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Method for synthesizing tris(dioxa-3,6-heptyl)amine

A technology for dioxeptyl and synthesis methods, which is applied in chemical instruments and methods, preparation of aminohydroxy compounds, preparation of organic compounds, etc., can solve the problems of poor selectivity and high reaction temperature, achieve high selectivity and reduce reaction temperature , improve the effect of selectivity

Inactive Publication Date: 2011-01-19
浙江皓华制药有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Experiments have confirmed that a single Raney nickel catalyzes the above reaction, which has the disadvantages of high reaction temperature and poor selectivity.

Method used

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  • Method for synthesizing tris(dioxa-3,6-heptyl)amine
  • Method for synthesizing tris(dioxa-3,6-heptyl)amine
  • Method for synthesizing tris(dioxa-3,6-heptyl)amine

Examples

Experimental program
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Effect test

preparation example Construction

[0020] Preparation of skeleton Cu-Ni catalyst:

[0021] (1) 315kg of 20% sodium hydroxide solution is put into a 1000L reactor, the stirring and cooling water are turned on, the temperature is controlled at 30°C, and 100kg of alloy powder (Cu 12.5%, Ni 37.5%, Al 50%) is put into the reactor in batches. About 2 hours, then heat up to 90°C, react for 2 hours, add 500kg of water, cool down to 30°C, let stand for 20 minutes, suck the upper layer of water by vacuum, add 500kg of water to stir, let stand, remove water, until pH 7~8 , the skeleton catalyst of making skeleton Cu-Ni catalyst A 62.5kg, under the protection of water is put into barrel for standby, wherein Cu content is 20%.

[0022] (2) Repeat the above preparation method with 100kg of alloy powder (Cu 20.5%, Ni 29.5%, Al 50%) to obtain 68.3Kg of skeleton Cu-Ni catalyst B, wherein Cu content is 30%.

[0023] (3) Repeat the above-mentioned preparation method with 100kg alloy powder (Cu10.5%, Ni39.5%, Al50%), obtain skele...

Embodiment 1

[0024] Embodiment 1: Get 250kg Diethylene Glycol Monomethyl Ether (mass purity 99%), 50kg skeleton Cu-Ni catalyst A, drop into enamel kettle, stir and heat up dehydration, when the temperature in the kettle reaches 150 ℃, start to pass ammonia and hydrogen, pass Ammonia 8m 3 / hour, hydrogen flow 1m 3 / hour, excess ammonia was absorbed by a falling film absorption tower, and after ventilating for 5 hours, it was detected that the mass ratio of diethylene glycol monomethyl ether and 3,6-dioxaheptylamine in the reaction solution was 2.0:1.

[0025] Stop logical ammonia then, after continuing logical hydrogen 2.5 hours, detect and find in the reaction solution: Diethylene glycol monomethyl ether mass percentage drops to 1.8%, formula (7) mass percentage drops to 0.5%, formula (4) mass percentage drops to 1.2%, target product 95.2%, other 1.3%.

[0026] The catalyst was removed by filtration, and 205.26 kg of the product tris(3,6-dioxaheptyl)amine was obtained by rectification,...

Embodiment 2

[0027] Embodiment 2: Get 250Kg Diethylene Glycol Monomethyl Ether (mass purity 99%), 100kg framework Cu-Ni catalyst B, drop into enamel kettle, stir and heat up dehydration, when the temperature in the kettle reaches 130 ℃, start to pass ammonia and hydrogen, pass Ammonia 10m 3 / hour, hydrogen flow 1.1375m 3 / hour, excess ammonia was absorbed by a falling film absorption tower, ventilated for 4.0 hours, and it was detected that the mass ratio of diethylene glycol monomethyl ether and 3,6-dioxaheptylamine in the reaction solution was 1.9:1.

[0028] Then stop flowing ammonia, continue to pass hydrogen after 2 hours and 10 minutes, detect and find in the reaction solution: Diethylene glycol monomethyl ether mass percentage drops to 2.0%, formula (7) mass percentage drops to 0.4%, formula (4) mass percentage Down to 1.2%, target product 95%, other 1.4%.

[0029] The catalyst was filtered off, and 204.81 kg of tris(3,6-dioxaheptyl)amine was obtained by rectification, with a ma...

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Abstract

The invention relates to a method for synthesizing tris(dioxa-3,6-heptyl)amine. The conventional method for synthesizing the tris(dioxa-3,6-heptyl)amine has low selectivity, low yield and long production period. The method comprises the following steps of: catalyzing diglycol simple methyl ether serving as a raw material by a framework Cu-Ni bimetallic catalyst in the absence of solvent; and introducing hydrogen and ammonia under normal pressure and at the temperature of between 130 and 150 DEG C with stirring so as to synthesize the tris(dioxa-3,6-heptyl)amine, wherein the feeding volume ratio of the hydrogen to the ammonia is controlled to be 1:(5-10); and when the mass ratio of the diglycol simple methyl ether to 3,6-dioxa amine in reaction solution reaches (1.5-2):1, ammonia introducing is stopped and hydrogen introducing speed is not changed until the mass percentage of the diglycol simple methyl ether is less than or equal to 2 percent. The method has the advantages of high selectivity, high yield, convenient subsequent separation and suitability for industrialized production and the production and preparation of the tris(dioxa-3,6-heptyl)amine.

Description

technical field [0001] The invention relates to a synthesis method of tris(3,6-dioxaheptyl)amine. Background technique [0002] Tris(3,6-dioxaheptyl)amine is an excellent surfactant and phase transfer catalyst. [0003] Regarding the synthesis and application of tris(3,6-dioxaheptyl)amine, Fine Chemical Industry 1998, Volume 15, page 208, "Synthesis of Tris(3,6-dioxaheptyl)amine and Its PTC Catalytic Activity "The article has comparatively detailed narration, and US6403834 and US4408075 documents also all relate to the synthesis of this product, but a general characteristic of seeing document report is to use Raney nickel as catalyst, and the selectivity of tertiary amine is lower, and the total yield Low, not conducive to industrial production. [0004] The tri(3,6-dioxaheptyl)amine involved in the present invention has a structural formula such as formula (1): [0005] [0006] In the synthesis process based on the mechanism of alcohol reductive amination, its main i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C217/08C07C213/02
Inventor 方慧忠方明奎方明朋王立虎
Owner 浙江皓华制药有限公司
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