Catalyst and method for preparing 2-methyl-2,4-pentanediol by diacetone alcohol hydrogenation

A technology of hydrogenation catalyst and diacetone alcohol, which is applied in the direction of physical/chemical process catalysts, chemical instruments and methods, preparation of hydroxyl compounds, etc., which can solve the discomfort of pilot scale-up and industrial production, complex catalyst preparation methods, and separation of products and solvents Difficulties and other problems, to achieve the effect of good recycling performance, low cost, and easy separation

Active Publication Date: 2017-10-10
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] Yet above-mentioned existing document is in the process of preparing 2-methyl-2,4-pentanediol by hydrogenation of diacetone alcohol, mostly adopts Ni series catalyst or adds basic compound in Ni series catalyst, and its catalyst preparation method is relatively Complex, Ni-based catalysts have serious loss and instability, small production capacity, and are not suitable for pilot scale-up and industrial production; and the use of toxic solvents or organic solvents in these processes makes it difficult to separate the product from the solvent, and the yield is low, and There are problems such as high production cost and difficult operation

Method used

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  • Catalyst and method for preparing 2-methyl-2,4-pentanediol by diacetone alcohol hydrogenation
  • Catalyst and method for preparing 2-methyl-2,4-pentanediol by diacetone alcohol hydrogenation
  • Catalyst and method for preparing 2-methyl-2,4-pentanediol by diacetone alcohol hydrogenation

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Embodiment

[0044] The present invention will be described in further detail below in conjunction with specific examples. In the following examples, unless otherwise specified, the methods used are conventional methods, and the reagents used can be obtained from commercial sources. The embodiments described below are exemplary, and are only for explaining the present invention, and should not be construed as limiting the present invention.

preparation example

[0046] The loaded metal catalyst used in the present invention can be prepared as follows:

[0047] Ruthenium supported catalyst: use 50-150mL of RuCl with a concentration of 0.126-1.265mg / mL in a 250mL round bottom flask 3 ·xH 2 A solution of O in acetone (purchased from Aladdin Reagent Co., Ltd.) impregnated 0.50-1.00 g of apatite carrier such as Ca 5 (PO 4 ) 3 (OH), Mg 2 Ca 3 (PO 4 ) 3 (OH), Ce 5 (VO 4 ) 6 (OH) 2 , Ca 5 (PO 4 ) 3 (HCO 3 ), Ca 5 (PO 4 ) 3 F or Na 10 (PO 4 ) 3 (OH) etc. (purchased from Aladdin Reagent Co., Ltd.), stirred by a magnetic stirrer for 12-24h to reach adsorption equilibrium, vacuum pumped and washed with acetone, dried in a drying oven at 20-100°C for 6-12h, and then used The tubular reduction furnace uses H at 150-400°C 2 After reduction for 1-6 hours, a supported ruthenium catalyst with ruthenium in Table 1 at 0.5% by weight to 5% by weight was obtained.

[0048] Palladium-loaded catalyst: 50-150 mL of Pd(OAC) with a concen...

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Abstract

The invention provides a catalyst and a method for preparing 2-methyl-2,4-pentanediol by diacetone alcohol hydrogenation. The method includes that diacetone alcohol and hydrogen are subjected to reaction in the presence of a catalyst to generate 2-methyl-2,4-pentanediol, wherein the catalyst is a supported metal catalyst formed by loading of an active metal component on a hydroxyapatite carrier. The method can be implemented in an environment-friendly solvent as well as under a solvent-free condition, and the conversion rate of diacetone alcohol in preparation of 2-methyl-2,4-pentanediol is up to 100%; a reaction process for preparing 2-methyl-2,4-pentanediol from diacetone alcohol is simple, and simple equipment, simplicity and convenience in operation and mild reaction conditions are realized; the catalyst is simple in preparation and low in cost, large-scale production can be realized, and the catalyst prepared according to an ion exchange method is high in hydrothermal stability and recyclability; reaction products can be easily separated from the catalyst and a solvent system, and short reaction period, suitableness for industrial production and a promising application prospect are realized.

Description

technical field [0001] The invention relates to the field of organic catalytic synthesis, and more specifically relates to a method and a catalyst for preparing 2-methyl-2,4-pentanediol through hydrogenation of diacetone alcohol. Background technique [0002] 2-Methyl-2,4-pentanediol is a colorless transparent slightly viscous liquid with a slightly fresh sweet smell, soluble in water, alcohol, ether and lower aliphatic hydrocarbons. It is completely miscible with water, has strong solubility in high-grade organic solvents, and has good dispersion ability for organic matter. 2-Methyl-2,4-pentanediol is a fine chemical product with a wide range of uses. It is widely used in building materials, cosmetics, textiles, pesticides, coatings, biochemical engineering, organic synthesis and other fields. It is mainly used as a solvent, coupling agent, emulsifier, penetrant, stabilizer, etc. 2-Methyl-2,4-pentanediol is used as a coupling agent to form a stable protease solution in th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/145B01J27/18B01J27/185C07C31/125
CPCB01J27/1817B01J27/1853B01J27/1856C07C29/145C07C31/125
Inventor 张颖李闯
Owner UNIV OF SCI & TECH OF CHINA
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