Method for continuously preparing 1, 5-pentanediol from tetrahydrofurfuryl alcohol

A technology for tetrahydrofurfuryl alcohol and pentanediol, which is applied in the field of continuous preparation of 1,5-pentanediol, can solve the problems of low selectivity of 1,5-pentanediol, dependence on petroleum resources for raw materials, difficulty in separation and purification, and the like, Achieving the effect of wide concentration range, simple process and high selectivity

Inactive Publication Date: 2013-02-27
NANJING UNIV OF TECH
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AI Technical Summary

Problems solved by technology

The method adopts batch reaction, and the products include 1,5-pentanediol, tetrahydrofurfuryl alcohol, 1,2-pentanediol, 2-methylfuran, 2-methyltetrahydrofuran, n-pentanol, 2-pentanol, etc. Various components, among which 1,5-pentanediol has low selectivity (<35%), and subsequent separation and purification are difficult
[0010] In the above methods, there may be problems such as dependence on petroleum resources for raw materials, harsh reaction conditions, or low selectivity of the target product 1,5-pentanediol.

Method used

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  • Method for continuously preparing 1, 5-pentanediol from tetrahydrofurfuryl alcohol

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Experimental program
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Effect test

Embodiment 1

[0025] Thoroughly mix 30.0 grams of zirconium hydroxide and 4.15 grams of ammonium metatungstate, add 20 ml of distilled water to adjust the rheological state, and carry out rheological phase reaction at 80~90 °C for 24 hours, then dry at 110 °C and dry at 700 °C Calcining at low temperature for 2-4 hours to obtain tungsten-zirconium composite oxide. Take 10 grams of tungsten-zirconium composite oxide, impregnate it with 6.8 ml of chloroplatinic acid aqueous solution containing 30.0 mg platinum / ml for 10-12 hours, dry it at 110 °C, and roast it at 450 °C for 3 hours to obtain the metal element platinum: tungsten: Catalyst with zirconium molar ratio=0.19:1.0:13.0.

[0026] A tubular fixed-bed reactor with a length of 60 cm and an inner diameter of 10 mm was used. Load 5 grams of catalyst with a particle size of 20-40 mesh, and conduct hydrogen reduction activation at 200°C for 1 hour. , 2 MPa, the mass flow rate of tetrahydrofurfuryl alcohol is 0.75 g / hour, and the hydrogen / t...

Embodiment 2

[0028] Reaction raw material is the tetrahydrofurfuryl alcohol aqueous solution of mass concentration 80%, and other conditions are all identical with embodiment 1. The product obtained from the reaction was analyzed by gas chromatography. The conversion rate of tetrahydrofurfuryl alcohol was 65.1%, the selectivity of the target product 1,5-pentanediol was 86.1%, the selectivity of the by-product n-pentanol was 10.5%, and the selectivity of other by-products was 3.4%.

Embodiment 3

[0030] Reaction raw material is mass concentration 60% tetrahydrofurfuryl alcohol aqueous solution, other conditions are all identical with embodiment 1. The product obtained from the reaction was analyzed by gas chromatography. The conversion rate of tetrahydrofurfuryl alcohol was 81.5%, the selectivity of the target product 1,5-pentanediol was 88.0%, the selectivity of the by-product n-pentanol was 10.9%, and the selectivity of other by-products was 1.1%.

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Abstract

The invention discloses a method for continuously preparing 1, 5-pentanediol from tetrahydrofurfuryl alcohol. According to the method, platinum loaded tungsten-zirconium composite oxide is taken as a catalyst, and a 10-90% solution tetrahydrofurfuryl alcohol aqueous 10-90% solution and hydrogen are simultaneously and continuously introduced into a fixed bed reactor for reaction so as to generate1, 5-pentanediol under the reaction conditions that the temperature is 100-150 DEG C, the pressure is 1-5 MPa, the mass flow rate of the tetrahydrofurfuryl alcohol is 0.05-1 A/H (A is the mass of the catalyst in the reactor), and the mol ratio of hydrogen to tetrahydrofurfuryl alcohol is 10-100. The mol ratio of various metal elements in the catalyst is Pt: W: Zr=(0.05-0.5): 1: (5-30). The method is moderate in reaction condition, high in catalytic activity, good in product selectivity, simple in process and continuous in production; and the raw materials are from biomass, thereby meeting the green chemical development direction.

Description

technical field [0001] The invention relates to a method for continuously preparing 1,5-pentanediol by using tetrahydrofurfuryl alcohol as a raw material. Background technique [0002] 1,5-pentanediol is an important organic chemical raw material, mainly used in the production of saturated / unsaturated polyester resins, oil-free alkyd resins, polyester polyols and esters for synthetic lubricants, polyurethane foams and Elastomer plasticizers, high-grade lubricating oil additives and other fine chemicals, the polyurethane materials and polyester materials synthesized with them have excellent performance and have broad application prospects. [0003] At present, the methods for preparing 1,5-pentanediol mainly contain the following types: [0004] (1) Chinese patent CN101270032 discloses a method for preparing 1,5-pentanediol by hydrogenation of 1,5-glutaraldehyde using a supported Ru catalyst under the reaction conditions of 50-160 °C and 0.5-15.0 MPa. The raw material 1,5-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/20C07C29/132B01J23/652
Inventor 陈长林陈洪龙
Owner NANJING UNIV OF TECH
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