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Preparation method of magnetic solid base catalyst immobilized with dimethylbiguanide

The technology of a solid base catalyst and dimethyl biguanide, which is applied in the field of preparation of magnetic solid base catalysts, can solve the problems of difficult product separation and cannot be reused, and achieves the effects of convenient separation and recovery, good stability and easy dispersion.

Inactive Publication Date: 2016-07-27
HENAN UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In view of the fact that the free guanidine organic base catalyst belongs to a homogeneous catalyst, it is not easy to be separated from the product after the reaction, and it cannot be reused. A kind of immobilized dimethyl biguanide solid base catalyst that is easy to separate and recycle is technically needed, and It can efficiently catalyze the transesterification of oil to produce biodiesel, meeting the needs of clean production and improving production efficiency

Method used

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  • Preparation method of magnetic solid base catalyst immobilized with dimethylbiguanide
  • Preparation method of magnetic solid base catalyst immobilized with dimethylbiguanide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] (1) Preparation of carrier

[0035] ① Fe 3 o 4 Magnetic core preparation

[0036] Under nitrogen protection, 13.9gFeSO 4·7H 2 O and 27gFeCl 3 ·6H 2 Add O and 800mL of distilled water into the flask together, stir to dissolve completely, then quickly add 28% ammonia solution (110mL), and heat at 60°C for 1h. The mixture was cooled to room temperature, the solvent was removed by solid-liquid separation, the solid was transferred to a reaction kettle, 0.3 mol / L trisodium citrate solution (500 mL) was added, and stirred at 80°C for 1 h. After cooling to room temperature, the solid-liquid separation removes the solvent under the action of an external magnetic field, washes with acetone 4 times, and puts it in a vacuum drying oven at 60°C for 24 hours to obtain Fe 3 o 4 .

[0037] ② Fe 3 o 4 / SiO 2 Preparation of vector

[0038] will step Fe prepared in 3 o 4 (10g) in a flask, add 300mL of distilled water and stir vigorously to disperse, heat to 40°C, then ad...

Embodiment 2

[0045] (1) Fe 3 o 4 / SiO 2 The preparation method of the carrier is the same as in Example 1.

[0046] (2) Functional modification of the carrier

[0047] 5 g dry Fe 3 o 4 / SiO 2 Put the microspheres into a round-bottomed flask, then pour 200 g of dry toluene into the flask, stir at room temperature for 15 min, slowly add 7.54 g of 3-chloropropyltrimethoxysilane dropwise to the flask under stirring, and then place the mixture at 60 Stirring was continued for 18 h at °C. After the reaction, cool to room temperature, and carry out magnetic separation under the action of an external magnetic field. The obtained solid is put into a Soxhlet extractor and extracted with toluene for 24 hours (or fully washed with toluene 5 times), and then placed in a vacuum drying oven at 80 Dry at ℃ for 12 hours to obtain chloropropyl-modified Fe 3 o 4 / SiO 2 Microspheres.

[0048] (3) Immobilization of dimethyl biguanide

[0049] 5g chloropropyl modified Fe 3 o 4 / SiO 2 Put microsph...

Embodiment 3

[0051] (1) Fe 3 o 4 / SiO 2 The preparation method of carrier is the same as embodiment 1

[0052] (2) Functional modification of the carrier

[0053] 5 g dry Fe 3 o 4 / SiO 2 Put the microspheres into a round bottom flask, then pour 200g of dry toluene into the flask, stir at room temperature for 15min, slowly add 8.62g of 3-chloropropyltrimethoxysilane dropwise to the flask under stirring, and then place the mixture at 60 Stirring was continued for 18 h at °C. After the reaction, cool to room temperature, and carry out magnetic separation under the action of an external magnetic field. The obtained solid is put into a Soxhlet extractor and extracted with toluene for 24 hours (or fully washed with toluene 5 times), and then placed in a vacuum drying oven at 80 Dry at ℃ for 12 hours to obtain chloropropyl-modified Fe 3 o 4 / SiO 2 Microspheres.

[0054] (3) Immobilization of dimethyl biguanide

[0055] 5g chloropropyl modified Fe 3 o 4 / SiO 2 Put microspheres, 3.55...

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Abstract

The invention discloses a preparation method of a magnetic solid base catalyst immobilized with dimethylbiguanide. The preparation method comprises steps as follows: Fe3O4 is prepared from FeSO4*7H2O and FeCl3*6H2O firstly and is stirred and dispersed by adopting distilled water, ethanol and ammonia water sequentially, an ethanol solution of ethyl orthosilicate is dropwise added for sufficient reaction, a mixture is dried, and a magnetic Fe3O4 / SiO2 microsphere is prepared; the magnetic microsphere is modified, and a chloropropyl functionalized Fe3O4 / SiO2 microsphere carrier is prepared; the microsphere carrier, KI, metformin hydrochloride and NaOH are put together, an acetonitrile solvent is added for sufficient reaction, and after drying, the finished product of the magnetic solid base catalyst with the dimethylbiguanide loading quantity of 0.013-0.020 mmol / g is obtained. The process is simple, and the prepared finished catalyst product has high activity and good catalytic stability, is convenient to separate and recycle and has the advantage of repeated usability.

Description

technical field [0001] The invention relates to the fields of oleochemical and chemical application, in particular to a preparation method of a magnetic solid alkali catalyst immobilized with dimethyl biguanide. Background technique [0002] Fossil fuels play an important role in the national economy. Since fossil energy is a non-renewable energy, it will gradually become scarce and exhausted with the excessive exploitation and utilization of human beings, and the use of fossil energy will also cause relatively serious environmental pollution. Therefore, the development of green, environmentally friendly and renewable alternative energy sources has become one of the most important research topics for human beings today. Biodiesel is processed from bio-oil as raw material through transesterification with low-carbon alcohols. Its physical and chemical properties are equivalent to those of petrochemical diesel. It is non-toxic, renewable, biodegradable, high flash point, low fr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/28
CPCB01J31/0251B01J31/0275B01J31/28B01J2231/49B01J35/33
Inventor 谢文磊韩玉香王宏雁
Owner HENAN UNIVERSITY OF TECHNOLOGY
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