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Catalyst for synthesizing Trioctyl/tridecylaklylamines and preparation method and application of catalyst

A technology of octadecyl tertiary amine and catalyst, which is applied in the field of organic synthesis, can solve the problems of increased production cost, increased catalyst consumption, and slow conversion of trioctyl tertiary amine, so as to avoid catalyst deactivation and reduce catalyst wear , to reduce the effect of exposure

Active Publication Date: 2020-10-30
江苏万盛大伟化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the existing method, in order to reduce the by-product aldol condensation, intermediates such as primary amine and secondary amine, it is necessary to maintain the high activity of the catalyst at high temperature, reduce the residence time of the intermediate aldehyde in the reaction system, and generate water It is harmful to the copper-based catalyst. In the existing method, the activity of the catalyst decreases in the late stage of the reaction, resulting in a very slow conversion. The intermediate primary amine, secondary amine, and by-product aldol condensation will increase.
At the same time, the catalyst needs to be replaced in the next batch, resulting in an increase in catalyst consumption, an increase in the production cost of trioctyl tertiary amine, and a large amount of heavy metal waste catalyst.

Method used

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  • Catalyst for synthesizing Trioctyl/tridecylaklylamines and preparation method and application of catalyst
  • Catalyst for synthesizing Trioctyl/tridecylaklylamines and preparation method and application of catalyst
  • Catalyst for synthesizing Trioctyl/tridecylaklylamines and preparation method and application of catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-3

[0077] Embodiment 1-3: Catalyst for preparing long carbon chain aliphatic tertiary amine

[0078] 1. Raw material composition: see Table 1

[0079] Table 1: The proportioning of raw materials in embodiment 1-3

[0080] Example 1 Example 2 Example 3 Copper nitrate trihydrate Cu(NO 3 ) 2 ·3H 2 o

400 400 400 Nickel nitrate hexahydrate Ni(NO 3 ) 2 ·6H 2 o

150 100 100 Zinc nitrate nonahydrate Zn(NO 3 ) 2 ·6H 2 o

80 50 Iron nitrate nonahydrate Fe(NO 3 ) 2 9H 2 o

50 Magnesium nitrate hexahydrate Mg(NO 3 ) 2 ·6H 2 o

70 50 50 ionized water 1600+1000 1600+1000 1600+1000 activated clay 500 500 500 10% sodium carbonate adjust pH adjust pH adjust pH

[0081] 2. Preparation process

[0082] Taking the formula of Example 1 as an example, 400kg Cu(NO 3 ) 2 ·3H 2 O, 150kg Ni(NO 3 ) 2 ·6H 2 O, 80kg Zn(NO 3 ) 2 ·6H 2 O, 70kg Mg(NO 3 ) 2 ·6H 2 O was put in...

Embodiment 4

[0083] Embodiment 4: fixed bed reactor

[0084] Such as Figures 1 to 3 As shown, the fixed bed reactor includes:

[0085] Housing 1, the lower side of the housing 1 is provided with a heat transfer oil inlet 11 and a bottom temperature measurement port 13, and the upper side is provided with a heat transfer oil outlet 12 and a heat transfer oil temperature measurement port 14;

[0086] The upper head 2, the upper head 2 is installed on the upper end of the housing 1, and it is provided with a top temperature measuring port 21, a feed port 22 and a hydrogen or nitrogen gas inlet 23;

[0087]The lower sealing head 3, the lower sealing head 3 is installed on the lower end of the housing 1, and a discharge port 31 is arranged on it, and it is characterized in that it also includes:

[0088] A static distributor 4, the static distributor 4 is arranged in the upper head 2, and the static distributor 4 is provided with several liquid outlet holes 41 communicating with the housing ...

Embodiment 5

[0093] Embodiment 5: the preparation of trioctyl decanyl tertiary amine

[0094] 1. A fixed bed filled with catalyst (prepared in Example 1, height 350cm) (filled as in Example 4, the same below) is gradually heated up to 280°C under a mixture of nitrogen and hydrogen (the volume of nitrogen and hydrogen is 3:1) , and maintain the temperature for reduction for 72 hours, then cool to 200°C for use.

[0095] 2. After replacing the mixed gas in the fixed bed with hydrogen, set the hydrogen pressure to 1.5Mpa, pump in preheated octadecyl alcohol and vaporized liquid ammonia, pump in octadecyl alcohol and liquid ammonia to preheat The molar ratio of alcohol to ammonia is 3:1. The gas-liquid mixture passing through the preheater enters the fixed bed reactor. The temperature of the fixed bed is controlled at 210-230°C and the space velocity is 0.8h. -1 , the material that comes out is condensed to the gas-liquid separation of the oil-water separator, the oil layer is distilled to ob...

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Abstract

The invention discloses a catalyst for synthesizing Trioctyl / tridecylaklylamines and a preparation method and application of the catalyst. The catalyst is prepared from the following raw materials: copper nitrate trihydrate, nickel nitrate hexahydrate, ferric nitrate nonahydrate, magnesium nitrate hexahydrate, zinc nitrate hexahydrate, ionized water, a carrier and 10% soda water. According to themethod for synthesizing the Trioctyl / tridecylaklylamines, reaction raw materials are octyl alcohol and liquid ammonia, a reaction device is a fixed bed filled with the catalyst, and hydrogen serves asshielding gas.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a catalyst for synthesizing trioctadecanyl tertiary amine, a preparation method thereof and an application in the preparation of trioctadecanyl tertiary amine. Background technique [0002] Tri-captydecyl tertiary amine, English: Amines, tri-C8-10-alkyl, CAS number: 68814-95-9, industry code: N235 or 7301, chemical formula C 27 h 57 N, a colorless to light yellow transparent liquid, can be used as a precious metal extraction agent. In the metallurgical industry, it is used to extract and separate precious metals such as uranium, cobalt, molybdenum, nickel, actinides and lanthanides. It is also used in wastewater treatment to extract acidic compounds with benzene rings, especially in wastewater treatment and mineral flotation. Nowadays, the pressure of environmental protection is increasing, and the high-carbon chain lipophilic tertiary amines that can extract organ...

Claims

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Application Information

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IPC IPC(8): B01J23/78B01J23/80B01J37/03B01J35/02C07C209/16C07C211/07B01J8/06
CPCB01J23/78B01J23/80B01J37/03C07C209/16B01J8/06B01J35/00B01J35/30C07C211/07Y02P20/584
Inventor 陈红星赵竹元黄正祥孟小凤薛士林唐毅
Owner 江苏万盛大伟化学有限公司
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