Catalyst for synthesizing 6-aminocapronitrile, preparation method thereof and method for synthesizing 6-aminocapronitrile by using catalyst

A technology of aminocapronitrile and catalyst, which is applied in the direction of molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of reduced service life, low selectivity, and low conversion rate, and achieve low requirements for preparation equipment, The effect of simple preparation method and long catalyst life

Pending Publication Date: 2021-11-16
BEIJING RISUN TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Disclosed in CN107739318A is a liquid-phase synthetic process, phosphoric acid or phosphate is a catalyst, batch process, caprolactam conversion rate 55%, 6-aminocapronitrile selectivity 97%, conversion rate is low, catalyst separation and recycling make the process Complicated, low overall performance of the device
In the early years of the gas phase process, the U.S. patent US 2234566 A used silica gel as a catalyst to support copper, and the conversion rate was low, less than 25%, and the selectivity of 6-aminocapronitrile was low, less than 90%. Pay attention, patents such as CN110404582A, CN111992241A, CN111672526A, CN111672494A, CN111659463A and CN111659374A disclose their respective preparation methods of gas-phase catalyst systems. ℃ and the space velocity is low. According to past practical experience, high temperature and low space velocity are often prone to carbon deposition and shorten the service life

Method used

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  • Catalyst for synthesizing 6-aminocapronitrile, preparation method thereof and method for synthesizing 6-aminocapronitrile by using catalyst
  • Catalyst for synthesizing 6-aminocapronitrile, preparation method thereof and method for synthesizing 6-aminocapronitrile by using catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Catalyst preparation: Prepare a mixed aqueous solution of ternary active components: add accurately weighed 1.0g of ytterbium nitrate, 5.0g of calcium nitrate and 5.0g of copper nitrate to 300ml of desalted water, weigh 100g of ZSM-5 molecular sieve with a silicon-aluminum ratio of 100, and mix the molecular sieve The carrier was added to the mixed aqueous solution of the ternary active components, kept at 65°C and shaken for 6 hours, the excess water was evaporated under reduced pressure by a water pump, the residual solid was baked at 110°C for 4 hours, dried and molded, and calcined in a muffle furnace for 5 hours at 600°C to obtain the finished catalyst.

[0027] Catalyst performance evaluation: take 5g catalyst and fill it in a fixed bed reactor, preheater is filled with quartz sand, preheating temperature is 300°C, fixed bed layer is 300°C, mass space velocity of caprolactam is 6h -1 , the molar ratio of caprolactam to ammonia is 1:12. The molten caprolactam is fed...

Embodiment 2

[0030] Except that the amount of ytterbium nitrate, calcium nitrate and copper nitrate used in the preparation of ternary active component mixed aqueous solution is 1.0g ytterbium nitrate, except 10.0g calcium nitrate and 10.0g copper nitrate, prepare catalyst with the method identical with embodiment 1 .

[0031] The catalytic performance evaluation process of the catalyst was the same as in Example 1. As a result, the per-pass conversion of caprolactam was 85.2%, and the selectivity of 6-aminocapronitrile was 99%.

Embodiment 3

[0033] Except that the amount of ytterbium nitrate, calcium nitrate and copper nitrate used in the preparation of ternary active component mixed aqueous solution is 1.0g ytterbium nitrate, except 5.0g calcium nitrate and 10.0g copper nitrate, prepare catalyst with the method identical with embodiment 1 .

[0034] The catalytic performance evaluation process of the catalyst was the same as in Example 1. As a result, the per-pass conversion of caprolactam was 86.5%, and the selectivity of 6-aminocapronitrile was 99%.

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Abstract

The invention provides a preparation method of a catalyst for synthesizing 6-aminocapronitrile from caprolactam. The preparation method comprises the following steps: 1) preparing a mixed aqueous solution of ternary active components of ytterbium nitrate, calcium nitrate and copper nitrate for later use; (2) weighing a ZSM-5 silicon-aluminum molecular sieve, and adding the molecular sieve into the mixed aqueous solution of the ternary active components in the step (1); (3) dipping for 4-10 hours at the temperature of 25-80 DEG C; and 4) evaporating to dryness, drying, forming and roasting to obtain the catalyst. Wherein the mass ratio of the ytterbium nitrate to the calcium nitrate to the copper nitrate is 1: (1-20): (1-20), and the ratio of the total mass of the ytterbium nitrate, the calcium nitrate and the copper nitrate to the mass of the ZSM-5 silicon-aluminum molecular sieve is (0.01-0.4): 1. The catalyst disclosed by the invention is simple in preparation method, stable in quality, high in catalytic efficiency, high in product space-time yield, long in service life, low in requirements on catalyst preparation equipment and easy for industrial production.

Description

technical field [0001] The invention relates to the field of organic synthesis of 6-aminocapronitrile prepared from caprolactam, in particular to a method for preparing a catalyst for synthesizing 6-aminocapronitrile by using ZSM-5 silica-alumina molecular sieve as a carrier to load active components, A catalyst prepared by the method and a method for synthesizing 6-aminocapronitrile using the catalyst. Background technique [0002] Hexamethylenediamine is a key intermediate in the production of polyamides such as nylon 66 and nylon 610, and is also used in the preparation of diisocyanate and as a curing agent for epoxy resin and urea-formaldehyde resin. At present, the main synthetic route is the synthesis of adiponitrile by butadiene-hydrocyanic acid method, and the catalytic reduction of adiponitrile to hexamethylenediamine. In recent years, with the continuous expansion of caprolactam production capacity and the continuous reduction of costs, 6-aminocapronitrile (precur...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/46C07C253/20C07C255/24
CPCB01J29/46C07C253/20B01J2229/186C07C255/24
Inventor 杨学林谢增勇王耀红刘东磊王树平陈西波党伟荣
Owner BEIJING RISUN TECH CO LTD
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