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Hydrogenation catalyst, its preparation method and its application in preparation of hexahydrophthalic anhydride

A technology of hydrogenation catalyst and hexahydrophthalic anhydride, which is applied in chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, etc. Thoroughness and other issues, to achieve the effect of increased yield of the target product, low catalyst cost, and simple preparation method

Active Publication Date: 2015-07-22
SHANGYU SUNFIT CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

) The cost of this method is relatively high, and in the hydrogenation process, the double bond of tetrahydrophthalic anhydride is activated, and the double bond is prone to transfer, resulting in incomplete hydrogenation. Decomposition, cross-linking and other by-products generate high-boiling and low-boiling impurities that are difficult to separate, which not only affect the conversion rate and selectivity of the reaction, but also high-boiling by-products are easily coked and adsorbed on the surface of the catalyst, resulting in catalyst poisoning
Both tetrahydrophthalic anhydride and hexahydrophthalic anhydride have high and similar boiling points. After the reaction, it is difficult to effectively separate them by traditional separation methods such as rectification, which seriously affects product quality.
Betnev et al. (Betnev A.F., Obukhova T.A., Budanov N.A., etal.Synthesis of polycarboxylic acids of cyclohexane series and their derivatives[J].Russian Journal of Organic Chemistry, 1999,35(4):519-521.) adopted phthalic di Formic acid is used as raw material, RNU-5 is used as catalyst, pH=13-14 is adjusted with 10% KOH, and 1,2-cyclohexanedicarboxylic acid is prepared by hydrogenation under the conditions of 150°C and 3.5-5MPa, with a yield of 95%, 1, Dehydration of 2-cyclohexanedicarboxylic acid to prepare hexahydrophthalic anhydride, but the composition and preparation method of the RNU-5 catalyst are not disclosed

Method used

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  • Hydrogenation catalyst, its preparation method and its application in preparation of hexahydrophthalic anhydride
  • Hydrogenation catalyst, its preparation method and its application in preparation of hexahydrophthalic anhydride

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Embodiment 1

[0029] Preparation of carrier mesoporous carbon: Take 10g of commercial activated carbon, add 2g KOH, stir evenly, in the tube furnace, in the presence of nitrogen, treat at 900°C for 3h, naturally cool down to room temperature in the presence of nitrogen, take it out, and wash it repeatedly with deionized water , filter until the pH of the filtrate is equal to 9, and dry the solid at 120°C for later use. The specific surface area of ​​the obtained mesoporous carbon is 500-600m 2 / g, the average pore diameter is 17-20nm.

Embodiment 2

[0031] Preparation of carrier mesoporous carbon: Take 10g of commercial activated carbon, add 4g Na 2 CO 3 , stir evenly, in a tube furnace, in the presence of nitrogen, treat at 800°C for 5 hours, naturally cool down to room temperature in the presence of nitrogen, take it out, repeatedly wash with deionized water, filter until the pH of the filtrate is equal to 8, and dry the solid at 120°C for later use , the specific surface area of ​​mesoporous carbon is 800-900m 2 / g, the average pore diameter is 12-15nm.

Embodiment 3

[0033] Catalyst preparation: get mesoporous carbon 5g prepared in embodiment 1, add 50mg containing ruthenium (referring to Ru 3+ ) of ruthenium trichloride aqueous solution 10ml, stirred at room temperature for 2 hours, dried and treated at 300°C for 5 hours in the presence of nitrogen, and then reduced at 300°C for 3 hours in a hydrogen atmosphere to obtain a hydrogenation catalyst.

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Abstract

The invention discloses a hydrogenation catalyst, and a preparation method of hexahydrophthalic anhydride. The catalyst adopts meso-porous carbon as a carrier and Ru as an active component, and the load amount of the active component is 0.5-10% of the mass of the catalyst. The preparation method of hexahydrophthalic anhydride is characterized in that hexahydrophthalic anhydride is produced through highly selective hydrogenation of phthalic anhydride as a raw material in the presence of a solvent and the hydrogenation catalyst. The method has the characteristics of low cost, high selectivity, few byproducts, and easy recovery of a precious metal in the catalyst.

Description

technical field [0001] The invention relates to a production method of chemical products, in particular to a hydrogenation catalyst and a preparation method of hexahydrophthalic anhydride. Background technique [0002] Hexahydrophthalic anhydride (HHPA), also known as hexahydrophthalic anhydride, is a white to off-white crystalline solid with a low melting point, soluble in benzene, acetone, etc. Low toxicity, (LD501200mg / kg). Hexahydrophthalic anhydride is an indispensable raw material for the production of high-grade polyester coatings. It can replace amino alkyd paints, amino polyester paints, polyester paints, polyurethane paints, etc. of aromatic polyacids, which can significantly improve the gloss of paints and reduce viscosity. Increasing the solid content can especially greatly improve the weather resistance of the coating. Coatings made of hexahydrophthalic anhydride are mainly used in the following industries: outdoor vehicles, metal coils, electrical appliances,...

Claims

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Application Information

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IPC IPC(8): B01J23/46C07D307/89
Inventor 李文李明时石勇黄生建张伟陈炯明董斌钢
Owner SHANGYU SUNFIT CHEM
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