Carbon-based magnetic solid acid catalyst and application thereof in preparing biodiesel

A magnetic solid acid and biodiesel technology, applied in physical/chemical process catalysts, biofuels, fatty acid esterification, etc., can solve the problems of poor stability, low separation recovery rate, low surface activity, etc., and achieve excellent recycling capacity , good catalytic effect, good catalytic activity and application value

Active Publication Date: 2017-05-31
XISHUANGBANNA TROPICAL BOTANICAL GARDEN CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a carbon-based magnetic solid with high activity, strong magnetism, good stability and long life in view of the shortcomings of existing biodiesel magnetic solid acid catalysts, such as low surface activity, poor stability, and low separation recovery rate. acid catalyst

Method used

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  • Carbon-based magnetic solid acid catalyst and application thereof in preparing biodiesel
  • Carbon-based magnetic solid acid catalyst and application thereof in preparing biodiesel
  • Carbon-based magnetic solid acid catalyst and application thereof in preparing biodiesel

Examples

Experimental program
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Effect test

Embodiment 1

[0038]Take 2g of CMC into 100mL of pure water and heat to dissolve to make solution A; put 40g of ferric sulfate into 100mL of pure water and heat to dissolve to make solution B; under stirring condition, use a syringe to take 100mL of solution A and add dropwise to 100mL of solution In B, the solution was left standing for 3 hours after completion, the solid precipitate was filtered out, washed, dried and ground through a 40-mesh sieve. Take about 10g of the obtained solid and soak it in 50mL of 1mol / L ferric sulfate solution for 3h. The obtained samples were washed, filtered, dried and calcined at 400, 500 and 600 °C for 2 h to obtain the carbon-based magnetic material C 400 / 500 / 600 @Fe.

[0039] figure 1 for C 400 The scanning electron microscope image of @Fe shows that the particle size is about 200 μm.

[0040] figure 2 (a) is C 400 The magnetic saturation intensity curve of @Fe, the magnetic saturation intensity is 6.2Am 2 / g or so.

[0041] Take 3g Magnetic C ...

Embodiment 2

[0043] Repeat Example 1, the following difference is arranged: get 1g CMC powder and be dissolved in 100mL pure water and be made into CMC solution, get 80g ferric sulfate and put into 100mL pure water and heat and dissolve and be mixed with Fe 3+ solution. Calcined at 600°C for 2h to obtain carbon-based magnetic material C 600 @Fe-1.

[0044] Take 1g Magnetic C 600 Mix @Fe‐1 and 200mL CMC aqueous solution evenly, and then add dropwise to 200mL0.5mol / L Fe 2 (SO 4 ) 3 In the solution, the solution was continuously stirred on a magnetic stirrer during the dropwise addition to make the chelation reaction fully proceed, and left to stand for 3 hours, then the solid was filtered out and washed and dried. Take 1 g of the dried solid sample, add 100 mL of 98% concentrated sulfuric acid, and sulfonate it in an oil bath at 200 °C for 10 h, wash the solid obtained by sulfonation with pure water at 80 °C until neutral, freeze-dry, grind and pass 200 mesh sieves, prepared carbon-bas...

Embodiment 3

[0046] Repeat Example 1 with the following differences: 5g of CMC powder is dissolved in 100mL of pure water to form a CMC solution.

[0047] Take 5g Magnetic C 400 @Fe was mixed in 200mL CMC solution and dispersed into a suspension. The suspension was added dropwise to 200mL 4mol / L zirconium oxychloride solution, and allowed to stand for 3h. The precipitated solid was filtered off, washed neutral and dried in an oven at 105°C overnight. Take 1 g of the dried solid sample and add it to 10 mL of 98% concentrated sulfuric acid, and sulfonate it in an oil bath at 100° C. for 24 h. The solid produced by sulfonation was washed with hot water at 80°C until neutral, freeze-dried, ground and passed through a 200-mesh sieve to obtain a magnetic solid acid catalyst C 400 -SO 3 H@Zr‐C@Fe‐2.

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Abstract

The invention discloses a carbon-based magnetic solid acid catalyst and an application thereof in preparing biodiesel. The catalyst is prepared by the following steps: mixing a CMC solution and a Fe<3+> solution; precipitating a solid and then soaking the solid with the Fe<3+> solution; calcining and grinding the dried solid to obtain a magnetic material; then mixing the CMC with a Zr<2+>/ Fe<3+> solution; and after drying the solid material, sulfonating, filtering, washing, freezing and drying the solid material to obtain the carbon-based magnetic solid acid catalyst. The catalyst has Lewis acidity and acidity of a formula as shown in the description and has relatively proper saturated magnetic intensity, can be directly used for a reaction on high acid value oil, and is quite good in catalytic effect. The biodiesel yield is greater than 95% and the recovery rate of the catalyst is greater than 90%. The catalyst is relatively preferable in circulating capacity, and the yield of biodiesel after reactions for 5 times also can reach 80% or above. The deactivated catalyst is reacted circularly for 5 times through sulfonating treatment, and the biodiesel yield still can reach 90% or above.

Description

technical field [0001] The invention belongs to the technical field of biodiesel preparation and catalyst application, and in particular relates to a synthesis method of a new carbon-based magnetic solid acid catalyst. At the same time, the invention also relates to the specific application of the catalyst in biodiesel preparation. Background technique [0002] Currently, human society relies heavily on fossil fuels for energy. The burning of fossil fuels has led to the destruction of the ecological environment, and problems such as smog, greenhouse effect, and environmental pollution have seriously affected people's lives and health. The depletion of fossil fuels makes people realize that it is very important to develop clean, environmentally friendly and green renewable energy. Biodiesel is a renewable fuel produced by transesterification reaction of vegetable oil, animal oil, catering waste oil and low-priced alcohol under the action of acidic and basic catalysts, and h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/053C11C3/08C10L1/02
CPCB01J27/053B01J35/0033C10L1/02C10L2290/12C11C3/08Y02E50/10
Inventor 王一同罗嘉方真杨星霞张帆
Owner XISHUANGBANNA TROPICAL BOTANICAL GARDEN CHINESE ACAD OF SCI
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