Preparation method of loaded solid catalyst used in deacidification of high-acid-value grease

A solid acid catalyst, high acid value oil technology, applied in physical/chemical process catalysts, molecular sieve catalysts, chemical instruments and methods, etc., can solve the problems of time-consuming and energy-consuming, complex process, low catalytic efficiency, etc., and achieve easy separation. The effect of recovery, simple preparation and high catalyst activity

Inactive Publication Date: 2012-02-08
BEIJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The most commonly used method to produce biodiesel is to use animal and vegetable oils and alcohols to undergo alcohol transesterification through solid alkali catalysts, but waste oils and fats contain a large amount of free fatty acids and polymers, resulting in too high acid values. If these high If the acid value waste oil is converted into biodiesel, then the solid base catalyst will be deactivated quickly due to poisoning
Therefore, these waste oils with high acid value cannot be directly used as raw materials for the production of biodiesel by the alkali-catalyzed method.
[0004] CN101092569A, CN101063040A, CN1382762A, CN1412278A and other Chinese patents report the method of preparing biodiesel with waste oil with high acid value as raw material, but due to the use of homogeneous catalytic route, the catalytic efficiency is not high, and the equipment is severely corroded
US4652406, CN1556174, CN101074390 and other patents use pretreatment to reduce the acid value, but the process is complicated, the production cycle is long, and the energy consumption is high
CN1887417A, CN101067091A and other patents propose to use composite rare earth solid acid catalyst for pretreatment, but the catalyst composition is complex and the production cost is high
The CN1904013A patent uses a fixed bed reaction path to reduce the acid value, but this method requires high temperature and high pressure conditions
[0005] It can be seen from this that in the process of biodiesel preparation using high acid value oils and fats as raw materials, if solid base catalyzed transesterification technology is simply used, the resulting biodiesel must have low catalytic efficiency and high production costs. and the disadvantages of time-consuming and energy-consuming

Method used

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Examples

Experimental program
Comparison scheme
Effect test

specific Embodiment 1

[0022] Weigh 0.10g of phosphotungstic acid and dissolve it in 9ml of deionized water, add 1ml of nitric acid with a mass percentage concentration of 65%, adjust the pH of the solution to 1, and then dry 1g of SiO at 150°C for 3 hours 2 Mesoporous molecular sieve (with 3nm mesoporous and 20nm mesoporous at the same time, the specific surface area is 1000m 2 / g and a pore volume of 2.0cm 3 / g) was immersed therein, stirred at 80° C. for 12 hours, and evaporated to dryness to obtain a solid sample. After the solid sample was fully ground, under the protection of nitrogen, the temperature was raised to 250°C at a rate of 5°C / min, and kept at a constant temperature for 6 hours, then quickly placed in a desiccator to naturally cool to room temperature and sealed to obtain a supported solid acid catalyst.

[0023] In a 100ml three-necked flask, add grease with an acid value of 50mg KOH / mL, methanol, and the molar ratio of alcohol to oil is 10:1, preheat to 67°C, add the above-mentio...

specific Embodiment 2

[0024] Weigh 0.40g of phosphozirconic acid and dissolve it in 9ml of acetone, and add 1ml of nitric acid with a mass percentage concentration of 65%, adjust the pH value of the solution to 1, and then dry 1g of SiO2 at 100°C for 5 hours 2 Mesoporous molecular sieve (with 2nm mesoporous and 15nm mesoporous at the same time, the specific surface area is 1200m 2 / g and a pore volume of 3.0cm 3 / g) was immersed therein, stirred at 35° C. for 1 hour, and evaporated to dryness to obtain a solid sample. After the solid sample was fully ground, the temperature was raised to 600°C at a rate of 10°C / min under the protection of nitrogen, and the temperature was kept constant for 3 hours, then quickly placed in a desiccator to naturally cool to room temperature and sealed to obtain a supported solid acid catalyst.

[0025] In a 100ml three-necked flask, add grease with an acid value of 30mg KOH / mL, methanol, and the molar ratio of alcohol to oil is 5:1, preheat to 57°C, add the above-men...

specific Embodiment 3

[0026] Weigh 0.20g of phosphoniobic acid and dissolve it in 10ml of chloroform, and add 1ml of nitric acid with a mass percentage concentration of 65% to adjust the pH value of the solution to 1, and then dry 1g of SiO at 120°C for 5 hours 2 Mesoporous molecular sieve (with 2nm mesoporous and 10nm mesoporous at the same time, the specific surface area is 1500m 2 / g and a pore volume of 3.5cm 3 / g) was immersed therein, stirred at 40° C. for 6 hours, and evaporated to dryness to obtain a solid sample. After the solid sample was fully ground, the temperature was raised to 150°C at a rate of 8°C / min under the protection of nitrogen, and kept at a constant temperature for 5 hours, then quickly placed in a desiccator to naturally cool to room temperature and sealed to obtain a supported solid acid catalyst.

[0027] In a 100ml three-necked flask, add grease with an acid value of 100mg KOH / mL, methanol, and the molar ratio of alcohol to oil is 20:1, preheat to 60°C, add the above-m...

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Abstract

The invention relates to a preparation method of a loaded solid catalyst, in particular to a preparation method of a loaded solid catalyst used in deacidification of high-acid-value grease. In the method, a SiO2-based mesoporous molecular sieve with a dual-model duct structure is taken as a carrier; one of super acids such as phosphotungstic acid, phosphomolybdic acid, zirconium phosphate, phosphorus niobate and the like is loaded for serving as an active ingredient; in the deacidification process of high-acid-value waste grease, the acid value can be lowered from initially 30-100 mg KOH/mL to 5-10 mg KOH/mL; and the catalyst has the characteristics of high catalytic activity, easiness for separating and recovering, no corrosion of equipment by a reaction system, environmental friendliness and the like.

Description

Technical field: [0001] The invention belongs to the field of environmental catalysis and energy technology, and in particular relates to a SiO with dual-model pore structure. 2 Preparation method of supported solid acid catalyst based on mesoporous molecular sieve and its application in acid reduction treatment of waste oil with high acid value. Background technique: [0002] At present, raw material oil accounts for about 70% of the production cost of biodiesel. With the rapid development of social economy and the continuous improvement of people's living standards, a large number of waste edible oils are produced. How to use these waste edible oils to produce biodiesel , has become the focus of widespread attention in recent years, and has become an effective way to reduce the cost of biodiesel. [0003] The most commonly used method to produce biodiesel is to use animal and vegetable oils and alcohols to undergo alcohol transesterification through solid alkali catalysts...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/03C10G3/00
CPCY02P30/20
Inventor 孙继红戴群和张丽张黄高琳
Owner BEIJING UNIV OF TECH
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