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Preparation method of a catalyst for preparing neopentyl glycol by liquid-phase hydrogenation of hydroxypivalaldehyde

A technology of hydroxypivalaldehyde and neopentyl glycol, applied in the field of catalysis, can solve the problems of unmentioned catalyst strength and mechanical stability, unmentioned catalyst strength and loading, poor liquid resistance of copper-based catalysts, etc., and achieve Reduce the generation of tiny cracks, good liquid resistance, and low damage rate

Active Publication Date: 2016-05-18
WANHUA CHEM GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The catalyst disclosed in CN102728370A is composed of copper-zinc-aluminum-titanium-zirconium-hafnium-rhenium, which has high conversion rate and selectivity, but the strength and mechanical stability of the catalyst are not mentioned in the patent
CN102302937A discloses a copper-zinc-aluminum-manganese catalyst used to catalyze the hydrogenation of HPA to prepare NPG. The catalyst has high activity and good stability. At the same time, it also has good hydrogenation ability for hydroxypivalate hydroxypivalate and can tolerate a small amount of Acetal reaction catalysts such as triethylamine, the strength and loading of the catalyst after the reaction are not mentioned in the patent
[0006] In the prior art, the copper-based catalysts used for hydrogenation reactions need to go through the process of storage, filling, heating reduction, reaction, etc. from preparation to use, and are affected by various internal or external forces. When they are used in liquid phase reactions , but also due to liquid immersion, swelling and other reasons, the actual use strength of the catalyst will be greatly reduced, resulting in the catalyst being easily broken and pulverized in the liquid phase hydrogenation system, causing reactor blockage, threatening the stable operation of industrial devices, and affecting the life of the catalyst
[0007] In the prior art, the conventional copper-based catalyst prepared by the precipitation method has poor liquid resistance, and the catalyst is easily broken and pulverized during operation in the reactor, which will greatly affect the stable operation of the device

Method used

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  • Preparation method of a catalyst for preparing neopentyl glycol by liquid-phase hydrogenation of hydroxypivalaldehyde
  • Preparation method of a catalyst for preparing neopentyl glycol by liquid-phase hydrogenation of hydroxypivalaldehyde

Examples

Experimental program
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Embodiment 1

[0040] Add 3kg of water into the reaction kettle, and add 19.5g of nano-titanium oxide with a particle size of 20-40nm, and stir evenly. 384.1g copper nitrate, 619.3g aluminum nitrate, 90.8g zinc nitrate, 2.92g stannous chloride, 51.4g calcium nitrate were dissolved in 2.7kg water to make mixed salt solution, and sodium carbonate was dissolved in water to make 20wt% carbonic acid Sodium solution, respectively, the two solutions were heated to 60 ℃. The method of co-precipitation was adopted, and the two solutions were dropped into the reactor at the same time, and the temperature in the reactor was controlled to be 60° C., the pH of the system was 6.0, and the reaction time was 1 h during the precipitation process. After adding the mixed brine solution, use sodium carbonate solution to adjust the pH of the system to 7.5, and age at 70°C for 3h, then filter, wash and dry the filter cake at 110°C for 12h, and roast at 350°C for 3h to break Then press it into a 5*5mm cylinder (d...

Embodiment 2

[0044] Add 3kg of water into the reaction kettle, and add 11.7g of nano-titanium oxide with a particle size of 20-30nm, and stir evenly. 530.4g of copper nitrate, 358.6g of aluminum nitrate, 90.8g of zinc nitrate, 71.8g of magnesium nitrate, and 11.7g of stannous chloride were dissolved in 2.5kg of water to make a mixed salt solution, and sodium carbonate was dissolved in water to make 20wt% carbonic acid Sodium solution, the two solutions were heated to 80 ℃. The method of co-precipitation is adopted, and the two solutions are dropped into the reaction kettle at the same time, and the temperature in the kettle is controlled to be 80° C., the pH of the system is 5.5, and the reaction time is 1.5 hours during the precipitation process. After adding the mixed brine solution, adjust the pH of the system to 7.0 with sodium carbonate solution, and continue to age at 70°C for 3h, then filter, wash and dry the filter cake at 110°C for 12h, and roast at 500°C for 3h. The calcined cat...

Embodiment 3

[0047] Add 3 kg of water into the reaction kettle, and add 15.6 g of nano-zirconia with a particle size of 20-30 nm, and stir evenly. Dissolve 439.0g copper nitrate, 358.6g aluminum nitrate, 181.6g zinc nitrate, 33.2g barium nitrate, 5.84g tin protochloride in 2.5kg water to configure mixed brine solution, dissolve sodium carbonate in water to make 20wt% sodium carbonate solution, the two solutions were heated to 60 ° C. The method of co-precipitation was adopted, and the two solutions were dropped into the reactor at the same time, and the temperature in the reactor was controlled to be 60° C., the pH of the system was 5.5, and the reaction time was 2 hours during the precipitation process. After adding the mixed brine solution, adjust the pH of the system to 7.7 with sodium carbonate solution, and continue to age at 80°C for 3h, then filter, wash and dry the filter cake at 110°C for 12h, and roast at 650°C for 3h. The calcined catalyst was crushed and pressed into a 5*5mm c...

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Abstract

The invention relates to a preparation method of a catalyst for hydroxypivalaldehyde liquid phase hydrogenation preparation of neopentylene glycol. The catalyst comprises 20-65wt% of copper oxide, 15-50wt% of alumina, 2-25wt% of zinc oxide, 0.1-5wt% of tin oxide, 0.5-25wt% of alkaline earth oxide and 0-20wt% of titanium oxide and / or zirconia. The compounds containing copper, aluminum, zinc, tin and alkaline earth metal are mixed to form a mixture aqueous solution according to a certain ratio, the solution and an alkaline precipitant are added into a nanometer oxide-containing dispersion liquid in parallel, the mixture undergoes a precipitation reaction, the reaction product is aged and filtered, and the filter residues are washed, dried, roasted and compressed to form a molded catalyst. The catalyst prepared by the method has high activity and good selectivity in hydroxypivalaldehyde liquid phase hydrogenation preparation of neopentylene glycol, can promote 1115 ester conversion, can effectively improve liquid-repellency, and has high catalyst intensity and good stability.

Description

technical field [0001] The invention belongs to the technical field of catalysis, and in particular relates to a preparation method of a catalyst for preparing neopentyl glycol by liquid-phase hydrogenation of hydroxypivalaldehyde. Background technique [0002] Neopentyl glycol (NPG) is an important chemical intermediate, mainly used in the production of powder coatings, polyester resins, plasticizers, lubricating oil additives, water-soluble alkyd resins, etc., widely used in automobiles, textiles, medicine , coatings and petroleum and other fields; it can also be used for the selective separation of aromatics and cycloalkanes, and has a broad market prospect. [0003] At present, there are two methods for industrially producing neopentyl glycol: sodium formate method and catalytic hydrogenation method. The sodium formate method is that the hydroxypivalaldehyde (HPA) generated by formaldehyde and isobutyraldehyde undergoes a cross-Connizzaro reaction with formaldehyde unde...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/835B01J37/18C07C29/141C07C31/20
Inventor 李作金初乃波詹吉山尹育王同济何光文黎源华卫琦于方骁
Owner WANHUA CHEM GRP CO LTD
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