Catalyst for preparing 1,3-butadiene through ethanol condensation, preparation method of catalyst and application of catalyst

A catalyst and butadiene technology, applied in chemical instruments and methods, heterogeneous catalyst chemical elements, physical/chemical process catalysts, etc., can solve the problem of poor crystallization performance affecting catalytic performance, single catalyst components, and lack of active components and other problems, to achieve the effect of easy industrial scale-up, low cost and simple preparation method

Active Publication Date: 2016-03-23
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these catalyst components are relatively single (lack of synergistic effect of active components), or poor crystal

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] 1. Add Cu(NO 3 ) 2 ·3H 2 O, Mg(NO 3 ) 2 ·6H 2 O, Al(NO 3 ) 3 9H 2 O was made into a (0.5M, 1000ml) solution in a molar ratio of (Cu / Mg / Al=0.175 / 0.375 / 0.45), and the template agent F127 (F127 was 1% W / V) A solution was added.

[0042] 2. Na 2 CO 3 and NaOH (Na 2 CO 3 (1M)+NaOH(2M)) mixed solution B, about 800ml, requires (CO 3 2- / Al 3+ =3).

[0043] 3. At 80°C, add A and B dropwise to 1000ml of water at the same time, and adjust the pH to 9 with 2M NaOH solution.

[0044] 4. The aging time is 3 hours, and it is placed overnight at room temperature, and the obtained precipitate is filtered and washed with deionized water until the pH is 7.

[0045] 5. Vacuum dry at 60°C for 12 hours.

[0046] 6. Heat treatment at 500° C. for 5 hours in an air atmosphere to obtain sample 1, wherein the atomic percentage of Cu / Mg / Al=14.98 / 37.21 / 47.81.

[0047] 7. Put 1.5 ml of the catalyst prepared above into a reaction tube, and fill the upper and lower sides of the reac...

Embodiment 2

[0050] 1. Add Cu(NO 3 ) 2 ·3H 2 O, Mg(NO 3 ) 2 ·6H 2 O, Al(NO 3 ) 3 9H 2 O was made into a (0.5M, 1000ml) solution in a molar ratio of (Cu / Mg / Al=0.175 / 0.375 / 0.45), and the template agent F127 (F127 was 3% W / V) A solution was added.

[0051] 2. Na 2 CO 3 and NaOH (Na 2 CO 3 (1.5M)+NaOH(3M)) mixed solution B, about 800ml, requires (CO 3 2- / Al 3+ = 3.75).

[0052] 3. At 80°C, add A and B dropwise to 1000ml of water at the same time, and adjust the pH to 10 with 3M NaOH solution.

[0053] Steps 4-6 are the same as in Example 1 to obtain sample 2, wherein the atomic percentage of Cu / Mg / Al==15.03 / 37.86 / 47.11.

[0054] 7. Put 1.5 ml of the catalyst prepared above into a reaction tube, and fill the upper and lower sides of the reaction tube with quartz sand. Inject 3700ml / ml cat h -1 Nitrogen, at 500 ° C for 6 hours, then lowered to 350 ° C, with a space velocity of 3900ml / ml cat h -1 The hydrogen was reduced for 3 hours, the temperature was lowered to the reacti...

Embodiment 3

[0057] 1. Add Cu(NO 3 ) 2 ·3H 2 O, Mg(NO 3 ) 2 ·6H 2 O, Al(NO 3 ) 3 9H 2 O was made into a (0.5M, 1000ml) solution in a molar ratio of (Cu / Mg / Al=0.175 / 0.375 / 0.45), and the template agent F127 (F127 was 7% W / V) A solution was added.

[0058] 2. Na 2 CO 3 and NaOH (Na 2 CO 3 (2M)+NaOH(4M)) mixed solution B, about 800ml, requires (CO 3 2- / Al 3+ =5).

[0059] 3. At 80°C, add A and B dropwise to 1000ml of water at the same time, and adjust the pH to 11 with 4M NaOH solution.

[0060] Step 4-5 is the same as embodiment 1.

[0061] 6. Heat treatment at 500° C. for 6 hours in an air atmosphere to obtain sample 3, wherein the atomic percentage of Cu / Mg / Al=15.9 / 36.72 / 47.38.

[0062] 7. Put 1.5 ml of the catalyst prepared above into a reaction tube, and fill the upper and lower sides of the reaction tube with quartz sand. Inject 4000ml / ml cat h -1 Nitrogen, keep warm at 420°C for 3h, then drop to 320°C, and use a space velocity of 4200ml / ml cat h -1The hydrogen was...

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Abstract

The invention relates to a catalyst for preparing 1,3-butadiene through ethanol condensation. The catalyst is acid-base bifunctional mesoporous CuZnZrMgAl mixed metal oxide, wherein the atomic percent ratio of metal elements, i.e., Cu/Zn/Zr/Mg/Al in the catalyst is (9.68 to 36.43): (0 to 7.34): (0 to 7.62): (18.22 to 62.56): (20.93 to 48.12). The catalyst has the advantages of low reaction temperature, multielement active ingredient synergetic effect and good catalyst performance.

Description

technical field [0001] The invention relates to a catalyst for preparing 1,3-butadiene by condensation of ethanol, a preparation method and application. Background technique [0002] 1,3-Butadiene is an important basic raw material in the petrochemical field, especially for the synthesis of rubber, resin and other organic chemical products. Its preparation method is usually: 1) Extraction method, the C4 fraction by-product of ethylene cracking device is extracted with solvent extraction method to extract butadiene. This method is the main preparation method of 1,3-butadiene at present. 2) Naphtha cracking, direct dehydrogenation of n-butene and oxidative dehydrogenation of n-butene. Naphtha cracking requires high temperatures and produces other products. The direct dehydrogenation of n-butene is an endothermic reaction, which needs to be carried out under high temperature and low pressure conditions, which is not conducive to commercialization. [0003] To meet the growi...

Claims

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Application Information

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IPC IPC(8): B01J23/80C07C11/167C07C1/20
CPCB01J23/80B01J2523/00C07C1/20C07C11/167B01J2523/17B01J2523/27B01J2523/48B01J2523/22B01J2523/31
Inventor 房克功周娟韩有信张立功赵路穆晓亮
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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