Preparation of hydrogenated pyromellitic acid ester

A technology for hydrogenating pyromellitic acid esters and pyromellitic acid, which is applied in the preparation of organic compounds, carboxylate esters, organic chemistry, etc., can solve the problems of rapid catalyst deactivation, frequent regeneration, and short service life. Achieve the effects of improving anti-sintering ability, improving dispersion and high selectivity

Active Publication Date: 2012-03-21
威海新元科盛新材料有限公司
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  • Application Information

AI Technical Summary

Problems solved by technology

This invention solves the shortcomings of the existing technology of directly using pyromellitic acid as raw material to hydrogenate hydrogenated pyromellitic acid to prepare hydrogenated pyromellitic acid, such as rapid catalyst deactivation, short service life, and frequent regeneration during use. Aluminum oxide

Method used

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  • Preparation of hydrogenated pyromellitic acid ester
  • Preparation of hydrogenated pyromellitic acid ester
  • Preparation of hydrogenated pyromellitic acid ester

Examples

Experimental program
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Example Embodiment

[0028] Example 1

[0029] Take the commercially available pseudo-boehmite and aluminum hydroxide powders and mix them into a uniform powder in a certain proportion, weigh out quantitative dilute nitric acid and phosphoric acid to prepare an aqueous solution, and spray the prepared solution evenly in the powder in the kneader , Then spray the quantitative polyethylene glycol aqueous solution into the mixture uniformly, after aging for a certain period of time, extrude it on a twin-screw extruder, dry and calcinate under the preset temperature control to obtain strip compound alumina , Crushing and sieving to obtain a certain particle size carrier to obtain the compound catalyst carrier used in the present invention. Prepare the following 1-7 carriers according to different raw material ratios:

[0030] Table 1 Preparation and characterization of composite alumina carrier

[0031]

Example Embodiment

[0032] Example 2

[0033] Weigh 100g of the carriers 1-7 in Example 1, respectively, put them in 100ml (0.012g Sr / ml) of strontium nitrate aqueous solution for 24 hours, dry at 120°C for 12 hours, and then calcinate at 400°C for 3 hours to obtain rare earth modification Compound alumina carrier.

[0034] Put the above-mentioned pretreated carrier into 125ml of mixed aqueous solution containing ruthenium chloride and rhodium chloride, in which Ru content is 0.002g / m1 and Rh content is 0.0004g / ml, immersed for 24 hours and dried at 120°C for 6 hours, repeat The above operations were performed 4 times, and then calcined at 400°C for 4 hours after drying to obtain the corresponding H-1, H-2, H-3, H-4, H-5, H-6, H-7 catalysts loaded with 1% Ru and 0.2% Rh.

Example Embodiment

[0035] Example 3

[0036] The tetrabutyl pyromellitic acid was dissolved in butanol to form a butanol solution containing 23% (wt) of tetrabutyl pyromellitic acid, which was used as the reaction raw material solution. A single-tube fixed-bed reactor was filled with catalyst, and it was reductively activated at a programmed temperature in a hydrogen atmosphere. The raw material solution was fed into the reactor via a metering pump for hydrogenation reaction. Reaction conditions: pressure 6.0Mpa, bed temperature 220 ℃, liquid space velocity 4.0h 1 (V), hydrogen space velocity 250h 1 (V) After the hydrogenated mixed product is cooled, a mixed product of hydrogenated pyromellitic acid tetrabutyl ester containing solvent butanol is obtained, which is subjected to chromatographic analysis as follows:

[0037] Table 2 Evaluation of catalyst activity

[0038] catalyst Conversion rate(%) Selectivity (%) H-1 99.6 98.4 H-2 99.1 98.0 H-3 99.4 98.2 H-4 99.0 9.6 H-5 99.8 ...

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Abstract

In the invention, a catalyst used for hydrogenation reaction of pyromellitic acid ester to prepare hydrogenated pyromellitic acid ester is prepared, the catalyst is prepared by loading multi-component noble metal on a rare-earth modified and compounded aluminum oxide carrier, and the hydrogenation catalyst has high activity, high selectivity and long life.

Description

technical field [0001] The invention relates to the preparation and use of a catalyst for preparing hydrogenated pyromellitic acid esters. The hydrogenated pyromellitic acid esters are prepared by hydrogenation reaction of pyromellitic acid esters. Under certain temperature, hydrogen pressure and catalyst action, the After the benzene ring in the pyromellitic acid ester molecule is subjected to saturated hydrogenation, an alicyclic tetrabasic ester is obtained, which is used as a fine chemical intermediate to prepare hydrogenated pyromellitic dianhydride. The catalyst prepared in the invention is suitable for the catalytic hydrogenation process of pyromellitic acid esters, and has the characteristics of high activity and high selectivity. Background technique [0002] Hydrogenated pyromellitic dianhydride (HPMDA) is a new type of alicyclic anhydride used to prepare hydrogenated pyromellitic dianhydride polyimide (PI). Since HPMDA does not contain aromatic components in its ...

Claims

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Application Information

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IPC IPC(8): C07C69/75C07C67/303B01J27/18
Inventor 李璐王超杨丰华
Owner 威海新元科盛新材料有限公司
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