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Preparation method for chiral beta zeolite

A beta zeolite and chiral technology, applied in the field of preparation of chiral compounds, can solve problems such as insufficient chiral resolution technology, and achieve huge commercial value

Active Publication Date: 2015-01-14
天津海赛纳米材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to solve the problem that many enantiomerically pure chiral drugs used in China rely heavily on imports due to the lack of chiral resolution technology in my country, and most of the chiral synthetic drugs produced are still sold in the form of racemates. The present invention provides A preparation method of chiral β zeolite is proposed. The chiral β zeolite obtained by the preparation method can be used as a chiral stationary phase of liquid chromatography for chiral resolution, which makes up for the deficiency of chiral resolution technology and is beneficial to life. Science, Medicinal Chemistry, Materials Chemistry and other fields have a huge boost

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  • Preparation method for chiral beta zeolite

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preparation example Construction

[0023] A preparation method of chiral beta zeolite according to the present invention: according to a certain proportion, the aluminum source is uniformly mixed with the mixed template agent composed of tetramethylammonium bromide, tetraethylammonium bromide and tetrapropylammonium bromide , to obtain solution A; mix silicon source, appropriate amount of seed crystals and pure water in a certain proportion to obtain mixture B; slowly pour A into B and stir evenly to obtain material C; add chiral directing agent to material C , to obtain material D; transfer material D into an autoclave for crystallization under autogenous pressure. The crystallized product is washed and calcined to obtain crystal powder, which is chiral zeolite beta.

[0024] According to the method of the present invention, the proportioning of reaction material will satisfy: xNa 2 O: AL 2 o 3 :ySiO 2 :mR + :oL:nH 2 O, where x ranges from 0.2 to 2, y ranges from 5 to 300, m ranges from 1 to 40...

Embodiment 1

[0036] Embodiment 1: sodium metaaluminate 99g2 O concentration is 17.34%, Al 2 o 3 The concentration is 10.28%> mixed with tetramethylammonium bromide 266g , tetraethylammonium bromide 334g mixed uniformly to obtain solution A; silica gel 200g 2 The content is 95%>, 10g of seed crystals and 428g of pure water are mixed evenly to obtain mixture B; slowly pour A into B and stir evenly to obtain material C; add 20g of L-alanine (content 100%) to material C , to obtain material D; the material D was transferred into a 2L autoclave, and crystallized under autogenous pressure at 145°C for 60 hours. The crystallized product is washed and calcined to obtain crystal powder. The crystal powder is chiral β zeolite. The X-ray diffraction pattern of chiral beta zeolite obtained in the present embodiment 1 like figure 2 Shown, the obtained chiral beta zeolite scanning electron micrograph (SEM) is as follows image 3 shown.

[0037] The crystal powder is made into a liquid ...

Embodiment 2

[0038] Embodiment 2: sodium metaaluminate 99g2 O concentration is 17.34%, Al 2 o 3 Concentration of 10.28%> mixed with tetraethylammonium bromide 334g , tetrapropylammonium bromide 314g to obtain solution A; silica gel 200g 2 The content is 95%>, 10g of seed crystals and 428g of pure water are mixed evenly to obtain mixture B; slowly pour A into B and stir evenly to obtain material C; add 20g of L-alanine (content 100%) to material C , to obtain material D; the material D was transferred into a 2L autoclave, and crystallized under autogenous pressure at 145°C for 60 hours. The crystallized product is washed and calcined to obtain crystal powder. The crystal powder is chiral β zeolite. The crystal powder is made into a liquid chromatography stationary phase, and the separation degree of racemic ketamine reaches 1.70.

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Abstract

The invention provides a preparation method for chiral beta zeolite. The method comprises: uniformly mixing an aluminium source and a mixed solution composed of tetramethylammonium bromide, tetraethylammonium bromide and tetrapropylammonium bromide according to a certain ratio, so as to obtain a solution A; mixing a silicon source, proper amount of a crystal seed and pure water according to a certain ratio, so as to obtain a solution B; slowly pouring the solution A into the solution B and stirring uniformly, so as to obtain a material C; adding a chiral guiding agent into the material C, so as to obtain a material D; transferring the material D into a high-pressure kettle, and performing crystallization under an automatically-generated pressure; and washing the crystallized product, and calcining to obtain the chiral beta zeolite. The obtained chiral beta zeolite obtained by employing the preparation method can be used as a chiral stationary phase of liquid chromatogram for chiral resolution, makes up the disadvantages of chiral resolution technology, has important meaning on fields such as life science, medicinal chemistry, material chemistry and the like, and possesses great business value.

Description

technical field [0001] The invention relates to the field of preparation of chiral compounds, in particular to a preparation method of chiral zeolite beta, which is used as a chiral stationary phase of liquid chromatography. Background technique [0002] Beta zeolite is a high silica zeolite with a three-dimensional structure, a twelve-membered ring skeleton structure, and a silicon-aluminum ratio of 5-300. Due to its unique structure, it is widely used in catalytic cracking, alkylation, etherification and automobile exhaust purification devices. As a molecular sieve, it has a moderate pore size and can be used in some special separation fields. [0003] The current research on chiral compounds is the most important and active part in stereochemistry and medicinal chemistry. Because enantiomers of chiral compounds usually have different biological activities, the preparation of enantiomerically pure chiral compounds is of great significance in the fields of life sciences, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04
CPCC01B39/04C01P2002/72C01P2004/03
Inventor 窦树华沈益新
Owner 天津海赛纳米材料有限公司
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