Method for preparing hexitol or hydroxy-acetone

A technology of hydroxyacetone and hexitol, which is used in the preparation of carbon-based compounds, chemical instruments and methods, and the preparation of hydroxyl compounds.

Active Publication Date: 2012-08-01
PEKING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But so far, the efficient conversion of cellulose and its derivatives to hydroxyacetone has not been reported

Method used

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  • Method for preparing hexitol or hydroxy-acetone
  • Method for preparing hexitol or hydroxy-acetone
  • Method for preparing hexitol or hydroxy-acetone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Embodiment 1, hydrolysis cellulose prepares hexitol

[0021] Supported Metal Catalyst Pt-SnO x / Al 2 o 3 Preparation: SnCl 2 2H 2 O and H 2 PtCl 6 ·6H 2 O was mixed at a molar fraction ratio of 0.3, then 1 drop of 37% hydrochloric acid solution was added dropwise and water was added, and after a uniform solution was formed, Al was added 2 o 3 ; After drying at room temperature, place it in an oven at 110°C for drying overnight, then successively roast (calculate at 400°C and air atmosphere for 4 hours) and reduce (at 400°C and 20% H 2 / N 2 Reduction under the atmosphere of 4 hours) that is.

[0022] 1g of microcrystalline cellulose (microcrystalline cellulose, available from Alfa Aesar) is placed in a 100ml reaction kettle with a sufficient amount of water (50ml), and 0.4g of the 2% prepared above (the mass percent of metal Pt in the active component) is added. content) Pt-SnO x / Al 2 o 3 (Sn / Pt=0.3, x is 0~4), filled with H 2 , the pressure in the reacto...

Embodiment 2

[0034] Embodiment 2, hydrolyzing cellulose to prepare hexitol

[0035] Supported Metal Catalyst Pt-SnO x / Al 2 o 3 Preparation: the specific preparation method is the same as in Example 1, the difference is: SnCl 2 2H 2 O and H 2 PtCl 6 ·6H 2 The molar fraction ratio of O is 0.5.

[0036] 1g of microcrystalline cellulose (microcrystalline, purchased from Alfa Aesar) was placed in a 100ml reaction kettle filled with sufficient water (50ml), and 0.4g of 2% Pt-SnO x / Al 2 o 3 (Sn / Pt=0.5, x is 0~4), filled with H 2 , the pressure in the reactor was 20atm, heated to 240°C, and reacted for 30 minutes.

[0037] According to the following method, the conversion rate of cellulose and the selectivity of hexitol were detected:

[0038] The unreacted cellulose was weighed on a balance, and it was 0g; the reaction product was analyzed by high performance liquid phase and quantified (Shimadazu LC-20A HPLC; separation column: BioRad Aminex HPX-87H; analysis conditions: mobile phase...

Embodiment 3

[0041] Embodiment 3, hydrolysis cellulose prepares hydroxyacetone

[0042] Supported Metal Catalyst Pt-SnO x / Al 2 o 3 Preparation: the specific preparation method is the same as in Example 1, the difference is: SnCl 2 2H 2 O and H 2 PtCl 6 ·6H 2 The mole fraction ratio of O was 4.0.

[0043] 1g of microcrystalline cellulose (microcrystalline, purchased from Alfa Aesar) was placed in a 100ml reaction kettle filled with sufficient water (50ml), and 0.4g of 2% Pt-SnO x / Al 2 o 3 (Sn / Pt=4.0, x is 0~4), filled with H 2 , make the pressure in the reactor be 80atm, heat to 200°C, and react for 30 minutes.

[0044] According to the following method, the conversion rate of cellulose and the selectivity of hydroxyacetone are detected:

[0045] The unreacted cellulose was weighed on a balance, and it was 0.779g; the reaction product was analyzed and quantified by high performance liquid phase (Shimadazu LC-20A HPLC; separation column: BioRad Aminex HPX-87H; analysis conditio...

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Abstract

The invention discloses a method for preparing hexitol or hydroxy-acetone, which comprises the steps as follows: cellulose reacts with glucose or fructose in water under the action of hydrogen atmosphere and catalytic agents, so as to obtain hexitol or hydroxy-acetone; the catalytic agents are supported metal catalysts; active constituents of the supported metal catalysts are metal modified by modifiers; the metal is any one of Pt, Ru, Ni and Cu; and a carrier of the supported metal catalysts is any one of Al2O3, TiO2, ZrO2, SiO2 and activated charcoal. The provided method selectively obtains hexitol or hydroxy-acetone through a one-pot reaction based on cellulose and glucose or fructose, achieves simple process, rapid reaction, high efficiency and energy conservation, and is easy to industrialize; the catalytic agents can be recovered and recycled, so that the cost is saved, and environmental protection can be achieved; in addition, the method has low requirements on equipment, cannot corrode equipment, and achieves low investment.

Description

technical field [0001] The invention relates to a method for preparing hexitol or hydroxyacetone. Background technique [0002] Biomass is rich in sources, renewable, and contains carbon elements and hydroxyl functional groups. It is a potential substitute for fossil resources. Cellulose is one of the most important components of biomass, and its effective conversion is an important content of biomass utilization. Cellulose is glucose monomers polymerized into chains through 1,4-β-glucosidic bonds, and the chains are connected by abundant hydrogen bonds to form a crystal structure with a high degree of polymerization and high crystallinity. Depolymerization of cellulose into glucose monomers and hydrogenation of them into polyols is one of the feasible routes for the efficient conversion of cellulose. [0003] Polyols are widely used in food, solvents, antifreeze, pharmaceuticals and cosmetics. At present, there are few methods for efficiently synthesizing polyols from ce...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/26C07C29/00C07C49/17C07C45/00B01J23/62B01J23/835
Inventor 刘海超邓甜音
Owner PEKING UNIV
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