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Preparation method of tris(2-ethylhexyl)amine

A technology of triisooctylamine and diisooctylamine, which is applied in the field of preparation of triisooctylamine, can solve the problems of unfavorable industrial production, difficult acquisition of raw material isooctyl aldehyde, and high price, and achieves simple post-processing, simple operation, high cost, and high cost. active effect

Inactive Publication Date: 2018-01-09
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

The main disadvantage is that the raw material isooctylaldehyde is not easy to obtain, and the price is high, which is not conducive to industrial production

Method used

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  • Preparation method of tris(2-ethylhexyl)amine
  • Preparation method of tris(2-ethylhexyl)amine
  • Preparation method of tris(2-ethylhexyl)amine

Examples

Experimental program
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Effect test

Embodiment 1

[0042] Catalyst preparation: Cu(NO 3 )2·3H 2 O, Ni(NO 3 )2·6H 2 O, Zn(NO 3 )2·6H 2 O, Mg(NO 3 )2·6H 2 Dissolve O in a certain amount of water, acetone or ethylene glycol, and then add ZrO corresponding to the volume of the solution 2 As a catalyst carrier, stir evenly to form a paste, age in a water bath at 50±5°C for 5±1h, filter and dry with suction, roast at 450±10°C for 4±0.5h, and crush to below 200 mesh to obtain the catalyst.

[0043] Put diisooctylamine (400g) and catalyst (20g) into a 1-liter four-necked reaction flask equipped with a hydrogen circulation and water separation device. After nitrogen replacement and hydrogen replacement, reduce the catalyst at 200-210°C for 2 hours, then add isooctyl alcohol (260g) dropwise, the reaction temperature is 200-210°C, water is continuously generated during the reaction, and after 20 hours, almost no water is produced. Sampling GC analysis, di-isooctylamine 1%, tri-isooctylamine 74%. The obtained crude product is dir...

Embodiment 2

[0045] Catalyst preparation: Cu(NO 3 )2·3H 2 O, Ni(NO 3 )2·6H 2 O, Zn(NO 3 )2·6H 2 O, Mg(NO 3 )2·6H 2 O is dissolved in a certain amount of water, acetone or ethylene glycol, and then Ca is added corresponding to the volume of the solution 2 CO 3 As a catalyst carrier, stir evenly to form a paste, age in a water bath at 50±5°C for 5±1h, filter and dry with suction, roast at 450±10°C for 4±0.5h, and crush to below 200 mesh to obtain the catalyst.

[0046] Diisooctylamine (450g) and catalyst (20g) were put into a 1 liter four-necked reaction flask equipped with a hydrogen circulation and water separation device. After nitrogen replacement and hydrogen replacement, reduce the catalyst at 190-200°C for 2 hours, then add isooctyl alcohol (260g) dropwise, the reaction temperature is 200-210°C, water is continuously generated during the reaction, and after 18 hours, almost no water comes out. Sampling GC analysis, di-isooctylamine 2%, tri-isooctylamine 80%. The obtained cru...

Embodiment 3

[0048] Catalyst preparation: Cu(NO 3 )2·3H 2 O, Ni(NO 3 )2·6H 2 O, dissolved in a certain amount of water, acetone or ethylene glycol, and then add Ca corresponding to the volume of the solution 2 CO 3 As a catalyst carrier, stir evenly to form a paste, age in a water bath at 50±5°C for 5±1h, filter and dry with suction, roast at 450±10°C for 4±0.5h, and crush to below 200 mesh to obtain the catalyst.

[0049] Diisooctylamine (450g) and catalyst (20g) were put into a 1 liter four-necked reaction flask equipped with a hydrogen circulation and water separation device. After nitrogen replacement and hydrogen replacement, reduce the catalyst at 190-200°C for 2 hours, then add isooctyl alcohol (260g) dropwise, the reaction temperature is 200-210°C, water is continuously generated during the reaction, and after 18 hours, almost no water comes out. Sampling GC analysis, di-isooctylamine 3%, tri-isooctylamine 78%. The obtained crude product is directly used in the rectification ...

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Abstract

The invention discloses a preparation method of tris(2-ethylhexyl)amine. The preparation method comprises preparation steps as follows: nitrogen displacement is performed, after nitrogen displacement,bis(2-ethylhexyl)amine and a catalyst are subjected to a reduction reaction at the temperature of 180-230 DEG C, isooctyl alcohol is dropwise added, hydrogen circulation and heating reaction are performed, a crude tris(2-ethylhexyl)amine product is obtained after no water is produced basically, and a product is obtained through distillation, wherein the content of the product is higher than 98wt%. A small amount of unreacted isooctyl alcohol can be recycled, the operation is simple, and no corrosive or irritant substances are produced in the production process, so that corrosion to productionequipment and pollution to the environment are prevented. The catalyst has higher activity, selectivity and stability, aftertreatment is simple, the catalyst can be recycled, and industrialization isfacilitated; conversion rate of isooctyl alcohol is as high as 89.5%, and product selectivity is as high as 81.3%.

Description

Technical field [0001] The invention belongs to the field of organic synthesis, and specifically relates to a preparation method of triisooctylamine. Background technique [0002] Tris(2-ethylhexyl)amine is a special secondary amine product. It is a colorless to yellow liquid compound with an amine smell. The chemical formula is C 24 H 51 N. CAS number is 1860-26-0, molecular weight 353.6684, weakly alkaline, density (g / mL, 25 / 4°C): 0.816, melting point -94°C, boiling point: 334.8°C at 1013.25hPa, flash point: 162°C at 1013. 25hPa, refractive index: n20 / D 1.4501 (lit.). Insoluble in water, soluble in ethanol and ether. [0003] Usage: extraction agent, paper processing aid, powder coating. [0004] The current main synthesis route of triisooctylamine: [0005] Isooctyl aldehyde and diisooctylamine are used to generate crude triisooctylamine in an autoclave under the action of a catalyst, and the product is obtained through distillation. The main disadvantage is that t...

Claims

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Application Information

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IPC IPC(8): C07C209/16C07C211/07
CPCY02P20/584
Inventor 陈红星黄德周史豫蒙陈敏锋唐毅
Owner 江苏万盛大伟化学有限公司
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