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Catalyst, preparation method thereof and method for synthesizing hexamethylenediamine intermediate

A catalyst and carrier technology, applied in the field of synthesizing hexamethylenediamine intermediates, catalysts and their preparation, can solve the problem of many by-products, and achieve the effects of reducing by-products, improving selectivity, and reducing mutual influence

Pending Publication Date: 2020-09-15
JIANGSU YANGNONG CHEM GROUP +3
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The main purpose of the present invention is to provide a kind of catalyst and preparation method thereof, the method for synthesizing hexamethylenediamine intermediate, to solve the problem in the prior art that there are more by-products of 6-aminocapronitrile by ammoniation of caprolactam

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  • Catalyst, preparation method thereof and method for synthesizing hexamethylenediamine intermediate
  • Catalyst, preparation method thereof and method for synthesizing hexamethylenediamine intermediate
  • Catalyst, preparation method thereof and method for synthesizing hexamethylenediamine intermediate

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preparation example Construction

[0028] In another typical embodiment of the present application, a preparation method of the aforementioned catalyst is provided, the preparation method comprising: step S1, mixing the shell-forming solution and the carrier to obtain a mixture; step S2, adjusting the pH value of the mixture To coat the carrier to obtain the coated system; and step S3, subjecting the coated system to solid-liquid separation, drying for the first time, and roasting for the first time to obtain a catalyst, wherein the shell-forming solution is selected from aluminum nitrate solution , any one or more of zinc nitrate solution, copper nitrate solution, ferric nitrate solution, aluminum sulfate solution.

[0029] Fully mix the above-mentioned shell-forming solution with the carrier, and adjust the pH so that the shell-forming solution forms a precipitate and coats the carrier to obtain the coated system, and then separate the obtained solid components by solid-liquid separation of the coated system ...

Embodiment 1

[0047] Weigh 10g of aluminum nitrate and dissolve it in 100g of water, slowly add 30g of calcium oxide to the aluminum nitrate solution at 90°C, and stir for 4h to obtain a mixture, after stirring the mixture for 30min, slowly add 10% ammonia solution dropwise until the pH value is 8 Between ~10, continue to stir for 1 hour, so that the aluminum ions are completely precipitated and coated on the calcium oxide carrier, and the coated system is obtained. After the coated system is filtered and washed twice, the filter residue is dried in an oven at 60°C After drying for 20 hours, the catalyst was further roasted in a muffle furnace at 650°C for 5 hours to obtain the desired catalyst Al with a core-shell structure. 2 o 3 -CaO, the shell thickness of the catalyst is 10nm, Al 2 o 3 The molar ratio with CaO is 0.045:1, Al 2 o 3 The pore diameter of the shell layer is 30-40 μm.

[0048] Take 20g of the above-mentioned catalyst and put it into a kneader, add 2g of turnip powder a...

Embodiment 2

[0050] The difference between embodiment 2 and embodiment 1 is that

[0051] Weigh 1.14g of aluminum nitrate and dissolve it in 100g of water, add 30g of calcium oxide to obtain the required catalyst Al with a core-shell structure 2 o 3 -CaO, the Al 2 o 3 -CaO catalyst with shell thickness of 0.1nm, Al 2 o 3 The molar ratio with CaO is 0.005:1, Al 2 o 3 The pore diameter of the shell layer is 10-30 μm, and a cylindrical catalyst with a diameter of 4 mm is finally obtained after molding.

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Abstract

The invention provides a catalyst, a preparation method thereof and a method for synthesizing a hexamethylenediamine intermediate. The catalyst is of a core-shell structure, the core of the core-shellstructure is a carrier, the carrier is selected from any one or more of magnesium oxide, silicon dioxide, calcium oxide and titanium oxide, and the shell layer of the core-shell structure is of a porous structure and comprises any one or more of aluminum oxide, zinc oxide, copper oxide and iron oxide. The core of the core-shell structure provides a loading effect for the shell layer; the shell layer of the core-shell structure comprises the active metal oxide component; therefore, the catalyst with the specific core-shell structure can simultaneously and respectively carry out catalytic reaction on the core and the shell layer and the thus catalytic activity of catalyst is improved, especially for a continuous step-by-step catalytic reaction system, the catalyst with the core-shell structure is beneficial to respectively carrying out different catalytic steps of the catalytic reaction system on the core and the shell of the catalyst so that the mutual influence among different catalytic steps is reduced, and byproducts of the catalytic reaction system are reduced.

Description

technical field [0001] The invention relates to the technical field of preparation of 6-aminocapronitrile, in particular to a catalyst, a preparation method thereof, and a method for synthesizing a hexamethylenediamine intermediate. Background technique [0002] 6-Aminocapronitrile is an important chemical intermediate for the synthesis of hexamethylenediamine, which is obtained by catalytic amination of caprolactam. The U.S. patent application with the patent application number US2234566 adopts silica gel-loaded copper as a dehydration catalyst, and synthesizes 6-aminocapronitrile under the conditions of a reaction temperature of 360 ° C and an ammonia / caprolactam mol ratio of 6, and the conversion rate of caprolactam is 21.7%, and 6- Aminocapronitrile yield is only 25%. In the U.S. patent application whose patent application number is US3855267, the mixed gas of ammonia gas and caprolactam passes through the alumina and molecular sieve catalyst of supporting aluminum phos...

Claims

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Application Information

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IPC IPC(8): B01J23/02B01J35/10B01J37/03B01J37/08B01J37/00C07C231/10C07C237/06C07C253/20C07C255/24
CPCB01J23/02B01J23/002B01J37/035B01J37/082B01J37/0018C07C231/10C07C253/20B01J35/397B01J35/657C07C237/06C07C255/24Y02P20/52
Inventor 王根林许越丁克鸿徐林王刚王铖殷剑虎李良善韩东旭聂庆超
Owner JIANGSU YANGNONG CHEM GROUP
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