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Porous zirconium pyrophosphate catalyst and application thereof to piperaldehyde hydrogenation reaction

A zirconium pyrophosphate and catalyst technology, applied in physical/chemical process catalysts, organic chemistry, chemical recovery and other directions, can solve the problems of easy separation and reuse of catalysts that do not meet the requirements, cannot be recycled, and Ni is expensive, and achieves good catalysis. effect, easy recycling, highly selective effect

Active Publication Date: 2018-07-24
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As an intermediate in the synthesis of the antibacterial drug berberine, piperonyl alcohol has been gradually studied and is committed to finding a method for preparing piperonyl alcohol with mild conditions. Tang Yueping mentioned in the book "Pharmaceutical Synthesis Technology" a method for the reduction of piperonal to prepare piperonyl alcohol. The alcohol method uses Raney Ni combined with hydrogen to achieve hydrogenation reduction of the carbonyl of piperonal. However, when hydrogen pressure is used, it still depends on pressurized equipment, and the price of Ni is relatively expensive, and it is special during use. It is easy to deactivate and does not meet the goal of easy separation and reusability of the catalyst. Liu et al. used NaBH 4 Reduction of piperonal in a silica sol medium yielded 93% yield of piperonol, also during the use of NaBH 4 Loss is more, can't recycle (disclosed in 2001 "OrganicPreparations and Procedures International"), in addition Li etc. obtain the piperonyl alcohol of 10% yield (J.T.Li et al, Synthetic Communications, 2002, 32(4), 547-551.), is still overly dependent on metal magnesium, so seeking a clean, efficient and stable catalyst is still the top priority of current research

Method used

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  • Porous zirconium pyrophosphate catalyst and application thereof to piperaldehyde hydrogenation reaction
  • Porous zirconium pyrophosphate catalyst and application thereof to piperaldehyde hydrogenation reaction
  • Porous zirconium pyrophosphate catalyst and application thereof to piperaldehyde hydrogenation reaction

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Preparation of zirconium pyrophosphate: Na 4 P 2 o 7 10H 2 O and ZrOCl 2 ·8H 2 Each of O was dissolved in 25mL deionized water to form solutions with a concentration of 0.04mol / L and 0.08mol / L respectively (the ratio of zirconium to phosphorus was 1:1), and the obtained zirconium oxychloride solution was added dropwise to sodium pyrophosphate After 14-18 minutes, the solution was dropped, and the mixture was continuously stirred at room temperature for 10 hours. The white precipitate was separated by centrifugation at 8500r / min, washed with deionized water and ethanol three times to remove Na + and Cl － , dried at 80°C for 12h.

Embodiment 2

[0031] (1) Take by weighing 1mmol piperonal, 200mg of zirconium pyrophosphate catalyst (the ratio of zirconium to phosphorus is 1:1) joins in the reactor that fills 5mL isopropanol;

[0032] (2) The above-mentioned reactor was placed in an oil bath at 160° C. and stirred for 10 h. After the reaction was cooled, a small amount of the reacted solution was taken to measure the yield of piperonyl alcohol and the conversion rate of piperonal with GC.

[0033] Change the isopropanol in (1) to other solvents, such as methanol, ethanol, isobutanol, and the reaction conditions of the remaining steps are the same. After getting a small amount of reaction, solution measures the conversion rate of piperonyl alcohol productive rate and piperonal with GC, the result is as follows image 3 Shown, corresponding methanol, ethanol, isopropanol and isobutanol make the conversion rate of the piperonal that solvent obtains be respectively 94%, 94%, 96%, 96%, and the productive rate of piperonyl al...

Embodiment 3

[0035] (1) Take by weighing 1mmol piperonal, 200mg of zirconium pyrophosphate catalyst (the ratio of zirconium to phosphorus is 1:1) joins in the reactor that fills 5mL isopropanol;

[0036] (2) The above-mentioned reactor was placed in an oil bath at 160° C. and stirred for 10 h. After the reaction was cooled, a small amount of the reacted solution was taken to measure the yield of piperonyl alcohol and the conversion rate of piperonal with GC.

[0037] Change the amount of zirconium pyrophosphate in (1) from 200 mg to 50, 100, 150, and 250 mg, and the reaction conditions of the remaining steps are the same. Cooling after completion of the reaction, get a small amount of reaction back solution and measure the conversion rate of piperonyl alcohol productive rate and piperonal with GC, the result is as follows Figure 4Shown, the addition of zirconium pyrophosphate amount is 50,100,150,200 and the conversion rate of the piperonal that 250mg obtains is respectively 46%, 58%, 81%...

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Abstract

The invention discloses a porous zirconium pyrophosphate catalyst and application thereof to piperaldehyde hydrogenation reaction and belongs to the technical field of solid acid catalysis. The porouszirconium pyrophosphate catalyst and the application thereof disclosed by the invention have the beneficial effects that the prepared catalyst is simple in synthetic step, raw materials used are cheap and easy to obtain, and the obtained catalyst self carries a large number of acidic sites and alkaline sites and can efficiently catalyze and reduce piperitol obtained from piperaldehyde; the catalyst is easy to separate after reaction, can be recycled for many times and meets the requirements of green and sustainable development.

Description

technical field [0001] The invention relates to a porous zirconium pyrophosphate catalyst and its application in the hydrogenation reaction of piperonal, belonging to the field of solid acid catalysis. Background technique [0002] With the development of society, tumor has become the main killer threatening human health. The incidence and mortality of malignant tumors are increasing year by year. The prevention, early detection and treatment of malignant tumors have become medical hotspots and problems worldwide. At present, the treatment methods for malignant tumors are mainly surgical treatment, chemical drug treatment, and radiotherapy. However, hepatocellular carcinoma is highly invasive and metastatic, and is less sensitive to conventional anti-tumor chemical drugs. Therefore, finding new anti-tumor drugs and controlling the recurrence of liver cancer has become an urgent problem in the field of cancer research. . With the development of medical science and the con...

Claims

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Application Information

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IPC IPC(8): C07D317/54B01J27/16
CPCY02P20/584C07D317/54B01J27/16
Inventor 王海军王健佳王瑞英
Owner JIANGNAN UNIV
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