Novel integrated solid acid catalyst with carbon-based structure as well as preparation of integrated solid acid catalyst and application in preparation of biodiesel

A solid acid catalyst, biodiesel technology, applied in the direction of physical/chemical process catalysts, biofuels, fatty acid esterification, etc., can solve the problems of temperature sensitivity and easy swelling, and achieve less acid site loss, thermal stability and structure The effect of good stability and novel preparation method

Inactive Publication Date: 2013-09-25
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Overcome the shortcomings of acidic ion exchange resins that a...

Method used

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  • Novel integrated solid acid catalyst with carbon-based structure as well as preparation of integrated solid acid catalyst and application in preparation of biodiesel
  • Novel integrated solid acid catalyst with carbon-based structure as well as preparation of integrated solid acid catalyst and application in preparation of biodiesel
  • Novel integrated solid acid catalyst with carbon-based structure as well as preparation of integrated solid acid catalyst and application in preparation of biodiesel

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Dissolve 5 g of ferric nitrate in 8 mL of oleylamine, then heat to 180°C and stir for 60 minutes. The above slurry was uniformly coated on the surface of the stainless steel wire mesh, and then dried under vacuum at 60° C. for 24 hours. Then put the sample into the tube furnace, under the protection of nitrogen (the flow rate of nitrogen is 30mL / min), raise the temperature from room temperature to 750°C, and keep it for 3 hours, and then use H 2 (Hydrogen flow rate 5mL / min) reduction for 3h. Afterwards, it was naturally cooled to room temperature to obtain a stainless steel wire mesh / sheet of catalyst particles. The Raman spectrum of the product is shown in figure 1 , TEM photo see figure 2 , SEM scanning electron microscope photo see image 3 .

[0046] Put the above-mentioned catalyst particle stainless steel wire mesh into a tube furnace, benzene is used as a carbon source, and nickelocene is mixed and dissolved in it, and injected into the tube furnace at 10mL...

Embodiment 2

[0049] Dissolve 10g of ferric chloride in 15mL of oleylamine, then heat to 300°C and stir for 60min. The above slurry was uniformly coated on the surface of the stainless steel wire, and then dried in vacuum at 60°C for 24h. Then put the sample into the tube furnace, under the protection of nitrogen (the flow rate of nitrogen gas is 60mL / min), raise the temperature from room temperature to 750°C, and keep it for 3 hours, and then use H 2 (Hydrogen flow rate 5mL / min) reduction for 3h. Afterwards, it was naturally cooled to room temperature to obtain a stainless steel wire sheet of catalyst particles.

[0050] Put the above-mentioned catalyst particle stainless steel wire into a tube furnace, ethanol is used as a carbon source, and ferrocene is mixed and dissolved in it, and injected into the tube furnace at 10mL / h, and the mixture is formed by Ar+H 2 (60mL / min+10mL / min) gas is carried into the center of the tube furnace, and catalytically cracked at 800°C for 30min to obtain ...

Embodiment 3

[0053] Dissolve 1 g of cobalt nitrate in 4 mL of oleylamine, then heat to 100° C. and stir for 60 minutes. The above slurry was uniformly coated on the surface of the stainless steel wire mesh, and then dried under vacuum at 60° C. for 24 hours. Then put the sample into the tube furnace, under the protection of nitrogen (the flow rate of nitrogen is 30mL / min), raise the temperature from room temperature to 750°C, and keep it for 3 hours, and then use H 2 (Hydrogen flow rate 5mL / min) reduction for 3h. Afterwards, it was naturally cooled to room temperature to obtain a stainless steel mesh of catalyst particles.

[0054] Put the stainless steel mesh of the above catalyst particles into a tube furnace, methanol is used as a carbon source, and cobalt dicene is mixed and dissolved in it, and injected into the tube furnace at 15mL / h, and the mixture is formed by Ar+H 2 (90mL / min+5mL / min) gas is carried into the center of the tube furnace, and catalytically cracked at 800°C for 40m...

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Abstract

The invention discloses a novel integrated solid acid catalyst with a carbon-based structure. The novel integrated solid acid catalyst is a sulfonating carbon nano tube (CNT-SO3H@) stainless steel material and is prepared by using the stainless steel material as a support material, growing a carbon nano tube on the surface of the support material, vulcanizing through polysulfide and oxidizing. The invention simultaneously discloses a preparation method of the novel catalyst and an application in preparation of biodiesel by means of catalytic distillation. The loss of an acid position of the solid acid catalyst with the carbon-based structure is reduced; because of high heat stability and structure stability, the catalyst is easily made into various shapes and is filled into a catalytic distillation tower to be used. An original element having functions of catalyzing and separating is used for coupling a reaction process with a separation process, and because of the process, the complicated processes of pre-esterification, purification and subsequent separation are avoided; meanwhile, a glycerinum product which is used for catalyzing waste oil and methyl alcohol ester to perform exchange reaction is converted into products of glyceraldehydes, glyceric acid, hexanal dimethyl acetal, acraldehyde dimethyl acetal and the like, so that the reaction is greatly intensified; finally, a biodiesel product with high purity can be directly obtained on the top of the tower and at the bottom of the tower.

Description

technical field [0001] The invention relates to a catalyst, in particular to a carbon-based monolithic catalyst, its preparation method and its application in the preparation of biodiesel. Background technique [0002] Carbon-based solid acid usually refers to the acidification modification on the surface of carbon materials, the introduction of acid groups (-SO 3 H, -COOH) prepared solid acid material. Carbon materials mainly include porous carbon, activated carbon, carbon fiber, carbon black, carbon microspheres, graphite flakes, glass carbon, carbon nanotubes, graphene, graphite ribbons, carbon molecular sieves, and many other forms, among which there are currently many studies on solid acid materials The most popular are porous carbon, carbon nanotubes and graphene. The acidification process chooses different routes according to different materials. This study mainly takes carbon nanotubes as the acidification object. There are four main methods of acid functionalizat...

Claims

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Application Information

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IPC IPC(8): B01J27/053C11C3/10C10L1/02
CPCY02E50/10
Inventor 丁维平张冬冬魏大力李骐薛念华彭路明郭学锋陈懿
Owner NANJING UNIV
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