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Process and catalyst for preparing 1,4-butanediol

A technology of catalyst and butanediol, which is applied in the fields of Raney-type catalysts, catalyst activation/preparation, physical/chemical process catalysts, etc., and can solve problems such as extremely high demand for nickel

Pending Publication Date: 2019-05-21
EVONIK OPERATIONS GMBH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] A disadvantage of the methods used to date for the production of BDO in industrial applications is the extremely high demand for nickel, which is used in these methods as a hydrogenation catalyst of the Raney type

Method used

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  • Process and catalyst for preparing 1,4-butanediol
  • Process and catalyst for preparing 1,4-butanediol
  • Process and catalyst for preparing 1,4-butanediol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] Nickel foam commercially available in roll form with a thickness of 1.9 mm, a width of 300 mm, and an average pore diameter of 580 μm was sprayed with a commercially available adhesion promoter solution, coated with aluminum powder and heat-treated at 700°C. After cooling, the material thus obtained was laser cut into square pieces measuring 4 mm x 4 mm on a side and 1.9 mm thick.

[0055] The resulting bulk material was placed in a fixed bed for catalytic activation, followed by wet chemical treatment by pumping through 5M NaOH solution (sodium hydroxide in water). Part A of the bulk material was subjected to this wet chemical post-treatment at 70°C for 5 minutes. Part B of the bulk material was post-treated with aqueous sodium hydroxide solution at 60° C. for 15 minutes.

[0056] Both fractions were subsequently washed with water until the pH of the wash solution reached <10 after pumping through the fixed bed.

[0057] The composition of the two catalytically activ...

Embodiment 2

[0076] The catalyst was prepared as described in Example 1, wherein the wet chemical workup was carried out with 10% by weight aqueous sodium hydroxide solution at 60° C. for 60 minutes. The composition of the resulting catalytically active bulk material (Catalyst C) was analyzed by ICP-OES to give a composition of 89% by weight nickel and 11% by weight aluminum. The bulk density of the material d Sch =0.3kg / L. Bulk density was determined according to the procedure described in Example 1.

[0077] The catalytic efficiency of catalyst C for the hydrogenation of butyne-1,4-diol (BYD) to 1,4-butanediol (BDO) in a stirred tank reactor was also investigated. Experimental setup, procedures and evaluations were performed as described in Example 1.

[0078] The results are summarized in the table below:

[0079] BYD conversion rate

BDO yield

BDO selectivity

STY BDO,V

97％

90％

93％

1.37kg / (L cat*h)

[0080] From the bulk density of catalys...

Embodiment 3

[0084] The catalyst was prepared as described in Example 1, wherein the wet-chemical workup was carried out with 10% by weight aqueous sodium hydroxide solution at 80° C. for 90 minutes. Molybdenum was precipitated on the catalyst from an aqueous molybdate solution after completion of the wet chemical treatment with aqueous sodium hydroxide. Analysis by ICP-OES gave a composition of the resulting catalytically active bulk material (Catalyst D) of 91% by weight nickel, 8.7% by weight aluminum and 0.3% by weight molybdenum. The bulk density of the material is d Sch =0.32kg / L. Bulk density was determined according to the procedure described in Example 1.

[0085] BDO Catalyst D was used in a pilot-scale fixed-bed reactor for the hydrogenation of 4-hydroxybutyraldehyde (HBA) to BDO at a temperature of 60 °C and a hydrogen pressure of 100 bar and showed almost quantitative conversion of HBA , which has very good BDO yield and BDO selectivity.

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Abstract

The present invention relates to a process for preparing 1,4-butanediol (BDO) by hydrogenating 2-butyne-1,4-diol (BYD) or 4-hydroxybutanal (4-HBA) in the presence of a catalyst of the Raney type having a porous foam structure, wherein the macroscopic pores have sizes in the range of 100 to 5000 mum, and a bulk density of up to 0.8 kg / L.

Description

technical field [0001] The present invention relates to a process for the production of 1,4-butanediol (BDO) and a catalyst for the process. Background technique [0002] 1,4-Butanediol itself is used especially in the textile, leather, food and pharmaceutical industries. As an intermediate, it is mainly used in the preparation of thermoplastic polyesters. Furthermore, BDO is a synthetic precursor in the production of some important chemical intermediates and solvents, such as tetrahydrofuran (THF), γ-butyrolactone or pyrrolidine. [0003] The most commonly used industrial process for the production of BDO is based on the continuous hydrogenation of 2-butyne-1,4-diol (BYD) catalyzed by a modified nickel catalyst. This one-step variant of the process is generally carried out in a fixed-bed reactor at 80-160° C. at a pressure of about 300 bar. A two-step hydrogenation of BYD is also known, wherein in the first stage mainly 2-butene-1,4-diol (BED) is produced, at a lower pre...

Claims

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Application Information

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IPC IPC(8): B01J25/02B01J35/02B01J35/10B01J37/08B01J37/00C07C29/17C07C31/20B01J23/755B01J35/04B01J37/02
CPCB01J37/0225B01J37/08B01J23/755B01J37/0018B01J37/0063B01J37/0215B01J37/0217C07C29/172B01J25/02B01J35/50B01J35/40B01J35/56B01J35/657C07C31/207B01J8/008B01J23/862B01J23/866C07C29/14B01J35/31B01J23/26B01J23/28B01J23/745
Inventor M·贝尔魏勒M·格特林格M·罗斯M·施瓦茨R·波斯
Owner EVONIK OPERATIONS GMBH
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