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Method for preparing novel isobutyl triethoxy silane

A new technology of isobutyltriethoxysilane, which is applied in the field of preparation of new isobutyltriethoxysilane, can solve the problem of rare isobutyltriethoxysilane, expensive catalyst, high production cost, etc. problems, to achieve the effect of easy separation and purification, easy operation, and small investment in equipment

Inactive Publication Date: 2011-10-19
GUANGZHOU SUPER CHEM COATING CO LTDGUANGZHOU SUPER CHEM COATING CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] As mentioned above, the traditional production method of isobutyltriethoxysilane has the disadvantages of long reaction cycle, expensive catalyst and high production energy consumption, resulting in high production cost.
At present, there are few reports on the new preparation method of isobutyltriethoxysilane in patent documents at home and abroad

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] The first step, in terms of mass in grams, gets 2 grams of magnesium chips and 15 grams of ethyl orthosilicate and joins it in a tank equipped with a reflux device, a stirring device and N 2 In the reactor connected to the device, after stirring and passing N 2 Raise the temperature to 90°C under the conditions, add 1 gram of iodine pellets, add 10 grams of bromoisobutane dropwise within 1 hour, then keep warm and reflux for 2 hours;

[0036] In the second step, the mixture obtained in the first step is cooled to 30° C., and filtered to obtain the filtrate;

[0037] In the third step, the filtrate obtained in the second step was distilled under the condition of 4.0 kPa, and the distilled fraction at 100° C. to 102° C. was collected to obtain 15 grams of isobutyltriethoxysilane product.

Embodiment 2

[0039] The first step, in terms of mass in grams, gets 5 grams of magnesium chips and 30 grams of tetraethyl orthosilicate and joins it in a tank equipped with a reflux device, a stirring device and N 2 In the reactor connected to the device, stirring and passing N 2 Under the conditions, the temperature was raised to 150°C, 3 grams of iodine particles were added, and 21 grams of bromoisobutane was added dropwise within 1.5 hours, and then kept at reflux for 4 hours;

[0040] In the second step, the mixture obtained in the first step is cooled to 60° C., and filtered to obtain the filtrate;

[0041] In the third step, the filtrate obtained in the second step was distilled under the condition of 4.0 kPa, and the distilled fraction at 100° C. to 102° C. was collected to obtain 27.5 grams of isobutyltriethoxysilane product.

Embodiment 3

[0043] The first step, in terms of mass grams, takes 2.9 grams of sodium particles and 22 grams of tetraethyl orthosilicate and joins it in a container equipped with a reflux device, a stirring device and N 2 In the reactor connected to the device, stirring and passing N 2 Under the conditions, the temperature was raised to 130°C, 2 grams of iodine particles were added, 10 grams of chloroisobutane was added dropwise within 1 hour, and then kept at reflux for 3 hours;

[0044] In the second step, the mixture obtained in the first step is cooled to 50° C., and filtered to obtain the filtrate;

[0045] In the third step, the filtrate obtained in the second step was distilled under the condition of 4.0 kPa, and the distilled fraction at 100° C. to 102° C. was collected to obtain 23 grams of isobutyltriethoxysilane product.

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Abstract

The invention discloses a method for preparing novel isobutyl triethoxy silane, and belongs to the field of anticorrosive materials. The method comprises the following steps of: adding 2 to 5 mass parts of active metal and 15 to 30 mass parts of ethyl orthosilicate into a reactor with a reflux device, a stirring device and an N2 introducing device, heating to the temperature of between 90 and 150 DEG C under the condition of stirring and introducing N2, adding 1 to 3 mass parts of iodine granules, dripping 10 to 21 mass parts of halogenated iso-butane in 1 to 1.5 hours, keeping the temperature and refluxing for 2 to 4 hours, cooling and filtering to obtain filter liquor; and distilling the filter liquor under reduced pressure, and collecting distillation fractions to obtain an isobutyl triethoxy silane product. In the preparation method, a process is simple, expensive catalyst and volatile solvent are not needed, the reaction conversion rate and yield are high, the production period of the product is short, and equipment is simple.

Description

technical field [0001] The invention belongs to the field of anticorrosion materials, and in particular relates to a preparation method of novel isobutyltriethoxysilane. Background technique [0002] Isobutyltriethoxysilane, also known as triethoxyisobutylsilane, is an important intermediate in the production of various silane coupling agents. In terms of ion erosion, isobutyltriethoxysilane treatment is one of the most economical methods, and its reasonable service life is greater than 30 years. [0003] In the prior art, the preparation method of isobutyltriethoxysilane is generally obtained by esterifying isobutyltrichlorosilane with ethanol at 80-100°C and 0.03MPa as a raw material, and the reaction formula is: [0004] CH 3 CH(CH 3 )CH 2 SiCl 3 +CH 3 CH 2 OH→CH 3 CH(CH 3 )CH 2 Si(OCH 2 CH 3 ) 3 +3HCl [0005] During the reaction process, ethanol is added in batches, the reaction time is about 6 hours, and after the reaction, it is refluxed at 0.03MPa for a...

Claims

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Application Information

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IPC IPC(8): C07F7/18
Inventor 杨金鑫皮丕辉周子鹄文秀芳
Owner GUANGZHOU SUPER CHEM COATING CO LTDGUANGZHOU SUPER CHEM COATING CO LTD
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