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Two-step-method hydrogenation process for preparing neopentyl glycol

A technology of neopentyl glycol and hydrogenation reaction, applied in the preparation of hydroxyl compounds, preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of increasing methanol energy consumption, decreasing HPA yield, etc. The effect of strong anti-toxic ability and low price

Active Publication Date: 2011-11-23
SHANGHAI HUAYI ENERGY CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Yet even if adopting the method for vacuum distillation, it is also difficult to completely remove catalysts such as triethylamine in the solution obtained by acetal, if adopt methods such as crystallization, extraction to purify HPA from the solution obtained by acetal, the yield of HPA will be relatively low big drop
Similarly, this patent also introduces methanol as a solvent, which increases the energy consumption of recycling methanol

Method used

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  • Two-step-method hydrogenation process for preparing neopentyl glycol
  • Two-step-method hydrogenation process for preparing neopentyl glycol
  • Two-step-method hydrogenation process for preparing neopentyl glycol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0069] Carry out the hydrogenation reaction of HPA in continuous spray bed reactor, experiment arrangement is as follows:

[0070] Reactor: stainless steel tubular reactor with an inner diameter of 10mm and a length of 400mm;

[0071] Catalyst: Cu-Zn-Al, prepared by co-precipitation method, the molar ratio of copper and aluminum in the catalyst is 1.0:1.34; the molar ratio of copper and zinc is 1.0:0.55, and the catalyst is crushed to 20-40 mesh

[0072] Feed: Crude HPA without any purification operations from the acetalization reaction catalyzed with triethylamine

[0073] Solvent: a mixture of main components NPG and water (from hydrogenation product return)

[0074] Catalyst dosage: 2.56g

[0075] Liquid feed rate: 23.3g / hr

[0076] Liquid hourly space velocity: WHSV=9.1g / gcat / hr

[0077] HPA liquid hourly space velocity: 1.0g / gcat / hr

[0078] Temperature: 141°C

[0079] Pressure: 3.5MPa

[0080] Mode of operation: The feed is continuously pumped through the reactor ...

Embodiment 2

[0088] Carry out the hydrogenation reaction of HPA in continuous spray bed reactor, experiment arrangement is as follows:

[0089] Reactor: stainless steel tubular reactor with an inner diameter of 10mm and a length of 400mm;

[0090] Catalyst: Cu-Zn-Al-Mn, prepared by co-precipitation method, containing 39.7wt% of copper oxide, 21.0wt% of zinc oxide,

[0091] Aluminum oxide 34.1wt%, manganese oxide 5.2%, catalyst crushed to 20-40 mesh;

[0092] Feed material: crude HPA solution without any purification operation obtained from the acetal reaction of isobutyraldehyde and formaldehyde, the acetal reaction is catalyzed by triethylamine;

[0093] Solvent: a mixture of main components NPG and water (from hydrogenation product return);

[0094] Catalyst dosage: 2.52g;

[0095] Temperature: 135°C;

[0096] Pressure: 3.5;

[0097] Liquid feed rate: 4.6g / hr;

[0098] Airspeed: WHSV=1.84g / gcat / hr

[0099] HPA liquid hourly space velocity: 0.2g / gcat / hr

[0100] Mode of operation:...

Embodiment 3

[0108] Equivalent to the first hydrogenation reactor as described in Example 1, the hydrogenation product obtained from Example 1 is distributed as follows: about 85 wt% is directly mixed with the reaction solution obtained from the acetal reaction of isobutyraldehyde and formaldehyde, It is formulated as raw material for the first hydrogenation reactor, and the rest enters the second hydrogenation reactor for further hydrogenation conversion.

[0109] table 3

[0110]

[0111]

[0112] The second hydrogenation reactor experimental arrangement is as follows:

[0113] Carry out the hydrogenation reaction of HPA in the continuous spray bed reactor;

[0114] Reactor: stainless steel tubular reactor with an inner diameter of 10mm and a length of 400mm;

[0115] Catalyst: Cu-Zn-Al-Mn, prepared by co-precipitation method, the catalyst contains 39.7wt% copper oxide, 21.0wt% zinc oxide, 34.1wt% aluminum oxide, 5.2% manganese oxide, and the catalyst is crushed to 20-40 mesh;

...

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Abstract

The invention provides a two-step-method hydrogenation process for preparing neopentyl glycol. The two-step-method hydrogenation process for preparing the neopentyl glycol comprises the following steps of: inputting a solution containing hydroxyl pivalaledhyde (HPA) into a hydrogenation procedure and carrying out a hydrogenation reaction on the solution containing the HPA and hydrogen gas under the effect of a hydrogenation catalyst to obtain a solution containing a neopentyl glycol product, wherein the hydrogenation procedure comprises a first hydrogenation reactor and a second hydrogenation reactor which are connected in series, the catalyst which is filled into the first hydrogenation reactor comprises three metal elements, such as copper, zinc and aluminum, and the catalyst which is filled into the second hydrogenation reactor comprises four metal elements, such as copper, zinc, aluminum and manganese. According to the process provided by the invention, the HPA of the HPA solution obtained condensation can be almost completely transformed in the hydrogenation procedure by utilizing a second-grade hydrogenation process with serial connection of copper-zinc-aluminum and copper-zinc-aluminum-manganese; and the HPA has a higher selectivity of NPG (Neopentyl Glycol) and the selectivity can be not less than 97%.

Description

technical field [0001] The invention relates to a method for preparing neopentyl glycol, in particular to a two-step hydrogenation process for preparing neopentyl glycol by catalytic hydrogenation of hydroxypivalaldehyde. Background technique [0002] Neopentyl glycol is an important chemical intermediate. Neopentyl glycol is mainly used in the production of oil-free alkyd resins, polyester powder coatings, unsaturated polyester resins, printing inks, synthetic plasticizers and aviation lubricants. It has good thermal stability, acid resistance, alkali resistance and weather resistance. Widely used in coatings, construction and insulation materials industries, 80% of the world's neopentyl glycol is used in the coatings industry. [0003] Neopentyl glycol is usually produced industrially by two methods: disproportionation and condensation hydrogenation. The disproportionation method is to use a strong basic catalyst, such as sodium hydroxide, potassium hydroxide or calcium ...

Claims

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Application Information

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IPC IPC(8): C07C31/20C07C29/141
Inventor 金生亚蒋文张佶璘陈建伟
Owner SHANGHAI HUAYI ENERGY CHEM
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