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Crystalline calcium-based microporous framework material and preparation method thereof

A frame material, calcium-based technology, applied in the field of crystalline calcium-based microporous frame material and its preparation, can solve the problems of the humectant being unable to build a microporous structure, unstable water locking performance, weak water storage capacity, etc. It is suitable for large-scale popularization and application, the preparation method is simple and diverse, and the effect of promoting moisturizing performance

Active Publication Date: 2020-07-10
SHANGHAI TOBACCO GRP CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, traditional humectants cannot build a microporous structure to achieve the purpose of structural water retention
In addition, traditional crystalline inorganic humectants and amorphous organic humectants have the problems of weak water storage capacity and unstable water-locking performance. If the water absorption performance is too high in an over-humid environment, it will cause moldy tobacco; Medium and easy to lose water, resulting in dryness

Method used

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  • Crystalline calcium-based microporous framework material and preparation method thereof
  • Crystalline calcium-based microporous framework material and preparation method thereof
  • Crystalline calcium-based microporous framework material and preparation method thereof

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preparation example Construction

[0047] Another aspect of the present invention provides a method for preparing a crystalline calcium-based microporous framework material, wherein the preparation method for a calcium-based microporous framework material in a single crystal state comprises the following steps:

[0048] 1) Prepare 1.5mol / L calcium salt solution A1 and stir at room temperature for 10 minutes;

[0049] 2) Prepare 2mol / L solution B1 of 1,3,5-tris(4-carboxy-substituted phenyl)benzene ligand, and stir at room temperature for 10 minutes;

[0050] 3) Mix solution A1 and solution B1, and stir at room temperature for 30 minutes to obtain mixed solution C1;

[0051] 4) Transfer the solution C1 to a stainless steel reaction kettle lined with a polytetrafluoroethylene liner, seal it, and react at T°C for t hours;

[0052] 5) Naturally cool to room temperature after the reaction, filter and wash to obtain a single crystal calcium-based microporous framework material.

[0053] In step (1), the calcium salt...

Embodiment 1

[0067] Embodiment 1 Preparation of crystalline calcium-based microporous framework material

[0068] Dimethylacetamide and water (volume ratio 8:2) solution A with 1.5mol / L calcium chloride, and dimethylacetamide with 2mol / L 1,3,5-tris(4-carboxyphenyl)benzene Amide and water (volume ratio 8:2) solution B, the above two solutions were mixed in a volume ratio of 1:1, stirred for 30 minutes, then the mixed solution was transferred to a stainless steel reaction kettle lined with a polytetrafluoroethylene liner, React at 120°C for 72 hours, cool naturally, filter, wash, and dry to obtain a rod-shaped crystalline calcium-based microporous framework material, the molecular structure of which is shown in Figure 1, according to the formula: The calculated yield is 78% (mass of the calcium substance in the medium)*100. The calcium substance in the product in this embodiment is a crystalline calcium-based microporous framework material, and the calcium substance in the feed is calcium ch...

Embodiment 2

[0069] Embodiment 2 Preparation of crystalline calcium-based microporous framework material

[0070] Configure solution C of 1.5mol / L calcium nitrate in dimethylformamide and water (volume ratio 8:2), configure 2mol / L 1,3,5-tri(4-carboxy-2,6-difluorobenzene base) dimethylformamide of benzene and water (volume ratio 8:2) solution D, the above two solutions were mixed at a volume ratio of 1:1, stirred for 30 minutes, and then the mixed solution was transferred to the liner polytetrafluoroethylene In a stainless steel reactor with an inner tank, react at 90°C for 24 hours, cool naturally, filter, wash, and dry to obtain a rod-shaped crystalline calcium-based microporous framework material. According to the formula (the quality of the calcium substance in the product / the quality of the calcium substance in the feed)*100, the calculated yield is 51%. In this embodiment, the calcium substance in the product is a crystalline calcium-based microporous framework material, and the calci...

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Abstract

The invention relates to a novel porous material, in particular to a crystalline calcium-based microporous framework material and a preparation method thereof. The general molecular formula of the crystalline calcium-based microporous framework material is shown in the specification as Ca6(L)4(H2O)4, L is a completely deprotonated 1, 3, 5-tri (4-carboxyl substituted phenyl) benzene ligand, the crystalline calcium-based microporous framework material belongs to a monoclinic system, and the cell parameters are as shown in the specification; the invention also provides the preparation method andapplication of the crystalline calcium-based microporous framework material. The crystalline calcium-based microporous framework material has a two-dimensional hexagonal microporous channel structure,so that the moisture retention performance of the material is promoted; the preparation method is simple and diverse and suitable for large-scale popularization and application.

Description

technical field [0001] The invention relates to a novel porous material, in particular to a crystalline calcium-based microporous frame material and a preparation method thereof. Background technique [0002] Cut stems are one of the components of tobacco products. Compared with shredded tobacco, the content of polyphenolic natural products in cut stems is lower. One of the characteristics of polyphenolic compounds is that they can lock water molecules through hydrogen bonds at the molecular level, so as to achieve the effect of moistening smoke and reducing the burning sensation. At the same time, shredded tobacco has a natural microporous structure, which is also very helpful for the storage of water molecules. In contrast, cut stems have been shown to contain super-large pore structures, and the inner surface is very smooth. From the perspective of structural chemistry, the composition and morphology are obviously not conducive to the capture and storage of water molec...

Claims

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Application Information

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IPC IPC(8): C07D213/80A24B5/16C07C51/41C07C63/331C07C63/72C07D213/803
CPCC07D213/80C07D213/803C07C63/331C07C63/72C07C51/418A24B5/16C07B2200/13
Inventor LOU JIAYINGWU DAFEI TINGZHANG WEIZHOU KAIMINZHANG JING
Owner SHANGHAI TOBACCO GRP CO LTD
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