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Preparation method and application of vanadyl phosphate catalyst

A technology of vanadyl phosphate catalyst and vanadium source, which is applied in the fields of vanadyl phosphate catalyst, vanadyl phosphate catalyst preparation, and deep eutectic solvent enhanced preparation, and can solve the loss cost of additive elements, complicated preparation process, and low reaction yield etc. to achieve the effects of increased selectivity and conversion rate, simple operation, and simple synthesis

Active Publication Date: 2018-07-06
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The method of the present invention uses a cheap, non-toxic deep eutectic solvent to assist in the synthesis of the vanadyl phosphate catalyst, can prepare the vanadyl phosphate catalyst in an environmentally friendly manner, and can overcome the traditional reliance on noble metals to improve its performance, secondary pollution, high cost, and difficult preparation process Complicated and other disadvantages
When the catalyst is used to catalyze the reaction of n-butane selective oxidation to maleic anhydride, it improves the low yield of n-butane selective oxidation of maleic anhydride, catalyst selectivity, low conversion rate, loss of additive elements and cost in the prior art. advanced questions

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  • Preparation method and application of vanadyl phosphate catalyst
  • Preparation method and application of vanadyl phosphate catalyst
  • Preparation method and application of vanadyl phosphate catalyst

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preparation example Construction

[0022] The embodiment of the present invention provides a kind of preparation method of vanadyl phosphate catalyst, it comprises the following steps:

[0023] (1) Vanadium source, deep eutectic solvent, benzyl alcohol and C 3 ~C 8 The monohydric alcohol is mixed, obtains compound, reacts, and wherein, described deep eutectic solvent is: the deep eutectic solvent that choline chloride and organic polyhydric alcohol form;

[0024] (2) Mix the reaction product obtained in step (1) with the phosphorus source, raise the temperature to 100°C to 200°C, and continue the reaction to obtain the vanadyl phosphate precursor;

[0025] (3) Roasting to obtain the vanadyl phosphate catalyst.

[0026] Among the present invention, the deep eutectic solvent that described deep eutectic solvent choline chloride and organic polyhydric alcohol forms is referred to as choline chloride-organic polyhydric alcohol deep eutectic solvent, the low eutectic solvent that choline chloride and organic polyh...

Embodiment 1

[0063] Preparation of vanadyl phosphate catalyst:

[0064] (1) Weigh 10g V 2 o 5 Place in a 250mL three-necked flask, add a mixture of 1g choline chloride-ethylene glycol deep eutectic solvent, 80mL isobutanol and 20mL benzyl alcohol, stir and mix evenly, reflux at 135°C for 3h and then cool down to 60°C .

[0065] (2) Slowly add 7.53mL of 85% H 3 PO 4 , and continued to reflux for 16 hours at a temperature of 135° C. Filter and wash with absolute ethanol to obtain a blue precipitate, and dry it in air at 120° C. for 24 hours to obtain a catalyst precursor powder.

[0066] (3) The obtained catalyst precursor powder was pressed into tablets under a pressure of 15 MPa, crushed, and 20-40 mesh catalyst particles were sieved.

[0067] (4) Afterwards, the catalyst particles were activated in situ at a rate of 2°C / min to 430°C for 12 hours in an atmosphere of n-butane / oxygen / nitrogen reaction gas with a volume ratio of 1.5:17:81.5 to obtain phosphoric acid oxygen Vanadium cat...

Embodiment 2

[0072] Preparation of acid vanadyl catalyst:

[0073] (1) Weigh 10g V 2 o 5 Place in a 250mL three-neck flask, add a mixture of 1g choline chloride-butanediol deep eutectic solvent, 80mL isobutanol and 20mL benzyl alcohol, stir and mix evenly, reflux at 135°C for 3h and then cool down to 60°C .

[0074] (2) Slowly add 7.53mL of 85% H 3 PO 4 , and continued to reflux for 16 hours at a temperature of 135° C. Filter and wash with absolute ethanol to obtain a blue-black precipitate, and dry it in air at 120° C. for 24 hours to obtain a catalyst precursor powder.

[0075] (3) The obtained catalyst precursor powder was pressed into tablets under a pressure of 15 MPa, crushed, and 20-40 mesh catalyst particles were sieved.

[0076] (4) Afterwards, the catalyst particles were activated in situ from room temperature to 430° C. for 12 hours at a rate of 2° C. / min under a reaction gas atmosphere to obtain a vanadyl phosphate catalyst.

[0077] Detection:

[0078] Take by weighing...

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Abstract

The invention relates to a vanadyl phosphate catalyst, an intensified preparation method by low congruent melting solvent, and application of the vanadyl phosphate catalyst. The method comprises the following steps: 1) mixing a vanadium source, low congruent melting solvent, benzyl alcohol and C3-C8 monohydric alcohol to obtain mixed materials, and reacting, wherein the low congruent melting solvent is formed by choline chloride and organic polyhydric alcohols; 2) mixing a reaction product obtained in 1) with a phosphorus source, raising the temperature to 100-200DEG C, and continuously reacting to obtain a vanadyl phosphate precursor; 3) roasting to obtain the vanadyl phosphate catalyst. The method is characterized in that green and low-price low congruent melting solvent is subjected tointensified preparation to obtain the vanadyl phosphate catalyst, the defects of secondary pollution, high cost, complex preparation process and the like since the performance of the vanadyl phosphatecatalyst is improved on the basis of noble metal are overcome. When the vanadyl phosphate catalyst is used for catalytic normal butane selectivity oxidation maleic anhydride reaction, the difficulties including low yield, poor selectivity and the like, are solved, and defects of high cost and serious pollution in a traditional catalyst improvement method are overcome.

Description

technical field [0001] The invention belongs to the field of chemical catalysis, and relates to a preparation method and application of a vanadyl phosphate catalyst, in particular to a vanadyl phosphate catalyst, a method for strengthening the preparation by using a deep eutectic solvent, and an application thereof. Background technique [0002] Due to the low price and low environment of alkane, it is a raw material with great potential in the preparation of high value-added chemicals. So far, the selective oxidation of butane to maleic anhydride using vanadium phosphorus oxygen catalyst is the only process that has been successfully industrialized. [0003] So far, the main reason restricting the performance improvement of vanadium phosphorus oxygen catalyst is that the catalyst will be deeply oxidized during use. It is generally believed that the active phase (VO) of the catalyst 2 P2O 7 is made from the precursor VOHPO 4 2H 2 O is transformed by activation, during w...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/198B01J35/10B01J37/00C07D307/60
CPCC07D307/60B01J23/002B01J27/198B01J37/0009B01J35/61
Inventor 刘瑞霞贺滨张瑞锐陈雪景代飞张锁江
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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