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Method for preparing ethanolamine hydrochlorides and coproduct ethanolamine

A technology of ethanolamine hydrochloride and ethanolamine, applied in chemical instruments and methods, preparation of organic compounds, preparation of amino hydroxyl compounds, etc., can solve the problems of many side reactions, high energy consumption, high reaction temperature, etc., to ensure product quality, The effect of less investment and increased energy consumption

Inactive Publication Date: 2012-01-04
薛荔
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to provide a high-quality, energy-saving and environmentally friendly method for preparing ethanolamine hydrochloride and co-product ethanolamine, which solves the reaction problem in the prior art High temperature, many side reactions, low efficiency, difficult dehydration, high energy consumption, etc. The reaction conditions are relatively easy, the investment in equipment is small, and the cost is significantly reduced. The by-product is table salt, which can be recycled and comprehensively utilized

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Example 1 Simultaneous preparation of mono, di and triethanolamine hydrochloride

[0033] Mix 214g (4 moles) of ammonium chloride in 150ml of water, add 204g of EO for the first time under stirring in the reactor, gradually raise the temperature to 50-60°C, and wait until the pressure of the kettle is zero, and the reaction ends. Nitrogen was introduced into the kettle to blow off the residual raw material EO. Remove the water under reduced pressure and bring it down to room temperature, fold the crystals and filter, wash with a small amount of methanol, drain, and vacuum-dry at a temperature of ≤50°C to obtain 195 g of industrial grade MEA·HCl, with a yield of about 50%.

[0034] After recovering the methanol from the lotion, combine it with the above-obtained filtrate, and then inject the remaining 264 grams (468 grams in total) of EO under stirring in the reactor, and gradually increase the temperature and control it at 70°C to 100°C until the reaction is complete....

Embodiment 2

[0037] Example 2 Preparation of technical grade monoethanolamine hydrochloride

[0038] Mix 214 grams (4 moles) of ammonium chloride in 150 ml of water, put 200 grams of EO into the reactor, gradually raise the temperature to 50-60 ° C, wait until the pressure of the kettle is zero, and the reaction is completed, and then blow nitrogen into the kettle. Clean the remaining raw material EO, remove the water under reduced pressure, drop to room temperature, fold crystals and filter, wash with a small amount of water, drain and dry to obtain 234 g of industrial grade MEA·HCl, with a yield of about 60%.

[0039] The above obtained filtrate and lotion are combined for feeding in the next batch.

Embodiment 3

[0040] Example 3 Preparation of technical grade triethanolamine hydrochloride

[0041] Mix 214 grams of ammonium chloride in the combined filtrate and washing liquid of the previous batch, and inject 530 grams of EO in batches for addition reaction, gradually increase the temperature, and react at 70 ° C ~ 100 ° C, the pressure of the reactor is controlled at ≤ 0.3Mpa , the pressure begins to drop gradually in the later stage, until it stops falling, the reaction ends, excess EO is removed and recovered, nitrogen is blown into the kettle to remove residual raw material EO, water is removed under reduced pressure, crystallization is carried out by cooling, filtered, and rinsed with a small amount of ethanol. Drained and dried to obtain about 668 g of technical grade TEA·HCl, yield 90%. The ethanol was recovered from the washing solution and combined with the above filtrate for later use.

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Abstract

The invention provides a method for preparing ethanolamine hydrochlorides and a coproduct ethanolamine, which comprises the following steps: carrying out addition reaction on ammonium chloride, which is used as a raw material, and EO (ethylene oxide), adjusting to a proper ratio to firstly synthesizing MEA.HCl (monoethanolamine hydrochloride) and DEA.HCl (diethanolamine hydrochloride), and separating out the MEA.HCl by utilizing the differences of physical properties; continuing adding the EO into the filtrate, sealing the reaction kettle, and gradually heating to react, wherein the reaction pressure must be sufficient to prevent the EO from gasifying at the reaction temperature, and the reaction temperature can be raised to 100 DEG C or so, so that the conversion rate of the TEA.HCl (triethanolamine hydrochloride) is maximized; cooling to room temperature, filtering, and drying to obtain the TEA.HCl; and merging the washing liquid and the filtrate, and dehydrating to obtain the DEA.HCl. The ethanolamine hydrochloride can be respectively dissociated in the presence of sodium hydroxide or sodium methoxide to obtain the MEA, DEA and TEA according to market demands.

Description

technical field [0001] The invention relates to a method for preparing petrochemical raw materials, in particular to a method for directly preparing ethanolamine hydrochloride and co-product ethanolamine through addition reaction of relatively cheap ammonium chloride and ethylene oxide. Background technique [0002] Ethanolamine hydrochloride. It is the general term for monoethanolamine hydrochloride (MEA·HCl), diethanolamine hydrochloride (DEA·HCl), and triethanolamine hydrochloride (TEA·HCl). Its direct preparation method has not been reported in the literature. Existing ethanolamine hydrochloride is generally obtained by using ethanolamine products as production raw materials, adding them dropwise to equimolar concentrated hydrochloric acid for salt formation reaction, and then dehydrating under reduced pressure at a controlled temperature of 50-150°C. Among them, MEA·HCl is an anionic surfactant, which is the raw material for the green chemical synthesis technology of p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C215/08C07C215/12C07C213/04
CPCC07C215/12C07C215/08C07C213/04
Inventor 薛守礼薛芳薛荔
Owner 薛荔
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