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Preparation method and application of framework Co catalyst

A catalyst and skeleton technology, which is applied in the field of preparation of skeleton Co catalysts, can solve problems such as alloy waste, many side reactions, and poor catalyst strength, and achieve the effects of reducing production costs, wide particle size distribution range, and improving activity

Active Publication Date: 2016-11-16
WANHUA CHEM GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, US6337300 discloses using 15% polyoxymethylene copolymer as a binder, molding Co-Al alloy powder, drying, and roasting at 800 ° C for 125 min, and then using 20 % NaOH solution to activate at 80 ° C for 120 min The catalyst is prepared; the catalyst is used for the hydrogenation of IPN to prepare IPDA, the IPN conversion rate is 99.9%, but the IPDA selectivity is only 89.7%, the product yield is low, and the particle crushing strength (Breaking Strength) is only 120N / particle
[0009] Therefore, it is necessary to seek a new preparation method of the skeleton Co catalyst, so as to solve the problem of low yield of the target alloy particles due to the crushing of the alloy block and serious waste of the alloy; the strength of the catalyst formed by the alloy powder is poor, and the active components are easily lost; 2 Or AlOOH is easy to remain in the pores of the catalyst, causing problems such as many side reactions during use

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Weigh 1600g of metal Co and 2400g of metal Al, and put them into a melting crucible. Turn on the power of the smelting furnace, start to heat up to about 1680°C, keep it for 5 minutes, stir for 1-2 minutes, pour the alloy liquid onto a graphite plate and cool to room temperature to obtain an alloy block. The alloy block is broken to collect 200-300 mesh Co-Al alloy powder.

[0051] Weigh 200g of Co-Al alloy powder, weigh 1g of Sesame powder, 5g of aluminum powder, 2g of copper powder, 2g of nickel powder, 1g of disodium hydrogen phosphate, 10g of polyvinylpyrrolidone, and 10g of gum arabic, and weigh the above with a mixer The obtained materials are fully mixed, then soaked with deionized water, and then kneaded with a kneader; the wet material obtained by kneading is formed with an extruder, and finally cut into particles with a length of about 3 mm with a honey pill machine. Bake the formed alloy particles in an oven at 120°C for 12 hours, and finally put them into a...

Embodiment 2

[0054] The preparation of Co-Al alloy powder is the same as in Example 1.

[0055]Weigh 200g of Co-Al alloy powder, and weigh 3g of Sesame powder, 12g of aluminum powder, 5g of molybdenum powder, 6g of chromium powder, 6g of disodium hydrogen phosphate, 15g of hydroxypropyl methylcellulose, and 15g of soluble starch. Fully mix the above weighed materials with a machine, then soak them with deionized water, and then knead them with a kneader; shape the wet materials obtained by kneading with an extruder, and finally cut them into particles with a length of about 3 mm with a honey pill machine. Bake the formed alloy particles in an oven at 120°C for 12 hours, and finally put them into a medium frequency induction furnace, adjust the heating power, quickly raise the temperature to 300°C, keep it for 3.0min, adjust the heating power, raise the temperature to 570°C, 3 Roasting under atmosphere for 5.5min, NH 3 The flow rate is 50ml / s. The average crushing strength (axial directio...

Embodiment 3

[0058] The preparation of Co-Al alloy powder is the same as in Example 1.

[0059] Weigh 200g Co-Al alloy powder, weigh 2g graphite, 9g aluminum powder, 2g iron powder, 2g manganese powder, 2g molybdenum powder and 3g disodium hydrogen phosphate, 5g polyvinylpyrrolidone, 5g gum arabic, 5g lignosulfonic acid Sodium, first use a mixer to fully mix the above weighed materials, then soak them with deionized water, and then knead them with a kneader; shape the wet materials obtained by kneading with an extruder, and finally cut them into a length of about 3mm with a honey pill machine particle. Bake the formed alloy particles in an oven at 120°C for 10 hours, and finally put them into a medium-frequency induction furnace, adjust the heating power, quickly raise the temperature to 350°C, keep it for 4.0min, adjust the heating power, raise the temperature to 600°C, and set the temperature in NH 3 Roasting under atmosphere for 5.0min, NH 3 The flow rate is 70ml / s. The average crush...

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Abstract

The invention discloses a preparation method and application of a framework Co catalyst. The method specially comprises the following steps of preparing Co-Al alloys through smelting, then crushing the Co-Al alloys into alloy powder, and then adding an organic binder, a lubricant, a high-temperature adhesive and a special adhesive; and performing shaping, performing drying, performing roasting, performing activation and performing post treatment, so as to obtain the catalyst. The catalyst is used for hydrogenation of 3-(aminomethyl)-3,5,5-trimethylcyclohexanamine (IPN) so as to prepare isophorone diamine(IPDA), wherein the conversion rate of IPN is as high as 100%, and the selectivity of the IPDA is as high as 98% or above.

Description

Technical field: [0001] The invention relates to a preparation method and application of a skeleton Co catalyst, which can be used as a fixed bed to prepare 3-aminomethyl-3,5, Hydrogenation catalyst for 5-trimethylcyclohexylamine. Background technique: [0002] 3-Aminomethyl-3,5,5-trimethylcyclohexylamine (isophoronediamine, referred to as IPDA) is a raw material for preparing isophorone diisocyanate (IPDI), polyamide, etc.; it can also be used as Epoxy resin curing agent. It is usually composed of 3-cyano-3,5,5-trimethylcyclohexanone (isophorone nitrile, referred to as IPN), NH 3 and H 2 Under the action of a hydrogenation catalyst, it can be obtained through ammoniation and high-pressure hydrogenation. Commonly used hydrogenation catalysts are skeleton Co (Raney Co) catalysts. [0003] Raney Co catalyst is a commercial catalyst. Such as U.S. published patent documents US6087296A, US7569513 etc. disclose its preparation method as follows: take metal Co and Al as the a...

Claims

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Application Information

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IPC IPC(8): B01J25/00C07C209/48C07C209/22C07C211/36
CPCB01J23/75B01J25/00C07C209/22C07C209/48C07C211/36
Inventor 叶飞王磊王同济杨立超初乃波崔娇英张礼昌黎源
Owner WANHUA CHEM GRP
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