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Catalyst for decarboxylation of levulinic acid, preparation method of catalyst, and method for preparing butanone through selective decarboxylation of levulinic acid

A technology of levulinic acid and catalyst, which is applied in the direction of catalyst activation/preparation, molecular sieve catalyst, and carbon-based compound preparation. It can solve the problems of low product yield and difficult recovery, and achieve high yield, high catalytic efficiency, and simple treatment. Effect

Pending Publication Date: 2022-02-18
PETROCHINA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] The main purpose of the present invention is to provide a kind of catalyst for decarboxylation of levulinic acid and preparation method thereof, the method for the selective decarboxylation of levulinic acid to prepare methyl ethyl ketone, to overcome the difficulty of recovery of levulinic acid decarboxylation catalyst in the prior art, need to The reaction is carried out in the buffer solution system, and the defect of low product yield

Method used

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  • Catalyst for decarboxylation of levulinic acid, preparation method of catalyst, and method for preparing butanone through selective decarboxylation of levulinic acid
  • Catalyst for decarboxylation of levulinic acid, preparation method of catalyst, and method for preparing butanone through selective decarboxylation of levulinic acid

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Effect test

Embodiment 1

[0047] Catalyst preparation: the carrier (SAPO-11 molecular sieve, SAPO-34 molecular sieve, HY molecular sieve, H-β molecular sieve, H-USY molecular sieve, MCM-22 molecular sieve, MCM-41 molecular sieve, SBA-15 molecular sieve, H-ZSM-5 molecular sieve and silica gel) placed in a muffle furnace, heated from room temperature at 8-15°C / min to 350-500°C, kept for 1-5 hours for thermal activation treatment, taken out after cooling down, and passed through a 100-mesh sieve Sieve, and take by weighing the porous material carrier after the above-mentioned activation treatment of 1g in the 25ml beaker for subsequent use; According to the ratio of CuO and PbO in the embodiment and the loading capacity calculation on the carrier and weigh the precursor salt Cu(NO 3 ) 2 ·3H 2 O and PbCl 2 Place in a 25ml round bottom flask, add 4-20ml of ultra-pure water, and stir evenly in an oil bath at 90-150°C. After it is completely dissolved, pour the metal precursor salt solution drop by drop int...

Embodiment 2

[0049] Weigh 0.15g of levulinic acid into a 50mL beaker, dissolve it with ultrapure water, adjust its pH value to 5-6 with NaOH solution, and prepare 25ml of levulinic acid reaction solution. Weigh 0.03g of supported copper-based composite catalyst CuO-PbO(28:12) / H-β into a 50ml autoclave, and then add the above-mentioned levulinic acid reaction solution. Afterwards, the reactor was sealed, and the N 2 Replace the air in the reactor with air, set the stirring speed to 400r / min, turn on the condensed water, the heating program is to raise the temperature from room temperature to 280°C after 40min, and keep it for 1h. Condensate, sampled and pretreated. Using Waters high performance liquid chromatography (model Waters Alliance 2695 HPLC, HPX-87H chromatographic column) for quantitative analysis of raw materials and products, the conversion rate of levulinic acid was 93.56%, and the yield of butanone was 76.48%.

[0050] Catalyst preparation parameters: carrier activation tempe...

Embodiment 3

[0053] Weigh 0.25g of levulinic acid into a 50mL beaker, dissolve it with ultrapure water, adjust its pH value to 5-6 with NaOH solution, and prepare 25ml of levulinic acid reaction solution. Weigh 0.075g of supported copper-based composite catalyst CuO-PbO(30:15) / H-ZSM-5 into a 50ml autoclave, and then add the above-mentioned levulinic acid reaction solution. Afterwards, the reactor was sealed, and the N 2 Replace the air in the reactor with air, set the stirring speed to 400r / min, turn on the condensed water, the heating program is to raise the temperature from room temperature to 260°C after 40min, and keep it for 3.5h. and condensate, sampled and pretreated. Using Waters high performance liquid chromatography (model Waters Alliance 2695 HPLC, HPX-87H chromatographic column) for quantitative analysis of raw materials and products, the conversion rate of levulinic acid was 91.45%, and the yield of butanone was 69.23%.

[0054] Catalyst preparation parameters: carrier activ...

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Abstract

The invention provides a catalyst for decarboxylation of levulinic acid, a preparation method of the catalyst, and a method for preparing butanone through selective decarboxylation of levulinic acid. The catalyst comprises a carrier and active components, wherein the active components are loaded on the carrier and comprise CuO and PbO. The preparation method comprises the following steps: dipping the carrier in a solution containing a copper precursor and a lead precursor, and carrying out ultrasonic treatment, drying and calcining successively to obtain the catalyst for decarboxylation of levulinic acid. According to the catalyst for decarboxylation of levulinic acid, the active components comprise copper oxide and lead oxide; and under the condition that a buffer solution system is not used, the reactant levulinic acid is allowed to be high in conversion rate, and the product butanone is allowed to be high in yield.

Description

technical field [0001] The invention relates to the technical field of bioenergy, in particular to a catalyst for decarboxylation of levulinic acid and a preparation method thereof, and a method for preparing methyl ethyl ketone through selective decarboxylation of levulinic acid. Background technique [0002] Levulinic acid (abbreviated as LA, with the following structural formula) is a biomass-based platform compound prepared by acid hydrolysis of renewable biomass resources, which provides a rich source of raw materials for the development of biomass-based chemicals. [0003] [0004] Butanone (MEK for short), also known as methyl ethyl ketone, methyl ethyl ketone or 2-butanone, has the following structural formula. It is a high-quality oxygenated solvent that is widely used. Extraction, paint, ink and various resin dissolution, oil extraction and refined azeotropic distillation, can also be used as a binder for dyes, a photolithography developer, a vulcanization accel...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/85B01J29/14B01J29/76B01J29/04B01J29/46B01J23/835B01J37/08B01J37/02C07C45/67C07C49/10
CPCB01J29/85B01J29/146B01J29/7615B01J29/7676B01J29/044B01J29/46B01J23/835B01J23/002B01J37/08B01J37/024B01J37/088C07C45/676B01J2229/186C07C49/10
Inventor 雪晶侯丹孙勇张鑫
Owner PETROCHINA CO LTD