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A kind of method for synthesizing zsm-23 zeolite without solvent

A ZSM-23, solvent-free technology, applied in the field of molecular sieve preparation, can solve the problems of unfavorable zeolite production, high synthesis cost, strong volatility, etc., and achieve the effects of good catalytic reaction activity, low cost and low toxicity

Active Publication Date: 2019-03-05
JIAXING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, in the ZSM-23 zeolite synthesis, there are mainly two problems: its synthesis is carried out under hydrothermal conditions, the synthesis cost is high and the efficiency is low; most of the organic templates used are organic amines (such as iso Propylamine, dimethylamine, etc.), which are highly toxic and volatile
However, the synthesis cost of 1,3-diisopropylimidazole hydroxide is relatively high, and HF, which is extremely volatile and highly toxic, is used in the synthesis, which is not conducive to the production of zeolite

Method used

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  • A kind of method for synthesizing zsm-23 zeolite without solvent
  • A kind of method for synthesizing zsm-23 zeolite without solvent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Embodiment 1: Solvent-free synthesis of ZSM-23 zeolite

[0023] Put 1.6g of solid silica gel, 1g of ammonium fluoride, and 0.37g of 1,3-diisopropylimidazolium iodide (T) in a grinding mill, then crystallize at 160°C for 3 days to complete crystallization, and the product is suction filtered , the product can be obtained after drying. The ratio of reaction raw materials is as follows (molar ratio):

[0024] 1SiO 2 :1NH 4 F:0.05T

[0025] Obtain its structure through XRD analysis and be ZSM-23 zeolite ( figure 1 ), and it can be seen from the SEM photo that the typical rod-shaped morphology attributed to ZSM-23 zeolite ( figure 2 ).

Embodiment 2

[0026] Embodiment 2: Solvent-free high-temperature synthesis of ZSM-23 zeolite

[0027] Grind 1.6g of solid silica gel, 2g of ammonium fluoride and 0.74g of 1,3-diisopropylimidazolium iodide in a grinder, then crystallize at 200°C for 1 day to complete crystallization, the product is suction filtered and dried The product is then available. The ratio of reaction raw materials is as follows (molar ratio):

[0028] 1SiO 2 :2NH 4 F:0.1T

Embodiment 3

[0029] Embodiment 3: Solvent-free low-temperature synthesis of ZSM-23 zeolite

[0030] Put 1.6g of solid silica gel, 0.5g of ammonium fluoride, 2.22g of 1,3-diisopropylimidazolium iodide salt and 0.16g of ZSM-23 zeolite seed crystals in a grinding mill, and then crystallize at 100°C for 15 days. After complete crystallization, the product was suction filtered and dried to obtain the product. The ratio of reaction raw materials is as follows (molar ratio):

[0031] 1SiO 2 :0.5NH 4 F:0.3T

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Abstract

The invention relates to a preparation method of a molecular sieve, and aims at providing a method for synthesizing ZSM (Zeolite Socony Mobil)-23 zeolite in a solvent-free manner. The method comprisesthe following steps of putting a silicon source, an aluminum source, a fluorine source and 1,3-diisopropyl imidazole iodine, which is used as an organic template, into a mortar, wherein a range of amolar ratio of the silicon source to the aluminum source to the fluorine source to the organic template is 1 to (0 to 0.01) to (0.5 to 2) to (0.05 to 0.3); carrying out grinding treatment on raw materials, then transferring into a reaction kettle, and carrying out a crystallization reaction for 0.5d to 15d in a condition of 100 to 200 DEG C; carrying out suction filtration and oven-drying on a reaction product, so as to obtain the ZSM-23 zeolite. By using the method, a synthesis yield is improved; the use of the organic template is reduced; HF is completely replaced by using non-volatile ammonium fluoride; moreover, the synthesis operation is simple, easy and feasible. The used organic template has low toxicity and a low cost, and has an application prospect. Inorganic raw materials adopted for production are all environment-friendly and have lower price, and therefore, the method has important significance in the field of actual chemical production.

Description

technical field [0001] The invention belongs to a method for preparing molecular sieves, in particular to a method for synthesizing ZSM-23 zeolite without solvent. Background technique [0002] ZSM-23 zeolite is a high silica zeolite with medium pore size and MTT topological structure, which contains five-membered ring, six-membered ring and ten-membered ring channels. Scientists such as Plank reported for the first time the method of using pyrrolidine as an organic template to synthesize ZSM-23 molecular sieves (USP4076,842). Later, researchers found that it showed excellent performance in butene isomerization, xylene isomerization and MTG reactions, which aroused people's enthusiasm for studying ZSM-23 zeolite. [0003] At present, in the ZSM-23 zeolite synthesis, there are mainly two problems: its synthesis is carried out under hydrothermal conditions, the synthesis cost is high and the efficiency is low; most of the organic templates used are organic amines (such as iso...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/48
CPCC01B39/48C01P2002/72C01P2004/03
Inventor 朱龙凤曹雪波吴勤明宋利武军
Owner JIAXING UNIV