Industrial prepn process of triphenyl bismuth compounds

A technology of triphenyl bismuth and compounds, applied in the direction of bismuth organic compounds, etc., can solve the problems of being unsuitable for industrial production, and achieve the effect of mild reaction conditions

Inactive Publication Date: 2007-08-22
庄罗元
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Existing preparation method 2: use bromobenzene and magnesium to react under anhydrous, anaerobic and nitrogen protection to generate phenylmagnesium bromide...

Method used

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  • Industrial prepn process of triphenyl bismuth compounds
  • Industrial prepn process of triphenyl bismuth compounds
  • Industrial prepn process of triphenyl bismuth compounds

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0018] The preparation of example 1, triphenylbismuth

[0019] In a 500L reaction flask, add 6Kg of magnesium chips, 0.2Kg of iodine particles, 0.2Kg of bromobenzene, 10L of tetrahydrofuran and 30L of toluene, heat to 64°C, activate the magnesium chips for about 30 minutes, add dropwise a mixture of 38kg of bromobenzene and 150L of toluene For the mixed solution, control the dropping speed to maintain the reaction solution in a slightly boiling state. After the dropwise addition, react at 65-75°C for 5 hours to make the action of magnesium chips complete, cool to room temperature, and add dry bismuth trichloride 24.2 Kg and 100L dry toluene mixture was added in batches, after the addition was completed, reacted at 110°C for 4 hours, after the reaction was completed, cooled, stopped the reaction with a saturated aqueous solution made of 10Kg ammonium chloride, extracted with toluene, recrystallized, and filtered , After drying, 30.1 Kg of milky white crystalline triphenylbismut...

example 2、 3

[0020] The preparation of example 2, three (p-methylphenyl) bismuth

[0021] In a 500L reaction flask, add 6Kg, 0.2Kg iodine particles, 0.2Kg p-bromotoluene, 10L N-methylpyrrolidone and 30L benzene, heat to 80°C to activate magnesium chips for about 30 minutes, cool to 20°C, Add a mixture of 41.5Kg p-bromotoluene and 150L benzene dropwise at ℃, control the rate of addition, and control the reaction temperature at about 20℃. After the dropwise addition, continue to react at 20℃ for 15 hours to complete the reaction of magnesium chips. Add 24.2Kg of dry bismuth trichloride and 100L of dry benzene mixture in batches under stirring. After the addition is complete, react at 80°C for 9 hours. The aqueous solution was used to stop the reaction, extracted with benzene, recrystallized, filtered, and dried to obtain 34.2Kg of white crystal tris(p-methylphenyl)bismuth, with a yield of 92.4%, melting point: 88°C to 89°C, (literature value: 86°C ~87°C).

example 3

[0022] The preparation of example 3, three (m-methylphenyl) bismuth

[0023] In a 500L reaction flask, add 6.2Kg of magnesium chips, 0.2Kg of iodine grains, 0.2Kg of m-bromotoluene, 10L of N-methylpyrrolidone and 30L of ethylbenzene, heat to 120°C, activate the magnesium chips for about 30 minutes, then add For the mixture of 41.5Kg bromotoluene and 150L ethylbenzene, control the rate of addition to maintain the reaction temperature at 120°C. After the dropwise addition, continue to react at 120°C for 1 hour to make the action of magnesium chips almost complete. Cool to room temperature and add dry The mixture of 24.2Kg of bismuth trichloride and 100L of dry ethylbenzene was added in batches. After the addition was completed, it was reacted at 120°C for 1 hour. After extraction with ethylbenzene, recrystallization, filtration and drying, 34Kg of white crystalline tris(m-methylphenyl)bismuth was obtained, with a yield of 92.0%. Melting point: 78°C-79°C (literature value: 78°C-7...

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Abstract

The present invention discloses industrial preparation process of serial triphenyl bismuth compounds. Serial benzene bromide compounds as material are made to produce Grignard reaction with metal magnesium in anhydrous solvent to produce organic magnesium compounds, which are then reacted with anhydrous bismuth trichloride at 20-120 deg.c to produce serial triphenyl bismuth compounds. The serial benzene bromide compounds include bromobenzene, parabromotoluene, m-bromotoluene, o-bromotoluene, etc; and the anhydrous solvent may be tetrahydrofuran, benzene, toluene, ethyl benzene, etc or their mixture. The reaction time is 2-24 hr. The present invention adopts organic solvent with high boiling point for high safety and easy activation of magnesium, and has mild reaction condition and yield over 90 %.

Description

Technical field: [0001] The invention relates to a preparation method of triphenylbismuth series compounds, in particular to an industrial preparation method of triphenylbismuth series compounds. Background technique: [0002] Solid propellant is an important part of the rocket engine, its weight accounts for about 90% of the total weight of the rocket engine, and its cost accounts for 20% of the total launch cost of the space shuttle, so the performance and cost of solid propellant play an important role in the development of the aerospace industry. to a very significant effect. Organic bismuth compounds are important combustion catalysts in solid propellants. Studies have shown that organic bismuth-based propellants can be solidified at room temperature, reducing the propellant solidification temperature and achieving room temperature solidification, reducing and eliminating the shrinkage stress of the propellant charge, improving The mechanical properties of the propella...

Claims

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Application Information

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IPC IPC(8): C07F9/94
Inventor 庄罗元
Owner 庄罗元
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