Tri-n-octylamine preparation method

A technology of tri-n-octylamine and di-n-octylamine, which is applied in the field of preparation of tri-n-octylamine, can solve the problem of cost, is not suitable for industrialized production, etc., and achieves the effects of reducing three-waste discharge, realizing waste utilization, and increasing economic benefits

Active Publication Date: 2018-01-05
江苏万盛大伟化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Another report: Use n-octylamine and n-octanol to react under the catalyst to generate the target product. Due to cost issues, this route is not suitable for industrial production

Method used

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Examples

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Embodiment 1

[0046] Preparation of alkaline earth metal oxide catalysts: 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 was dissolved in water, neutralized with sodium carbonate to neutrality, then ZrO was added 2 As a catalyst carrier, stir evenly into a paste, age in a water bath at 50±5°C for 5±1h, dry with suction filtration, calcinate at 450±10°C for 4±0.5h, and crush to below 400 mesh to obtain alkaline earth metal oxides catalyst.

[0047] Put 150 g of di-n-octylamine, 89 g of n-octanol, and 1.5 g of alkaline earth metal oxide catalyst into a 500-milliliter four-neck reaction flask, which is equipped with a hydrogen circulation and water separation device. After nitrogen replacement and hydrogen replacement, the catalyst was reduced under a hydrogen atmosphere at 160-180 ° C for 1 hour, and then the reaction temperature was increased to 210-220 ° C, and water was continuously generated in the reaction. Di-n-octylamine 0.8%, tri-n-octylamine 94...

Embodiment 2

[0049] Preparation of alkaline earth metal oxide catalysts: 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 was dissolved in water, neutralized with ammonia water to neutrality, then calcium carbonate was added as a catalyst carrier, stirred to form a paste, aged in a water bath at 50±5°C for 5±1h, dried by suction filtration, and roasted at 450±10°C for 4 ±0.5h, crushed to less than 400 mesh, namely the alkaline earth metal oxide catalyst was obtained.

[0050] Put 150 g of di-n-octylamine, 97.2 g of n-octanol, and 3 g of alkaline earth metal oxide catalyst into a 500-milliliter four-necked reaction bottle with a hydrogen circulation and water separation device. After nitrogen replacement and hydrogen replacement, the catalyst was reduced under a hydrogen atmosphere at 160-190 ° C for 1 hour, and then the reaction temperature was raised to 200-230 ° C, and water was continuously generated in the reaction. Di-n-octylamine 0.3%, tri-n-octyl...

Embodiment 3

[0052] Preparation of alkaline earth metal oxide catalysts: Cu(NO 3 )2·3H 2 O, Ni (NO 3 )2·6H 2 O, dissolved in a certain amount of water, neutralized with ammonia water to neutrality, and then added calcium carbonate as a catalyst carrier, stirred uniformly into a paste, aged in a water bath at 50±5 °C for 5±1 h, and dried by suction filtration, 450± The alkaline earth metal oxide catalyst was prepared by roasting at 10°C for 4±0.5h and crushing to below 400 mesh.

[0053]Put 150 g of di-n-octylamine, 97.2 g of n-octanol, and 3 g of an alkaline earth metal oxide catalyst into a 500 ml four-necked reaction flask equipped with a hydrogen circulation and water separation device. After nitrogen replacement and hydrogen replacement, reduce the catalyst under a hydrogen atmosphere at 160-190°C for 1 hour, then raise the reaction temperature to 200-230°C, water will continue to be generated during the reaction, and after 4 hours there is almost no water, then sample GC analysis, ...

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Abstract

The invention discloses a tri-n-octylamine preparation method. The preparation method comprises the following preparation steps: throwing di-n-octylamine, n-caprylic alcohol and an alkaline earth metal oxide catalyst into a reactor; keeping hydrogen atmosphere after nitrogen displacement and hydrogen displacement are performed, reducing the catalyst for 1+ / -0.5 hour at 160 to 190 DEG C; heating and reacting, sampling and performing GC detection when the collected generated water amount reaches 95 percent or above a theoretical amount and the change amount in half an hour does not exceed 2 weight percent, and ending the reaction to obtain crude tri-n-octylamine when the content of the di-n-octylamine is less than or equal to 2 weight percent; cooling, precipitating the crude tri-n-octylamine, and finally, rectifying to obtain the tri-n-octylamine. According to the process route, the initial raw materials come from distillation residues of the tri-n-octylamine; a byproduct of the companyis changed from waste into treasure, so that waste utilization is realized; the emission of waste water, waste gas and solid waste is reduced; the environmental protection is benefited; the economicbenefit is increased.

Description

technical field [0001] The invention belongs to the field of organic synthesis, in particular to a preparation method of tri-n-octylamine. Background technique [0002] Tri-n-octylamine (Triotylamine) is a special tertiary amine product, which is a colorless to pale yellow liquid compound with an amine smell and is alkaline. The chemical formula is C 24 H 51 N. The CAS number is 1116-76-3. Pure melting point -34 ℃. Boiling point 365.8 ℃. Density 0.811. Refractive index 1.449 (20°C). Insoluble in water, soluble in ethanol and ether. [0003] Uses: It can be used as extraction agent for precious metals. 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 to extract acidic compounds with benzene rings in wastewater treatment. [0004] The main route of synthesis of tri-n-octylamine at present: [0005] Using n-octanol and ammonia under the action of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/60C07C211/07B01J23/80B01J23/78
Inventor 陈红星黄德周勇新黄正祥史豫蒙唐毅
Owner 江苏万盛大伟化学有限公司
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