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Pd/C-SiC catalyst for p-phthalic acid hydrorefining, preparation method and application thereof

A technology for terephthalic acid and hydrorefining reactions, which is used in physical/chemical process catalysts, carboxylate preparation, organic compound preparation, etc.

Inactive Publication Date: 2014-06-11
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are few reports on the use of SiC as a catalyst support for CBA hydrogenation reactions.

Method used

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  • Pd/C-SiC catalyst for p-phthalic acid hydrorefining, preparation method and application thereof
  • Pd/C-SiC catalyst for p-phthalic acid hydrorefining, preparation method and application thereof
  • Pd/C-SiC catalyst for p-phthalic acid hydrorefining, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] [Example 1] Preparation of C-SiC carrier

[0028] (a) First, put 1.2g a-phase SiC particles (particle size is 2um) into a tube furnace, and program the temperature to 800°C, 900°C, and 1000°C respectively under the He gas atmosphere, and the heating rate is 5°C / min , then pure CCl 4 The liquid is passed through the form of He gas bubbling (that is, He is passed into the CCl-containing 4 After the solvent is removed, the He carrying the chlorine-containing organic solvent is introduced into the reaction system where the SiC particles are located at room temperature), the helium flow rate is 51ml / min, and CCl is continuously introduced into the reaction system. 4 2h, and then switch to a pure He atmosphere to lower the temperature. The prepared material is named C-SiC-T (T is the preparation temperature).

[0029] Such as figure 1 The surface of SiC shown in the electron microscope photo is uniformly covered with carbon layer, figure 2 The Raman spectrum shows the c...

Embodiment 2

[0032] [Example 2] Preparation of Pd / C-SiC catalyst

[0033] (a) The C-SiC carrier of [Example 1] was calcined in air at 400°C for 2 hours.

[0034] (b) Add 0.577g PdCl dropwise to the calcined 0.521g C-SiC carrier with stirring 2 Aqueous solution (Pd mass percentage: 0.457%), stirred until dry, dried overnight at 60°C, reduced with hydrogen at 250°C for 2 hours, to obtain 0.5% Pd / -C-SiC-T (T represents the preparation temperature), And Pd / O-C-SiC-900, Pd / N-C-SiC-800 samples. The comparative Pd / AC (coconut shell carbon) catalyst was prepared as described above using chloropalladium acid as the precursor.

Embodiment 3

[0035] [Example 3] CBA hydrogenation reaction

[0036] Activity evaluation of Pd / C-SiC catalyst for hydrorefining of terephthalic acid was carried out in a batch reactor. 0.200 g of 4-CBA was added to 70 ml of water, and 0.050 g of the Pd / -C-SiC catalyst of [Example 2] was added. 130 DEG C of temperature, hydrogen pressure 0.4MPa, 50 minutes of reaction time, regular sampling, adopt the content of the 4-CBA in the high performance liquid chromatography analysis reaction process, utilize reaction formula ln(C 0 / C i )=kt(C 0 is the concentration of CBA before the reaction, C i is the instant concentration of CBA, k is the kinetic coefficient, and t is the reaction time) in the k value to reflect the catalytic performance of the catalyst. Depend on Figure 5 As shown, the activity of the Pd catalyst supported on C-SiC-900 and C-SiC-1000 is significantly higher than that of the catalyst supported on coconut shell carbon, and the activity of the Pd catalyst supported on C-SiC...

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Abstract

The present invention relates to a Pd / C-SiC catalyst having high activity in a p-phthalic acid hydrorefining reaction, a preparation method and an application thereof. According to the present invention, high strength macroporous silicon carbide is adopted as a carrier, a carbon layer is produced on the surface, carbon dioxide activation and nitrogen atom doping modification are performed, and then the Pd catalyst is dispersed so as to substantially increase the catalysis activity, wherein the high strength silicon carbide carrier is adopted as the hard skeleton, such that the problems of carbon carrier breaking and the like during the reaction process can be avoided, the service life of the catalyst can be increased, and the potential industrial application values are provided in the p-phthalic acid hydrorefining reaction.

Description

technical field [0001] The invention relates to a Pd / -C-SiC catalyst used in the hydrorefining reaction of terephthalic acid and its preparation and application. Background technique [0002] Purified terephthalic acid (PTA) is an important precursor for the industrial production of polyethylene terephthalate, with an annual output of more than 24,000,000 tons. Terephthalic acid is produced by catalytic oxidation of terephthalate in acetic acid ( Kuo-Tseng Li, Catalysis Communications 9 (2008) 2257–2260). The prepared terephthalic acid (CTA) contains 2000-6000ppm p-benzaldehyde (CBA). These impurities seriously affect the quality of the produced polyester, so the impurities need to be removed. Industrially, Pd / C is used as a catalyst, and CBA is hydrogenated into p-toluic acid (PT) under H2 atmosphere, and then PTA products are obtained through steps such as crystallization, centrifugation, and drying. The main problem facing the catalysts used in CBA hydrogenation is that...

Claims

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Application Information

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IPC IPC(8): B01J27/224C07C63/26C07C51/487
Inventor 包信和李星运潘秀莲
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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