Tetrahydro furfuryl alcohol preparing process

A tetrahydrofurfuryl alcohol production method technology, applied in the field of tetrahydrofurfuryl alcohol production method, can solve the problems of high temperature, high pressure, fracture, etc.

Inactive Publication Date: 2012-07-04
淄博华澳化工有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its disadvantages are: (1) According to the reaction mechanism of furfuryl alcohol hydrogenation, when furfuryl alcohol is hydrogenated to generate tetrahydrofurfuryl alcohol, the carbon-oxygen single bond on the side chain of the furfuryl ring of furfuryl alcohol may also be broken and undergo hydrogenolysis to generate 2-methylfurfuryl alcohol. Barking
Theoretically, the pressure of the reaction is high, the temperature is high, and by-products are easily produced; (2) the preparation method of the catalyst is complicated and not suitable for large-scale industrial production

Method used

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  • Tetrahydro furfuryl alcohol preparing process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Preparation of catalyst

[0025] 10Kg of nickel-aluminum alloy was slowly added to 50Kg of 30% sodium hydroxide solution. Because the reaction exothermed violently, the addition rate was controlled so that the temperature was 30°C-40°C. After the addition is complete, when the foam disappears, the temperature is raised to 65° C., the temperature is kept for 1 hour, and after washing twice, a catalyst with a composition content of 45% nickel, 51% aluminum and 4% molybdenum is obtained. Soak in water for later use.

[0026] (2) Preparation of tetrahydrofurfuryl alcohol

[0027] Add 1000Kg of furfuryl alcohol (purity ≥98.5%, moisture ≤0.2%, residual aldehyde ≤0.5%) and 6Kg of the catalyst prepared into the reaction kettle, vacuum out the air in the kettle, and carry out hydrogenation in the form of a suspended bed. During the reaction, the reaction pressure was 1.5 MPa, the temperature was 40°C-50°C, after hydrogenation for 7 hours, the temperature was raised to 95-100°C, a...

Embodiment 2

[0029] (1) Preparation of catalyst

[0030] 10Kg of nickel-aluminum alloy was slowly added to 57Kg of 35% sodium hydroxide solution. Because the reaction exothermed violently, the addition rate was controlled so that the temperature was 45°C-50°C. After the addition is complete, when the foam disappears, the temperature is increased to 55° C., the temperature is kept for 2 hours, and after washing twice with water, a catalyst with a composition content of 20% nickel, 70% aluminum and 10% molybdenum is prepared. Soak in water for later use.

[0031] (2) Preparation of tetrahydrofurfuryl alcohol

[0032] Add 1000Kg of furfuryl alcohol (purity ≥98.5%, moisture ≤0.2%, residual aldehyde ≤0.5%) and 1Kg of the prepared catalyst into the reaction kettle, vacuum out the air in the kettle, and carry out hydrogenation in the form of a suspended bed. During the reaction, the pressure was 1.6 MPa, and the temperature was 45°C to 55°C. After hydrogenation for 7 hours, the temperature was raised ...

Embodiment 3

[0034] (1) Preparation of catalyst

[0035] 10Kg of nickel-aluminum alloy was slowly added to 62.5Kg of 40% sodium hydroxide solution. Because the reaction exothermed violently, the addition rate was controlled so that the temperature was 40°C to 45°C. After the addition is complete, when the foam disappears, the temperature is raised to 65° C., the temperature is kept for 1 hour, and after washing twice, a catalyst with a composition content of 50% nickel, 49% aluminum and 1% molybdenum is prepared. Soak in water for later use.

[0036] (2) Preparation of tetrahydrofurfuryl alcohol

[0037] Add 1000Kg of furfuryl alcohol (purity ≥98.5%, moisture ≤0.2%, residual aldehyde ≤0.5%) and 3Kg of the catalyst prepared into the reaction kettle, vacuum out the air in the kettle, and carry out hydrogenation in the form of a suspended bed. During the reaction, the pressure was 2.0MPa, the temperature was 60℃~70℃, after 6h of hydrogenation, the temperature was raised to 100~105℃, and the temper...

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Abstract

The preparation process of tetrahydro furfuryl alcohol belongs to the field of preparing technology of quinary heterocyclic compound with only one hetero atom. The preparation process includes liquid phase hydrogenation of furfuryl alcohol in the presence of catalyst at pressure of 1.5-2 MPa and temperature of 30-80 DEG C for 6-7 hr; heating after reaction to 95-105 DEG C and maintaining for 1-2 hr; discharging and precipitating for 8 hr; and vacuum distillation to produce tetrahydro furfuryl alcohol product. The catalyst consists of Ni 20-60 wt%, aluminum 30-70 wt% and Mo 0.1-10 wt%. The preparation process of the present invention has mild reaction condition and high catalyst selectivity, and the tetrahydro furfuryl alcohol product has purity over 99.5 % and may be used in medicine industry.

Description

technical field [0001] The invention belongs to the technical field of five-membered heterocyclic compounds containing an oxygen atom as the only ring heteroatom, and specifically relates to a method for preparing tetrahydrofurfuryl alcohol. Background technique [0002] Tetrahydrofurfuryl alcohol (THFA), also known as THFA, is a special solvent with a wide range of applications. For example: it can be used to prepare pesticide sprays for protecting grains; it can also be used as a wetting and diffusing agent for pigments in the formulation of water-based paints and varnishes of various colors; it can be used in the dyeing and finishing of fabrics and leather; Catalyst and solvent; as a plasticizer of oleic acid vinegar, it can dissolve cellulose derivatives, polyvinyl chloride, polystyrene, polymethacrylic acid, artificial and natural resins, rubber, etc., and can improve the low temperature flexibility of polyethylene film , to give the film flakes inherent lubricity and ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/44
Inventor 黄信礼韩克林韩克英赵成文
Owner 淄博华澳化工有限公司
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