Continuous preparation method for phthalide and derivatives thereof

A derivative, phthalide technology, applied in chemical instruments and methods, physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problems of low carbonyl hydrogenation selectivity and limited application. , to achieve the effect of more reaction, low cost and uniform pore size distribution

Active Publication Date: 2012-09-19
如东文园投资开发有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The catalyst preparation methods of previous studies are mainly impregnation method, mixing method and deposition-precipitation method. When Ni and Co in Group VIII metals are used as active components, the catalyst has a low selectivity for carbonyl hydrogenation. When noble metals such as Pd and Au are used as active components, they show good conversion and selectivity, but the price of noble metals limits their industrial application.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Take 38.5g of tetraethyl orthosilicate in a three-necked flask, add 21.3g of butyl titanate alcohol solution, stir at 80°C for 4h, dissolve 14.7g of nickel nitrate in 7ml of ethylene glycol to make a solution, add it to the above mixture and stir for 3h , add distilled water at a ratio (molar ratio) of ethyl orthosilicate: distilled water = 1:15, add absolute ethanol at a ratio (molar ratio) of ethyl orthosilicate: absolute ethanol = 1:3, and continue stirring for 2 hours , transferred to a dish to obtain a colorless and transparent wet gel, kept in an oven at 70°C for 30 hours to obtain a dry gel, then roasted in a muffle furnace at 600°C for 24 hours, ground and sieved to obtain a 40-60 mesh catalyst for use.

[0038] Put 10ml of the above 40~60mesh catalyst in a fixed bed reaction tube, adjust the hydrogen pressure to 1.0Mpa, slowly raise the temperature to 450°C, and the hydrogen volume space velocity is 2000h -1 , Under these conditions the catalyst was reduced for...

Embodiment 2

[0040] Take 38.5g of ethyl orthosilicate in a three-necked flask, add 18.6g of butyl titanate alcohol solution, stir at 80°C for 4 hours, dissolve 13g of nickel nitrate in 10ml of ethylene glycol to make a solution, and dissolve 0.04g of PdCl in 2ml of ethylene glycol 2, add to the above mixture and stir for 3 hours, add distilled water at the ratio (molar ratio) of ethyl orthosilicate: distilled water = 1:16, and add distilled water at the ratio (molar ratio) of ethyl orthosilicate: absolute ethanol = 1:2 Add absolute ethanol, continue to stir for 2 hours, transfer to a dish to obtain a colorless and transparent wet gel, keep it in an oven at 80°C for 30 hours to obtain a dry gel, then bake it in a muffle furnace at 600°C for 24 hours, grind and sieve to obtain 40~60 mesh catalysts are used for standby.

[0041] Put 10ml of the above 40~60mesh catalyst in a fixed bed reaction tube, adjust the hydrogen pressure to 1.0Mpa, slowly raise the temperature to 450°C, and the hydrogen...

Embodiment 3

[0043] Take 58.5g of ethyl orthosilicate in a three-necked flask, add 29g of butyl titanate alcohol solution, stir at 60°C for 4h, dissolve 13.5g of nickel nitrate in 10ml of ethylene glycol to make a solution, add it to the above mixture and stir for 3h, Add distilled water at a ratio (molar ratio) of ethyl orthosilicate: distilled water = 1:18, add absolute ethanol at a ratio (molar ratio) of ethyl orthosilicate: absolute ethanol = 1:2, and continue stirring for 2 hours. Transfer to a dish to obtain a colorless and transparent wet gel, keep it in an oven at 80°C for 30 hours to obtain a green dry gel, then bake it in a muffle furnace at 600°C for 24 hours, grind and sieve to obtain a 40-60 mesh catalyst for use.

[0044] Put 10ml of the above 40~60mesh catalyst in a fixed bed reaction tube, adjust the hydrogen pressure to 1.0Mpa, slowly raise the temperature to 450°C, and the hydrogen volume space velocity is 2000h -1 , Under these conditions the catalyst was reduced for 4h....

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Abstract

The invention discloses a continuous preparation method for phthalide and derivatives thereof, and belongs to the technical field of chemical industry. A catalyst is prepared by a sol-gel method, the catalyst is a low-content nickel-based catalyst, and the content of nickel is 5 to 35 percent based on nickel oxide; one or more of noble metal, alkali metal and alkaline-earth metal elements is / are used as aid(s); the catalyst carrier is a TiO2-SiO2 composite oxide; and the reaction is implemented in a fixed bed hydrogenation device. According to the preparation method, because the active ingredient Ni of the catalyst has a superfine particle structure, the pore size distribution is uniform, the catalyst has high catalytic activity and selectivity, the conversion rate of phthalic anhydride can reach 99.4 percent under experimental conditions, and the selectivity of the phthalide can reach about 92.5 percent. The continuous preparation method for the phthalide is high in activity and selectivity.

Description

technical field [0001] The invention relates to a method for preparing phthalide by continuous catalytic hydrogenation of phthalic anhydride (phthalic anhydride) and its derivatives, which belongs to the technical field of chemical industry. Background technique [0002] Phthalide, also known as o-hydroxymethylbenzoic acid lactone, is an important fine chemical intermediate, which is used in the production of anticoagulant drugs phenylindandione and phenylthiazine, and anxiolytic drug doxepin , analgesic raw material drug talniflunate crude product, pharmaceutical intermediate 3-bromophthalide and laxatives, etc.; pesticides are used to produce fungicides tetrachlorophthalide, phenoxystrobin, etc.; in addition, it can also be used for dye intermediates 1, Synthesis of 4-dichloroanthraquinone and 1-chloroanthraquinone, etc., also used for dye reduction brown BR, etc. [0003] The synthesis methods of phthalide mainly include phthalimide method, chemical reduction method of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/88B01J23/755B01J23/89
Inventor 李为民魏国辉邱玉华任庆功郭登峰姚超
Owner 如东文园投资开发有限公司
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