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The industrialized preparation method of 1-naphthylamine

A technology of naphthylamine and catalyst is applied in the field of preparation of 1-naphthylamine, which can solve the problems of complex catalyst preparation method, and achieve the effects of energy saving, strong operation safety and low processing cost.

Active Publication Date: 2020-05-01
九江常宇化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The preparation methods of the catalysts claimed in the above two patent documents are relatively complicated, and the respective preferred embodiments are laboratory experiments

Method used

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  • The industrialized preparation method of 1-naphthylamine
  • The industrialized preparation method of 1-naphthylamine
  • The industrialized preparation method of 1-naphthylamine

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Experimental program
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Embodiment 1）

[0033] See figure 1 The device used in the industrialized preparation method of 1-naphthylamine of the present embodiment comprises a catalytic hydrogenation kettle 1, a nitronaphthalene storage tank 2, a solvent storage tank 3, a catalyst supplement tank 4, a catalyst settling tank 5, and a desolventizer 6 , Distillation unit 7 and recovery solvent storage tank 8.

[0034] The catalytic hydrogenation still 1 comprises the first catalytic hydrogenation still 11 and the second catalytic hydrogenation still 12 with the same volume in series, and the nitronaphthalene storage tank 2 is located at the top of the first catalytic hydrogenation still 11 through a pump and a pipeline. The feed port is connected, and the pump used in this embodiment is a metering pump. The top of the body of the first catalytic hydrogenation kettle 11 is provided with a discharge port, the top of the body of the second catalytic hydrogenation kettle 12 is provided with a feed port and a discharge port,...

Embodiment 2）

[0052] All the other of the industrialized preparation method of 1-naphthylamine of the present embodiment are identical with embodiment 1, difference is:

[0053] Step 1. the solvent that feeds in catalytic hydrogenation tank 1 is ethanol, and step 5. obtains the 1-naphthylamine that purity is 96.5% through distillation process, and amino total value 99.37%, the yield of 1-naphthylamine (by nitro naphthalene) was 97.6%.

Embodiment 3）

[0055] All the other of the industrialized preparation method of 1-naphthylamine of the present embodiment are identical with embodiment 1, difference is:

[0056] 10m in step ① 3 Add 6000L of reaction solvent methanol into the first catalytic hydrogenation kettle 11 and the second catalytic hydrogenation kettle 12 respectively, and then open the switch of the catalyst replenishment tank 4 above each catalytic hydrogenation kettle 1 to feed the first catalytic hydrogenation kettle 11 Add Raney nickel 75kg respectively in the second catalytic hydrogenation kettle 12.

[0057] Step ③ Heat each reactor and keep the temperature in each reactor at 120°C.

[0058] Step ④ Under the condition of 120°C, continuously feed hydrogen into the first catalytic hydrogenation tank 11 and the second catalytic hydrogenation tank 12 until the internal pressure of each catalytic hydrogenation tank 1 is 1.3 Mpa, and keep each catalytic hydrogenation tank 1 The internal pressure is 1.3 MPa.

[00...

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Abstract

The invention discloses an industrial preparation method of 1-naphthylamine. The 1-naphthylamine is prepared by hydrogenation reduction of 1-nitronaphthalene, and the reaction is continuously carried out in tandem catalytic hydrogenation kettles. The method comprises the following steps: sequentially and respectively adding a reaction solvent and a catalyst Raney nickel into each tandem catalytic hydrogenation kettle; replacing the reaction device system by using nitrogen and hydrogen sequentially; heating each reaction kettle; respectively and continuously introducing hydrogen into each catalytic hydrogenation kettle; continuously introducing the 1-nitronaphthalene and a solvent into the first tandem catalytic hydrogenation kettle; discharging from the previous catalytic hydrogenation kettle to the next catalytic hydrogenation kettle while continuously feeding the first catalytic hydrogenation kettle, discharging from the last tandem catalytic hydrogenation kettle to a catalyst settling tank, settling the materials after the reaction, enabling the reaction solution to enter a desolventizing device, enabling the separated crude product to enter a distilling apparatus, thereby obtaining the product 1-naphthylamine after distillation. According to the method disclosed by the invention, the industrialization problem during continuous preparation of 1-naphthylamine through catalytic hydrogenation is solved.

Description

technical field [0001] The invention relates to a preparation method of 1-naphthylamine, in particular to an industrialized preparation method of 1-naphthylamine by catalytic hydrogenation of 1-nitronaphthalene. Background technique [0002] 1-Naphthylamine (also known as menaphthylamine) is used as an analytical reagent, a fluorescent indicator and a stationary liquid for gas chromatography; it is also used in organic synthesis, an intermediate for the production of various dyes, and the main raw material for rubber antioxidants. [0003] At present, the industrial production method of 1-naphthylamine at home and abroad is mainly to reduce 1-nitronaphthalene through sodium polysulfide composed of alkali sulfide and sulfur, and the reduced material is washed with water and distilled to obtain the finished product. This reduction method has a low yield (the yield is about 85%), and a large amount of sulfide-containing wastewater is generated during the production process, and...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C209/36C07C211/58
CPCC07C209/36C07C211/58
Inventor 周武勇陆益马燕东周应剑
Owner 九江常宇化工有限公司
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