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Regeneration method of catalyst for preparation of unsaturated acid or unsaturated acid ester

A technology for regenerating catalysts and catalysts, applied in molecular sieve catalysts, chemical instruments and methods, catalyst regeneration/reactivation, etc., can solve problems such as inability to meet large-scale production, easy loss of active components, and complex influencing factors, and achieve good industrial applications. Prospect, easy separation, simple effect of industrial preparation

Active Publication Date: 2018-06-01
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Most of the catalysts used in the above studies are basic catalysts or acid-base bifunctional catalysts. The preparation process generally uses methods such as impregnation, ion exchange, and co-precipitation to load the active components on the carrier. There are cumbersome preparations, complex influencing factors and The shortcomings of low repeatability and easy loss of active ingredients cannot meet the needs of industrial mass production

Method used

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  • Regeneration method of catalyst for preparation of unsaturated acid or unsaturated acid ester
  • Regeneration method of catalyst for preparation of unsaturated acid or unsaturated acid ester
  • Regeneration method of catalyst for preparation of unsaturated acid or unsaturated acid ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0080] Preparation of H-MOR catalyst

[0081] 100 grams of roasted Na-ZSM-35 molecular sieves purchased from Shanghai Zhuoyue Chemical Technology Co., Ltd. with an atomic silicon-aluminum ratio of 25 were exchanged three times with 1mol / L ammonium nitrate for 2 hours each time, washed with deionized water, and dried , calcined at 550°C for 4 hours, and then extruded to prepare a 20-40 mesh catalyst, named as 1# catalyst.

[0082] Fill 5g of 1# catalyst into the fixed bed reactor for pretreatment. Catalyst pretreatment conditions are: N 2 The flow rate is 30mL / min, starting from 25°C over 150min to 500°C, and maintaining at 500°C for 180min. A mixture of methylal (DMM) and methyl acetate (MAc) carried by nitrogen gas was passed through the reactor at a temperature of 250° C., a pressure of 5 MPa, and a space velocity of 2400 mL / g / h. Wherein the gas flow rate is 200mL / min, and the molar ratio DMM / MAc=2 / 1. The results of the catalyst reaction and the regeneration results are...

Embodiment 2

[0086] Ga-ZSM-35 catalyst

[0087] 50g Ga(NO 3 ) 3 Dissolve in 90mL deionized water to make the corresponding nitrate aqueous solution. Add 100 g of the 1# catalyst prepared in Example 1 into the above-mentioned nitrate aqueous solution, let it stand for 24 hours, then separate and wash with deionized water, and the obtained sample is dried in an oven at 120° C. for 12 hours, and the dried sample is placed in a horse In a Furnace, heat up to 550°C at a heating rate of 2°C / min, roast for 4 hours, then exchange with 1mol / L ammonium nitrate three times, each time for 2 hours, wash with deionized water, dry, and roast at 550°C for 4 hours, Prepared by extrusion into 20 to 40 mesh catalyst, named as 2# catalyst.

[0088] Fe-ZSM-35 catalyst

[0089] 22g Fe(NO 3 ) 3 Dissolve it in 90mL of deionized water to prepare the corresponding nitrate aqueous solution. The rest of the operations are the same as that of the 2# catalyst. The obtained 20 to 40 mesh catalyst is named as t...

Embodiment 3

[0094] H-ZSM-5 catalyst molding

[0095] Take 80g Na-ZSM-35 with an atomic silicon-aluminum ratio of 2.5, mix 28g pseudoboehmite with 10% dilute nitric acid and extrude into strips, after roasting, exchange with 1mol / L ammonium nitrate three times, each time for 2 hours, Wash with deionized water, dry, and bake at 550° C. for 4 hours to obtain a catalyst, which is named 4# catalyst.

[0096] Take 80g Na-ZSM-35 with an atomic silicon-aluminum ratio of 15, mix 20g magnesium oxide with 10% dilute nitric acid and extrude it into a strip. After roasting, exchange it with 1mol / L ammonium nitrate three times for 2 hours each time. Washed with water, dried, and calcined at 550° C. for 4 hours to obtain a catalyst named as 5# catalyst.

[0097] 1g of 4# catalyst and 5# catalyst were respectively packed into the fixed bed reactor for pretreatment. Catalyst pretreatment conditions are: N 2 The flow rate is 30mL / min, starting from 25°C over 150min to 500°C, and maintaining at 500°C f...

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Abstract

The invention relates to a regeneration method of a catalyst for preparation of unsaturated acid or unsaturated acid ester. The method comprises the step of regenerating the catalyst at a temperatureof 250-600 DEG C in an atmosphere containing hydrogen.

Description

technical field [0001] The invention relates to a method for regenerating a catalyst for the preparation of unsaturated acids or unsaturated esters. Background technique [0002] Acrylic acid and methyl acrylate are important chemical raw materials, which can be used as coatings, flocculants, dispersants and binders, and are widely used in construction, water treatment, daily chemical, soil treatment and leather industries. People's daily life is closely related. At present, the most commonly used method in the industry to prepare acrylic acid and methyl acrylate is the two-stage oxidation of propylene, that is, the first step of oxidizing propylene to acrolein, and further oxidation to obtain acrylic acid. However, the raw material propylene comes from petroleum, which is a non-renewable resource and does not conform to the concept of sustainable development. [0003] With the rapid development of C1 chemistry, there is an overcapacity of acetic acid and methyl acetate. ...

Claims

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Application Information

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IPC IPC(8): C07C51/353C07C57/04C07C67/24C07C69/54B01J29/90B01J29/65B01J29/68B01J29/40B01J38/10
CPCB01J29/40B01J29/65B01J29/655B01J29/68B01J29/90B01J38/10C07C51/353C07C67/24C07C57/04C07C69/54Y02P20/584
Inventor 马占玲朱文良马现刚刘红超刘勇倪友明刘世平陈其伟刘中民
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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