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Process for producing tertiary butylamine ethoxy ethyl alcohol with space steric effect

A technology of tert-butylaminoethoxyethanol and steric hindrance effect, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of aminohydroxyl compounds, etc., which can solve the problem of large volatilization loss, increased purification cost, and reduced economic benefits and other problems, to achieve the effect of high solvent boiling point, saving operating costs, and high purification efficiency

Inactive Publication Date: 2005-06-08
四川省精细化工研究设计院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As a selective desulfurization solvent, N-methyldiethanolamine (MDEA) is increasingly unsatisfactory for higher CO 2 The demand for gas purification treatment with high content and acid gas load
In view of this situation, the applicant adds 5 to 20% of the amine solvent tert-butylaminoethanol (TBE) with steric hindrance effect to the traditional selective desulfurization solvent N-methyldiethanolamine, and then mixes and stirs it evenly to prepare Composite organic desulfurization solvent, although the solvent has the ability to convert H 2 The selectivity of S is increased by about 30%, and the energy saving is more than 25%. However, since the boiling point of tert-butylaminoethanol is only 90°C (25mmHg), it is highly volatile, and will cause a large amount of solvent volatilization under most acid gas purification temperature conditions. , increase purification cost and reduce economic benefits
Therefore, this technology has defects such as low boiling point, large volatilization loss, and high cost of use.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] A. 2 liters of ethanol with a purity of 97%, 657g of tert-butylamine with a content of 95%≥, and 450g of 2-chloroethoxyethanol are put into the reactor, heated to 100-120°C, and reacted under self-pressure for 2.0 hours;

[0013] B. After cooling the above reactant to 60°C, add 220g of KOH with a content of 95%, and neutralize it under reflux for 1.0 hour, then cool to ≤30°C to recover excess tert-butylamine;

[0014] C, the filtrate after above-mentioned solution filtration is placed in crude distillation under 160 ℃ of temperature and 0.03MPa vacuum;

[0015] D. After rectifying the crude distillate obtained from C at a temperature of 190° C. and a vacuum condition of 0.03 MPa, 442 g of a tert-butylaminoethoxyethanol product was obtained. The content of this product was 95.8% through chromatographic analysis.

Embodiment 2

[0017] The processing steps of this embodiment are the same as those of Embodiment 1.

[0018] First, mix 91g of tert-butylamine of industrial purity, 62g of 2-chloroethoxyethanol and 200ml (milliliters) of methanol into a 600-liter reactor, and react under pressure at 145°C for 1.5 hours, then cool to about 50°C, and then Add 22g of NaOH with a content of 98% and neutralize under reflux for 1.0 hour, then cool to about 25°C to recover excess tert-butylamine; then filter, reduce pressure, crude distillation and rectification to obtain tert-butylaminoethoxy Ethanol product 62g, product content 95.6%.

Embodiment 3

[0020] In this embodiment, water is used as the reaction medium, 46g of tert-butylamine, 31g of 2-chloroethoxyethanol (both industrially pure) and 30ml of water are mixed, placed in a steel reaction kettle, the reaction temperature is 160°C, and the pressure is 0.6-0.7MPa After reacting for 50 minutes, cool down to 65°C together with the reactor, then add 11g of 98% NaOH for neutralization treatment for 45 minutes, lower the temperature to room temperature (about 28°C) and recover excess tert-butylamine, then filter the reactant; The filtrate was crudely distilled at a temperature of 170°C and a pressure of 0.04MPa; the distillate was further rectified at a temperature of 190°C and a pressure of 0.04MPa to obtain 33g of a product with a content of 98.1%. In this embodiment, the reaction speed is fast, the effect is good, the medium does not need to be recycled, and the technical and economic benefits are obvious.

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Abstract

A process for preparing the tert-butylamino ethoxyethanol as the selective desulfurizing solvent with sterical hindering effect includes such steps as putting tert-butylamine, 2-chloroethyoxy ethanol and reaction medium in reactor, heating while reaction, alkali neutralizing, condensing to recover excessive tert-butylamine, filtering, distilling, and rectifying. Its advantages are high selectivity and absorptivity to H2S, high boilding point and high purification.

Description

technical field [0001] The invention belongs to a production method of a selective desulfurization solvent, in particular to a production method of a hindered amine desulfurization solvent tert-butylaminoethoxyethanol with steric hindrance effect. Background technique [0002] Traditionally used for CO removal from acid gases 2 and H 2 The solvent of S, N-methyldiethanolamine (MDEA), has been widely used at home and abroad for a long time, and it is very useful for the treatment of CO 2 The content is relatively low (CO 2 / H 2 S < 1.0) gas or used under the condition of small acid gas load (acid gas / amine ≤ 0.2), for H 2 S has a good selective removal effect, and can save energy by about 40% compared with ordinary amine solvents. But for handling CO 2 Higher content (CO 2 / H 2 S > 1.0) or gas with a large acid load (acid gas / amine > 0.2), the selectivity deteriorates significantly. In recent years, high CO 2 The content of gas, such as coal gas, oilfield a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C213/08C07C217/28
Inventor 高峻李世荣蒋吉平杨玉斌钟明黄淑芬
Owner 四川省精细化工研究设计院
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