Steric hindrance amine desulfurizing agent and preparation method thereof

A technology of sterically hindered amines and desulfurizers, applied in separation methods, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of complex reactions and great differences in reaction rates, and achieve large absorption capacity, low operating costs, Good desulfurization selectivity

Inactive Publication Date: 2015-02-18
SOUTHWEST PETROLEUM UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

while CO 2 The reaction between amines and amines is very complicated. A large number of studies have shown that CO 2 The reaction mechanism of primary amine, secondary amine and tertiary amine is different, and the reaction rate is very different

Method used

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  • Steric hindrance amine desulfurizing agent and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] A. Put 103.90ml of tert-butylamine with a purity of ≥99.0%, 32.9121g of 1,3-dichloro-2-propanol with a content of 98%, and 100ml of absolute ethanol into the reactor, heat to 130-145°C, and pressurize Respond for 2.0 hours;

[0024] B. Pour out the above reactant after cooling to 70°C, add saturated NaOH solution (10%), neutralize and react under reflux for 0.5 hours, then cool to ≤30°C;

[0025] C, the neutralized solution is extracted with ethyl acetate (3 * 70ml), to obtain the upper layer extract;

[0026] D. Dry the extract in C with anhydrous magnesium sulfate for 2 hours, and filter.

[0027] E. The liquid in D was distilled under reduced pressure and crystallized by cooling to obtain 48.6015 g of the target crystal, which was analyzed as 1,3-di-tert-butylaminoisopropanol by infrared and nuclear magnetic chromatography, with a yield of 96.1%.

Embodiment 2

[0028] Embodiment 2 The process steps of this embodiment are the same as those of Embodiment 1.

[0029] First, put 52..20ml of tert-butylamine with a purity of ≥99.0%, 16.4846g of 1,3-dichloro-2-propanol with a content of 98%, and 50ml of UP-grade pure water into the reactor, and heat it to 130-145°C. Reaction under self-pressure for 2.0 hours, cooled to about 65°C and poured out, then added saturated NaOH solution and refluxed and neutralized at 80°C for 0.5 hours, then cooled to about 25°C, extracted with EA, dried, filtered, and reduced Cooling and crystallization after pressure distillation yielded 24.1796 g of 1,3-di-tert-butylaminoisopropanol with a yield of 95.6%.

Embodiment 3

[0030] Example 3 In this example, distilled water and absolute ethanol were used as the reaction medium. 51.90ml of tert-butylamine, 16.4832g of 1,3-dichloro-2-propanol, 25ml of water, and 25ml of absolute ethanol were mixed and placed in a reaction kettle. The reaction temperature is 130-145°C. After 2.0 hours of self-pressurized reaction, cool down to 65°C together with the reactor and pour it out, then add saturated NaOH solution and reflux at 70°C for 0.5 hours, then lower the temperature to room temperature (about 28°C) , extracted with EA, dried, filtered, and distilled under reduced pressure, then cooled and crystallized to obtain 24.2793 g of 1,3-di-tert-butylaminoisopropanol, with a yield of 96.0%.

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Abstract

The invention belongs to the technical field of preparation of chemical reagents, and in particular relates to a preparation method for steric hindrance amine desulfurizing agent 1, 3-bi-tert-butylamine-2 propanol. 1, 3-bi-tert-butylamine-2 propanol crystals can be prepared through the following steps: adding 1, 3-dichloro-2 propanol and tert-butylamine, of which the proportion is 1: 2-4, as well as a reaction medium of which the inventory is 20-200wt% of the total inventory of the raw materials in percentage by weight into a reaction kettle, and performing self-compression reaction for 2-3 hours, and performing alkali neutralization reaction, extraction, drying, filtration, reduced pressure distillation and cooling crystallization on the reaction product to obtain the 1, 3-bi-tert-butylamine-2 propanol crystals. The desulfurizing agent synthetized by the preparation method disclosed by the invention has the advantages that the steric hindrance is large, the boiling point is high, the selectivity of a desulphurization process is greatly improved, and the usage scope is greatly expanded, so that the economic benefits, the environmental benefits and the social benefits of a gas purification technology of sulfur containing natural gas, refinery gas, liquified gas and the like are improved.

Description

technical field [0001] The invention belongs to the technical field of preparation of chemical reagents, in particular to a preparation method of 1,3-di-tert-butylamino-2-propanol, a sterically hindered amine desulfurizer. Background technique [0002] Sulfur-containing natural gas, refinery gas, and liquefied petroleum gas must be desulfurized before they can be used. The method is mainly amine desulfurization. In recent years, in CO 2 In the presence of a large amount, the selective absorption of H 2 S technology has received more and more attention. Because it not only saves equipment investment, reduces operating costs, but also can handle high CO 2 / H 2 The exhaust gas of the CLAUS device with S ratio meets the increasingly stringent environmental protection requirements. [0003] At present, the selective removal of H 2 There are two methods of S: thermodynamic selective desulfurization and kinetic selective desulfurization. Thermodynamic selective desulfurizati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D53/14C07C213/04C07C215/18
Inventor 诸林郭晓丹杨超越陈倬唐诗焦文超
Owner SOUTHWEST PETROLEUM UNIV
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