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Method for catalyzing selective hydrogenation of 1,3-butadiene with PdAgNi/N-C catalyst

A catalyst and butadiene technology, which is applied in catalyst activation/preparation, heterogeneous catalyst chemical elements, physical/chemical process catalysts, etc., can solve the problem of high catalyst cost, high butene-1 loss, and product butadiene content. Insufficient and other problems, to achieve the effect of good catalytic activity, high activity and stability

Active Publication Date: 2018-11-13
安徽工大化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese patent CN106582625A discloses a catalyst for selective hydrogenation of butadiene, which comprises the following components in parts by weight of the catalyst: (a) 0.05-0.5% metal Pd or its oxide; (b) 0.1- 2 parts of Group IB metals or their oxides; (c) the technical solution of 97.5-99.7 parts of carrier alumina, which effectively solves the problems of high butene-1 loss, high catalyst cost and preparation problems in the prior art. The technical problem of using toxic and harmful raw materials in the process, but the control of the content of butadiene in the product is slightly insufficient

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] (1) Preparation of catalyst

[0022] 0.02mmolPdCl 2 , 0.004mmolAgNO 3 and 0.002 mmol NiCl 2 Dissolve in 10mL of distilled water, stir evenly in an ice bath at 0°C, and then add 10mmol of N-C material to the above solution, wherein the N-C material is prepared by roasting melamine and glucose at 700°C for 2 hours at a mass ratio of 30:1; After stirring, dropwise add 0.1mol / L sodium borohydride solution for reduction for 2 hours, filter and dry in a drying oven at 80°C for 20 hours to obtain the catalyst PdAg 0.2 Ni 0.1 / N-C 500 , airtight storage.

[0023] (2) Hydrogenation reaction process

[0024] First, fill 1.5 mL of the catalyst prepared in step (1) into a tubular reactor with an inner diameter of 8 mm, then raise the temperature of the catalyst bed to 30 ° C, and then add 1,3-butane with a molar ratio of 1:1.2 The mixed gas of diene and hydrogen is introduced into the reactor, the reaction pressure is 1.5MPa, and the reaction space velocity is 1.0h -1 .

...

Embodiment 2

[0027] (1) Preparation of catalyst

[0028] 0.02mmolPdCl 2 , 0.008mmolAgNO 3 and 0.006 mmol NiCl 2 Dissolve in 10mL of distilled water, stir evenly in an ice bath at 0°C, and then add 16mmol N-C material to the above solution, wherein, the N-C material is prepared by roasting melamine and glucose at 900°C for 6 hours at a mass ratio of 60:1; After stirring, dropwise add 0.4mol / L sodium borohydride solution for reduction for 2 hours, filter and dry in a drying oven at 140°C for 10 hours to obtain the catalyst PdAg 0.4 Ni 0.3 / N-C 800 , airtight storage.

[0029] (2) Hydrogenation reaction process

[0030] First, fill 1.5 mL of the catalyst prepared in step (1) into a tubular reactor with an inner diameter of 8 mm, then raise the temperature of the catalyst bed to 60 ° C, and then add 1,3-butane with a molar ratio of 1:2.5 The mixed gas of diene and hydrogen is introduced into the reactor, the reaction pressure is 3.2MPa, and the reaction space velocity is 4.0h -1 .

[...

Embodiment 3

[0033] (1) Preparation of catalyst

[0034] 0.02mmolPdCl 2 , 0.006mmolAgNO 3 and 0.004 mmol NiCl 2 Dissolve in 10mL distilled water, stir evenly in an ice bath at 0°C, and then add 14mmol N-C material to the above solution, wherein the N-C material is prepared by roasting melamine and glucose at 800°C for 4 hours at a mass ratio of 50:1; After stirring, dropwise add 0.3mol / L sodium borohydride solution for reduction for 2 hours, filter and dry in a drying oven at 120°C for 15 hours to obtain the catalyst PdAg 0.3 Ni 0.2 / N-C 700 , airtight storage.

[0035] (2) Hydrogenation reaction process

[0036] First, fill 1.5 mL of the catalyst prepared in step (1) into a tubular reactor with an inner diameter of 8 mm, then raise the temperature of the catalyst bed to 50 ° C, and then add 1,3-butane with a molar ratio of 1:2.0 The mixed gas of diene and hydrogen is introduced into the reactor, the reaction pressure is 2.8MPa, and the reaction space velocity is 3h -1 .

[0037] ...

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PUM

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Abstract

The invention discloses a method for catalyzing selective hydrogenation of 1,3-butadiene with a PdAgNi / N-C catalyst. The method is characterized by comprising the following steps: firstly, putting a PdAgNi / N-C catalyst into a tubular reactor, increasing the temperature of a catalyst bed layer to 30-60 DEG C, further introducing a mixed gas of 1,3-butadiene and hydrogen into the reactor, and carrying out a reaction at pressure of 1.5-3.2MPa and an air speed of 1.0-4.0hour<-1>. By adopting the method, PdAgNi / N-C is adopted as a catalyst, selective hydrogenation of 1,3-butadiene is carried out with the catalyst, the content of 1,3-butadiene in a product is less than 900ppb, the content of butane is less than 2.3%, and high catalysis activity can be still maintained after the catalyst is continuous operated for 100 hours.

Description

technical field [0001] The invention relates to the technical field of chemistry and chemical engineering, in particular to a method for catalyzing the selective hydrogenation of 1,3-butadiene with a PdAgNi / N-C catalyst. Background technique [0002] In petrochemicals, steam cracking of naphtha produces abundant low-chain C 4 alkenes, but in these C 4 Olefins often contain a small amount of diolefins or alkynes; in the downstream olefin polymerization process, diolefins or alkynes are often more likely to adsorb on the surface of the polymerization catalyst than monoolefins to poison the catalyst, so people often use the selectivity of diolefins Hydrogenation to monoolefins solves this problem. [0003] The development of high-efficiency selective hydrogenation catalysts is a hot spot in current research. The SHP process (Oil Gas J, 1988, 86 (49) 40-43) of U.S. Universal Oil Company (UOP) uses noble metal catalysts, and the conversion rate of butadiene is as high as 99.8 ...

Claims

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Application Information

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IPC IPC(8): B01J27/24B01J23/44B01J23/50B01J23/755B01J35/00B01J37/02C07C11/08C07C5/05
CPCC07C5/05B01J23/44B01J23/50B01J23/755B01J27/24B01J37/0201C07C2523/44C07C2523/50C07C2523/755B01J2523/18B01J2523/824B01J2523/847B01J35/19C07C11/08
Inventor 万超许立信叶明富雷昭王金刚范立岩张建伟周伟汪玉喜罗贤进
Owner 安徽工大化工科技有限公司
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