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Synthesis method of dibutyltin dilaurate

A technology of dibutyltin laurate and synthesis method, which is applied in the direction of tin organic compounds, chemical instruments and methods, compounds of group 4/14 elements of the periodic table, etc., and can solve problems such as many process steps, ethanol residue, and long synthesis time , to achieve the effect of simple process, reduced product loss and short time consumption

Inactive Publication Date: 2017-09-15
NORTHWEST INSTITUTE FOR NON-FERROUS METAL RESEARCH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Notification number is CN102838631B " a kind of synthetic method of dibutyltin laurate " patent discloses a kind of technology that takes lauric acid and dibutyltin oxide as raw material, and ethanol is the technique of solvent synthesis dibutyltin laurate, and this technique saves Eliminate the alkalization process, no toxic dust and waste water, no pollution to the environment, but because of the use of ethanol as a solvent, it will cause ethanol residue in the product
The patent of "a synthetic method for preparing dibutyltin dilaurate" with the publication number CN104672276A discloses a process of using lauric acid and dibutyltin oxide as raw materials and adding a catalyst synthesis reaction under the action of a solvent. The recycling efficiency is improved, the production cost is reduced, and the production equipment is simple, and the environmental pollution is less in the process, but the process has many steps and the synthesis takes a long time

Method used

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  • Synthesis method of dibutyltin dilaurate
  • Synthesis method of dibutyltin dilaurate
  • Synthesis method of dibutyltin dilaurate

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Embodiment 1

[0021] The synthetic method of the present embodiment dibutyltin dilaurate comprises the following steps:

[0022] Step 1, stirring the solid mixture of 100g lauric acid and 62g dibutyltin oxide at 25°C to convert the solid mixture into a liquid mixture;

[0023] Step 2. Heat the liquid mixture obtained in Step 1 to 65°C, and then reflux for 2.5 hours;

[0024] Step 3. Cool the liquid mixture after the reflux reaction in step 2 to 20° C., collect the organic phase after standing and separating, add anhydrous magnesium sulfate to the organic phase to remove water for 9 hours, and then filter to obtain the filtrate It is dibutyltin dilaurate; the amount of anhydrous magnesium sulfate added is 8g of anhydrous magnesium sulfate per 100mL of organic phase.

[0025] This embodiment obtains 153.5g of dibutyltin dilaurate, the theoretical output value of dibutyltin dilaurate calculated according to the reaction equation is 157.9g, and the yield of dibutyltin dilaurate is 97.2%.

[0...

Embodiment 2

[0028] The synthetic method of the present embodiment dibutyltin dilaurate comprises the following steps:

[0029] Step 1, stirring the solid mixture of 176g lauric acid and 109g dibutyltin oxide at 20°C to convert the solid mixture into a liquid mixture;

[0030] Step 2, heating the liquid mixture obtained in Step 1 to 60°C, and then reflux for 2 hours;

[0031] Step 3. Cool the liquid mixture after the reflux reaction in step 2 to 10°C, and collect the organic phase after standing for stratification. Add anhydrous magnesium sulfate to the organic phase to remove water for 8 hours, and then filter to obtain the filtrate It is dibutyltin dilaurate; the amount of anhydrous magnesium sulfate added is 5g of anhydrous magnesium sulfate per 100mL of organic phase.

[0032] This embodiment obtains 266.3g of dibutyltin dilaurate, the theoretical output value of dibutyltin dilaurate calculated according to the reaction equation is 276.0g, and the yield of dibutyltin dilaurate is 97.2...

Embodiment 3

[0035] The synthetic method of the present embodiment dibutyltin dilaurate comprises the following steps:

[0036] Step 1, stirring the solid mixture of 264g lauric acid and 164g dibutyltin oxide at 30°C to convert the solid mixture into a liquid mixture;

[0037] Step 2, heating the liquid mixture obtained in step 1 to 70°C, and then reflux for 3h;

[0038] Step 3. Cool the liquid mixture after the reflux reaction in step 2 to 30° C., collect the organic phase after standing for stratification, add anhydrous magnesium sulfate to the organic phase to remove water for 10 hours, and then filter to obtain the filtrate It is dibutyltin dilaurate; the amount of anhydrous magnesium sulfate added is 10g of anhydrous magnesium sulfate per 100mL of organic phase.

[0039] This embodiment obtains 395.4g of dibutyltin dilaurate, the theoretical output value of dibutyltin dilaurate calculated according to the reaction equation is 416.2g, and the yield of dibutyltin dilaurate is 95.0%.

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Abstract

The invention discloses a synthesis method of dibutyltin dilaurate. The method comprises steps as follows: 1, a solid mixture of lauric acid and dibutyltin oxide is stirred at the temperature of 20-30 DEG C to be converted into a liquid mixture; 2, the liquid mixture is heated to 60-70 DEG C and then subjected to a reflux reaction for 2-3 h; 3, the liquid mixture subjected to the reflux reaction is cooled to 10-30 DEG C, left to stand for layering and then collected, an organic phase is obtained, anhydrous magnesium sulfate is added to the organic phase for water removal, the mixture is filtered, and obtained filtrate is dibutyltin dilaurate. The solid mixture of lauric acid and dibutyltin oxide is converted into the liquid mixture, then the liquid mixture is subjected to the reflux reaction, cooled, separated and dried, and dibutyltin dilaurate is obtained. The process is simple, requirements for equipment are lower, the method takes short time and is convenient, efficient and environment-friendly, and the obtained dibutyltin dilaurate has no solvent or catalyst residues.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a synthesis method of dibutyltin dilaurate. Background technique [0002] Dibutyltin dilaurate is an organic tin compound with excellent transparency, lubricity and weather resistance. It can not only be used as a catalyst in the synthesis of silicone rubber, acrylate rubber, carboxyl rubber and polyurethane foam, but also widely used in wood Production of lacquers, PU coatings, metallic inks, adhesives and sealants. [0003] In industry, tetrabutyltin or tin tetrachloride is often used as the starting material to synthesize the intermediate product, and then condensed with lauric acid to obtain dibutyltin dilaurate. This process will produce a large amount of waste water and pollute the environment. Therefore, research on the green and pollution-free dibutyltin dilaurate synthetic method has become a hotspot. Notification number is CN102838631B " a kind o...

Claims

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Application Information

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IPC IPC(8): C07F7/22
CPCC07F7/2208
Inventor 李延超李来平王晖张新
Owner NORTHWEST INSTITUTE FOR NON-FERROUS METAL RESEARCH
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