P-benzene dicarboxylic acid hydrogen refining catalyst and preparation method thereof

A technology for terephthalic acid and hydrorefining, which is applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of poor sulfur resistance and easy growth of palladium crystal grains.

Active Publication Date: 2009-05-13
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] One of the technical problems to be solved by the present invention is the problem that the palladium carbon catalyst has poor sulfur resistance and the palladium crystal grains are easy to grow in the prior art, and a new terephthalic acid hydrogenation refining catalyst is provided

Method used

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  • P-benzene dicarboxylic acid hydrogen refining catalyst and preparation method thereof
  • P-benzene dicarboxylic acid hydrogen refining catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Get 50 grams of granular coconut shell charcoal carriers for pretreatment, soak in 400 milliliters of concentration in a dilute nitric acid solution of 0.08 (weight) % for 4 hours, then wash with deionized water until neutral, drain, and dry at 105 ° C 24 hours, naturally cooled to room temperature.

[0032] Dissolve chloropalladium acid, lanthanum nitrate and tartaric acid in 20 milliliters of deionized water, adjust the pH value of the solution to 3.0 with 8 (weight)% sodium carbonate, and finally set the volume to 40 milliliters to obtain palladium glue.

[0033] The carrier is put into a rotating pan, and the prepared palladium glue solution is sprayed on the carrier to prepare a catalyst precursor. The catalyst precursor was left to age for 10 hours, then reduced with hydrogen at 200 °C for 6 hours, cooled naturally to room temperature under a hydrogen atmosphere, and finally washed with pure water to be free of Cl - So far, the catalyst of the present invention i...

Embodiment 2

[0035] Get 50 grams of granular coconut shell charcoal carriers for pretreatment, soak in 400 milliliters of concentration in 0.1 (weight) % dilute hydrochloric acid solution for 4 hours, then wash with deionized water until neutral, drain, and dry at 105 ° C 24 hours, naturally cooled to room temperature.

[0036] Palladium acetate, lanthanum nitrate, and tartaric acid were dissolved in 20 milliliters of deionized water, and the pH value of the solution was adjusted to 4.0 with 8 (weight)% sodium carbonate, and finally the solution was constant to 40 milliliters to obtain palladium glue.

[0037] The carrier is put into a rotating pan, and the prepared palladium glue solution is sprayed on the carrier to prepare a catalyst precursor.

[0038] Place the catalyst precursor for aging for 24 hours, prepare a reduction solution with 20 grams of 5 (weight)% hydrazine hydrate and 200 grams of pure water, soak the catalyst precursor in the reduction solution for 2 to 4 hours, and fin...

Embodiment 3～6

[0040] Catalysts Cat 3-Cat 6 were prepared by the same method as [Example 1]. See Table 1 for the weight percent composition of each component of the catalyst and the pH value of the palladium colloid solution.

[0041] Table 1

[0042] Example catalyst PD rare earth element oxide acid pH value of palladium colloid 1 Cat 1 Add 0.48% with chloropalladium acid La 2 o 3 (added as lanthanum nitrate) 0.2% Tartaric acid 0.02% 3.0 2 Cat 2 Add 0.49% as palladium acetate CeO 2 (added as cerium nitrate) 0.2% Tartaric acid 0.02% 4.0 3 Cat 3 Add 0.49% as palladium chloride SM 2 o 3 (Added as Samarium Nitrate) 0.2% Citric acid 0.03% 5.0

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Abstract

The invention relates to a catalyst used in a hydrofining reaction of terephthalic acid and a preparation method thereof, and mainly solves the problems that the prior Pd-C catalyst has poor sulfur resistance and the Pd grain is liable to grow. The components in weight percentages of the catalyst are as follows: a) 0.3% to 0.8% of Pd; b) 0.01% to 0.5% of oxides of at least one metal selected from rare-earth elements; and c) a carrier in balance amount, wherein the carrier is coconut shell charcoal with a particle size ranging from 4 meshes to 8 meshes and a specific surface area more than 1000 square meter/g; and the Pd and the oxides of rare-earth elements are distributed from the surface of the carrier to the superficial layer (at a depth ranging from 40micrometers to 100 micrometers). With the technical scheme, the catalyst overcomes the problems in the prior art and is applied to the commercial-scale hydrofining of terephthalic acid.

Description

technical field [0001] The invention relates to a terephthalic acid hydrogenation refining catalyst and a preparation method thereof. Background technique [0002] Purified terephthalic acid, commonly known as PTA, is the basic raw material for synthetic polyester. The domestic demand for PTA is increasing at a rate of more than 10% year by year. Purified terephthalic acid (PTA) is mainly produced by the Amoco method, that is, p-xylene (PX) is catalyzed and oxidized with Co / Mn / Br in acetic acid solvent to obtain crude terephthalic acid (CTA), and then Palladium carbon catalyst, high temperature and high pressure hydrogenation refining, crystallization, centrifugal separation and drying. In the oxidation stage, due to the complexity of the reaction, by-products are inevitable, such as p-carboxybenzaldehyde (4-CBA) produced by incomplete oxidation, benzil, fluorenone, anthraquinone, etc. produced by cyclopolymerization, And other colored impurities and their precursors. Amo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/63C07C63/26C07C51/487
CPCY02P20/52
Inventor 肖忠斌畅延青陈大伟
Owner CHINA PETROLEUM & CHEM CORP
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