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Molecular sieve based catalysts, preparation method and application thereof in crylic acid preparation by lactic acid dehydration

A technology of molecular sieve and catalyst, applied in the field of molecular sieve catalyst and its preparation and its application in the dehydration of lactic acid to prepare acrylic acid, to achieve the effects of high selectivity, less side reactions and long service life

Inactive Publication Date: 2009-12-16
SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0022] Take a ZSM-5 molecular sieve with a silicon-aluminum molar ratio of 40, and roast it at 550°C for 5hr;

[0023] Prepare 30ml of 9M aqueous ammonia solution, add 6g of roasted ZSM-5 molecular sieve to it, stir at room temperature for 2hr, suction filter, wash with water, and dry at 120°C; prepare 7ml of 15wt% sodium dihydrogen phosphate aqueous solution, and the above alkalized Molecular sieves were added, stirred and impregnated at room temperature for 8 hours, spin-dried at 60°C, and dried at 120°C to obtain modified molecular sieve JZSM-7;

[0024] 3 grams of the catalyst JZSM-7 prepared above are loaded into a fixed-bed reactor with an internal diameter of 10 mm and a height of 500 mm, and the catalyst is filled with inert small ceramic balls or quartz sand up and down. Reaction temperature 375°C, nitrogen flow rate 50ml / min, space velocity 1h -1 , the weight ratio of water and lactic acid in the raw material is 1:1. Under the above conditions, the catalyst JZSM-7 ...

Embodiment 2

[0026] Take a ZSM-5 molecular sieve with a silicon-aluminum molar ratio of 50, and roast it at 550°C for 5hr;

[0027] Prepare 30ml of 0.5M NaOH aqueous solution, add 6g of roasted ZSM-5 molecular sieve to it, stir at 80°C for 8hr, suction filter, wash with water, and dry at 120°C to obtain modified molecular sieve JZSM-10;

[0028] 3 grams of the catalyst JZSM-10 prepared above are loaded into a fixed-bed reactor with an inner diameter of 10 mm and a height of 500 mm, and the upper and lower parts of the catalyst are filled with inert small ceramic balls or quartz sand. Reaction temperature 350°C, nitrogen flow rate 30ml / min, space velocity 1h -1 , the weight ratio of water and lactic acid in the raw material is 1:1. Under the above conditions, the catalyst JZSM-10 catalyzed the dehydration of lactic acid to prepare acrylic acid with a conversion rate of 100% and acrylic acid selectivity of 71%.

Embodiment 3

[0030] Take a ZSM-5 molecular sieve with a silicon-aluminum molar ratio of 50, and roast it at 550°C for 5hr;

[0031]Prepare 30ml of 0.5M NaOH aqueous solution, add 6g of roasted ZSM-5 molecular sieves to it, stir at 80°C for 8hr, filter with suction, wash with water, and dry at 120°C; prepare 7ml of 11wt% sodium dihydrogen phosphate aqueous solution, and basify the above The treated molecular sieve was added, stirred and impregnated at room temperature for 8 hours, spin-dried at 60°C, and dried at 120°C to obtain modified molecular sieve JZSM-13;

[0032] 3 grams of the catalyst JZSM-13 prepared above are loaded into a fixed-bed reactor with an inner diameter of 10 mm and a height of 500 mm, and the upper and lower parts of the catalyst are filled with inert small ceramic balls or quartz sand. Reaction temperature 375°C, nitrogen flow rate 50ml / min, space velocity 1h -1 , the weight ratio of water and lactic acid in the raw material is 1:1. Under the above conditions, the ...

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Abstract

The invention discloses a molecular sieve based catalyst, a preparation method and an application thereof in crylic acid preparation by lactic acid dehydration. The method comprises the following steps: processing the ZSM-5 molecular sieve in aqueous alkali, or adopting an impregnation method to support phosphate, drying, roasting and finally obtaining the modified molecular sieve based catalyst. The catalyst realizes the reaction of crylic acid preparation by lactic acid dehydration in low temperature and has the advantages of high lactic acid conversion rate and crylic acid selectivity, and long-life of catalyst, the conversion rate of lactic acid dehydration reaction is 100%, and crylic acid selectivity can reach as high as 83.9%, thus having good industrial application prospect.

Description

technical field [0001] The invention belongs to the technical field of catalyst preparation and chemical industry, and in particular relates to a molecular sieve catalyst, its preparation and its application in the dehydration of lactic acid to prepare acrylic acid. Background technique [0002] Acrylic acid is an important polymer monomer and chemical raw material. It is widely used in textiles, chemical fibers, plastics, light industry, water treatment, oil recovery, metallurgy and other fields. The market demand is large and has been showing an upward trend in recent years. [0003] At present, acrylic acid is basically synthesized from petrochemical products. Except for a few companies that use acrylonitrile hydrolysis and Reppe method, most companies produce acrylic acid by two-step oxidation of propylene. Since propylene is mainly derived from the petroleum refining industry, the method of oxidizing propylene to produce acrylic acid has a great dependence on petroleum ...

Claims

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Application Information

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IPC IPC(8): B01J29/40B01J27/16B01J37/02B01J37/08C07C57/065C07C51/377
Inventor 姜标李青李丹丹王万军
Owner SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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