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Method for catalyzing esterification reaction by means of high-stable-acidity mesoporous-microporous molecular sieve

A technology of molecular sieve catalyzing esters and microporous molecular sieves, applied in molecular sieve catalysts, fatty acid esterification, chemical instruments and methods, etc., can solve the problems of low conversion rate of oleic acid and high reaction temperature of 160 °C, and achieve stable catalytic performance, high heat Strong stability and good repeatability

Inactive Publication Date: 2015-09-02
QINGDAO UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

At present, the molecular sieve used to catalyze the esterification of oleic acid is SBA-15 mesoporous molecular sieve, but the reaction temperature is 160°C (Chemical Industry and Engineering, 2011, 28, 2: 68-72; Journal of Liaoning University of Petroleum & Chemical Technology, 2008, 28, 4: 9-13) or the oleic acid conversion rate is low, only about 44% (Speciality Petrochemicals, 2007, 24, 2: 58-61)

Method used

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  • Method for catalyzing esterification reaction by means of high-stable-acidity mesoporous-microporous molecular sieve

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Experimental program
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Effect test

Embodiment 1

[0011] The preparation of β / Al-MCM-41 catalyst: the β / Al-MCM-41 catalyst of n(Si):n(Al)=30 is prepared by stepwise crystallization method, and the synthesis steps are as follows: NaOH, NaAlO 2 , SiO 2 Aqueous solution (mass fraction 30%) and mass fraction are the aqueous solution of TEAOH of 25% according to molar ratio n (Al 2 o 3 ) / n(SiO 2 ) / n(Na 2 O) / n(TEAOH) / n(H 2 (2) = 1.0 / 60 / 2.5 / 22 / 800 ratio mixing, and stirring, then the mixture is transferred to the autoclave, dissolved at 140 ° C for 4 hours, the resulting clear solution, namely Beta zeolite directing agent; Add the Beta zeolite directing agent into cetyltrimethylammonium bromide (CTAMBr) aqueous solution, mix and stir for 30min, adjust the pH value with 5mol / L sulfuric acid, add ethanol; In a tetrafluoroethylene-lined stainless steel reactor, seal it, and after crystallization, suction filter, wash, dry, and roast to obtain a β / Al-MCM-41 molecular sieve catalyst, which is ready for use.

[0012] With 10 grams o...

Embodiment 2

[0014] The preparation of β / Zr-MCM-41 catalyst: the β / Zr-MCM-41 catalyst of n(Si): n(Al)=30 is prepared by stepwise crystallization method, and the synthesis steps are as follows: NaOH, NaAlO 2 , SiO 2 Aqueous solution (mass fraction 30%) and mass fraction are the aqueous solution of TEAOH of 25% according to molar ratio n (Al 2 o 3 ) / n(SiO 2 ) / n(Na 2 O) / n(TEAOH) / n(H 2 (2) = 1.0 / 60 / 2.5 / 22 / 800 ratio mixing, and stirring, then the mixture is transferred to the autoclave, dissolved at 140 ° C for 4 hours, the resulting clear solution, namely Beta zeolite directing agent; Add the Beta zeolite directing agent into the cetyltrimethylammonium bromide (CTAMBr) aqueous solution, mix and stir for 30min, add Zr(SO 4 ) 2 The aqueous solution (Si / Zr=1 / 0.05) was continuously mixed and stirred for 30 min, the pH value was adjusted with 5 mol / L sulfuric acid, and ethanol was added; stirred for 1 h at room temperature, the mixed solution was transferred into a stainless steel reactor lin...

Embodiment 3

[0017] The preparation of β / Sn-MCM-41 catalyst: preparation condition and step are with embodiment 2, just Zr(SO 4 ) 2 The aqueous solution is changed into SnCl4 aqueous solution.

[0018] Experimental condition and step are the same as embodiment 1, just change catalyst β / Al-MCM-41 into catalyst β / Sn-MCM-41, when alcohol-oil ratio is 10: 1, catalyst consumption accounts for 5% of reactant quality, 120 The highest conversion rate of oleic acid was 70.12% when reacting at ℃ for 8 hours.

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Abstract

The invention relates to a method for catalyzing esterification reaction by means of a high-stable-acidity mesoporous-microporous molecular sieve. The method is characterized by comprising the following steps: compounding the high-stable-acidity mesoporous-microporous molecular sieve in a step-by-step crystallization method by using self-produced beta zeolite as a guiding agent, loading a rare-earth La element, and catalyzing the esterification reaction of oleic acid and methyl alcohol by using the compounded acidic mesoporous-microporous molecular sieve. When the ratio of alcohol to oil is 10:1, the consumption of catalyst is 5 percent of the total quantity, and reaction is performed for 8 hours at the temperature of 120 DEG C, the conversion rate of oleic acid is not less than 70 percent, and the catalyst is good in hydrothermal stability and reusability.

Description

technical field [0001] The invention belongs to the technical field of biomass energy conversion, and mainly relates to a method for generating biodiesel by catalyzing the esterification reaction of oil with highly stable acidic mesoporous-microporous molecular sieves. Background technique [0002] Biodiesel is one of the most important renewable liquid fuels for biomass energy. It has high energy density, good lubrication performance, safe storage and transportation, good anti-knock performance, and sufficient combustion. It is also renewable and environmentally friendly. It is the bulk bio-based liquid fuel with the most development potential. Among them, methyl oleate, which is representative, has been valued as a biofuel in recent years. Industrial production is generally prepared by the esterification reaction of oleic acid and methanol using liquid sulfuric acid as a catalyst. Due to the strong oxidizing property of sulfuric acid, there are many by-products of the es...

Claims

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Application Information

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IPC IPC(8): C11C3/04C10L1/02B01J29/80
Inventor 王志萍于世涛
Owner QINGDAO UNIV OF SCI & TECH
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