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Stannous benzoate synthesis method

A stannous benzoate, a newly synthesized technology, applied in carboxylate preparation, organic chemistry, etc., can solve the problems that the price reaction solvent cannot be carried out, cannot be applied to production, complex process flow, etc., and achieve low production cost and reduce production cost , The effect of simple production process

Active Publication Date: 2006-07-26
ZHEJIANG HISUN BIOMATERIALS +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention aims at the shortcomings of the prior art that a slurry-like mixture is formed during the preparation of stannous benzoate, which cannot be applied to production and cannot be carried out in large-scale industrial production due to the use of complex technological processes and expensive reaction solvents, and provides a kind of benzoic acid A New Synthetic Method of Stannous

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add benzoic acid (366g, 3.0mol) and water (2000ml) into a 5000ml three-necked flask, start stirring and heating for 15 minutes to 50°C, add NaOH (134g, 3.35mol) 500ml aqueous solution dropwise, and the addition is completed in 60 minutes. All dissolve, feed nitrogen into the solution then, remove the oxygen in the solution and in the reaction bottle, and add tin protochloride (SnCl 2 2H 2 (2, 339g, 1.5mol) 500ml aqueous solution, after 60 minutes dropwise, reacted 30 minutes at 50 ℃, stannous benzoate was precipitated in granular form, filtered, and air-dried product obtained 505g stannous benzoate, yield 505 / 541.4 x 100% = 93.3%. Elemental analysis value (composition C 14 h 10 o 4 Sn) (%) C: 42.03 (46.59), H: 3.23 (2.79), Sn: 32.70 (32.89), melting point 94~100°C (measured in air).

Embodiment 2

[0023] Add benzoic acid (366g, 3.0mol) and water (2000ml) into a 5000ml three-neck flask, start stirring and heating for 20 minutes to 55°C, add KOH (187g, 3.35mol) 500ml aqueous solution dropwise, dropwise in 45 minutes, benzoic acid All dissolve, feed nitrogen into the solution then, remove the oxygen in the solution and in the reaction flask, and add tin protochloride (SnCl 2 2H 2 (2,339g, 1.5mol) 500ml aqueous solution, after 45 minutes dropwise, reacted 20 minutes at 55 ℃, stannous benzoate was precipitated in granular form, filtered, and air-dried product obtained 510g stannous benzoate, yield 510 / 541.4 x 100% = 94.2%. Elemental analysis value (composition C 14 h 10 o 4 Sn) (%) C: 42.53 (46.59), H: 3.20 (2.79), Sn: 32.80 (32.89), melting point 94~100°C.

Embodiment 3

[0025] Add benzoic acid (366g, 3.0mol) and water (2000ml) into a 5000ml three-necked flask, start stirring and heating for 24 minutes to 60°C, add NaOH (134g, 3.35mol) 600ml aqueous solution dropwise, and dropwise add in 40 minutes, the benzoic acid All dissolve, feed nitrogen into the solution then, remove the oxygen in the solution and in the reaction bottle, and add tin protochloride (SnCl 2 2H 2 (2, 339g, 1.5mol) 500ml aqueous solution, after 40 minutes dropwise, reacted 20 minutes at 60 ℃, stannous benzoate was precipitated in granular form, filtered, and air-dried product obtained 520g stannous benzoate, yield 520 / 541.4 x 100% = 96.0%. Elemental analysis value (composition C 14 h 10 o 4 Sn) (%) C: 42.73 (46.59), H: 3.17 (2.79), Sn: 32.85 (32.89), melting point 94~100°C.

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Abstract

The invention provides a new synthesis method for stannous benzoate, which comprises: (1) adding benzoic acid into water, heating to 50~70Deg; stirring while dripping strong base solution to generate benzoate; (2) dripping stannite solution into former solution or water with dissolved benzoate for reaction to obtain the deposition; (3) filtering and drying to obtain the final product. This invention is practical and has high product purity.

Description

technical field [0001] The present invention relates to a kind of synthetic method of organometallic compound, relate in particular to a kind of new synthetic method of stannous benzoate. Background technique [0002] The method for preparing stannous benzoate in the early stage is to react with stannous chloride and benzoic acid in water to obtain a muddy mixture, and it is difficult to separate the solid mixture obtained by applying this method to prepare stannous benzoate, so it cannot be applied to production[J.D.Donaldson and A . Jelen, J. Chem. Soc. (A), 1986, (6): 1448]. [0003] Then there are people to switch to synthetic methylcyclopentadiene stannous or methoxy stannous intermediate and benzoic acid in benzene exchange preparation [Paul F.R.Ewings and Philip G.Harrison, J.Chem.Soc.1976, (16 ): 1717]. But this method at first will synthesize intermediates such as methylcyclopentadiene stannous or stannous methoxide, secondly, this reaction mainly prepares stannou...

Claims

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Application Information

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IPC IPC(8): C07C51/41C07C63/08
Inventor 陈学思白骅边新超陈志明黄景琴项盛梁奇志陈文启
Owner ZHEJIANG HISUN BIOMATERIALS