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Process for producing shell powder supported solid acid biodiesel catalyst

A technology of biodiesel and shell powder, applied in catalyst activation/preparation, preparation of liquid hydrocarbon mixture, physical/chemical process catalyst, etc., can solve problems such as environmental pollution, expensive lipase, large amount of alcohol, etc., to improve catalytic performance Effects of activity and service life, elimination of sewage discharge problems, and ease of industrial production

Inactive Publication Date: 2009-04-08
GUANGDONG OCEAN UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The liquid alkali catalysis process has the advantages of relatively cheap and easy-to-obtain catalyst, short reaction time, and high conversion rate, but there are still a series of inherent defects: high quality requirements for raw materials, the acid value of raw materials must be less than 1, and the water content must be Less than 0.5%, that is, the recycling rate of waste oil and industrial waste is low; saponification reaction is prone to occur; the process is complicated and energy consumption is high; the amount of alcohol is large and it is not easy to recycle; the by-product glycerin is difficult to recycle, and the catalyst is difficult to separate from the product. Thereby increasing the cost of follow-up treatment, the most important thing is that waste lye is discharged, forming a new source of environmental pollution
However, there are a series of defects in the preparation of biodiesel catalyzed by lipase: the reaction cycle is long; the enzyme is easily poisoned and inactivated, and if the lower alcohol in the reaction system reaches a certain amount, the enzyme will lose its catalytic activity; at the same time, the price of lipase is relatively expensive
Although liquid acid catalyst (such as CN1412278A adopts sulfuric acid as catalyst) does not have special requirement to the moisture of raw oil and free acid content, it has corrosiveness, very high to equipment requirement, and methyl alcohol and by-product glycerin are difficult to separate after reaction finishes, increase the cost
In addition, using liquid acid as a catalyst will discharge a large amount of sewage in the post-treatment process, causing environmental pollution

Method used

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  • Process for producing shell powder supported solid acid biodiesel catalyst
  • Process for producing shell powder supported solid acid biodiesel catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] At room temperature, dissolve 1 mmol of ethyl naphthalenesulfonic acid in 100ml of water, stir for 15 minutes, add 5 g of activated oyster shell powder to the sulfonic acid solution, load the sulfonic acid under stirring, dry at 60°C, and use the remaining sulfonic acid solution Rinse repeatedly to remove weakly bonded sulfonic acid, then dry at 60°C, bake in an oven, control the heating rate of 4K / min, heat up to 150°C, keep the temperature for 2 hours, then raise the temperature to 200°C, and keep the temperature for 10 hours. That is, the solid acid biodiesel catalyst immobilized by shell powder is obtained. In order to increase the load capacity, multiple loads can be carried out.

[0025] Catalyst activity test, in a 100ml three-neck flask equipped with electromagnetic stirring, a thermometer, and a reflux condenser, add 5g castor oil, 1.5g methanol, and 0.2g of the above-mentioned solid catalyst, heat and reflux and stir for 3h, distill methanol under reduced pres...

Embodiment 2

[0029] At room temperature, dissolve 1.5mmol of ethylnaphthalenesulfonic acid in 100ml of methanol, stir for 10min, add 5g of activated oyster shell powder to the sulfonic acid solution, load the sulfonic acid under stirring, dry at 70°C, and use the remaining sulfonic acid Rinse repeatedly with acid solution to remove weakly bonded sulfonic acid, then dry at 70°C, bake in an oven, control the heating rate of 5K / min, after heating to 150°C, keep the temperature constant for 3 hours, then raise the temperature to 180°C, and then keep the temperature constant After 15 hours, the solid acid biodiesel catalyst immobilized by shell powder was obtained. In order to increase the load capacity, multiple loads can be carried out.

[0030] The catalyst activity test was the same as in Example 1, and the yield of biodiesel reached 99.2%. The catalyst was recycled 12 times, and the yield of biodiesel was between 96-99.2%, and the catalytic activity did not decrease.

Embodiment 3

[0032] At room temperature, dissolve 2 mmol of p-ethylbenzenesulfonic acid in 100ml of methanol, stir for 10 minutes, add 5 g of activated oyster shell powder to the sulfonic acid solution, load the sulfonic acid under stirring, dry at 80°C, and use the remaining Rinse the sulfonic acid solution repeatedly to remove the weakly bonded sulfonic acid, then dry it at 80°C, bake it in an oven, control the heating rate of 6K / min, raise the temperature to 150°C, keep the temperature for 5h, then raise the temperature to 200°C, and then After constant temperature for 24 hours, the solid acid biodiesel catalyst immobilized by shell powder is obtained. In order to increase the load capacity, multiple loads can be carried out.

[0033] The catalyst activity test was the same as in Example 1, and the yield of biodiesel reached 99%. The catalyst was recycled 15 times, and the yield of biodiesel was between 96.5% and 99%, and the catalytic activity did not decrease.

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Abstract

The invention discloses a method for preparing a solid acid biodiesel catalyst loaded by shell powders. The method is to load sulfonic acid on a shell powder carrier through a solid phase synthesis method or a dipping method. The dipping method is as follows: firstly, preparing a sulfonic acid solution with proper concentration; secondly, loading the sulfonic acid; and finally obtaining the catalyst through roasting at a program-controlled temperature after pretreatments of stirring and the like. The solid phase synthesis method is as follows: fully mixing and grinding one or two precursors with certain mass and more than two of sulfonic acid mixtures with certain mass of activating shell powders, and then drying and roasting the mixture to obtain the solid acid biodiesel catalyst immobilized by the shell powders. The solid acid catalyst has the characteristics of high catalytic efficiency, good stability, excellent regenerability and the like, and can be applied in the fields of biodiesel synthesis, esterification, and ester exchange synthesis and the like. For the raw material source and the production process, the method not only reduces the production cost and improves the catalytic efficiency of the catalyst, but also is advantageous for controlling environment pollution, thereby having great meaning on environmental protection.

Description

Technical field: [0001] The invention relates to the technical field of solid acid catalysts and energy, in particular to a preparation method of shell flour-loaded solid acid biodiesel catalysts. Background technique: [0002] Biodiesel is a clean and renewable energy, known as "green gold", which occupies a special position in the energy field. At present, biodiesel is mainly obtained by transesterification, that is, short-chain alcohols such as methanol or ethanol are transesterified with triglycerides, the main component of natural vegetable oil or animal fat, to synthesize long-chain fatty acid A (B) esters - biodiesel. The transesterification method mainly includes homogeneous catalytic method, heterogeneous catalytic method, biocatalytic method and supercritical method. Among them, the chemical catalysis method includes homogeneous and heterogeneous catalysis methods. The homogeneous catalysis method uses liquid acid or liquid alkali as a catalyst to prepare biodies...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J37/02B01J31/02C10G3/00
CPCY02E50/13Y02E50/10Y02P30/20
Inventor 李泳张兆霞洪鹏志
Owner GUANGDONG OCEAN UNIVERSITY
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