Method for preparing MNPA, DNPA and TNPA

A new technology of propanolamine and propanolamine hydrochloride is applied in chemical instruments and methods, preparation of organic compounds, preparation of amino hydroxyl compounds, etc. It can solve the problems of decomposition into propylene glycol, simple investment and low investment, and achieve product quality Good, low equipment requirements, and the effect of reducing production costs

Inactive Publication Date: 2012-09-12
薛荔
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The purpose of the present invention is to provide a method for preparing new propanolamine, which solves the problem of side reactions such as the decomposition of raw material PO into propylene glycol under alkaline conditions. It adopts cheap ammonium chloride instead of liquid ammonia, and the relative temperature and pressure of the preparation process are relatively high Low cost, simple equipment, low investment, easy separation of main products, good quality, energy saving, emission reduction, low carbon, and environmental protection; the only by-product sodium chloride can be used to produce ammonium chloride as a raw material for self-use, and the added value is relatively high sodium bicarbonate products

Method used

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  • Method for preparing MNPA, DNPA and TNPA

Examples

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Embodiment 1

[0034] Mix 214 grams (4 moles) of ammonium chloride in 144 ml of deionized water, then inject nitrogen to replace the air in the autoclave to evacuate, and then inject nitrogen repeatedly to remove the air. After that, start to inject 280 grams of PO under stirring, gradually increase the temperature and control the reaction to 60~80°C, and control the pressure to ≤0.3MPa. After the pressure in the kettle is reduced to zero (gauge pressure), the reaction is completed. Nitrogen was introduced into the kettle to blow off the residual PO, recovered by ammonium chloride aqueous solution, dehydrated under reduced pressure, cooled, crystallized and filtered, washed with a small amount of water, drained, and vacuum-dried at ≤ 50°C to obtain MNPA. HCl, then add it to the methanol solution with equivalent caustic soda under stirring, free MNPA, filter out most of the sodium chloride at lower temperature, recover methanol, remove water and distill under reduced pressure, control 20mmHg a...

Embodiment 2

[0037] Mix 214 grams of ammonium chloride in 144 ml of deionized water, then inject nitrogen to replace the air in the reactor, vacuumize the air to remove it, then inject a total of 280 grams of PO under stirring, gradually increase the temperature and control the reaction to 60~80 ° C, the pressure ≤ 0.3MPa, until the internal pressure of the kettle reaches zero reaction. Recover residual PO, remove water under reduced pressure, cool down, crystallize and filter, wash the filter cake with methanol, drain, and dry to obtain MNPA. About 90 grams of HCl was recovered from the washing liquid and combined with the filtrate, and put into the kettle together with the "MNPA.HCl, TNPA.HCl mixture" in Example 1, and gradually injected about 230 grams of PO under stirring. Pressure ≤ 0.3MPa, stop injecting PO until the gauge pressure does not drop, and then stir for 30 minutes to complete the reaction, recover excess PO, remove water, cool down, crystallize and filter, wash with methan...

Embodiment 3

[0039] Get MNPA in embodiment 2. Add 100 grams of dry HCl to the methanol solution containing the equivalent of sodium methoxide in portions, free MNPA under stirring, filter out sodium chloride, recover methanol, and then distill under reduced pressure, control 20mmHg to take a fraction at about 81-83°C to obtain MNPA , content ≥ 95%,.

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Abstract

The invention provides a method for preparing MNPA, DNPA and TNPA. The method comprises the following steps: taking PO and ammonium chloride as raw materials for reacting; adding water, ammonium chloride and the PO into a reaction kettle; gradually injecting partial PO while stirring; reacting and synthesizing MNPA.HCL and partial DNPA.HCL under the conditions of temperature at 60-80 DEG C and pressure control lower than or equal to 0.3MPa; separating the MNPA.HCL by utilizing the difference of physical property; injecting the remained PO into filtrate; reacting at 70-100 DEG C; cooling, filtering and drying, thereby obtaining TNPA.HCL; merging the cleaning solution with the filtrate, and then dehydrating, thereby obtaining the DNPA.HCL; and respectively reacting the three hydrochlorides with equivalent methanol alkali, thereby obtaining MNPA, DNPA and TNPA. The method has unique advantages; the relative temperature and pressure are lower during the preparation process; the equipment is simple and is low in investment; the main products are easily separated; the raw material PO is prevented from being subjected to side reactions, such as hydrolyzing into propylene glycol, and the like, under an alkali condition; the energy-saving, emission-reducing, low-carbon and environment-friendly effects are achieved; and the only byproduct sodium chloride is used as a self-use raw material for producing the ammonium chloride and sodium bicarbonate with relative high additional value is obtained.

Description

technical field [0001] The present invention relates to a preparation method of petrochemical raw materials, in particular, the addition reaction of ammonium chloride and propylene oxide (PO) is carried out at a relatively cheap price, and new propanolamine hydrochloride is firstly prepared, which is freed from alcohol and alkali. Process for the preparation of neopropanolamines. technical background [0002] Propanolamine is a propanol compound containing an amino group, which is divided into three isomers: 3-amino-1-propanol (n-propanolamine), 1-amino-2-propanol (isopropanolamine, MIPA ), 2-amino-1-propanol (new propanolamine, MNPA); the former is prepared by ethylene cyanohydrin route and hydrogenation. The latter two are derived from propylene oxide as raw material. They have three derivative compounds respectively. This paper mainly discusses the latter two compounds. [0003] The synthesis of isopropanolamine was first seen in the US patent (US1988225) in 1935; unt...

Claims

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Application Information

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IPC IPC(8): C07C215/08C07C215/12C07C213/04
Inventor 薛守礼郭开兴孙源谦薛芳薛荔
Owner 薛荔
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