Method for hydrofining caprolactam in magnetically stabilized bed

A caprolactam, magnetically stabilized bed technology, applied in chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, organic chemistry, etc., can solve the problems of large catalyst dosage, low reactant concentration and high energy consumption, Achieve the effect of reducing energy consumption, optimizing refining process and improving processing capacity

Active Publication Date: 2011-05-11
CHINA PETROLEUM & CHEM CORP +3
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the above-mentioned patents all adopt the method of hydrogenating caprolactam aqueous solution, the concentration of reactants is low, the amount of catalyst is large, a large amount of water is required after the reaction, and the energy consumption is high.

Method used

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  • Method for hydrofining caprolactam in magnetically stabilized bed
  • Method for hydrofining caprolactam in magnetically stabilized bed
  • Method for hydrofining caprolactam in magnetically stabilized bed

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] The preparation of embodiment 1 catalyst carrier

[0015] (1), 250 grams of magnetic granular material and 1000 grams of Al 2 o 3 The sol (Al 2 o 3 The mass ratio is 40%), 30 grams of 20 nanometers of CaCO 3 Mix in a stirred mixer, where SiO in the magnetic granular material 2 The coating layer is uniformly dispersed in it with Fe with an average particle size of 108 nm 3 o 4 The ratio of magnetic particles is 0.3:1. Control the stirring speed to be greater than 500 rpm and mix for 1 hour, prepare micron-sized pellets in a nitrogen flow at 600°C by spray drying method, and soak the pellets in excess hydrochloric acid (10% mass concentration) at 40°C for 30 minutes , washed several times to remove CaCO 3 . Then calcined at 500° C. for 2 hours to obtain spherical particles, and sieved to obtain small balls with a diameter of 50-70 microns as spherical catalyst carriers for later use, namely Carrier-1.

[0016] (2), 250 grams of magnetic granular material and 100...

Embodiment 2

[0017] The preparation of embodiment 2 catalyst.

[0018] (1), according to the weight of palladium being 1% calculation of catalyst support weight, take by weighing an appropriate amount of Pd (NO 3 ) 2 , the palladium is loaded on the surface of the carrier-1 by impregnation method, the catalyst carrier loaded with palladium decants the liquid, puts it into a muffle furnace after drying, and bakes at 550° C. for 2 hours. The calcined catalyst was reduced with hydrogen at 500° C. for 4 hours, the heating was stopped, and the temperature was lowered to room temperature in a hydrogen atmosphere to obtain Catalyst-1.

[0019] (2), according to the weight of platinum is 1% calculation of catalyst carrier weight, take by weighing an appropriate amount of chloroplatinic acid, platinum is loaded on the surface of carrier-1 by dipping method, the catalyst carrier after loading platinum is decanted liquid, air After drying, put it into a muffle furnace and bake at 550°C for 2 hours....

Embodiment 3

[0022] Embodiment 3 crude caprolactam hydrogenation test

[0023] 10 milliliters of catalyst-1 with a particle size of 50-70 microns is loaded into a reactor with an inner diameter of 14 mm; seven coils with an inner diameter of 55 mm, an outer diameter of 165 mm, a height of 35 mm and a number of turns of 370 are reacted along the The device is axially arranged to provide a uniform magnetic field, and the distance between the coils is 27.5 millimeters; the reaction raw materials and hydrogen enter from the lower part of the magnetically stable bed reactor and flow out from the upper part, and the hydrogen / material ratio (volume ratio) is 6.0. 100℃, pressure 1.2MPa, liquid space velocity 30 hours -1 Hydrofining reaction is carried out under the condition of , the reaction raw material is caprolactam crude product containing impurities (PM value is 110 seconds), table 1 is the effect of caprolactam hydrofinishing under different magnetic field strengths.

[0024] Table 1 Effects...

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Abstract

The invention relates to a method for hydrofining caprolactam in a magnetically stabilized bed. The method comprises the following steps: the acidamide oil is extracted and distilled with benzene/cyclohexane to obtain the caprolactam crude product; in a magnetically stabilized bed reactor, the hydrogenation reaction is carried out under the action of a catalyst formed by active components such as platinum or/and palladium and a magnetic spherical carrier, so that the unsaturated substance in the liquid caprolactam crude product reacts with hydrogen to generate a saturated substance; and then the saturated substance is rectified to obtain the caprolactam product. The active components in the catalyst occupy 0.01-5 percent (wt); and the hydrogenation reaction conditions are as follows: temperature: 80 DEG C to 140 DEG C, pressure: 0.5 to 3.0 MPa, air speed: 2 to 60h-1, and magnetic field intensity: 10 to 1500 oersteds. Compared with the prior art, the method has the advantages that the procedures of water re-extraction and dehydration by evaporation are reduced, the refining process is greatly simplified, and the refining operation process is optimized; and the method is favorable for reducing energy consumption and environmental pollution and enhancing the processing capacity of the device.

Description

technical field [0001] The invention belongs to the technical field of chemical refining, and in particular relates to a method for removing impurities by performing hydrogenation reaction on liquid caprolactam crude product in the presence of a magnetically stable bed and a magnetic noble metal catalyst. technical background [0002] The post-refinement of caprolactam is an important step in the production of caprolactam. ε-caprolactam is one of the important raw materials for synthetic fibers and synthetic resins, mainly used in the manufacture of polyamide fibers (nylon-6), resins and films. At present, the production process of caprolactam is mainly divided into benzene process and toluene process. Among them, the toluene process includes the oxidation of toluene to benzoic acid, the hydrogenation of benzoic acid to produce cyclohexane carboxylic acid (CCA), the amidation reaction of cyclohexane carboxylic acid and nitrosyl sulfuric acid to produce amidated products, an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D223/10B01J23/89
CPCY02P20/52
Inventor 赵承军宗保宁孟祥堃仇振华张金利李韦华林德宝
Owner CHINA PETROLEUM & CHEM CORP
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