Preparation method of molecular sieve template high-purity hexamethonium hydroxide water solution

A technology of hexamethyldiammonium hydroxide and hexamethyldiammonium, which is applied in the direction of ammonium halide, electrolysis process, electrolysis components, etc., can solve the problems of poor product quality, residual silver ions, and high cost of precious metal raw materials, so as to improve service life and reduce production cost effect

Active Publication Date: 2017-01-25
KENTE CATALYSTS INC
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  • Application Information

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Problems solved by technology

The disadvantage is: the cost of using precious metal raw materials is too high, and there will be a small amount of silver ion residue
Defects are: there are flammable and explosive organic solvents in the product, the product yield is about 85% low, the product quality is poor, and the content of halide ions and alkali metal ions in the product reaches about 2000PPM, which is used as a template to prep...

Method used

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  • Preparation method of molecular sieve template high-purity hexamethonium hydroxide water solution
  • Preparation method of molecular sieve template high-purity hexamethonium hydroxide water solution
  • Preparation method of molecular sieve template high-purity hexamethonium hydroxide water solution

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Embodiment 1

[0021] The preparation method of molecular sieve template agent high-purity hexamethonium hydroxide aqueous solution includes the following steps: (1) 112g (1mol) of 1,6-hexamethylenediamine is dissolved in 168g of water to prepare a 40% aqueous solution, which is added dropwise into a 2L reaction bottle In the mixture of 405g (5mol) of 37% formaldehyde solution and 281g (6mol) of 98% formic acid; stir, reheat, react at 80°C~100°C for 24 hours, add 288g (7mol) of 97% sodium hydroxide to adjust the pH value to 12~14, separate layers, take the organic layer, rectify under reduced pressure, vacuum degree -0.098MPa, remove the front fraction, collect the fraction at 120°C~140°C, and obtain 99% tetramethylhexyl Diamine 172g, the yield reaches more than 99%. (2) Weigh 172g (1mol) of tetramethylhexamethylenediamine dissolved in 80g (2.5mol) of methanol and 246g (6mol) of acetonitrile, add it to a 1L pressure reactor, and feed 111g (2.2mol) of methyl chloride, At a reaction temperatu...

Embodiment 2

[0023]The preparation method of the molecular sieve template agent high-purity hexamethonium hydroxide aqueous solution comprises the following steps: (1) The preparation of tetramethylhexamethylenediamine is the same as in Example 1. (2) Weigh a mixture of 172g (1mol) of tetramethylhexamethylenediamine dissolved in 80g (2.5mol) of methanol and 246g (6mol) of acetonitrile, add it to a 1L pressure reactor, and feed 208g (2.2mol) of methyl bromide into the At a reaction temperature of 100°C and a pressure of 0.05MPa, the reaction was continued for 48 hours, cooled to 0-5°C, centrifuged, the solvent was recovered and applied mechanically, and the solid was dried at 80°C for 4 hours to obtain 357g of hexamethyldiammonium bromide, with a yield of about 98.62% . (3) Hexamethyldiammonium bromide is dissolved in pure water and enters the raw material room of the three-cavity two-membrane electrolyzer, the three-cavity two-membrane electrolyzer, the anode plate is a titanium substrate ...

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Abstract

The invention discloses a preparation method of a molecular sieve template high-purity hexamethonium hydroxide water solution. The method comprises the following steps: dissolving 1,6-hexamethylenediamine in a formaldehyde-formic acid mixed solution to obtain tetramethyl hexamethylenediamine, dissolving the prepared tetramethyl hexamethylenediamine in a methanol-acetonitrile mixture, introducing methyl chloride or bromomethane to prepare hexamethonium halide, finally adding the hexamethonium halide water solution into a three-chamber two-membrane electrolysis bath, and carrying out electrolysis to obtain the high-purity hexamethonium hydroxide water solution with low concentrations of metal ions, halogen ions and residual organic solvents. By adopting the technical scheme, the preparation method implements green high-yield low-cost industrial production of the hexamethonium hydroxide water solution.

Description

technical field [0001] The invention relates to a preparation method of a high-purity hexamethonium hydroxide aqueous solution as a molecular sieve template agent. Background technique [0002] Since the mid-1950s, the preparation and application of zeolite molecular sieves have developed rapidly, and the comprehensive development from low-silicon-alumina to medium-silicon-alumina and even high-silicon-alumina has greatly promoted the application of molecular sieves and the development of the industry. Among them, the application of templates in synthesis has brought a qualitative leap in the synthesis of molecular sieves. Templating agents act as structural templates during the formation of molecular sieves, leading to the generation of special structures with specific catalytic functions. Some molecular sieves have only found extremely limited templates, and can even be successfully synthesized only under the action of the only matching template. Hexamethyldiammonium hyd...

Claims

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Application Information

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IPC IPC(8): C25B3/00C01C1/16
CPCC01C1/16C25B3/00
Inventor 项飞勇吴尖平王新伟
Owner KENTE CATALYSTS INC
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