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A kind of diacetone alcohol hydrogenation catalyst and its preparation method and application

A diacetone alcohol and catalyst technology, applied in molecular sieve catalysts, chemical instruments and methods, preparation of hydroxyl compounds, etc., can solve the problems of harsh reaction conditions, difficult separation of catalysts and products, unsuitability for pilot scale-up and industrial production, and achieve high The effect of activity stability

Active Publication Date: 2017-05-17
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0014] The above patent documents prepare isohexanediol by hydrogenation of diacetone alcohol in a batch reaction mode, adopt Ni series catalysts or add basic compounds in Ni series catalysts, the catalyst preparation method is more complicated, the reaction conditions are harsh, the catalyst is expensive, and the production capacity Small, not suitable for pilot scale-up and industrial production; and this batch process has problems such as difficult separation of catalyst and product, low yield, etc.

Method used

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  • A kind of diacetone alcohol hydrogenation catalyst and its preparation method and application
  • A kind of diacetone alcohol hydrogenation catalyst and its preparation method and application

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preparation example Construction

[0032] The preparation method of modified Y molecular sieve of the present invention specifically comprises the following steps:

[0033] (1) Take an appropriate amount of ammonium fluoroborate crystals, gradually add them into distilled water stirred at a temperature of 30-60°C, filter out impurities in the solution, and prepare a clear, transparent and stable ammonium fluoroborate solution.

[0034] (2) Take an industrially produced low-sodium Y molecular sieve with a sodium oxide content of 0.5~2.0wt%, put it into the ammonium fluoroborate solution under stirring, the solid-liquid ratio is 3:1~10:1, and the temperature of the solution rises to 80~100°C , you can turn on the ultrasonic instrument, place the mixed slurry under ultrasonic irradiation, the ultrasonic frequency is 40-100kHz, and the power is 2-40W / m according to the volume of the solution. The following dealumination and boron supplementation reactions occur in the slurry system:

[0035] NH 4 BF 4 +Al 3+ +N...

Embodiment 1

[0040] Measure 219.0 g of ammonium fluoroborate and gradually add it into 2000 mL of distilled water under stirring at 50°C to prepare an aqueous solution of ammonium fluoroborate. Get 500g industrial production low-sodium ammonium Y molecular sieve (Na 2 The O content is 1.1%, the crystallinity is 102%, and the unit cell constant is 2.475nm), molecular sieves are gradually added to the stirred ammonium fluoroborate aqueous solution, the temperature of the slurry is increased to 95°C, and the treatment is 60 minutes; first, the slurry is mixed with solid particles (fluoroaluminum Sodium acid) separation, and then solid-liquid separation, the filter cake was dried at 120 ° C for 6 hours; take the above 500g molecular sieve, and 200mL organic silicone oil ethanol solution (concentration 18.4gSiO 2 / 100mL) evenly sprayed onto the molecular sieve. Dry the impregnated molecular sieve at a temperature of 80°C for 3 hours; carry out a hydrothermal treatment of the molecular sieve co...

Embodiment 2

[0042] Change the low-sodium ammonium Y in Example 1 to SSY molecular sieve, adjust the concentration of ammonium fluoroborate solution to 15.2g / 100mL, make the beating solid-liquid ratio 1:5, beating temperature 70°C, beating time 2h, organic silicon into silicon oxide Alkane, other with example 1, numbering is BCY-2.

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Abstract

The invention disclose a diacetone alcohol hydrogenation prepared iso-hexylene glycol catalyst which comprises an active component nickel and a modified Y molecular sieve, wherein the mass ratio of the active component nickel to the modified Y molecular sieve in oxide is (15:85)-(45: 55), preferably (20:80)-(35:65); the properties of the modified Y molecular sieve are as follows: the specific surface area is 500-900 m<2> / g and preferably 600-800 m<2> / g, the total pore volume is 0.20-0.6 ml / g, the average pore size is 1.9-3.0 nm, the relative crystallinity is 80-110%, the mole ratio of silicon to aluminum is 3-30 and preferably 10-20, the cell parameter is 2.425-2.445 nm, the proportion of medium-strong acid is 50-90%, and the boric oxide content is less than or equal to 4.0wt% and preferably less than or equal to 2.5wt%. The catalyst can be applied to the fixed bed process, shows excellent high activity and stability in long-period running process and can be used for continuously and stably producing iso-hexylene glycol.

Description

technical field [0001] The invention relates to a diacetone alcohol hydrogenation catalyst and its preparation method and application, in particular to a diacetone alcohol hydrogenation preparation isohexanediol catalyst and its preparation method and application. Background technique [0002] Isohexanediol (2-methyl-2,4-pentanediol, methylpentanediol-2,4, referred to as MPD) is a widely used fine chemical product, in building materials, cosmetics, textiles, pesticides, coatings , biochemical engineering, organic synthesis and other fields have been widely used, mainly used as solvents, coupling agents, emulsifiers, penetrants, stabilizers, etc. [0003] As a coupling agent, MPD can form a stable protease solution when used in the protease active composition solution. It has tough elasticity, high hardness, wear resistance and weather resistance coating made of PVC, ABS polyacrylate and other resins. It has been used in the fields of construction and shipbuilding; MPD is a ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/14C07C31/20C07C29/145
Inventor 李花伊霍稳周刘野魏晓霞田丹
Owner CHINA PETROLEUM & CHEM CORP