Preparation method of tetraphenyl phosphorus iodide
A technology of tetraphenylphosphorus iodide and phosphorus iodide, which is applied in the field of preparation of tetraphenylphosphorus iodide, can solve the problems of difficult large-scale production, high production cost, environmental pollution, etc., and achieve low production cost and low pollution , the effect of great commercial value
Pending Publication Date: 2021-12-03
西安思科赛实业有限公司
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Problems solved by technology
It solves the problems of high production cost, serious environmental pollution and difficulty in large-scale production in the existing preparation method of tetraphenylphosphorus iodide
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Embodiment
[0030] This embodiment provides a kind of preparation method of tetraphenyl phosphorus iodide, and the steps are as follows:
[0031] S1. Take 546g of triphenylphosphine, 429ml of benzene iodide, NiI 2 2H 2 O 264g, Ni-CaO 320g with K and La added, added to the reaction flask and heated for 3h, the temperature was kept at 80°C; the mass ratio of La, K and Ni-CaO was 1:1:1;
[0032] S2. Raise the temperature to 200°C at a heating rate of 25°C / min, and keep it warm for 5 hours;
[0033] S3. cooling the reaction flask to 100°C;
[0034] S4. Add boiling water at 100°C to the reaction flask, and keep stirring for 2 hours;
[0035] S5. The reaction bottle is left to stand for 1h, separated into layers, and cooled to room temperature;
[0036] S6. The solution in the reaction bottle was filtered, rinsed with cooling water to obtain white wet crystals, and dried to obtain 480 g of tetraphenylphosphorus iodide powder crystals.
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The invention discloses a preparation method of tetraphenyl phosphorus iodide, and relates to the technical field of preparation of tetraphenyl phosphorus iodide. The preparation method comprises the following steps: S1, adding triphenylphosphine, benzene iodide and a catalyst into a reaction bottle, adding divalent halogenated metal salt with crystal water, heating the reaction bottle for 2-6 hours, and keeping the temperature at 80 DEG C; s2, raising the temperature in the reaction bottle to 180-210 DEG C, and keeping the temperature for 2-6 hours; s3, cooling the reaction bottle; s4, adding boiling water at 100 DEG C into the reaction bottle, and carrying out heat preservation and stirring for 1-1.5 h; s5, standing the reaction bottle for 1-2 hours, and cooling the reaction solution; s6, filtering and washing the solution in the reaction bottle to obtain white wet crystals, and drying the solution to obtain tetraphenylphosphorus iodide powder crystals, wherein the catalyst is La, K and Ni-CaO. The preparation method of tetraphenyl phosphorus iodide has the advantages of low production cost and low pollution, is suitable for large-scale production, and has great commercial value.
Description
technical field [0001] The invention relates to the technical field of preparation of tetraphenylphosphorus iodide, in particular to a preparation method of tetraphenylphosphorus iodide. Background technique [0002] Tetraphenylphosphorus iodide is a kind of chemical agent with excellent performance, which is often used as a catalyst for supporting dielectric, electrolytic reduction and phase transfer. The existing preparation of tetraphenylphosphorus iodide often uses expensive NiCl 2 Catalyst and poisonous benzonitrile reagent have high production cost and serious environmental pollution, thereby limiting its large-scale production. [0003] At present, there is no preparation method of tetraphenylphosphorus iodide with low production cost, low pollution, suitable for large-scale production and high commercial value. Contents of the invention [0004] Aiming at the defects in the prior art, the invention provides a preparation method of tetraphenylphosphorus iodide. T...
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IPC IPC(8): C07F9/535
CPCC07F9/535
Inventor 陈伟王鹏宝
Owner 西安思科赛实业有限公司