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Preparation technique of dibutyl tin diacetate

A technology for the preparation of dibutyl diacetic acid, which is applied in the direction of tin organic compounds, can solve the problems of reduced production, high production cost, and low tin content, and achieve the effect of promoting complete reaction, ensuring product purity, and high purity

Inactive Publication Date: 2015-04-08
CHANGSHA LUOSI TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The tin content of the product in the traditional dibutyltin diacetate processing is low, which cannot meet the production requirements
And if the amount of feed is not well controlled, it will easily cause more by-products, reduce production, cause higher production costs, reduce product quality, and be easy to crystallize, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] A kind of dibutyl tin diacetate preparation technology, specifically comprises the following steps:

[0019] (1) add in the reactor after weighing 264g glacial acetic acid;

[0020] (2) Open the stirring device, the stirring speed is 250r / min, and add 276g dibutyltin oxide while stirring;

[0021] (3) Raise the temperature, wait until the temperature rises to between 60-80°C, keep the temperature for 2 hours, until the dibutyltin oxide is completely dissolved;

[0022] (4) Vacuumize, heat, stop heating when the temperature reaches 105°C, and keep warm for 30min;

[0023] (5) Continue heating to 110°C, keep warm, and vacuumize for 2 hours until no low boilers are distilled out;

[0024] (6) Blowing and weighing to obtain the required dibutyltin diacetate.

[0025] The tin content in the prepared product was detected to be 27%.

Embodiment 2

[0027] A kind of dibutyl tin diacetate preparation technology, comprises the following steps:

[0028] (1) weigh 320g glacial acetic acid and add in the reactor;

[0029] (2) Open stirring device, stirring speed 200r / min, add 276g dibutyltin oxide while stirring;

[0030] (3) Raise the temperature, wait until the temperature rises to between 60-80°C, keep the temperature for 1.5h until the dibutyltin oxide is completely dissolved;

[0031] (4) Vacuumize, heat, stop heating when the temperature reaches 105°C, and keep warm for 25 minutes;

[0032] (5) Continue heating to 110°C, keep warm, and evacuate for 2.5 hours until no low boilers are distilled out;

[0033] (6) Blowing and weighing to obtain the required dibutyltin diacetate.

[0034] The tin content of the prepared dibutyltin diacetate was detected to be 30%.

Embodiment 3

[0036] A kind of dibutyl tin diacetate preparation technology, comprises the following steps:

[0037] (1) weigh 330g glacial acetic acid and add in the reactor;

[0038] (2) Open stirring device, control stirring speed to be 170r / min, add 276g dibutyltin oxide while stirring;

[0039] (3) Raise the temperature, wait until the temperature rises to between 60-80°C, keep the temperature for 1.5h until the dibutyltin oxide is completely dissolved;

[0040] (4) Vacuumize, heat, stop heating when the temperature reaches 105°C, and keep warm for 20 minutes;

[0041] (5) Continue heating to 110°C, keep warm, and evacuate for 3.5 hours until no low boilers are distilled out;

[0042] (6) Blowing and weighing to obtain the required dibutyltin diacetate.

[0043] The tin content in the detected product is 33%.

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Abstract

The invention belongs to the technical field of catalyst preparation, and particularly relates to a preparation technique of dibutyl tin diacetate. The technique comprises the following steps: (1) weighing excessive glacial acetic acid for reaction, and adding into reaction kettle; (2) starting a stirring device, and adding dibutyl tin oxide while stirring; (3) heating to 60-80 DEG C, and keeping the temperature to react for 1-2 hours until the dibutyl tin oxide is completely dissolved; (4) vacuumizing, heating to 105 DEG C, stopping heating, and keeping the temperature for 20-30 minutes; (5) continuing heating to 110 DEG C, keeping the temperature, and vacuumizing for 2-3.5 hours until no low-boiling-point substance is distilled off; and (6) discharging, and weighing to obtain the required dibutyl tin diacetate. The technique has the advantages of complete reaction, low production cost and good product quality.

Description

technical field [0001] The invention belongs to the technical field of catalyst preparation, and in particular relates to a preparation process of dibutyltin diacetate. Background technique [0002] Dibutyl tin diacetate, English name Dibutyl tin diacetate, is light yellow or colorless transparent liquid with acetic acid smell, solid or semi-solid below 10°C, freezing point: 8~10°C, density: 1.32±0.005(20 ℃), boiling point: 140~144℃ / 10mmHg. It is mainly used as a curing catalyst for silicone rubber at room temperature, especially for deacetate-type silicone products. It is characterized by fast catalytic speed. In order to reduce its acetic acid smell, it can be used in conjunction with dibutyltin dilaurate. It is easily hydrolyzed when exposed to the air, and solids are precipitated at the bottle mouth. It can also be used as a polyurethane coating catalyst. [0003] At present, the preparation method of dibutyltin acetate mostly adopts glacial acetic acid and dibutyltin ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/22
Inventor 罗丁袁再春禹康
Owner CHANGSHA LUOSI TECH
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