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A kind of tin-containing heteroatom functional molecular sieve and its synthesis and application

A molecular sieve and hydrothermal synthesis technology, applied in molecular sieve and alkali exchange compound, molecular sieve catalyst, chemical instrument and method, etc., can solve the problems of difficult operation, easy agglomeration of tin source, difficult to control, etc., and achieve the effect of good catalytic performance

Active Publication Date: 2017-05-10
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For tin-containing heteroatom molecular sieves, P.Wu et al. studied the post-synthesis method of Beta molecular sieves dealuminated by nitric acid using gas-phase SnCl4 isomorphic substitution [P.Li, G.Liu, H.Wu, Y.Liu, J.Jiang, and P.Wu, J.Phys.Chem.C, dx.doi.org / 10.1021 / jp1076966], but the gas-phase crystal substitution method has the disadvantages of being difficult to operate and difficult to control
I.Hermans etc. carry out the research [C.Hammond, S.Conrad, and I.Hermans, Angew.Chem.Int.Ed., DOI: 10.1002 / anie.201206193], this method has obvious disadvantages that the tin source used is easy to agglomerate and difficult to disperse

Method used

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  • A kind of tin-containing heteroatom functional molecular sieve and its synthesis and application
  • A kind of tin-containing heteroatom functional molecular sieve and its synthesis and application
  • A kind of tin-containing heteroatom functional molecular sieve and its synthesis and application

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Experimental program
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Effect test

Embodiment 1

[0036] Treat 3 g of Beta molecular sieve (silicon-aluminum ratio=21) with concentrated nitric acid (concentration 65%) at 100°C for 24 hours at a liquid:solid ratio (weight ratio) of 20 to obtain Beta molecular sieve seed crystals (silicon-aluminum ratio>2000 ).

[0037] Add 0.15g of Beta molecular sieve seed crystals into 30g of deionized water, keep stirring vigorously for 24 hours to obtain a completely dispersed seed crystal solution.

[0038] Add 10.4g of tetraethylammonium hydroxide (concentration 50%) and 120g of water into another reactor, then add 12.3g of tetraethyl orthosilicate, raise the temperature to 50°C under stirring for 24 hours, then add 1.6g of boric acid to continue After reacting for 5 hours, a solution prepared by dissolving 0.17 g of tin tetrachloride in 20 g of water was added dropwise to the above reaction system within 1 hour, and reacted for 4 hours under strong stirring, and then added the seed liquid to continue the reaction for 2 hours. Finally...

Embodiment 2

[0041] Treat 3 g of borosilicate Beta molecular sieve (silicon-boron ratio = 25) with concentrated nitric acid (concentration 65%) at a ratio of liquid:solid of 20 (weight ratio) for 10 hours under ultrasonically strengthened heating conditions at 100°C to obtain Beta molecular sieve crystals. species (silicon-boron ratio>1300).

[0042] Add 0.7g of Beta molecular sieve seed crystals into 60g of deionized water, keep stirring vigorously for 24 hours to obtain a completely dispersed seed crystal solution.

[0043] Add 200g of water to another reactor, weigh 2.6g of tetraethylammonium hydroxide (concentration 50%) and 12.3g of divinyltriamine, then add 5.3g of boric acid to continue the reaction for 5 hours, and then tetrachloride The solution prepared by dissolving 0.02g of tin in 20g of water was added dropwise to the above reaction system within 1 hour, and reacted for 4 hours under strong stirring, then added the seed liquid and continued to react for 2 hours, finally added ...

Embodiment 3

[0046] 3 g of pure silicon Beta molecular sieves were treated with tetraethylammonium hydroxide (concentration 25%) at a liquid:solid ratio (weight ratio) of 20 under microwave-enhanced heating at 50°C for 10 hours to obtain Beta molecular sieve seed crystals.

[0047] Add 0.05g of Beta molecular sieve seed crystals into 60g of deionized water, keep stirring vigorously for 24 hours to obtain a completely dispersed seed crystal solution.

[0048] Add 200g of water to another reactor, weigh 2.6g of tetraethylammonium hydroxide (concentration 50%) and 12.3g of divinyltriamine, then add 5.3g of boric acid to continue the reaction for 5 hours, and then tetrachloride The solution prepared by dissolving 0.02g of tin in 20g of water was added dropwise to the above reaction system within 1 hour, and reacted for 4 hours under strong stirring, then added the seed liquid and continued to react for 2 hours, finally added 12.3g of ethyl orthosilicate, stirred Lower the temperature to 50°C a...

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Abstract

The invention discloses a functional molecular sieve containing tin heteroatoms and a synthesis method thereof. The tin-containing heteroatom functional molecular sieve has BEA topological structure characteristics, the silicon-tin ratio (atomic ratio) ranges from 80 to 1000, and a synthesis method for preparing the tin-containing Beta molecular sieve by using boric acid-assisted hydrothermal synthesis technology. Mix tin source, silicon source, boric acid, templating agent, water and seed crystal uniformly according to a certain ratio and feeding method, crystallize at a certain temperature for a certain period of time, and obtain Sn-Beta heteroatom functional molecular sieve after separation, washing and drying , the crystallized product can be directly used as a catalyst or a catalyst carrier. The Sn-Beta heteroatom functional molecular sieve has good catalytic performance in biomass catalytic conversion and many fine chemical reaction processes.

Description

technical field [0001] The invention relates to a functional molecular sieve containing tin heteroatoms and a synthesis method thereof. Specifically, the tin-containing heteroatom functional molecular sieve has BEA topological structure characteristics, the silicon-tin ratio (atomic ratio) ranges from 80 to 1000, and a tin-containing Beta molecular sieve is prepared by boric acid-assisted hydrothermal synthesis technology. resolve resolution. Background technique [0002] Molecular sieves are classified according to their basic composition, mainly silicate-based molecular sieves and phosphate-based molecular sieves. Since different chemical reactions have different requirements on the pore structure and surface properties of porous catalytic materials, on the one hand, the synthesis of new structural molecular sieve materials is always an important research content in materials science and catalytic science; on the other hand, the function of molecular sieve materials The ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/08C01B39/12B01J29/70B01J29/86B01J32/00
Inventor 王炳春田志坚马怀军曲炜徐仁顺徐竹生
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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