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Preparation method of catalyst for coproducing isopropanol and methyl isobutyl ketone by acetone hydrogenation

A technology of methyl isobutyl ketone and catalyst, applied in the field of catalysis, can solve problems such as high cost, reduce MIBK production cost, and easy loss of active components, achieve stable performance, overcome the easy loss of precious metal palladium, and have good industrial application prospects Effect

Active Publication Date: 2012-12-05
CHINA NAT OFFSHORE OIL CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The use of non-precious metal nickel as the active component overcomes the disadvantages of easy loss of active components and high cost of palladium-based catalysts, and can greatly reduce the production cost of MIBK; in addition, due to the use of inorganic carriers, there is no Pd / resin catalyst in the initial stage of operation. Corrosion of equipment caused by loss of acid radicals

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Prepare catalyst of the present invention

[0029] Mix 200g of alumina and 4g of methyl cellulose for 30 minutes, add 170mL of 3wt% dilute nitric acid solution, mix for 20 minutes, roll the ball in a granulator to form a 3mm ball, dry at 120°C for 12 hours, and roast at 650°C for 4 hours. Alumina carrier was prepared; then 210g of magnesium nitrate was dissolved in deionized water to make 200mL clear solution, impregnated with alumina carrier, dried at 120°C for 12 hours, and roasted at 480°C for 3 hours to obtain a semi-finished catalyst; then 356g of nitric acid Nickel was dissolved in 800 grams of deionized water to prepare a nickel nitrate solution, and the semi-finished catalyst was impregnated twice. The excess filtrate filtered out could be used as an impregnation solution again next time. After each impregnation, it was dried at 120°C for 12 hours, and roasted at 450°C for 3 hours. Hours, the finished catalyst is finally obtained.

[0030] The catalyst prepared...

Embodiment 2~6

[0033] Other catalysts B to F were prepared according to the method of Example 1, except that the calcination temperature of the carrier and the concentration of the metal salt in the impregnation solution were changed. The catalyst preparation conditions and component contents are shown in Table 1.

[0034] Table 1

[0035] example Catalyst number Nickel content, wt% Magnesium content, wt% Carrier calcination temperature, ℃ Carrier roasting time, hours Calcination temperature after impregnating magnesium nitrate, ℃ Calcination temperature after impregnating nickel nitrate, ℃ 2 B 11.8 3.6 680 3 480 380 3 C 14.6 3.9 650 6 450 380 4 D 15.9 5.2 700 5 450 420 5 E 17.2 6.5 720 5 420 400 6 F 17.5 7.1 725 4 475 445

[0036] Catalysts B~F were loaded into a fixed-bed reactor and reduced in a hydrogen flow. After reduction, the hydrogenation performance of the catalyst was evaluated under selected reactio...

Embodiment 7

[0044] Activity stability evaluation experiment

[0045] 100 mL of Catalyst A was loaded into a 100 mL fixed-bed reactor respectively, and technical grade acetone was used as raw material, and the acetone content was 98 wt%. The catalyst is first subjected to reduction treatment, the reduction condition is pressure 0.5MPa, temperature 380°C, time 8 hours, reduction atmosphere is H 2 / N 2 The mixed gas, the hydrogen content is 20.0v%, the flow rate of the reducing gas is 200mL / h; after the reduction, the acetone raw material is passed into the hydrogenation reaction, the total reaction pressure is 1.5MPa, the temperature is 140 °C, and the liquid hour volume of the acetone feed Airspeed 1.5h -1 , The volume ratio of hydrogen and acetone is 200, and a long-term operation test of 2000 hours is carried out.

[0046] The test results show that the conversion rate of acetone and the yield of products isopropanol and MIBK are kept very stable, and the activity of the catalyst does...

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PUM

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Abstract

The invention relates to a preparation method of a catalyst for coproducing isopropanol and methyl isobutyl ketone by acetone hydrogenation. The catalyst comprises an alumina carrier and Ni and Mg loaded on the gamma-Al2O3 carrier, and particularly comprises, by total weight, 10-18% of the Ni, 3-8% of the Mg and the balance alumina; and the BET specific surface area of the catalyst ranges from 100m<2> / g to 180m<2> / g, and the pore volume of the catalyst ranges from 0.35mL / g to 0.55mL / g. The preparation method includes steps of (1), preparing the carrier by details of weighing pseudo-boehmite powder, adding binders and extrusion assistants into the pseudo-boehmite powder, forming by strip extrusion or granulating by rotation, drying and calcining, cooling to reduce temperature so as to obtain the stripped or spherical carrier; (2), impregnating the carrier into magnesium nitrate by details of loading a magnesium additive onto the carrier by means of saturated impregnation, drying and then calcining for 2-6 hours at the temperature ranging from 400 DEG C to 500 DEG C; (3), loading the actively metallic nickel by details of impregnating for 10-24 hours and calcining for 2-6 hours at the temperature ranging from 350 DEG C to 480 DEG C; and (4), loading the actively metallic nickel again by details of drying a semi-finished product, impregnating the dried semi-finished product into impregnation liquid of nickel nitrate again, repeating the step (3) once, and calcining the semi-finished product for 2-4 hours at the temperature ranging from 400 DEG C to 450 DEG C so as to obtain the finished catalyst.

Description

technical field [0001] The invention belongs to the technical field of catalysis; it is a method for preparing a catalyst for acetone hydrogenation to co-produce isopropanol and methyl isobutyl ketone, more specifically, the invention relates to acetone hydrogenation with nickel as the main active component of the catalyst The preparation method of the catalyst for the hydrogen synthesis of isobutanol and methyl isobutyl ketone. Background technique [0002] Isopropanol is an important chemical product and raw material. It is mainly used as dehydrating agent and cleaning agent in pharmaceutical, cosmetics, plastics, spices, coatings and electronic industries. Isopropanol is used as a low-cost solvent and as an extractant in many industrial and consumer products. Isopropanol is also used as a solvent for oils and colloids, and in the manufacture of fishmeal feed concentrates. Additionally, low-quality isopropanol is used in automotive fuel. The production of isopropanol c...

Claims

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Application Information

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IPC IPC(8): B01J23/755C07C31/10C07C29/145C07C49/04C07C45/73C07C27/00
Inventor 南军于海斌张景成张玉婷耿姗刘新普曲晓龙
Owner CHINA NAT OFFSHORE OIL CORP
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