Preparation method of di-N-octyltin oxide

A technology of dioctyltin oxide and dioctyltin dichloride, which is applied in the field of preparation of dioctyltin oxide, can solve the problems of many steps, high toxicity of organotin chloride, and high additional cost

Active Publication Date: 2017-07-28
启东市强强贸易有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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] Dioctyl

Method used

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  • Preparation method of di-N-octyltin oxide

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Example Embodiment

[0028] The invention provides a method for preparing dioctyl tin oxide, which comprises the following steps:

[0029] (1) Add tetraoctyl tin chloride, activated clay, and modified diatomaceous earth to the reactor, pour nitrogen into it, stir evenly, slowly add tin tetrachloride, after the addition is complete, stir for 30 minutes, and heat to 160-190℃, heat preservation reaction for 4-8h, filter to obtain dioctyltin dichloride;

[0030] (2) Add isopropanol and surfactant to step (1), and slowly add sodium hydroxide solution dropwise. After the dropwise addition is completed, the temperature is raised to 75-80°C, the reaction is kept for 4-6h, the temperature is reduced to room temperature, and filtered, Obtain crude dioctyl tin oxide, wash the crude dioctyl tin oxide with water to neutrality, and dry under reduced pressure at 80°C for 12 hours to obtain dioctyl tin oxide;

[0031] Wherein, the modified diatomaceous earth is dodecylamine polyoxyethylene ether modified diatomaceous e...

Example Embodiment

[0068] Example 1

[0069] The preparation method of dioctyl tin oxide includes the following steps:

[0070] (1) Add tetraoctyl tin chloride, activated clay, and modified diatomaceous earth to the reactor, pour nitrogen into it, stir evenly, slowly add tin tetrachloride, after the addition is complete, stir for 30 minutes, and heat to 180°C, heat preservation and reaction for 6h, filter to obtain dioctyltin dichloride;

[0071] (2) Add isopropanol and surfactant to step (1), and slowly add sodium hydroxide solution dropwise. After the dropwise addition is completed, the temperature is raised to 80°C, the temperature is kept for 5 hours, the temperature is lowered to room temperature, and then filtered to obtain dioctyl For crude tin oxide, wash the crude dioctyl tin oxide with water to neutrality, and dry under reduced pressure at 80°C for 12 hours to obtain dioctyl tin oxide;

[0072] Wherein, in the step (1), the weight ratio of the tetraoctyltin chloride to the activated clay and ...

Example Embodiment

[0083] Example 2

[0084] The preparation method of dioctyl tin oxide includes the following steps:

[0085] (1) Add tetraoctyl tin chloride, activated clay, and modified diatomaceous earth to the reactor, pour nitrogen into it, stir evenly, slowly add tin tetrachloride, after the addition is complete, stir for 30 minutes, and heat to 180°C, heat preservation and reaction for 6h, filter to obtain dioctyltin dichloride;

[0086] (2) Add isopropanol and surfactant to step (1), and slowly add sodium hydroxide solution dropwise. After the dropwise addition is completed, the temperature is raised to 80°C, the temperature is kept for 5 hours, the temperature is lowered to room temperature, and then filtered to obtain dioctyl For crude tin oxide, wash the crude dioctyl tin oxide with water to neutrality, and dry under reduced pressure at 80°C for 12 hours to obtain dioctyl tin oxide;

[0087] Wherein, the weight ratio of the tetraoctyl tin chloride to the activated clay and the modified dia...

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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...

Claims

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Application Information

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IPC IPC(8): C07F7/22
CPCC07F7/2224
Inventor 杨学强俞永峰
Owner 启东市强强贸易有限公司
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