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Sulfo-(combination) tin reverse-ester, preparation method and application

A technology of reverse ester tin and sulfuration, which is applied in the field of preparation of reverse ester tin thio, can solve the problem of high cost, and achieve the effects of simple operation, excellent lubricity, and good application prospects

Active Publication Date: 2014-12-17
湖北犇星新材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it is mainly used in the fields of sheets, films, card bases, etc., and has relatively large limitations in the fields of PVC pipes, pipe fittings and profiles, and the cost is relatively high

Method used

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  • Sulfo-(combination) tin reverse-ester, preparation method and application
  • Sulfo-(combination) tin reverse-ester, preparation method and application
  • Sulfo-(combination) tin reverse-ester, preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Add 2.45mol of mercaptoethanol oleate, 1mol of monomethyl tin trichloride in the three-neck round bottom flask, add 150ml of pure water, stir well, then add 1 / 2 of the theoretical amount of ammonia (2.4mol) therein, and then Add 0.6 mol of ammonium sulfide, and finally add the remaining ammonia water, adjust the pH to 4.5-7, keep the reaction temperature at about 40°C, and the reaction time is 1.5 hours; then wash with water, and finally vacuumize and dehydrate to obtain the target product Thio (United) Reverse ester tin 807.0 grams, yield 97.0% based on monomethyl tin trichloride.

[0031] 1 H NMR (300MHz, CDCl 3 ) characterization results are: chemical shift δ=0.9(6), δ=0.95-0.98(12), δ=1.27-1.35(80), δ=1.68(8), δ=1.96(16), δ=2.23- 2.26(8), δ=2.83-2.86(8), δ=4.33-4.39(8), δ=5.41-5.48(8).

[0032] MS m / z: 1687 [M+Na].

[0033] Elemental analysis value (composition: C 82 h 154 o 8 S 5 sn 2 )(%): C: 58.96 (59.16), H: 9.30 (9.26), S: 9.55 (9.62), Sn: 14.42 (14.27...

Embodiment 2

[0035] Add 2.25mol of mercaptoethanol oleate and 1mol of monomethyl tin trichloride into a three-neck round bottom flask, add 200ml of pure water, stir, then add 2 / 3 of the theoretical amount of ammonia (2.3mol) to it, and then add Ammonium sulfide 0.7mol, and finally add the remaining ammonia water, adjust the pH to 4.5-7, keep the reaction temperature at 50°C, and the reaction time is 2 hours; then wash with water, and finally vacuum dehydrate to obtain the target product thio(joint) reverse ester tin 807.8 grams, with a yield of 97.1% based on monomethyl tin trichloride.

Embodiment 3

[0037] Add 2.30 mol of mercaptoethanol oleate and 1 mol of monomethyl tin trichloride into a three-neck round bottom flask, add 250 ml of pure water, stir, then add 2 / 3 of the theoretical amount of ammonia water (2.25 mol) to it, and then add Sodium sulfide 0.75mol, and finally add the remaining ammonia water, adjust the pH to 4.5-7, keep the reaction temperature at 60°C, and the reaction time is 2 hours; then wash with water, and finally vacuum dehydrate to obtain the target product thio(joint) reverse ester 802.9 grams of tin, with a yield of 96.5% based on monomethyl tin trichloride.

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Abstract

The invention relates to sulfo-(combination) tin reverse-ester which adopts the structure shown in a formula (I). The invention further provides a preparation method of the sulfo-(combination) tin reverse-ester and the application of the sulfo-(combination) tin reverse-ester in PVC heat stabilizer. The sulfo-(combination) tin reverse-ester creates sulfur bridges, increases sulfur tin bonds, and increases molecular weight; all the performances of the sulfo-(combination) tin reverse-ester are superior to those of the conventional tin reverse-ester heat stabilizer; and the sulfo-(combination) tin reverse-ester can be used as the novel PVC heat stabilizer with a better effect. In the preparation method, raw materials has low prices and are easy to get, a synthetic method adopts mild conditions and is simple and convenient to operate, and a favorable application prospect can be achieved.

Description

technical field [0001] The invention relates to the field of fine chemical industry, in particular to a thio(joint) reverse ester tin, its preparation method and its application. Background technique [0002] Organotin heat stabilizers are an important class of fine chemicals and excellent raw materials for preparing heat stabilizers for polyvinyl chloride (PVC) plastic products. However, it is mainly used in the fields of sheets, films, card bases, etc., and has relatively large limitations in the fields of PVC pipes, pipe fittings and profiles, and the cost is relatively high. [0003] The main reason for this situation is that the existing mercapto esters for the preparation of organotin are esters obtained from mercapto acids and fatty alcohols. Such esters are usually called normal esters, and the synthesized organotin compounds are commonly known as organotins. In order to change this situation, the existing research has adjusted the structure of the ester group accor...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K5/58C07F7/22C08L27/06
Inventor 戴百雄宫廷吴勇徐善武张建广温志鹏罗斌
Owner 湖北犇星新材料股份有限公司
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