Al-pillared paligorskite modified solid acid catalyst and preparation and application thereof

A technology of solid acid catalyst and palygorskite, which is applied in the chemical industry, can solve the problems of large consumption of n-octanol, high reaction temperature, and poor thermal stability, and achieve good catalytic effect, no pollution to the environment, and low raw material cost.

Inactive Publication Date: 2009-04-15
NORTHWEST NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

with SnCl 4 Although the esterification rate is higher as a catalyst, it consumes a large amount of n-octanol, and the reaction temperature is high, which will lead to an increase in production costs
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Method used

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  • Al-pillared paligorskite modified solid acid catalyst and preparation and application thereof
  • Al-pillared paligorskite modified solid acid catalyst and preparation and application thereof
  • Al-pillared paligorskite modified solid acid catalyst and preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] Embodiment 1, SO 4 2- Preparation of / Al-PGS solid acid catalyst

[0061] ① At a concentration of 0.2-0.3mol / L AlCl 3 Add NaOH solution to the solution to make Al and OH in the mixture - The molar ratio is 1:2.2~1:2.5, the temperature is controlled at 70~90°C, and the aging is stirred for 18~36 hours to obtain the polyhydroxyaluminum ion solution;

[0062] ② Prepare the purified palygorskite into a slurry with a mass fraction of 0.8-1.5%, stir for 1-1.5 hours, and let it stand for 20-30 hours to fully soak and delaminate to make a suspension; add polyhydroxyl Aluminum ion solution, make Al / PGS at 5-8mmol / g, control the temperature at 70-90°C, stir for 20-26h, and centrifuge, the obtained solid is washed with distilled water and centrifuged until the supernatant is washed with AgNO 3 detect no Cl - ;Dry at 70-80°C, grind, pass through a 100-mesh sieve, and then roast at a constant temperature of 450-550°C for 3-5 hours to make pillared clay;

[0063] ③Slowly add H ...

Embodiment 2

[0064] Example 2, SO 4 2- Synthesis of Trioctyl Citrate Catalyzed by Al-PGS Solid Acid Catalyst

[0065] Add citric acid and n-octanol with a molar ratio of 1:4.5 to a two-necked flask with a water separator and a condenser, mix and heat to 80-100°C and reflux for 10-15 minutes while stirring, when the citric acid is completely dissolved , measure the initial acid value of the mixed solution; add citric acid mass 10.5% SO in the mixed solution 4 2- / Al-PGS catalyst, control the temperature at 150°C, react for 6 hours, and separate the water produced by the reaction in time. After the reaction, take the reaction solution to measure the acid value, and calculate the esterification rate of trioctyl citrate: 99.1%.

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Abstract

The invention provides an al-pillared palygorskite modified solid acid catalyst, which is obtained by taking palygorskite raw soil (PGS) as a carrier, preparing al-pillared palygorskite (Al-PGS) by an ion exchange method and then modifying the Al-PGS through SO4<2->. The larger specific surface area of palygorskite can effectively improve the effective active acid site of the acid catalyst in catalytic reaction; meanwhile, the acid catalyst can be better contacted with reaction substrates in the catalytic reaction through good adsorption performance of palygorskite clay, so as to be the acid catalyst which is good in performance and takes the palygorskite as the carrier. When the al-pillared palygorskite modified solid acid catalyst (SO4<2->/Al-PGS) is used for the catalytic synthesis reaction of trioctyl citrate, the esterification rate of the trioctyl citrate is 99.1 percent. The catalyst still has good catalytic activity after the catalyst is continuously used for five times, thereby showing that the catalyst is worthy to be reclaimed.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and relates to a solid acid catalyst with palygorskite as a carrier, in particular to a catalyst using SO 4 2- Modified aluminum pillared palygorskite solid acid catalyst——SO 4 2- / Al-PGS; the present invention also relates to the preparation method of the solid acid catalyst and its application in catalytic synthesis of trioctyl citrate. Background technique [0002] As a new green and environment-friendly plasticizer, citrate products have the advantages of non-toxicity, good biodegradability, low volatility, anti-bacteria, and high plasticizing efficiency, and have been widely used in many fields. my country is the world's largest producer of citric acid, and has unique advantages in the research and development of citric acid ester plasticizers and their downstream products. The key to developing citric acid esters is to increase the conversion rate, and the core technology to i...

Claims

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Application Information

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IPC IPC(8): B01J27/053C07C67/08C07C69/704
Inventor 常玥王勇刚查飞吕学谦鲁峰吕玉荣
Owner NORTHWEST NORMAL UNIVERSITY
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