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Method for preparing isosorbide based on cellulose

A technology for isosorbide and cellulose, applied in the field of preparing isosorbide based on cellulose and isosorbide, can solve the problems of inevitable equipment corrosion, increase equipment investment and maintenance costs, environmental pollution, etc., and achieve high selectivity. The effect of sexual transformation, small investment and low corrosion

Inactive Publication Date: 2013-09-04
SUZHOU INST OF NANO TECH & NANO BIONICS CHINESE ACEDEMY OF SCI +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The problem with this method is that the addition of inorganic liquid acid is a non-green process, and there is the discharge of waste acid liquid, causing environmental pollution, and there is inorganic liquid acid at a temperature of 190-250 ° C, which imposes harsh requirements on equipment, which is unavoidable Cause corrosion of equipment, increase equipment investment and maintenance costs

Method used

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  • Method for preparing isosorbide based on cellulose
  • Method for preparing isosorbide based on cellulose
  • Method for preparing isosorbide based on cellulose

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Put 0.06g of 5wt% ruthenium / hydrous niobium oxide catalyst, 0.6g of cellulose (microcrystalline, Alfa Aesar) and 30mL of water into a 100mL reaction kettle, and replace the gas with hydrogen gas for 6 times, fill it with hydrogen gas to 6MPa, and raise the temperature to 220°C for reaction After 1 h, the temperature was rapidly lowered after the reaction, and the supernatant liquid after centrifugation was taken for high-performance liquid chromatography analysis.

[0027] After the reaction finishes, measure the amount of isosorbide in the reaction solution according to the following method:

[0028] Quantitative analysis of the reaction products was carried out by high performance liquid chromatography (Agilent1260series HPLC, Beijing Agilent Co., Ltd.), the separation column was Alltech Prevail Carb ES, with acetonitrile and water as the mobile phase, the flow rate was 0.8mL / min, the column temperature was 30°C, and the evaporating light Scattering detector.

[0029...

Embodiment 2

[0035] Put 0.06g of 5wt% ruthenium / niobium-silicon composite oxide catalyst, 0.6g of cellulose (microcrystalline, Alfa Aesar) and 30mL of water into a 100mL reactor, and replace the gas with hydrogen gas for 6 times, fill it with hydrogen to 6MPa, and raise the temperature to 210 ℃ for 1.5 h, after the reaction was completed, the temperature was rapidly lowered, and the centrifuged supernatant liquid was taken for high-performance liquid chromatography analysis.

[0036] According to the method described in Example 1, measure and calculate the amount of isosorbide in the reaction solution.

[0037] The results showed that the conversion rate of cellulose was 98%, the selectivity of isosorbide was 32%, and the yield of isosorbide was 31.4%.

Embodiment 3

[0039] Put 0.04g of 5wt% ruthenium / niobium-molybdenum composite oxide catalyst, 0.6g of microcrystalline cellulose (microcrystalline, Alfa Aesar) and 30mL of water into a 100mL reaction kettle, replace the gas with hydrogen gas for 6 times, fill it with hydrogen gas to 6MPa, and raise the temperature React at 230°C for 0.5h. After the reaction, the temperature is rapidly lowered, and the supernatant liquid after centrifugation is taken for high-performance liquid chromatography analysis.

[0040] According to the method described in Example 1, measure and calculate the amount of isosorbide in the reaction solution.

[0041] The results showed that the conversion rate of cellulose was 99%, the selectivity of isosorbide was 33%, and the yield of isosorbide was 32.7%.

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Abstract

The invention relates to the technical field of fine chemical engineering and discloses a method for preparing isosorbide based on cellulose. The method comprises the following steps of: adding a cellulose raw material into an airtight high-pressure reactor containing enough water, wherein the reaction pressure is 1-12 MPa, and the reaction temperature is 180-300DEG C; and carrying out hydrolysis, hydrogenation and hydration reactions in water for 0.5-48 hours in the presence of a catalyst to obtain the isosorbide. The catalyst is a metal / solid acid bifunctional catalyst and has the addition amount of 0.03-2.0g / g cellulose. The method disclosed by the invention has low corrosion to equipment as no inorganic liquid acid needs to be added, and is low in cost, simple in reaction system and easy to industrialize; and the catalyst is long in service life and free of loss.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and relates to a method for preparing isosorbide, in particular to a method for preparing isosorbide based on cellulose. Background technique [0002] Vigorously developing bio-based chemicals can not only reduce the consumption of petroleum resources by the chemical industry, but also help create a new high value-added market. Isosorbide is one of the representatives of bio-based chemicals, which has the characteristics of rigidity, chirality and non-toxicity. Isosorbide and its derivatives are an important class of fine chemical raw materials, widely used in the synthesis of medicines, skin care products, food, fuels and polymers. Especially in the pharmaceutical industry, isosorbide derivatives are used in the treatment of cardiovascular diseases or as penetrating solvents for other drugs. The substitution of isosorbide derivatives for traditional toxic plastics has also gained consid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D493/04
Inventor 李福伟孙鹏
Owner SUZHOU INST OF NANO TECH & NANO BIONICS CHINESE ACEDEMY OF SCI
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