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Method for preparing 1,5-pentanediol by using catalyst containing molybdenum disulfide for catalytic hydrogenation of tetrahydrofurfuryl alcohol

A technology for catalytic hydrogenation of tetrahydrofurfuryl alcohol, applied in catalyst activation/preparation, physical/chemical process catalysts, molecular sieve catalysts, etc., can solve problems such as copper chromate environmental pollution, increased processing costs, and long synthesis routes, etc., to achieve The effect of high selectivity, good stability and good application prospects

Active Publication Date: 2019-06-18
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In 1946, Schniepp L E et al. used copper chromate catalyst to successfully prepare 1,5-pentanediol through a three-step method with a yield of 70%. The use will cause serious pollution to the environment and greatly increase the cost of follow-up treatment

Method used

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  • Method for preparing 1,5-pentanediol by using catalyst containing molybdenum disulfide for catalytic hydrogenation of tetrahydrofurfuryl alcohol
  • Method for preparing 1,5-pentanediol by using catalyst containing molybdenum disulfide for catalytic hydrogenation of tetrahydrofurfuryl alcohol
  • Method for preparing 1,5-pentanediol by using catalyst containing molybdenum disulfide for catalytic hydrogenation of tetrahydrofurfuryl alcohol

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Experimental program
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Effect test

Embodiment 1

[0019] Preparation of supported molybdenum sulfide catalyst: 2.5 mmol of sodium molybdate and 20 mmol of sodium sulfide are co-dissolved in 100 ml of deionized water to form a mixed solution, 10 ml of ethanol is added to it, and then 1 g of ceria powder is dispersed in the above solution. After the cerium dioxide was uniformly dispersed, 2 ml of concentrated hydrochloric acid was added to form a precipitate. The catalyst carrier and the precipitate were filtered, washed with deionized water, and dried at 120° C. overnight. The obtained catalyst was reduced in a tube furnace at 450 °C for 0.5 h under a hydrogen atmosphere to obtain a supported molybdenum sulfide catalyst MoS 2 / CeO 2 .

[0020] In the same way, MoS can be prepared separately by replacing the carrier with alumina, silica, titania, zirconia, ceria, molecular sieve, activated carbon, and carbon fiber. 2 / Al 2 O 3 , MoS 2 / SiO 2 , MoS 2 / TiO 2 , MoS 2 / ZrO 2 , MoS 2 / Beta, MoS 2 / AC, MoS 2 / CF and othe...

Embodiment 2

[0022] Hydrogenation metal loading: 1 g MoS 2 / CeO 2 Put it in a beaker, add a chloroplatinic acid solution containing 0.2 mmol Pt, stir evenly, place it at room temperature for 12 hours, and place it in a 120°C oven overnight to dry. 4Pt / MoS can be prepared by reducing the obtained catalyst at 300C for 1 h under a hydrogen atmosphere in a tube furnace 2 / CeO 2 .

[0023] 4Pt / MoS can be prepared by the same method 2 / Al 2 O 3 , 4Pt / MoS 2 / SiO 2 , 4Pt / MoS 2 / TiO 2 , 4Pt / MoS 2 / ZrO 2 , 4Pt / MoS 2 / Beta, 4Pt / MoS 2 / AC, 4Pt / MoS 2 / CF.

[0024] commercial MoS 2 As a carrier, 4Pt / MoS can be obtained by the same method 2 catalyst.

[0025] Molybdenum sulfide catalysts containing different hydrogenation metals can be obtained by changing the hydrogenation metal components.

Embodiment 3

[0027] Experiment of catalytic conversion of tetrahydrofurfuryl alcohol:

[0028] 20g of 5wt% tetrahydrofurfuryl alcohol aqueous solution was added to a 100ml Hastelloy reactor, 0.1g of catalyst and a magnetic stirring rotor were added at the same time, nitrogen was introduced for three times, and then replaced by hydrogen five times. The initial pressure of hydrogen was 4MPa, and magnetic stirring was set. The rotational speed of 800rpm / min, the reaction temperature was 250°C, and the reaction time was 8 hours. After the reaction was completed, the raw materials and products were quantified by the internal standard method using the FID detector. Conversion and selectivity are calculated in moles of carbon.

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Abstract

The invention provides a method for preparing 1,5-pentanediol by using a catalyst containing molybdenum disulfide for catalytic hydrogenation of tetrahydrofurfuryl alcohol. The method is characterizedin that the molybdenum disulfide is loaded onto carriers such as compounds of one, two or more of aluminium oxide, silicon oxide, titanium dioxide, zirconium dioxide, cerium dioxide, molecular sieves, active carbon and carbon fibers; meanwhile, hydrogenation active components are loaded; and the catalyst is applied to catalytic conversion of the tetrahydrofurfuryl alcohol for preparation of the 1,5-pentanediol. The reaction temperature is 180-300 DEG C; and the pressure is 2-7 Mpa. The catalyst provided by the invention is prepared by a relatively simple process, and is high in selectivity and good in stability.

Description

technical field [0001] The invention relates to a method for catalytically converting tetrahydrofurfuryl alcohol to prepare 1,5-pentanediol, in particular to the preparation of a molybdenum sulfide-containing catalyst and the reaction of preparing 1,5-pentanediol by hydrogenation of tetrahydrofurfuryl alcohol Applications. Background technique [0002] 1,5-Pentanediol is an important chemical raw material, and polyesters and polyurethanes synthesized with it as a monomer have lower performance than when other diols such as 1,6-hexanediol and 1,4-butanediol are used. The advantages of viscosity, low glass transition temperature and better flexibility have led to the price of 1,5-pentanediol as high as $6000 / ton, but its annual production is only about 3000 tons, mainly because of the Shortage of effectively available C5 resources (Faraday Discussions, 2017.). [0003] At present, the main production route of industrial production of 1,5-pentanediol is prepared by hydrogenat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/00C07C29/132C07C31/20B01J27/051B01J29/78B01J37/03B01J37/18
Inventor 郑明远李新生张涛
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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