Molecular sieve catalyst, preparation method and use in preparing ethylene by dehydrating ethanol

A technology of ethanol dehydration and molecular sieve, which is applied in the direction of molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., to achieve the effects of improving production capacity, improving ethylene selectivity, and prolonging service life

Inactive Publication Date: 2008-12-24
SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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  • Molecular sieve catalyst, preparation method and use in preparing ethylene by dehydrating ethanol
  • Molecular sieve catalyst, preparation method and use in preparing ethylene by dehydrating ethanol
  • Molecular sieve catalyst, preparation method and use in preparing ethylene by dehydrating ethanol

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Embodiment 1

[0027] [embodiment 1] measure 5ml titanium tetrachloride, at room temperature, N 2 Under the atmosphere and good stirring, slowly add 4.6ml of isopropanol to it, after the reaction is complete, add 20ml of acetone to dissolve the yellow precipitate, and obtain titanium isopropoxide-acetone solution; at room temperature and under rapid stirring, distilled water , nitric acid, and absolute ethanol are added dropwise into the titanium isopropoxide-acetone solution, and stirred for 0.5 to 3 hours to obtain an impregnation solution containing titanium ions. Among them, titanium isopropoxide-acetone, distilled water, nitric acid, and ethanol The volume ratio is 1:0.08:0.02:1;

[0028] Treat the ZSM-5 molecular sieve with a silicon-aluminum molar ratio of 25 with 1M ammonium acetate aqueous solution at 95°C for 2 to 4 times, each time for 4 hours, wherein 5ml of ammonium acetate aqueous solution is added to each gram of ZSM-5; Dry at 120°C, roast at 500°C for 3 hours to obtain HZSM-...

Embodiment 2

[0030] [Example 2] Put 6 grams of the catalyst Ti-1 / HZSM-5 prepared above into a fixed-bed reactor with an inner diameter of 32 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℃, space velocity 13.1h -1 , the weight ratio of water to ethanol in the raw material is 0.1:1. Under the above conditions, the catalyst Ti-1 / HZSM-5 catalyzed the dehydration of ethanol to prepare ethylene with a conversion rate of 90.8% and a selectivity of ethylene of 94.6%. The gas chromatographic analysis results of the liquid phase components are shown in Table 1, wherein the retention time is 1.24min is the water peak, and the retention time is 4.74min is the ethanol peak, the original spectrum of chromatographic analysis can refer to the attached figure 1 . After 72 hours of continuous operation under this condition, the activity of the catalyst did not decrease.

[0031] Table 1. Chromat...

Embodiment 3

[0034] [Example 3] Using HZSM-5 with a silicon-aluminum molar ratio of 48 as a carrier, the titanium ion-modified molecular sieve catalyst Ti-2 / HZSM-5 was prepared in the same method and material ratio as in Example 1. Put 3.2 grams of the catalyst Ti-2 / HZSM-5 prepared above into a fixed-bed reactor with an inner diameter of 32 mm and a height of 500 mm. The reaction temperature is 350 °C and the space velocity is 10.2 h. -1 , the raw material is analytically pure ethanol. Under the above conditions, the catalyst Ti-2 / HZSM-5 catalyzes the dehydration of ethanol to prepare ethylene with a conversion rate of 80.9% and a selectivity of ethylene of 99.4%.

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Abstract

The present invention discloses a molecular sieve catalyst, a preparation method thereof and the application of the molecular sieve catalyst for preparing for ethene by dehydrating ethanol. The catalyst uses ZSM-5 molecular sieve or HZSM-5 which is obtained by acidifying the ZSM-5 as a support; oxide or salt of heteropoly acid or vanadium (V) or titanium (Ti) is used as active component; the active component is introduced into the support by a dipping method or a surface chemical reaction modifying method to be dried and calcined in a muffle furnace to obtain the molecular sieve catalyst. The catalyst is used in ethanol dehydration to prepare for the ethene and not only has high ethanol conversion rate and ethene selectivity and long service life, the maximum conversion rate of ethanol dehydration reaction can be 100 percent, and the maximum selectivity of the ethene can be 99.4 percent; but the catalyst also solves the technical problems of low airspeed, high temperature, high energy consumption, and the like, in the reaction of preparing for the ethene by dehydrating the ethanol; the catalyst is applicable to the industrial production of preparing for the ethene by dehydrating the ethanol and has the effects of improving production efficiency and saving energy source.

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 ethanol dehydration to prepare ethylene. Background technique [0002] Ethylene is one of the most important basic raw materials in the petrochemical industry. About 75% of chemical products are prepared from ethylene. Therefore, the size of ethylene production has become an important symbol to measure the development level of a country's petrochemical industry. At present, the method of producing ethylene is mainly by using natural gas or light petroleum distillate as raw material and adopting steam cracking process. However, with the increasingly tense relationship between the supply and demand of global oil resources, the price of natural gas and light petroleum distillates continues to rise, and the environmental pollution caused by the petrochemical industry is b...

Claims

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Application Information

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IPC IPC(8): B01J29/48B01J29/40C07C11/04C07C1/24
CPCY02P20/10Y02P20/52
Inventor 姜标李青王英雄陈锦峰王万军
Owner SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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