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A kind of preparation method and application of quaternary ammonium salt template agent

A technology of template agent and quaternary ammonium salt, which is applied in the field of compounds with molecular sieve and base exchange properties, can solve problems such as limitations, and achieve the effects of reducing synthesis costs, high safety, and reducing use costs

Active Publication Date: 2021-02-05
KENTE CATALYSTS INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the limitation of template concentration, the synthesis of SSZ-39 zeolite by solid phase method is still limited.

Method used

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  • A kind of preparation method and application of quaternary ammonium salt template agent
  • A kind of preparation method and application of quaternary ammonium salt template agent
  • A kind of preparation method and application of quaternary ammonium salt template agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Embodiment 1: the preparation of 2,6-dimethylpiperidine

[0042] The first step supports rhodium catalyst preparation

[0043] After mixing 11.2 g (0.1 mol) of triethylenediamine and propylene chloride at a molar ratio of 1:2, and stirring and reacting at room temperature for 72 hours, a white solid was obtained, which was filtered, washed with ethyl acetate and dried to obtain an ionic liquid mono Dissolve it in DMF, add an azobisisobutyronitrile initiator, stir evenly, transfer to an autoclave, and place in an oven for 12 hours of heating solvent thermal polymerization at 120°C to obtain a super-crosslinked porous polyionic liquid. Dissolve ammonium chlororhodate in ethanol to make a 2% solution, add the above-mentioned hypercrosslinked porous polyionic liquid, control the molar ratio of ammonium chlororhodate to the ionic liquid center to be 1:8, and carry out stirring and exchange at room temperature for 12 hours After filtering, washing and drying with ethanol, a ...

Embodiment 2

[0048] Embodiment 2: Preparation of 3,5-dimethylpiperidine

[0049] Step 1: Preparation of supported rhodium catalyst

[0050] After mixing 11.2 g (0.1 mol) of triethylenediamine and propylene chloride at a molar ratio of 1:2, and stirring and reacting at room temperature for 72 hours, a white solid was obtained, which was filtered, washed with ethyl acetate and dried to obtain an ionic liquid mono Dissolve it in DMF, add an azobisisobutyronitrile initiator, stir evenly, transfer to an autoclave, and place in an oven for 16 hours of heating solvent thermal polymerization at 110°C to obtain a super-crosslinked porous polyionic liquid. Dissolve ammonium chlororhodate in ethanol to make a 2% solution, add the above-mentioned hypercrosslinked porous polyionic liquid, control the molar ratio of ammonium chlororhodate to the ionic liquid center to be 1:4, and carry out stirring and exchange at room temperature for 12 hours After filtering, washing and drying with ethanol, a loaded ...

Embodiment 3-8

[0055] Embodiment 3-8: Catalyst recycling

[0056] The catalyst in Example 1 was recovered and reused. The basic process was the same as that in Example 1. Table 1 shows the results of the impact of the repeated use of the catalyst on the reaction.

[0057] Table 1 The impact of catalyst recycling times on the reaction

[0058] Example Reuse times Yield / % Proportion of trans product / % 3 1 99 87 4 2 98 88 5 3 99 87 6 4 98 87 7 5 99 87 8 6 98 88

[0059] As can be seen from Table 1, the supported rhodium catalyst prepared by the method of the present application has high activity, and when applied to the hydrogenation reaction of dialkylpyridine, the catalytic hydrogenation of dialkylpyridine can be converted into dioxane with high efficiency and high selectivity. Even if the base piperidine is reused six times, the activity is basically not reduced, and its catalytic conversion rate is still as high as 98%, and the ...

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Abstract

The application provides a preparation method and application of a quaternary ammonium salt template, which belongs to the technical field of compounds with molecular sieve and base exchange properties. Using dialkylpyridine as raw material, through the synthesis of dialkylpiperidine, tertiary amination of dialkylpiperidine, quaternization of dialkylpiperidine, hydrogenation of N,N-dialkylated dioxane The synthesis of base piperidine quaternary ammonium base obtains high-concentration template agent, which is used for solid-phase synthesis of SSZ-39 zeolite to synthesize SSZ-39 zeolite molecular sieve. Applying the present application to template agent and SSZ‑39 zeolite synthesis has the advantages of good safety, low reaction pressure, high yield and good selectivity.

Description

technical field [0001] The application relates to a preparation method and application of a quaternary ammonium salt template agent, which belongs to compounds with molecular sieve and base exchange properties. Background technique [0002] In 1999, Chevron Corporation of the United States reported for the first time to synthesize a new type of structural zeolite - SSZ-39 zeolite (US5958370). The rings are linked by some four-membered rings to form a three-dimensional channel structure with a maximum of eight-membered rings. SSZ-39 zeolite is mainly used in diesel engine exhaust NO x removal. [0003] Diesel engines have good thermal efficiency and economy, and are widely used in transportation vehicles. In the face of increasingly stringent exhaust emission laws and regulations, control NO in diesel engine exhaust x The emissions have become one of the most prominent difficulties in the field of catalytic purification of exhaust gas at home and abroad. Selective cataly...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25B3/20C25B3/05C25B3/09C25B3/13C01B39/48B01J31/30
CPCC25B3/00C01B39/48B01J31/30B01J31/0282B01J2231/646B01J35/617B01J35/615
Inventor 王新伟沈永淼李青山梁学正施旭升董柱永吴尖平吴勤明
Owner KENTE CATALYSTS INC
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