Improved preparation method of tetramethyl ammonium bicarbonate

A technology of tetramethylammonium bicarbonate and dimethyl carbonate is applied in the preparation of amino-substituted functional groups, chemical instruments and methods, organic compounds/hydrides/coordination complex catalysts, etc. The reactor is bulky and the device is complicated.

Inactive Publication Date: 2021-12-03
信联电子材料(山东)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] However, in the above-mentioned prior art, Chinese patent application publication CN101314572A has the technical defects of high partial pressure of trimethylamine and high equipment energy consumption; Chinese patent application publication CN107417539A and CN107281994A have the technical defects of large reactor volume and complex devices; Zhou Yulu The method such as Zhang Guiju adopts two-step method, and the method such as Zhang Guiju adopts one-step method; The former step is loaded down with trivial details, and hydrolysis reaction easily reduces product yield; The latter step is simple, but product yield is still unsatisfactory

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] 2g of SBA-15 molecular sieves were added to 30mL of anhydrous toluene, and then 0.8g of 3-aminopropyltriethoxysilane was added thereto, and the reaction was refluxed at 108°C for 12h. After the reaction is completed, filter, wash with anhydrous toluene three times, dry at 120° C. for 24 hours, and cool to room temperature to obtain an organic amine-modified SBA-15 molecular sieve.

Embodiment 2

[0042] Add 9.0 g (0.1 mol) of dimethyl carbonate and 17.9 g (containing 0.1 mol) of trimethylamine aqueous solution with a mass fraction of 33% in the autoclave; then add 1.0 g of the organic amine modified SBA-15 of Example 1 Molecular sieve. Inflate with nitrogen, check the airtightness of the autoclave and empty it, and pressurize to 1.2MPa. Turn on the heater and stirrer, raise the temperature to 105°C, and stir the reaction for 5h. After the reaction is finished, depressurize, cool, and filter to remove the organic amine-modified SBA-15 molecular sieve. A small amount of by-product methanol was distilled off under reduced pressure to obtain an aqueous solution of tetramethylammonium bicarbonate. The aqueous solution was concentrated and dried to obtain a white solid, namely the product.

Embodiment 3

[0044] Add 9.0 g (0.1 mol) of dimethyl carbonate and 21.5 g (containing 0.12 mol) of trimethylamine aqueous solution with a mass fraction of 33% in the autoclave; then add 1.0 g of Example 1 organic amine modified SBA-15 Molecular sieve. Inflate with nitrogen, check the airtightness of the autoclave and empty it, and pressurize to 1.2MPa. Turn on the heater and stirrer, raise the temperature to 105°C, and stir the reaction for 5h. After the reaction is finished, depressurize, cool, and filter to remove organic amine-modified SBA-15 molecular sieves. A small amount of by-product methanol was distilled off under reduced pressure to obtain an aqueous solution of tetramethylammonium bicarbonate. The aqueous solution was concentrated and dried to obtain a white solid, namely the product.

[0045] Samples were taken and HPLC was used to analyze the product yields of Examples 2 and 3, which were 94.1% and 96.3% respectively.

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Abstract

The invention discloses an improved preparation method of tetramethyl ammonium bicarbonate. According to the improved preparation method, dimethyl carbonate and a trimethylamine aqueous solution are taken as reaction raw materials, and tetramethyl ammonium bicarbonate is prepared by adopting a one-step method; wherein the reaction is carried out in the presence of an organic amine modified molecular sieve. The organic amine modified molecular sieve with a specific proportion is added, so that the product yield is further improved. The organic amine modified molecular sieve interacts with dimethyl carbonate or a product thereof, so that the probability of side reaction of the final product is reduced.

Description

technical field [0001] The invention relates to an improved preparation method of tetramethylammonium bicarbonate, which belongs to the technical field of organic synthesis. Background technique [0002] Tetramethylammonium bicarbonate is the key raw material for the preparation of tetramethylammonium hydroxide by ion membrane electrolysis, which has a wide range of uses in many fields, including but not limited to, catalysts, surfactants, templating agents, organic synthesis reagents, etc. In particular, in recent years, high-purity tetramethylammonium hydroxide has been used as a cationic developer in large-scale integrated circuits and as a cleaning agent in microelectronic chips, which not only reduces the content of impurity ions, but also reduces costs. Thereby, researching the preparation method of tetramethylammonium bicarbonate is the prerequisite for the preparation of high-purity tetramethylammonium hydroxide. [0003] Chinese patent application publication CN10...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/20C07C211/63B01J31/02B01J29/03
CPCB01J31/0274B01J31/0275B01J29/0308C07C209/20B01J2229/32C07C211/63
Inventor 刘颂军孙炜冯亚楠吕国文
Owner 信联电子材料(山东)有限公司
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