Solid acid catalyst for preparing bio-based para-xylene as well as preparation and application thereof

A solid acid catalyst and p-xylene technology, which is applied in the direction of carbon compound catalysts, physical/chemical process catalysts, catalysts, etc., can solve the problems of many by-products, serious hydrolysis, and poor selectivity

Inactive Publication Date: 2016-08-31
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Some other solid acid catalysts such as niobic acid, TiO 2 , γ-Al 2 o 3 The selectivity of etc. is relatively poor, mostly below 60%
In addition, the experimental results also found that the hydrolysis of 2,5-dimethylfuran under the catalysis of non-molecular sieve solid acid is serious and the by-products are many and complex

Method used

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  • Solid acid catalyst for preparing bio-based para-xylene as well as preparation and application thereof
  • Solid acid catalyst for preparing bio-based para-xylene as well as preparation and application thereof
  • Solid acid catalyst for preparing bio-based para-xylene as well as preparation and application thereof

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Experimental program
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preparation example Construction

[0040] The preparation method of the above-mentioned solid acid catalyst involved in the second aspect of the present invention includes:

[0041] Step L: Disperse the silica material in an acid solution to make a silica acid suspension

[0042] Step M, adding hydrogen peroxide and 3-mercaptopropyltrimethoxysilane (MPTMS) to the acidic silica suspension, mixing and reacting to obtain a catalyst precursor solution;

[0043] In step N, the catalyst precursor solution is heat-treated, and then the solid powder is filtered out, washed with water and ethanol one or more times, and dried to obtain a powdery solid acid catalyst.

[0044] In the above preparation method of the present invention, the weight content of silica in the acidic silica suspension is 0.1% to 5%.

[0045] In the present invention, the acidic solution is an aqueous acid solution, wherein the acid includes hydrochloric acid, sulfuric acid, and phosphoric acid. In some embodiments of the present invention, the concentratio...

Embodiment 1

[0076] (1) Disperse 0.1g of silica material into 100g of acidic solution to prepare a silica acid suspension with a concentration of 0.1%;

[0077] (2) Add 0.4g 30% hydrogen peroxide and 0.163g MPTMS to the acidic silica suspension, mix and react for 2h to obtain a catalyst precursor solution;

[0078] (3) Transfer the catalyst precursor solution into a hydrothermal reactor, heat treatment at 100°C for 0.5 h, filter out the solid powder, wash it with water and ethanol several times, and dry to obtain a powdered solid catalyst.

[0079] (4) Add 0.1g of the above solid catalyst, 1.0g 2,5-dimethylfuran, 30mL n-heptane, 0.43g internal standard n-decane into a 50mL reactor, fill with 1.5MPa ethylene, and react at 250℃ 6h, PX was prepared. According to formulas (III) and (IV), the measurement and calculation show that the conversion rate of 2,5-dimethylfuran is 60%, and the PX selectivity is 63%.

Embodiment 2

[0081] (1) Disperse 0.4g of silica material into 100g of acidic solution to prepare a silica acid suspension with a concentration of 0.4%;

[0082] (2) Add 0.4g 30% hydrogen peroxide and 0.2g MPTMS to the acidic silica suspension, mix and react for 4 hours to prepare a catalyst precursor solution;

[0083] (3) Transfer the catalyst precursor solution to a hydrothermal reactor, heat treatment at 100°C for 5 hours, filter out the solid powder, wash it with water and ethanol several times, and dry to obtain a powdered solid catalyst.

[0084] (4) Add 0.2g of the above solid catalyst, 1.0g of 2,5-dimethylfuran, 30mL of n-heptane, 0.43g of n-decane into a 50mL reactor, fill with 1.5MPa ethylene, and react at 250°C for 6 hours to prepare Get PX. According to formula (III) and (IV), the measurement and calculation show that the conversion rate of 2,5-dimethylfuran is 70%, and the PX selectivity is 81%.

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Abstract

The invention relates to a solid acid catalyst for preparing bio-based para-xylene (PX) as well as preparation and application thereof. A novel solid catalyst with a mesoporous structure is prepared by carrying out acid modification on the surface of a silicon dioxide material. The catalyst has proper acidity and is used for the reaction for catalyzing addition of 2,5-dimethyl furan and ethylene and dehydrating to prepare the PX; the coupling of reaction-separation in a PX preparation process is realized and a novel method for highly selectively preparing the bio-based PX is provided; and in a reaction process, excellent catalytic activity, selectivity and stability are represented and a firm foundation is laid for industrial production of the bio-based PX.

Description

Technical field [0001] The invention belongs to the field of bio-based chemicals, and relates to a solid acid catalyst for preparing bio-based para-xylene (PX), and a preparation method and application thereof. Background technique [0002] Para-xylene, its English name is para-xylene, or PX for short. Colorless and transparent liquid with aromatic odor. It is industrially used to produce terephthalic acid and then produce terephthalic acid polyester resin. The polyester resin is the raw material for the production of polyester flakes, polyester hollow containers and my country's largest synthetic fiber polyester fiber. It is also used as a raw material for paints, dyes and pesticides. [0003] In recent years, my country’s demand for PX has increased year by year, and China’s external dependence on PX has also risen from 38.7% in 2007 to 52.4% in 2014. If there is no new capacity, my country’s PX is expected to have a gap of 15 million tons by 2020. [0004] The traditional PX p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/02C07C15/08C07C1/24
CPCY02P20/52B01J31/0275B01J2231/324B01J2231/70C07C1/24C07C2531/02C07C15/08
Inventor 谭天伟申春冯心强田晨郴纪凯悦薛国振
Owner BEIJING UNIV OF CHEM TECH
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