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A kind of dimethyl terephthalate (DMT) hydrogenation catalyst and preparation method thereof

A technology of dimethyl cyclohexanedicarboxylate and catalyst, which is applied in the field of catalysis, can solve problems such as low yield, high equipment cost and operating cost, and reduce reaction pressure, and achieve high reaction efficiency, low cost, and improved hydrogenation activity Effect

Active Publication Date: 2022-03-08
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

[0007] In summary, the use of palladium catalysts has a high reaction yield, but it needs to be carried out under high pressure, and the equipment and operating costs are high.
Using rhodium, ruthenium or ruthenium-M bimetallic catalyst can significantly reduce the reaction pressure, but the yield is low

Method used

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  • A kind of dimethyl terephthalate (DMT) hydrogenation catalyst and preparation method thereof
  • A kind of dimethyl terephthalate (DMT) hydrogenation catalyst and preparation method thereof
  • A kind of dimethyl terephthalate (DMT) hydrogenation catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Take by weighing 50.0g process and dry pine activated carbon (400 mesh, specific surface area 1200m 2 / g, pore volume 0.8ml / g), added to 200mL ammonium tungstate solution containing tungsten mass fraction of 10%, stirred and impregnated for 2h, filtered, and the filter cake was dried in an oven at 120°C for 5h to obtain ammonium tungstate loaded Activated carbon precursor. Put the precursor in a tube furnace, under a hydrogen atmosphere, the gas flow rate is 5ml / g min, the furnace temperature is raised to 400°C at 5°C / min, and the carbonization is kept for 6h. After the end, it is lowered to room temperature, and a small amount of air is introduced. passivation to obtain a tungsten carbide-activated carbon composite carrier with a mass fraction of tungsten carbide of 5%.

[0033] According to the mass content of metal ruthenium in the catalyst as 5%, the equal volume impregnation method is used to impregnate the ruthenium trichloride hydrochloric acid solution on the t...

Embodiment 2

[0035] Take by weighing 50.0g process and dry pine activated carbon (400 mesh, specific surface area 1200m 2 / g, pore volume 0.8ml / g), join in the ammonium paramolybdate solution that 200mL contains molybdenum mass fraction and be 5%, stir and impregnate 4h, filter, and filter cake is dried 5h in 120 ℃ oven and obtains loaded with paramolybdate Ammonium activated carbon precursor. Put the precursor in a tube furnace, under a hydrogen atmosphere, the gas flow rate is 5ml / g min, the furnace temperature is raised to 400°C at 5°C / min, and the carbonization is kept for 6h. After the end, it is lowered to room temperature, and a small amount of air is introduced. passivation to obtain a molybdenum carbide-activated carbon composite carrier with a molybdenum carbide mass fraction of 3%.

[0036] According to the mass content of metal ruthenium in the catalyst as 5%, the equal volume impregnation method is used to impregnate the ruthenium trichloride hydrochloric acid solution on the...

Embodiment 3

[0038] Take by weighing 50.0g process and dry pine activated carbon (400 mesh, specific surface area 1200m 2 / g, pore volume 0.8ml / g), added to 200mL ammonium paratungstate solution containing 10% tungsten mass fraction, stirred and impregnated for 2h, filtered, and the filter cake was dried in an oven at 120°C for 5h to obtain an activated carbon precursor loaded with ammonium paratungstate. Put the precursor in a tube furnace, under a hydrogen atmosphere, the gas flow rate is 5ml / g min, the furnace temperature is raised to 400°C at 5°C / min, and the carbonization is kept for 6h. After the end, it is lowered to room temperature, and a small amount of air is introduced. passivation to obtain a tungsten carbide-activated carbon composite carrier with a mass fraction of tungsten carbide of 5%.

[0039] According to the mass content of metal ruthenium in the catalyst as 3%, the equal volume impregnation method is used to impregnate the ruthenium trichloride hydrochloric acid solut...

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Abstract

The invention discloses a catalyst for hydrogenating dimethyl terephthalate (DMT) to produce dimethyl 1,4-cyclohexanedicarboxylate (DMCD) and a preparation method thereof. The hydrogenation catalyst carrier adopts pine activated carbon, and a layer of metal carbide is supported on the surface of the activated carbon carrier, and the active component is metal ruthenium with a mass fraction of 1% to 5%. The invention also discloses a preparation method of the hydrogenation catalyst. The method of using the catalyst is as follows: DMT is dissolved in ethyl acetate, and at a certain temperature and pressure, the solution is passed through the hydrogenation catalyst layer together with hydrogen, and DMT undergoes a highly selective hydrogenation reaction of benzene ring to generate DMCD. Under the temperature of 50-80°C, hydrogen pressure of 1-4MPa, stirring speed of 500-800rpm under low temperature, low pressure and mild conditions, the DMT conversion rate reaches 99.9%, and the selectivity is over 98.8%. The hydrogenation catalyst prepared by the invention has the characteristics of low cost, high activity, high selectivity and long application life, and has good industrial application prospect.

Description

technical field [0001] The invention belongs to the technical field of catalysis, and in particular relates to a catalyst for hydrogenating dimethyl terephthalate (DMT) to produce dimethyl 1,4-cyclohexanedicarboxylate (DMCD) and a preparation method thereof. Background technique [0002] Terephthalic acid (PTA) is one of the compounds with the largest output in the world. The annual production capacity in mainland China alone exceeds 30 million tons, mainly for the production of polyester PET. The development of bulk chemicals, polymer materials and products with PTA as the starting raw material can enhance the added value of the PTA industry chain and the profitability of enterprises. Dimethyl 1,4-cyclohexanedicarboxylate (DMCD) is one of the most important derivatives in the PTA industry chain. It is an important organic chemical raw material and can be used as a polymer modification material. An important intermediate of cyclohexanedimethanol (CHDM), a series of polyeste...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/22B01J37/08B01J37/02B01J37/16B01J37/18B01J35/10C07C67/303C07C69/75
Inventor 史海赵许群邹展张旭王杰
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI