.2PPM. [0003] Phospanes are used in a wide variety of applications and are often used as a...

Claims

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Application Information

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IPC IPC(8): C01B25/06
CPCY02P20/10
Inventor 李达刚李松
Owner 李达刚
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