Method for preparing ITQ-2 molecular sieve

A technology of ITQ-2 and molecular sieve, applied in the field of preparation of ITQ-2 molecular sieve, can solve the problems of high cost, unfavorable industrial application, poor effect, etc., and achieve the effect of rationalized yield, simple and feasible method, and pollution reduction.

Inactive Publication Date: 2011-02-16
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the existing ITQ-2 molecular sieve preparation method uses tetrapropyl ammonium hydroxide in a large amount, so the cost is high, which is not conducive to industrial application
Existing literature attempts to reduce the amount of the above-mentioned valuable organic substances, but the effect is not good

Method used

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  • Method for preparing ITQ-2 molecular sieve
  • Method for preparing ITQ-2 molecular sieve
  • Method for preparing ITQ-2 molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041]First prepare 80ml of 0.2mol / L NaOH solution, then add 0.8g of white carbon black into the lye to obtain A solution, then add the solution containing 12.5g of cetyltrimethylammonium bromide to A solution, stir The B solution was obtained uniformly, and then the obtained mixture was transferred to a three-neck flask for heating in a water bath, and 5 g of MCM-22 molecular sieves were added under constant stirring, and then expanded at 80° C. for 24 h. After the mixed liquid is cooled, it is treated with 50KHz ultrasonic waves for 1 hour, and the pH value is quickly adjusted to be less than 2 with 6mol / L HCl. The solid is collected by centrifugation, washed, dried, and calcined at 540°C for 6 hours. The yield is calculated as 87%. XRD crystal phase analysis of the samples showed that the prepared samples were pure phase ITQ-2 molecular sieves. Spectrum see attached image 3 .

Embodiment 2

[0043] Repeat Example 1, but change the NaOH solution concentration into 0.05mol / L, 0.1mol / L, 0.5mol / L, 0.8mol / L, 1.0mol / L respectively, and the yield of the solid product obtained as a result is respectively 103%, 95%, 60%, 56%, 50%. XRD crystal phase analysis was carried out on the sample, and the results showed that the product distribution of the prepared sample was a mixture of MCM-22 and a small amount of amorphous substance, a mixture of a small amount of MCM-22 and a large amount of ITQ-2, a small amount of amorphous substance and a large amount of ITQ-2 A mixture of a small amount of ITQ-2 and a large amount of amorphous material, amorphous material. Wherein the yield obtained by the NaOH solution of 0.05mol / L is greater than 100%, the main reason is that the low alkalinity cannot completely dissolve the white carbon black, and the amount of the remaining white carbon black is greater than the amount lost by the MCM-22 molecular sieve.

Embodiment 3

[0045] Repeat Example 1, but change the amount of white carbon black into 0.1g, 0.5g, 1.6g, 5g respectively, and the yield of the solid product obtained as a result is 64%, 84%, 95%, 190% respectively. XRD crystal phase analysis was carried out on the sample, and the results showed that the prepared samples were pure phase ITQ-2 molecular sieve, pure phase ITQ-2 molecular sieve, mixture of amorphous substance and a large amount of ITQ-2 molecular sieve, amorphous substance and ITQ-2 molecular sieve mixture. The yield obtained by adding 5g of white carbon black is greater than 100%, the main reason is that excessive white carbon black is mixed in the product in an amorphous form.

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Abstract

The invention provides a method for preparing an ITQ-2 molecular sieve, which is characterized in that an MCM-22 molecular sieve is prepared, NaOH, KOH or mixture of NaOH and KOH or silicate containing NaOH and KOH is taken as an alkali source to prepare alkali solution; a silicon source is added in the obtained alkali solution and stirred to obtain solution A; an expanding agent is added into the solution A to obtain solution B; the solution B is heated and stirred continuously, then the MCM-22 molecular sieve is added in the solution B for expanding treatment, the expanded pulp is treated by ultrasonic wave, and the pH value of the solution after ultrasonic treatment is adjusted by acid solution. In the method, quaternary ammonium base for synthesizing the ITQ-2 molecular sieve is completely replaced by inorganic base, the production cost is low, desilicication by adding the silicon source is restrained, and the rationalization of the yield of target products is guaranteed. The method is simple and available and does not require the addition of organic base, thus reducing the pollution to the environment due to decomposition of the organic matters in the process of subsequent processing.

Description

technical field [0001] The invention belongs to the field of molecular sieve material preparation and relates to a preparation method of ITQ-2 molecular sieve. Background technique [0002] ITQ-2 molecular sieve is prepared by expansion and exfoliation of MCM-22 molecular sieve. It has a single-layer structure of MCM-22 molecular sieve and belongs to the MWW topology. MCM-22 molecular sieve has three sets of independent pore systems: a pore system connected by a supercage (0.71×0.71×1.82nm) and an interlayer 10-membered ring (0.4×0.54nm), and a two-dimensional sinusoidal pore system with an intralayer 10-membered ring. And the 12-membered ring hole (0.71×0.71×0.71nm) on the outer surface of the crystal. In contrast, ITQ-2 molecular sieve has two independent pore systems: a 10-membered ring two-dimensional sinusoidal channel system in the layer and a 12-membered ring hole (0.71×0.71×0.71nm) on the outer surface of the crystal. Disorder and short-range order. At the same ti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/02
Inventor 郭洪臣钱吉聂彬剑刘玲郑步梅
Owner DALIAN UNIV OF TECH
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