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Method of preparing ZSM-5 using variable temperature without organic template

A ZSM-5, particle size distribution technology, applied in chemical instruments and methods, crystalline aluminosilicate zeolites, chemical/physical processes, etc., which can solve problems such as long reaction times

Inactive Publication Date: 2007-05-30
SK INNOVATION CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method requires a reaction time of not less than 48 hours
[0009] As mentioned above, common methods for the synthesis of ZSM-5 without organic templates are outlined, i.e. by using seeds to promote crystallization, or neutralizing the alumina source with acid solutions to form suitable gel precursors, However, the disadvantage of these methods is that they require a long reaction time.

Method used

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  • Method of preparing ZSM-5 using variable temperature without organic template
  • Method of preparing ZSM-5 using variable temperature without organic template
  • Method of preparing ZSM-5 using variable temperature without organic template

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Embodiment approach

[0101] According to a first preferred embodiment of the present invention, a silicon dioxide source, an alkali metal oxide source (eg, alkali metal hydroxide) and water are mixed to prepare a first aqueous solution. Thus, it is desirable to control the amount of silica source in the first aqueous solution to be in the range of about 21.5-26.7% by weight. This is because silica cannot be uniformly dissolved in water if the amount of water in the first aqueous solution is too small or too large. A source of alumina, a source of alkali metal oxides and water are additionally mixed to obtain a second aqueous solution. In this way, the amount of alumina source in the second aqueous solution is controlled at about 0.9-4.4% by weight. This is also because the alumina source should be homogeneously dissolved in water. Then, the second aqueous solution is added to the first aqueous solution. Considering the concentrations of the first aqueous solution and the second aqueous solution...

Embodiment 1

[0121] Put 60g of Ludox AS-40 as a silica source into beaker 1, slowly add 21.4g of 10% by weight NaOH solution to the beaker while stirring at 200rpm, then add 30g of distilled water, and then stir at 200rpm for 3 hours. Separately, 1.65 g of sodium aluminate powder, 48.8 g of distilled water, and 8.8 g of a 10% by weight NaOH solution were added to the beaker 2, and mixed for 3 hours using a magnetic stirrer. After that, the solution in beaker 2 and another 18.8 g of distilled water were slowly added to the solution in beaker 1, followed by mixing for 1 hour. Subsequently, the resulting mixture was transferred to a 300 ml Teflon vessel, and by using an autoclave equipped with a sampling port as shown in Figure 1, the reaction temperature was raised to 190°C while stirring at 200 rpm for 2 hours. Then, the reaction temperature was cooled to 150°C and held for 40 hours. After completion of the reaction, the reaction product was filtered through a membrane filter with a pore s...

Embodiment 2

[0125] Put 60g of Ludox AS-40 as a silica source into beaker 1, slowly add 21.4g of 10% by weight NaOH solution to the beaker while stirring at 200rpm, then add 30g of distilled water, and then stir at 200rpm for 3 hours. 2.0 g of sodium aluminate powder, 49.4 g of distilled water and 7.5 g of 10% by weight NaOH solution were added to beaker 2, and mixed for 3 hours using a magnetic stirrer. After that, the solution in beaker 2 and another 19.4 g of distilled water were slowly added to the solution in beaker 1, followed by mixing for 1 hour. Subsequently, by using the same autoclave as in Example 1, the reaction temperature of the formed mixture was raised to 190° C. while stirring at 200 rpm, and maintained for 2 hours. Then, the reaction temperature was cooled to 150°C and held for 35 hours. After the reaction was completed, the properties of the formed reaction product were analyzed in the same manner as in Example 1. The results are shown in Figures 3a and 3b and Table 1...

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Abstract

Disclosed is a method of preparing ZSM-5 having substantially 100% crystallinity by using variable temperatures in the absence of an organic template, characterized in that a reaction mixture having a molar composition of M2O / SiO2 (M: alkali metal ion) of 0.07-0.14, H2O / SiO2 of 15-42 and SiO2 / Al2O3 of 20-100 is nucleated at relatively high temperatures (180-210 DEG C.) and then crystallized at relatively low temperatures (130-170 DEG C.), thus easily controlling a crystal size and a particle size distribution of the ZSM-5.

Description

technical field [0001] The present invention relates to a method for preparing ZSM-5 without an organic template using variable temperatures. More specifically, the present invention relates to a method for the preparation of ZSM-5, which is characterized in that the reaction mixture for the preparation of ZSM-5 is subjected to a two-step process, namely, nucleation at a relatively high temperature and subsequent crystallization at a relatively low temperature, without the use of Organic templates and seeds, so it is easy to control the crystal size and particle size distribution to a uniform particle size distribution and obtain essentially 100% crystallinity. Especially in nucleation, the reaction time is adjusted to freely control the crystal size and particle size distribution. Background technique [0002] Since Mobil Co. first developed ZSM-5 with a high silica content in the early 1970s, this class of materials has been extensively studied due to the unique catalytic...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/38B01J29/00C01B39/36
CPCC01B39/38
Inventor 金和重金信东
Owner SK INNOVATION CO LTD
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