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Cyclamine catalyst

A catalyst and cyclic amine technology, applied in the field of cyclic amine catalysts, can solve the problems of low space-time yield and short service life of cyclic amine catalysts

Active Publication Date: 2011-04-06
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to improve the space-time yield of cyclic amine catalysts, CN1442402A discloses a ZSM-5 cyclic amine catalyst modified by alkali metal K, which can make the conversion rate of ethanolamine up to 99%, triethylenediamine accounts for piperazine and triethylenediamine 95% of the total amount of amine, but the space-time yield of the cyclic amine catalyst is low, the space-time yield is only 200g / h.L, and the life is short, only 260h

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Embodiment 1

[0025] The cyclic amine catalyst precursor of the present invention is implemented according to the following weight percentages:

[0026] Component A 6%

[0027] Anatase TiO 2 30%

[0028] Component B 64%

[0029] Where component A is Pb 3 (PO 4 ) 2 ; Component B is dealuminated H-ZSM-5 with SiO 2 / Al 2 O 3 The molar ratio is 150.

[0030] The preparation process of the cyclic amine catalyst of the present invention is as follows:

[0031] a) First prepare 200mL of Pb(NO) with a concentration of 0.22moL / L 3 ) 2 Aqueous solution, 60g anatase TiO 2 After adding the aqueous solution, add 40mL of 0.74moL / L dihydrogen phosphate aqueous solution to the above aqueous solution under stirring, soak for 8h at 80℃, and obtain impregnated TiO after filtering, washing and drying treatment steps 2 .

[0032] b) The TiO obtained by impregnation in step a) 2 It is mixed with 128g of component B uniformly and then granulated, compressed and molded to obtain the cyclic amine catalyst precursor, which ...

Embodiment 2

[0034] The cyclic amine catalyst precursor of the present invention is implemented according to the following weight percentages:

[0035] Component A 13%

[0036] Anatase TiO 2 40%

[0037] Component B 47%

[0038] Where component A is Pb 3 (PO 4 ) 2 ; Component B is dealuminated H-ZSM-5 with SiO 2 / Al 2 O 3 The molar ratio is 250.

[0039] The preparation process of the cyclic amine catalyst of the present invention is as follows:

[0040] a) First prepare 200mL Pb(NO) with a concentration of 0.36moL / L 3 ) 2 Aqueous solution, 60g anatase TiO 2 After adding the aqueous solution, add 40mL of 1.20moL / L hydrogen phosphate aqueous solution to the above aqueous solution under stirring, soak for 8h at 80℃, and obtain the impregnated TiO after filtering, washing and drying. 2 .

[0041] b) The TiO obtained by impregnation in step a) 2 It is mixed with 70.5g of component B uniformly and then granulated and pressed into a shape to obtain a cyclic amine catalyst precursor, which is calcined at...

Embodiment 3

[0043] The cyclic amine catalyst precursor of the present invention is implemented according to the following weight percentages:

[0044] Component A 20%

[0045] Anatase TiO 2 50%

[0046] Component B 30%

[0047] Where metal ion A is Pb 3 (PO 4 ) 2 ; Component B is dealuminated H-ZSM-5 with SiO 2 / Al 2 O 3 The molar ratio is 350.

[0048] The preparation process of the cyclic amine catalyst of the present invention is as follows:

[0049] a) First prepare 200mL of Pb(NO) with a concentration of 0.44moL / L 3 ) 2 Aqueous solution, 60g anatase TiO 2 After adding the aqueous solution, add 40mL of 1.48moL / L ammonium phosphate aqueous solution to the above aqueous solution under stirring, soak for 8h at a temperature of 80℃, and obtain the impregnated TiO after filtering, washing and drying treatments. 2 .

[0050] b) The TiO obtained by impregnation in step a) 2 After mixing with 36g of component B uniformly, granulation, compression molding, cyclic amine catalyst precursor, calcined at ...

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Abstract

The invention discloses a cyclamine catalyst, which is characterized in that the precursor of the cyclamine catalyst comprises the following compositions in percentage by mass: 6 to 20 percent of a composition A, 30 to 50 percent of anatase TiO2, and 30 to 64 percent of a composition B, wherein the composition A is Pb3 (PO4)2, Zr3 (PO4) 2 or Cd3 (PO4) 2; and the composition B is H-ZSM-5 (mole ratio of SiO2 to Al2O3 is 150 to 350); the cyclamine catalyst is prepared through the following steps: loading the composition A on the anatase TiO2, and drying the obtained product; mixing the obtained product with the composition B; then carrying out pelletizing and forming on the obtained mixture so as to obtain the precursor of the cyclamine catalyst; and finally, roasting the precursor so as to obtain the cyclamine catalyst. The cyclamine catalyst of the invention is mainly used for synthesizing piperazidine and triethylene diamine by a gas-phase catalytic reaction of ethanolamine.

Description

Technical field [0001] The invention relates to a cyclic amine catalyst, in particular to a cyclic amine catalyst for the reaction of ethanolamine and ammonia to synthesize piperazine and triethylenediamine. Background technique [0002] It is well known that various acidic oxides and modified zeolite molecular sieves are used as catalysts in the synthesis of piperazine and triethylenediamine using various amine compounds as raw materials. [0003] For example, CN1106000A discloses a kind of γ-Al 2 O 3 As a carrier, a cyclic amine catalyst supporting Fe and Ni; and a cyclic amine catalyst containing Cu, Mg, Ca, Al, Co, Cr or Zn phosphate is disclosed. The cyclic amine catalyst can achieve a conversion rate of 98 %, the reaction product is mainly piperazine, and its selectivity can reach 85%, but the space-time yield of cyclic amine of this catalyst is only 55g / hL, and the catalyst life data has not been reported. [0004] In order to improve the space-time yield of the cyclic amine ...

Claims

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Application Information

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IPC IPC(8): B01J29/40C07D295/027C07D295/023C07D487/08
Inventor 赵锋伟吕剑杨建明王伟封利民淡保松崔文华何飞
Owner XIAN MODERN CHEM RES INST