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Preparation method of butene oxidative dehydrogenation catalyst

A technology for oxidative dehydrogenation and catalysts, applied in metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, chemical instruments and methods, etc., can solve metal loss and zinc utilization rate is only 70-75% , can not be completely precipitated and other problems, to achieve the effect of maintaining the original activity

Active Publication Date: 2018-09-04
PETROCHINA CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

According to the material balance and waste water analysis in the catalyst preparation process, Zn cannot be completely precipitated at the optimum gelling pH, Zn loss is 25-30%, and the zinc utilization rate is only 70-75%.
[0005] In view of the serious phenomenon of metal loss, the present invention proposes an improved catalyst preparation process to achieve the purpose of avoiding or reducing the percentage of metal zinc loss

Method used

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  • Preparation method of butene oxidative dehydrogenation catalyst
  • Preparation method of butene oxidative dehydrogenation catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Accurately weigh analytically pure Fe(NO 3 ) 3 9H 2 O 216.4g, analytically pure Zn(NO 3 ) 2 ·6H 2 O 71.2g, analytically pure Ca(NO 3 ) 2 ·6H 2 O 2.4g, add 1000ml deionized water to prepare a mixed solution. Gained solution is precipitated with 10% ammonia solution, and the pH value of the solution is monitored with a pH meter until the pH value is 7.6, the dropwise addition is stopped, and the first part of gelling is completed. At this time, carbon dioxide is passed into the solution at 600ml / min. Continued for 1 hour, stopped feeding carbon dioxide, then added 1.8g of scallop powder, after mixing well, the obtained precipitate was aged at 80°C for 1.0 hour. Wash 4 times with deionized water, 500ml of water for each wash. The loss of zinc in waste water is 12.6%, and the utilization rate of zinc in solid is 87.6%. It is dried at 120°C for 24 hours, placed in a muffle furnace at 700°C for 10 hours of roasting and activation, ground and sieved to take 20-60 mesh...

Embodiment 2

[0030] After 75g iron powder is dissolved completely through 540ml of 54% nitric acid, add analytically pure Zn (NO 3 ) 2 ·6H 2 O56.8g, analytically pure CaCl 2 0.8g, Ca(OH) 2 0.9g, add 1000ml deionized water to prepare a mixed solution. The resulting solution is precipitated with 10% ammonia solution, and the pH value of the solution is monitored with a pH meter until the pH value is 7.8, the dropwise addition is stopped, and the first part of gelling is completed. At this time, 400ml / min is passed into the solution for 1 hour, and the solution is stopped. Carbon dioxide was introduced, and 1.3 g of scallop powder was added. After mixing well, the obtained precipitate was aged at a constant temperature of 80° C. for 1.0 hour. Wash 4 times with deionized water, 500ml of water for each wash. The loss of zinc in wastewater is 9.45%, and the utilization rate of zinc in solids is 90.55%. After drying at 120°C for 24 hours, place it in a muffle furnace at 700°C for 10 hours of...

Embodiment 3

[0032] Accurately weigh analytically pure Fe(NO 3 ) 3 9H 2 O 536.9g, analytically pure Zn(NO 3 ) 2 ·6H 2 O125.6g, analytically pure CaCl 2 2g, Ca(OH)2 2g, add 2000ml deionized water to prepare a mixed solution. The resulting solution is precipitated with 10% ammonia solution, and the pH value of the solution is monitored with a pH meter, until the pH value is 7.9, the dropwise addition is stopped, and the first part of gelling is completed. At this time, 400ml / min is passed into the solution for 1 hour, and the solution is stopped. Carbon dioxide was passed through, and 3 g of scallop powder was added. After mixing well, the obtained precipitate was aged at a constant temperature of 85° C. for 1.0 hour. Wash 4 times with deionized water, 1000ml of water for each wash. The loss of zinc in waste water is 7.45%, and the utilization rate of zinc in solid is 92.55%. After drying at 120°C for 24 hours, put it in a muffle furnace for 700°C roasting and activation for 10 hours...

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Abstract

A preparation method of a butylene oxidative dehydrogenation catalyst is characterized in that the catalyst is prepared through a two-step gel formation and coprecipitation technology, and the method comprises the following steps: 1, adding ammonia water to an aqueous solution containing Fe, Zn and Ca series elements in a dropwise manner to control the pH value of a system to 7.0-8.0; and 2, stopping dropwise addition of the ammonia water, continuously introducing CO2 for 0.5-2h, keeping the pH value of the system unchanged, adding Sesbaria cannabina powder, mixing to obtain a precipitate, ageing the precipitate, washing the aged precipitate, drying the washed precipitate, and roasting the dried precipitate to obtain the butylene oxidative dehydrogenation catalyst.

Description

technical field [0001] The invention relates to a catalyst, in particular to an iron-based catalyst for producing butadiene by oxidative dehydrogenation of n-butene, a preparation method and application thereof. Background technique [0002] Butadiene is an important monomer for synthetic rubber and the like. The main production method is the extraction of butadiene, a by-product of steam cracking of naphtha, which is greatly affected by the price of petroleum. Butadiene has been produced industrially by oxidative dehydrogenation of butane or butene. Because alkanes are relatively stable, the butane dehydrogenation process generally has a higher temperature and more side reactions. The typical reaction temperature is 600 ° C, and the yield of butadiene based on butane is 65%. Butene is relatively active. The most typical butene oxidative dehydrogenation process is the Petro-Tex Oxo-D process, which has a high butadiene selectivity, generally greater than 90%, and fewer sid...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/80C07C11/167C07C5/48
CPCY02P20/141
Inventor 宋立红张玉东齐晓梅王家杰苗勇王中平田存轩刘月英
Owner PETROCHINA CO LTD
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