Method for preparing 4-hexene-3-ketone by carrying out dehydration on 4-hydroxy-3-hexanone
A technology of hexanone and hydroxyl, applied in the field of dehydration of 4-hydroxy-3-hexanone to prepare 4-hexen-3-one, which can solve the problems of low space velocity, poor catalyst activity and high reaction temperature
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Embodiment 1
[0020] By 1SiO 2 : 0.01Al 2 O 3 : 0.41TEAOH: 0.31 Acetylacetone: 31.76H 2 O Weigh each material, dissolve sodium aluminate in distilled water, add tetraethylammonium hydroxide dropwise, stir for 1 hour, add ethyl orthosilicate dropwise, stir for 1 hour, add acetylacetone, stir for 1 hour , adjust pH=13.0 with 0.1N sodium hydroxide solution, and continue stirring for 5 hours. The obtained mixture was crystallized under hydrothermal conditions at 170° C. for 4 days, washed, filtered and dried. The obtained product had characteristic diffraction peaks of ZSM-5 and preferentially grew in the (010) direction (b-axis). XRD spectrum see figure 2 In curve 1, the relative intensities of (020), (040), (060) and (080) peaks in the diffraction spectrum are significantly increased, which is obviously due to the preferred orientation of ZSM-5 single crystal on the powder diffraction sample plate, its (0h0) The surface, that is, the cylindrical surface of the single crystal, is paralle...
Embodiment 2
[0023] By 1SiO 2 : 0.01Al 2 O 3 : 0.25TPAOH: 0.05 Sodium oxalate: 32.0H 2 O Weigh each material, dissolve sodium aluminate in distilled water, add tetrapropylammonium hydroxide dropwise, stir for 1 hour, add silica sol dropwise, stir for 1 hour, add sodium oxalate, stir for 1 hour, use 0.1 N sodium hydroxide solution was adjusted to pH=12.0 and stirring was continued for an additional 5 hours. The resulting mixture was crystallized under hydrothermal conditions at 200°C for 3 days, washed, filtered and dried. XRD spectrum see figure 2 Middle curve 2. The synthesized ZSM-5 zeolite raw powder was treated with 0.8 mol / L acetic acid at 70° C. for 5 hours for 4 consecutive times, wherein the weight ratio of the acid solution and the ZSM-5 zeolite was 9 to obtain HZSM-5, that is, the catalyst.
[0024] The performance of the catalyst was evaluated according to the steps of [Example 1]. The reaction conditions and reaction results are shown in Table 1.
Embodiment 3
[0026] By 1SiO 2: 0.02Al 2 O 3 : 0.23TEAOH: 0.278-hydroxyquinoline: 44.64H 2 O Weigh each material, dissolve aluminum triethoxide in distilled water, add tetraethylammonium hydroxide dropwise, stir for 1 hour, add silica sol dropwise, stir for 1 hour, add 8-hydroxyquinoline, stir for 1 hour , adjust pH=11.0 with 0.1N sodium hydroxide solution, and continue stirring for 5 hours. The resulting mixture was crystallized under hydrothermal conditions at 150°C for 6 days, washed, filtered and dried. XRD spectrum see figure 2 Middle curve 3. The synthesized ZSM-5 zeolite raw powder was treated with 0.8 mol / L acetic acid at 80° C. for 5 hours for 3 consecutive times, wherein the weight ratio of the acid solution and the ZSM-5 zeolite was 8, to obtain HZSM-5, that is, the catalyst.
[0027] The performance of the catalyst was evaluated according to the steps of [Example 1]. The reaction conditions and reaction results are shown in Table 1.
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