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Co(II)-based crystalline catalyst with layer pillaring structure and preparation method thereof

A catalyst and pillared technology, which is applied in the field of polymers, Co-based crystalline catalysts with a layered pillared structure and its preparation, can solve the problems of unpredictability in the synthesis process, uncontrollable assembly process, and poor stability of the catalyst. Good recycling effect, good selectivity and yield, and high stability

Active Publication Date: 2017-05-17
江苏昂格生物科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Aiming at the above-mentioned technical problems in the prior art, the present invention provides a Co(II)-based crystalline catalyst with a layered pillared structure and a preparation method thereof. The Co(II)-based crystal with a layered pillared structure State catalyst and its preparation method should solve the technical problems such as the uncontrollable assembly process of most PCPs in the prior art, the structure is variable, and the synthesis process is relatively unpredictable. Technical problems such as cumbersome preparation steps and low activity

Method used

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  • Co(II)-based crystalline catalyst with layer pillaring structure and preparation method thereof
  • Co(II)-based crystalline catalyst with layer pillaring structure and preparation method thereof
  • Co(II)-based crystalline catalyst with layer pillaring structure and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0023] Embodiment 1: Synthesis and application of Co(II) crystalline catalyst 1

[0024] (1) According to 2,4,6-tris(4-pyridyl)-1,3,5-triazine and H 2 The molar ratio of BDC is 1:1, weighed and mixed to form a mixed compound;

[0025] (2) Weigh cobalt nitrate hydrate according to the ratio of 2:1 molar ratio between cobalt nitrate hydrate and 2,4,6-tris(4-pyridyl)-1,3,5-triazine in (1);

[0026] (3) The hydrated cobalt nitrate and the mixture were mixed in DMF / EtOH / H under ultrasound or stirring 2 O (DMF / EtOH / H 2 The volume ratio of O is 4:4:2) and mixed in a solvent to form a Co(II)-tpt precursor solution;

[0027] (4) Transfer the precursor solution obtained in (3) into a hydrothermal kettle with a volume ratio of 1 / 3, and conduct a solvothermal reaction at 100°C for 72 hours. Finally, filter, wash, and dry to obtain a layered pillared Structure Co(II) crystalline material.

[0028]Use the Bruker APEX II diffractometer to collect diffraction intensity data to obtain a h...

Embodiment 2

[0030] Embodiment 2: Synthesis and application of Co(II) crystalline catalyst 2

[0031] (1) According to 2,4,6-tris(4-pyridyl)-1,3,5-triazine with CH 3 -H 2 The BDC molar ratio is 1:1 and weighed, and it is a mixed compound after mixing;

[0032] (2) Weigh cobalt nitrate hydrate according to the ratio of 2:1 molar ratio between cobalt nitrate hydrate and 2,4,6-tris(4-pyridyl)-1,3,5-triazine in (1);

[0033] (3) Combine the hydrated cobalt nitrate and the mixture under ultrasonic or stirring in H 2 O / CH 3 CN (H 2 O and CH 3 The volume ratio of CN is 4:4) and mixed in a solvent to form a Co(II)-tpt precursor solution;

[0034] (4) Transfer the precursor solution obtained in (3) into a hydrothermal kettle with a volume ratio of 1 / 3, and conduct a solvothermal reaction at 130°C for 72 hours. Finally, filter, wash, and dry to obtain a layered pillared Structure Co(II) crystalline material.

[0035] In a typical Knoevenagel condensation reaction, a flask containing a single...

Embodiment 3

[0036] Embodiment 3: Synthesis and application of Co(II) crystalline catalyst 3

[0037] (1) According to 2, 4, 6-tris(4-pyridyl)-1, 3, 5-triazine and NO 2 -BDC molar ratio is 1:1 and weighed, mixed into a mixed body;

[0038] (2) Weigh cobalt nitrate hydrate according to the ratio of 2:1 molar ratio between cobalt nitrate hydrate and 2,4,6-tris(4-pyridyl)-1,3,5-triazine in (1);

[0039] (3) Mix the hydrated cobalt nitrate and the compound in the solvent of isopropanol / water (the volume ratio of isopropanol and water is 4:2) under ultrasonic or stirring, and configure the precursor of Co(II)-tpt solution;

[0040] (4) Transfer the precursor solution obtained in (3) into a hydrothermal kettle with a volume ratio of 1 / 3, and conduct a solvothermal reaction at 130°C for 72 hours. Finally, filter, wash, and dry to obtain a layered pillared Structure Co(II) crystalline material.

[0041] The diffraction intensity data was collected on the Bruker APEX II diffractometer to obtain...

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Abstract

The invention provides a Co(II)-based crystalline catalyst with a layer pillaring structure. A mixed ligand is formed by 2,3,6-tri(4-pyridyl)-1,3,5-triazine(tpt) and a 5-substituted isophthalate derivative; Co(II) is used as a center ion, and the mixed ligand and the CO(II) are assembled into the Co(II)-based crystalline catalyst with the layer pillaring structure. The invention also provides a preparation method of the catalyst. The preparation method comprises the following steps of mixing the mixed ligand and cobalt nitrate hexahydrate, so as to prepare into a Co(II)-tpt precursor solution; transferring the precursor water solution into a hydrothermal kettle, performing solvent thermal reaction, sucking and filtering, washing, drying, and separating, so as to obtain the Co(II)-based crystalline material with the layer pillaring structure. The Co(II)-based crystalline material has the advantages that the specific surface area is larger, the conjugate system is larger, the catalysis activity on the Knoevenagel condensation is higher, and the maximum catalysis efficiency is 99%.

Description

technical field [0001] The invention belongs to the field of chemical industry and relates to a polymer, specifically a Co(II)-based crystalline catalyst with a layered pillar structure and a preparation method thereof. Background technique [0002] As an emerging research field, Porous Coordination Polymers (PCPs) have shown attractive physical and chemical properties and potential application values ​​in many aspects such as magnetism, optics, ion exchange, gas storage, and catalysis. , attracting the attention of scientists in the fields of chemistry and materials in the world. The design and synthesis of PCPs is also one of the most popular scientific research directions today. PCPs has specific advantages such as ordered porosity, large specific surface area and adjustable pore morphology, and it is insoluble in most organic solvents, so it has natural advantages in the application of heterogeneous catalysis. . However, there are certain limitations in the applicatio...

Claims

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Application Information

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IPC IPC(8): B01J31/22C07C253/30C07C255/41
CPCC07C253/30B01J31/1691B01J31/2217B01J2531/845B01J2531/0238B01J35/50C07C255/41
Inventor 张建勇邓维史军霞黄嫣崔鹏辉温鲜妮
Owner 江苏昂格生物科技有限公司
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