Preparation method of di-N-octyltin oxide

Abstract

The invention provides a preparation method of di-N-octyltin oxide. The preparation method comprises following steps: 1, tetraoctyltin chloride, activated clay, and modified diatomite are delivered into a reactor, nitrogen is introduced into the reactor, an obtained mixture is stirred to be uniform, stannic chloride is added dropwise slowly, after adding of stannic chloride, an obtained mixed material is stirred for 30min, is heated to 160 to 190 DEG C, and is subjected to thermal insulation reaction for 4 to 8h, an obtained product is filtered so as to obtain dioctyldichlorotin; 2, isopropanol and a surfactant are added, a sodium hydroxide solution is added dropwise slowly, after adding of the sodium hydroxide solution, an obtained mixed solution is heated to 75 to 80 DEG C, is subjected to thermal insulation reaction for 4 to 6h, is cooled to room temperature, and is filtered so as to obtain a di-N-octyltin oxide crude product, the di-N-octyltin oxide crude product is washed with water until pH value is adjusted to 7, pressure reduction drying is carried out at 80 DEG C for 12h so as to obtain di-N-octyltin oxide, wherein the modified diatomite is dodecylamine polyoxyethylene ether-modified diatomite, and the surfactant is a mixture of a chitosan-modified imidazoline ampholytic surfactant and hexadecyltrimethylammonium chloride.

Description

technical field [0001] The invention relates to the field of preparation of organotin heat stabilizers, in particular, the invention relates to a preparation method of dioctyltin oxide. Background technique [0002] At present, the methods for producing organotin at home and abroad mainly include the Grignard method, the Wutz method, the alkyl aluminum method and the direct iodine method. The Grignard method is mostly used in European and American countries. The alkyl aluminum method is also used in East Germany. The direct iodine method is widely used in Japan. The advantage of the Grignard method is that it can control the composition of the product at any time, but there are many steps, and the Grignard reaction is an exothermic reaction, and the boiling point of the solvent is very low, so the temperature and reaction speed must be carefully controlled to avoid explosions; although the iodine method has fewer steps than the Grignard method , but it must be recovered ac...

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Problems solved by technology

The advantage of the Grignard method is that it can control the composition of the product at any time, but there are many steps, and the Grignard reaction is an exothermic reaction, and the boiling point of the solvent is very low, so the temperature and reaction speed must be carefully controlled to avoid explosions; although the iodine method has fewer steps than the Grignard method , but it must be recovered according to regulations. The common point of the two methods is that the price of metal magnesium, iodine and raw metal tin is relatively expensive, and the organotin chloride is highly toxic, so general industrial production seeks a method that does not use iodide

[0003] Dioctyltin oxide is the main intermediate for synthesizing high-efficiency and non-toxic organotin heat stabilizers for PVC. It has strong heat resistance and is used in food and pharmaceutical packaging materials because it is non-toxic to the human body. High cost, especially in the synthesis process of dioctyltin oxide, the raw material price is high, the route is complicated, and the additional cost is high, resulting in great restrictions on its application

[0004] In addition, in the prior art, surfactants are added to improve the side reactions produced during the reaction between dioctyltin dichloride and alkali, but there are problems such as serious adsorption in the existing surfactants

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