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Process for preparing tetramethylolphosphonium chloride by catalyzing phosphines with copper chlorides

A technology of tetrakis hydroxymethyl phosphorus chloride and phosphine, which is applied in the new process field of preparation of flame retardant THPC by the high-efficiency liquid phase catalytic oxidation of phosphine by copper chloride

Inactive Publication Date: 2015-06-03
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Considering the catalytic characteristics of the catalyst and the difficulty of separating the product THPC from the catalyst, no catalyst is currently used in the industrial production of THPC, and the conversion rate of phosphine is 60% to 70%. Therefore, it is necessary to find a catalyst that is efficient and easy to separate from the product in the reaction. To improve the conversion rate of phosphine and the separation degree of catalyst and product

Method used

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  • Process for preparing tetramethylolphosphonium chloride by catalyzing phosphines with copper chlorides

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Experimental program
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Effect test

Embodiment 1

[0015] Embodiment 1: the technique that this cupric chloride catalyzes phosphine to prepare tetrakis hydroxymethyl phosphorus chloride, specific content is as follows:

[0016] First feed nitrogen to purge the reaction system for 30 minutes, then mix the gas of nitrogen and phosphine through flow meter I 1 and flow meter II 3 and then pass it into the reaction system. The concentration of phosphine gas in the mixed gas is 500,000ppm. Add 38% formaldehyde and 38% hydrochloric acid to the absorption reactor 4 and mix evenly. The molar ratio of formaldehyde and hydrochloric acid is 4:1. The amount of copper chloride added as catalyst is 0.05g / g formaldehyde. Phosphine gas is chlorinated The copper catalyst reacts with formaldehyde and hydrochloric acid in the absorption reactor, and the gas after the reaction is further absorbed by the concentrated sulfuric acid in the exhaust gas absorption bottle 5 and then discharged. At 45°C, the space velocity is 200h -1 Under these conditi...

Embodiment 2

[0017] Embodiment 2: the technique that this cupric chloride catalyzes phosphine to prepare tetrakis hydroxymethyl phosphorus chloride, specific content is as follows:

[0018] Purge the reaction system with nitrogen for 25 minutes, mix nitrogen and phosphine gas into the reaction system, the concentration of phosphine gas in the mixed gas is 150,000ppm, add 36% formaldehyde and 37% hydrochloric acid into the absorption reactor respectively Mix evenly, the molar ratio of formaldehyde and hydrochloric acid is 4.25:1, and the amount of catalyst copper chloride added is 0.1g / g formaldehyde, and the phosphine gas reacts with formaldehyde and hydrochloric acid in the absorption reactor through the action of copper chloride catalyst. The final gas is further absorbed by the concentrated sulfuric acid in the waste gas absorption bottle and then discharged. At 50°C, the space velocity is 150h -1 Under these conditions, the conversion rate of phosphine is 99%. After the reaction, th...

Embodiment 3

[0019] Embodiment 3: the technique that this cupric chloride catalyzes phosphine to prepare tetrakis hydroxymethyl phosphorus chloride, specific content is as follows:

[0020] Introduce nitrogen to purge the reaction system for 20 minutes to discharge the air, and mix nitrogen and phosphine gas into the reaction system. The concentration of phosphine gas in the mixed gas is 300,000ppm, and 30% formaldehyde and 31% hydrochloric acid are respectively Add it into the absorption reactor and mix evenly. The molar ratio of formaldehyde and hydrochloric acid is 4.5:1, and the amount of catalyst copper chloride added is 0.25g / g formaldehyde. Phosphine gas reacts with formaldehyde in the absorption reactor through the copper chloride catalyst. , Hydrochloric acid reaction, the gas after the reaction is further absorbed by the concentrated sulfuric acid in the waste gas absorption bottle and then discharged. At 65°C, the space velocity is 100h -1 Under these conditions, the conversio...

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Abstract

The invention discloses a process for preparing a fire retardant which is tetramethylolphosphonium chloride (THPC) by catalyzing and oxidizing high-concentration phosphine gas with copper chlorides. The process comprises the following steps of: effectively preparing the fire retardant THPC by using the copper chlorides as unsupported catalysts, and catalyzing the high-concentration phosphine gas with formaldehyde and hydrochloric acid with the copper chlorides under protection of nitrogen and by action of carrier gas. Due to high-efficiency catalysis properties of the process, the conversion ratio of phosphines is up to 99 %, and the THPC can be effectively separated from the catalysts. Compared with the conventional industrial production of THPC, the phosphines can be fully absorbed by primary catalytic oxidation so as to reduce the yield of the waste phosphine gas; and a primary absorber just is arranged so as to increase convenience in technological operations and reduce investment cost.

Description

technical field [0001] The invention belongs to the field of flame retardant tetrakishydroxymethylphosphine chloride (THPC) production, and in particular relates to a new process for preparing the flame retardant THPC by catalyzing and oxidizing phosphine in a high-efficiency liquid phase with copper chloride. Background technique [0002] The current THPC preparation process is basically through the reaction of phosphine, hydrochloric acid and formaldehyde under mixed conditions, and then concentrated under reduced pressure to obtain the product THPC. Related patent CN 102167709 A reports that phosphine is added to a gas-liquid circulation mixing reaction device to synthesize THPC. Patent CN 101224378A and patent CN101134763A report that hydrochloric acid, formaldehyde and THPC is synthesized by contacting the gas-liquid phase of phosphine. Since the catalyzer is not reported in these two patents, the conversion rate of phosphine is not high in the reaction process, and th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/535
Inventor 黄小凤魏燕富宁平范莹莹普红平周涛覃扬颂
Owner KUNMING UNIV OF SCI & TECH