Preparation method for efficient tetramethylammonium hydroxide

A technology of tetramethylammonium hydroxide and tetramethylammonium bicarbonate salt, which is applied in the preparation of amino-substituted functional groups, organic chemistry, electrolysis process, etc., can solve the problems that the cost is difficult to meet market requirements, product pollution, consumption, etc., and achieve The effect of reducing the generation of industrial waste, production safety, and simple process flow

Inactive Publication Date: 2009-12-09
HANGZHOU XINDE ENVIRONMENTAL PROTECTION TECH
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  • Abstract
  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the domestic production of tetramethylammonium hydroxide all adopts the silver oxide method, that is, tetramethylammonium hydroxide is generated by the reaction of tetramethylammonium chloride and silver oxide. The process route of this method needs to consume precious silver oxide, and in the product There are traces of silver ions, which will pollute the product. This production method is difficult to meet the market requirements in terms of quality and cost.

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  • Preparation method for efficient tetramethylammonium hydroxide

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Embodiment 1

[0010] Embodiment 1: the preparation method of this high-efficiency tetramethylammonium hydroxide, make tetramethylammonium bicarbonate salt with dimethyl carbonate and trimethylamine as reaction substance, wherein dimethyl carbonate: the mol ratio of trimethylamine is 1~1.5, and then use the three-chamber two-membrane electrolytic cell method to prepare tetramethylammonium hydroxide; ~100℃, trimethylamine gas space velocity: 50~100kg / h.

[0011] The specific method is: dimethyl carbonate is weighed and poured into the reaction kettle, after being fully mixed, the mixing temperature is controlled to be 30~100°C, trimethylamine is introduced at normal pressure according to the specified flow rate, and the heat preservation reaction is completed for four hours, and then poured into the third chamber Two-membrane electrolyzer for electrolysis, alkali flow at 5m 3 / h, the temperature rise rate is 1.5°C / 10 minutes, the current rise rate is 500A / 3 minutes, and the current rises to ...

Embodiment 2

[0012] Embodiment 2; According to the ionic membrane central control operation described in embodiment 1:

[0013] Confirm the start-up conditions: including the brine section, rectification power supply, public works (water, electricity, gas and gas), etc., have the start-up conditions, and the secondary brine system has the start-up conditions.

[0014] Send direct current to detect membrane leakage: first increase the current to 200A, check the voltage of each cell, and use a multimeter to measure the cell with abnormal voltage. Then increase the current to 500A, and increase the current to 4KA at a speed of 500A / 3 minutes. The conclusion is shown in Table 1.

[0015] Table 1 Conclusion table

[0016]

[0017] Single-tank driving: reduce the current speed to 500A / 3 minutes, check the overflow of lye and light salt water in each unit tank, and prevent the flow from being cut off. Single-tank parking: reduce the current speed to 500A / 3 minutes, check the overflow of lye ...

Embodiment 3

[0021] Embodiment 3: According to the resin tower treatment described in Embodiment 1: the flow rate of brine at full load of the resin tower is 32kg / h, and the two resin towers operate in series when they are normal.

[0022] The premise of resin tower regeneration: when the calcium and magnesium content at the outlet of the first resin tower exceeds 30ppb, it should be regenerated off-line. When the calcium and magnesium content at the outlet of the second resin tower exceeds the standard due to poor regeneration, it should be regenerated off-line. A tower must be regenerated every 48 hours. The basic steps of resin tower regeneration: place the resin tower to be regenerated offline, and run the other tower as a single tower, drain the brine in the tower into the waste water tank for 15 minutes, make the tower half full, and use 8M3 / h pure water Clean the resin tower from top to bottom for 1 hour, and drain the waste liquid into the waste liquid tank. Then fill the resin t...

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Abstract

The invention relates to preparation method for efficient tetramethylammonium hydroxide, which comprises the following steps: methyl-carbonate and trimethylamine are taken as reactive substances to be prepared into tetramethyl ammonium bicarbonate, wherein the molar ratio of methyl-carbonate: trimethylamine is 1 to 1:5; and then a three-room two-membrane electrobath method is used for preparing the tetramethylammonium hydroxide; the reaction is carried out in gap phase and liquid phase; a kettle-type single reactor is used for production; the specific operation conditions thereof are that the pressure is the normal pressure, the temperature is 30 to 100 DEG C, and gas airspeed of the trimethylamine is 50 to 100kg/h. The preparation method has the advantages that an ion-exchange membrane electrodialysis is quite an ideal method for preparing tetramethylammonium hydroxide, firstly, the process flow of the ion-exchange membrane electrodialysis is simpler, secondly, both of the quality and purity of the tetramethylammonium hydroxide products prepared by the ion-exchange membrane electrodialysis can reach very high degree and meet the manufacturing requirements of cutting-edge high-tech industries, in addition, the ion-exchange membrane electrodialysis can effectively reduce the generation of three industrial wastes and has no pollution and the production is relatively safe.

Description

technical field [0001] The invention relates to the field of tetramethylammonium hydroxide, and mainly relates to a preparation method of efficient tetramethylammonium hydroxide. Background technique [0002] Tetramethylammonium hydroxide has two characteristics: (1) The decomposition temperature is low, and it becomes gas after decomposition, leaving no residue; (2) It is an organic strong base, completely ionized in water, and has low metal content . The characteristics of tetramethylammonium hydroxide make it widely used in chemical production and semiconductor fields, and there are very high requirements for the quality and quantity of tetramethylammonium hydroxide: the mass concentration of chloride ions in 20% TMAH solution shall not exceed 5mg / L, and the mass concentration of various metal ions must be less than 0.01mg / L. Tetramethylammonium hydroxide is mainly used in the synthesis of organic silicon to play a catalytic role. It is to open the organic silicon ring...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B3/00C07C211/63C07C209/20
Inventor 吴建华唐文忠惠健朱大明
Owner HANGZHOU XINDE ENVIRONMENTAL PROTECTION TECH
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