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Preparation method and application of 6-aminocapronitrile catalyst prepared by caprolactam ammonification

An aminocapronitrile and caprolactam technology, which is applied in catalyst activation/preparation, carboxylic acid amide preparation, carboxylic acid amide dehydration preparation and other directions, can solve problems such as equipment blockage, and achieve the effects of low cost, improved catalyst strength and high activity

Pending Publication Date: 2022-06-21
CHAOHU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At a lower feed ratio of ammonia gas to caprolactam, the conversion rate of caprolactam is 67.3-96.5%. Because caprolactam is a heat-sensitive substance, high-concentration caprolactam will inevitably generate polymerization products during the reaction or separation process, which will easily cause equipment blockage

Method used

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  • Preparation method and application of 6-aminocapronitrile catalyst prepared by caprolactam ammonification
  • Preparation method and application of 6-aminocapronitrile catalyst prepared by caprolactam ammonification
  • Preparation method and application of 6-aminocapronitrile catalyst prepared by caprolactam ammonification

Examples

Experimental program
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Effect test

Embodiment 1

[0042]Put 150g of aluminum hydroxide powder into a round-bottomed flask with mechanical stirring, add 30g of pseudo-boehmite, 35g of succulent powder and 120g of water, after mixing evenly, add 14g of metaphosphoric acid and 10g of concentrated sulfuric acid and mix at 30°C for 2h , after 7 times of extrusion, drying at 40℃ for 20h; roasting the dried sample at 800℃ for 5h to obtain a 5×5mm cylindrical catalyst with a bulk density of 0.56g / ml.

Embodiment 2

[0044] Put 150g of γ-alumina powder into the kneader, add 15g of pseudoboehmite, 20g of polyvinyl alcohol and 120g of water, after mixing evenly, add 20g of phosphoric acid and 20g of oxalic acid and knead at 50 °C for 1 hour, and after 5 times of extrusion molding , dried at 80°C for 10h; calcined the dried sample at 850°C for 4h to obtain a 3×3mm cylindrical catalyst with a bulk density of 0.55g / ml.

Embodiment 3

[0046] Put 150g of sodium aluminate powder into the crusher, add 35g of pseudo-boehmite and 120g of water, mix well, add 15g of hypophosphorous acid and 15g of acetic acid, and knead for 1 hour at 30°C. Dry for 15h; roast the dried sample at 750℃ for 6h to obtain a 5×5mm cylindrical catalyst with a bulk density of 0.57g / ml.

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Abstract

The invention discloses a method for preparing a 6-aminocapronitrile catalyst by ammoniating caprolactam. The method comprises the following steps: adding a carrier, an adhesive and a solvent into a mixer for mixing and stirring; the carrier is any one or a mixture of two or more of aluminum hydroxide, boehmite, sodium aluminate, pseudo-boehmite, gamma-aluminum oxide and kaolin; wherein the mass ratio of the carrier to the adhesive is 0.01: 1; adding the modifier solution into the material system, blending, fully mixing and reacting, extruding the mixed material into strips to obtain a catalyst precursor, drying and roasting to obtain a formed catalyst; the modifier is one or a mixture of two or more of phosphoric acid, hypophosphorous acid, phosphorous acid, pyrophosphoric acid, P2O5, P2O3 and polyphosphoric acid. The 6-aminocapronitrile prepared through catalysis of the catalyst prepared through the method is good in stability, simple in preparation operation, high in reaction selectivity and high in reaction conversion rate.

Description

technical field [0001] The invention belongs to the technical field of catalyst for preparing 6-aminocapronitrile, and particularly relates to a preparation method and application of a catalyst for preparing 6-aminocapronitrile by amination of caprolactam. Background technique [0002] Hexamethylenediamine is an important chemical product, mainly used in the production of nylon 66, nylon 610, ion exchange resin and diisocyanate, as well as curing agent and organic crosslinking agent for urea-formaldehyde resin, epoxy resin, etc., mainly composed of adiponitrile Or 6-aminocapronitrile is obtained by hydrogenation. However, the production of adiponitrile is technically difficult and the catalyst is easily deactivated. Therefore, the hydrogenation of 6-aminocapronitrile to prepare hexamethylenediamine has become an important process route at present. [0003] 6-Aminocapronitrile is mainly obtained by amination of caprolactam or partial hydrogenation of adiponitrile. Based on t...

Claims

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Application Information

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IPC IPC(8): B01J27/14B01J27/16B01J37/08C07C253/20C07C255/24
CPCB01J27/14B01J27/16B01J37/082C07C253/20C07C231/08C07C255/24C07C237/06
Inventor 谢忠王新运李川吴凤义
Owner CHAOHU UNIV
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