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Preparation method of sulfur bridge-containing reverse ester thiol methyltin

A technology of retro ester mercaptan methyl tin and methyl tin trichloride, which is applied in the field of preparation of retro ester mercaptan methyl tin, can solve the problem that the bridging structure cannot be guaranteed, the reactant is easy to turn black, and the product quality is not good and other issues to achieve the best thermal stability, easy implementation, and cost reduction

Inactive Publication Date: 2012-06-27
HUBEI NANXING CHEM GENERAL FACTORY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] 1. In the process of producing mercaptoethanol oleate, the raw materials include oleic acid and mercaptoethanol. Since the two are heated during the reaction, a large amount of mercaptoethanol will be evaporated, and considering that mercaptoethanol is much more expensive than oleic acid, so In the prior art, the usage amount of oleic acid is more than the usage amount of mercaptoethanol, yet, the usage amount of oleic acid is more can cause the poor quality of product;
[0014] 2. Both U.S. Patents US4120845 and US5821274 mentioned that methyl tin chloride and mercaptoethanol oleate were first condensed to generate hydrogen chloride, and then hydrogen chloride was neutralized with aqueous sodium hydroxide solution, and then sodium sulfide was added dropwise for bridging Reaction, in recent years, domestic manufacturers have also followed this idea, but this process cannot guarantee that the Sn-S-Sn bridging structure will be formed according to the set ratio, resulting in the product being easily emulsified, difficult to wash and stratify, and the reactant is easy to turn black , at the same time, hydrogen sulfide may be generated during the production process

Method used

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  • Preparation method of sulfur bridge-containing reverse ester thiol methyltin
  • Preparation method of sulfur bridge-containing reverse ester thiol methyltin
  • Preparation method of sulfur bridge-containing reverse ester thiol methyltin

Examples

Experimental program
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Embodiment 1

[0039] Preparation of mercaptoethanol oleate comprises the following steps:

[0040] a) Add 415g of oleic acid, 2g of alkyl titanate, 1g of hydroquinone and 120g of mercaptoethanol into a 1000ml first reaction vessel;

[0041] b) vacuumize and heat the first reaction vessel until the vacuum degree in the first reaction vessel reaches 200mmHg (absolute pressure) and the temperature reaches between 75-85°C, and then maintains the temperature between 75-85°C, and shall not exceed 85°C;

[0042] c) When a distillate is produced, the distillate is condensed and recovered; mercaptoethanol can be extracted from the distillate recovered by condensation for next use;

[0043] d) when the output speed of the distillate begins to decline, make the vacuum degree in the first reaction vessel reach 150mmHg (absolute pressure);

[0044] e) Control the degree of vacuum in the first reaction vessel to decrease stepwise according to 150mmHg, 100mmHg, and 30mmHg, and at the same time carefully o...

Embodiment 2

[0048] The preparation of methyl tin mercaptide in reverse ester comprises the following steps:

[0049] A) 680g mercaptoethanol oleate (the product obtained in Example 1) is added in the second reaction vessel of 2000ml;

[0050] B) the 440ml monomethyl tin trichloride aqueous solution that concentration is 53% and the 220ml sodium sulfide aqueous solution that concentration is 20% are added dropwise in the mercaptoethanol oleate in the second reaction vessel simultaneously, in the process of dropping , control the reaction temperature below 30°C, and react for 1.5 hours after the dropwise addition is completed;

[0051] C) dripping ammonia water with a concentration of 17%, until the pH value of the reactant in the second reaction vessel reaches between 6.5 and 7;

[0052] D) raising the temperature of the second reaction vessel to between 50 and 60°C, and keeping it warm for 1 hour;

[0053] E) make the second reaction vessel cool down, then add the water of 400ml in the ...

Embodiment 3

[0057] The preparation of methyl tin mercaptide in reverse ester comprises the following steps:

[0058] A) 680g mercaptoethanol oleate (the product obtained in Example 1) is added in the second reaction vessel of 2000ml;

[0059] B) the mixed aqueous solution of monomethyl tin trichloride and dimethyl tin dichloride of 500ml (wherein, the quality of monomethyl tin trichloride accounts for 40% of aqueous solution quality, dimethyl tin dichloride The mass accounts for 10% of the aqueous solution mass) and the 210ml sodium sulfide aqueous solution with a concentration of 20% is simultaneously added dropwise to the mercaptoethanol oleate in the second reaction vessel, and during the dropping process, the reaction temperature is controlled below 30°C; After the dropwise addition was completed, react for 1.5 hours;

[0060] C) dripping ammonia water with a concentration of 17%, until the pH value of the reactant in the second reaction vessel reaches between 6.5 and 7;

[0061] D)...

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Abstract

The invention discloses a preparation method of sulfur bridge-containing reverse ester thiol methyltin. The method comprises two stages: in a first stage, preparing mercaptoethanol oleate, and controlling the vacuum degree in a first reaction container to descend stepwise in a reacting process; and in a second stage, preparing sulfur bridge-containing reverse ester thiol methyltin by taking mercaptoethanol oleate obtained at the first stage as a raw material, dropwise adding a methyl tin chloride aqueous solution and a sodium sulfide aqueous solution into the mercaptoethanol oleate simultaneously, and undergoing a condensation reaction and a bridging reaction simultaneously to control sulfur atoms in sodium sulfide and tin atoms in methyl tin chloride to be connected in a sulfur bridge form. The preparation method is easy to implement, the problems of emulsification, saponification and the like in a production process can be solved effectively, and the productivity and production efficiency are increased; and meanwhile, the ratio of a sulfur bridge is controlled, so that the thermal stability of a product is in an optimal state.

Description

technical field [0001] The invention relates to the technical fields of production of plastic additives and plastic processing, in particular to a preparation method of methyl tin mercaptide containing a sulfur bridge. Background technique [0002] Among the many PVC heat stabilizers, methyl tin mercaptide is recognized as a heat stabilizer with good effect in the industry. In the 1950s, the United States patent document US 2731484 mentioned the production and potential use of dialkyl tin mercaptide; from the early 1980s, methyl tin mercaptide began to be produced and applied on a large scale; in 1989, my country's first large-scale production line of methyl tin mercaptide was built in Hubei Nanxing Chemical General Factory. After more than 20 years of development, my country now has nearly 70% of the world's production and sales of methyl tin mercaptide. [0003] Usually, methyl tin mercaptide has the following general structural formula: (CH3) X Sn[S(R 1 ) MCOOR 2 ] 4-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/22
Inventor 李建丰李尖王爱红龙守奎钟新乐高勇
Owner HUBEI NANXING CHEM GENERAL FACTORY
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