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Method for preparing azelaic diamine

A technology of nonanediamine and azelaic nitrile, applied in the field of preparing nonanediamine, can solve problems such as low conversion rate of raw materials, lack of nonanediamine process, etc., and achieve the effects of wide source, great social significance and economic value, and simple process

Active Publication Date: 2016-12-14
南京荔枝生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved in the present invention is to provide a method for preparing nonanediamine, so as to solve the problems in the prior art such as the lack of azelaic acid for preparing nonanediamine and the low conversion rate of raw materials.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] This example describes the preparation of molecular sieve catalysts containing different oxidizing agents.

[0025] The HZSM-5 catalyst loaded with metal oxide was prepared by chemical precipitation method, and the preparation of 25wt%-ZnO / HZSM-5 catalyst (10.00g) was taken as an example: weigh 17.84g Zn(NO 3 ) 2 ·6H 2 O was dissolved in a 250mL beaker filled with 50mL deionized water. After the nitrate was fully dissolved, 7.50g of HZSM-5 was added to the beaker. The mixture was stirred for 4 hours, and then 30.00g of 3mol / L (NH 4 ) 2 CO 3 solution, stirred while adding, and the resulting precipitated mixture was left to age for 24 hours, then washed with deionized water and absolute ethanol in sequence, filtered with suction, put the filter cake in an oven at 120°C for 12 hours, and then roasted at 550°C for 5 hours , the obtained catalyst powder is sufficiently ground, pressed into tablets under a pressure of 10 MPa, and sieved to obtain 20-60 mesh particles to o...

Embodiment 2

[0028] In this example, the influence of molecular sieve catalysts loaded with different oxides on the oxidation reaction of the key step in the process of preparing crude azelaic acid from castor oil was investigated.

[0029] The preparation method of the crude product of azelaic acid is exemplified: Weigh 200 grams of castor oil, add 1 liter of aqueous solution containing 40 grams of KOH, and fully stir to form an emulsion. Measure 200mL of absolute ethanol and heat it to 80°C, and gradually add the molecular sieve catalyst to carry out the oxidation reaction for 12h under the state of full stirring. After the reaction, add 500 milliliters of 33% sulfuric acid aqueous solution, continue to heat and stir and heat filter, wash the filter cake with hot water and then filter, the filtrates are combined and then concentrated, and the crude crystals of azelaic acid are precipitated after cooling.

[0030] The conversion rate of azelaic acid corresponding to different supported ox...

Embodiment 3

[0034] This embodiment illustrates the process of preparing nonanediamine by clarifying the crude crystals of azelaic acid. In order to obtain nonanediamine, the following process is established:

[0035] The crude crystals of azelaic acid are adjusted to pH 8.5 with ammonia water, and the pressure of the concentrated tank is controlled at -0.09Mpa and the temperature is 60°C by means of vacuum distillation. The crystal is transferred into a 500mL reactor, under normal pressure, the temperature is controlled at 190°C for 3 hours, and the effluent is mainly water and some ammonia gas, which can be directly connected to the waste water collection tank; connected to a vacuum pump to control the vacuum degree of the reactor at 8~ 9kpa, the temperature is controlled at 180°C for 2 hours, and the distillate is collected, that is, azelanitrile; the distillate is added to the hydrogenation reactor, and ethanol is used as a solvent. The amount added is 1.1 times (volume ratio) of azelan...

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PUM

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Abstract

The invention discloses a method for preparing azelaic diamine. Azelaic acid is taken as a raw material, azelaic dinitrile is prepared through a neutralization reaction, a dehydration reaction and a decompression reaction sequentially, and azelaic diamine is prepared through a hydrogenation reaction of the azelaic dinitrile. Compared with the prior art, the method has the advantages as follows: a process route with a simple process and extremely high efficiency and yield is provided; meanwhile, renewable biomass resources are taken as raw materials and are wide in source, and all the processes are relatively simple and can be implemented, so that the method has great social significance and great economic value.

Description

technical field [0001] The invention belongs to the field of chemical engineering, and in particular relates to a method for preparing nonanediamine. Background technique [0002] Azelaic acid, also known as rhododendronic acid, 1,7-heptanedicarboxylic acid, is white to light yellow monoclinic prism, needle crystal or powder at room temperature. Slightly soluble in cold water, ether and benzene, soluble in hot water, ether, easily soluble in ethanol, stable in nature. Azelaic acid is an important organic synthesis intermediate, which can be used to synthesize dioctyl azelate plasticizer, synthetic perfume, lubricating oil and polyamide and other products; azelaic acid is also used in the production of nylon-69 and nylon-9 Production. In addition, other applications of azelaic acid include dielectric liquids, demulsifiers, anti-moth agents, polyurethane methyl vinegar foams, hydraulic oils, turbine oils, high-solubility coatings, adhesives, water-soluble resins and cosmeti...

Claims

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Application Information

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IPC IPC(8): C07C209/48C07C211/09C07C253/22C07C255/04
CPCC07C209/48C07C253/22C07C211/09C07C255/04
Inventor 马江锋罗继宏
Owner 南京荔枝生物科技有限公司
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