Sepiolite loaded metal phthalocyanine catalyst, and applications thereof in catalytic preparation of humic acid

A technology for supporting metals and metal phthalocyanines, applied in physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, chemical instruments and methods, etc., can solve the problem of large amount of oxidant and low yield of humic acid , long reaction time and other problems, to achieve the effect of high humic acid content, great application value and short reaction time

Active Publication Date: 2016-04-13
济南市农业科学研究院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this process has always had problems such as large amount of oxidant, long reaction time, and low yield of humic acid. Selecting and applying a suitable catalyst is an effective measure to solve the above process problems.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Example 1 Preparation of sepiolite loaded nitrophthalocyanine iron

[0018] Methods as below:

[0019] (1) Immerse sepiolite in 6mol / L hydrochloric acid, the volume ratio of the two is 1:9, after soaking for 72, suction filter, wash, dry, grind to 80 mesh particles, and set aside.

[0020] (2) Take 10.0 g of the above-mentioned pretreated sepiolite, 200 mg of nitrophthalocyanine iron, and 10 mL of N, N-dimethylformamide (DMF), put them in a flask, stir for 20 h, filter with suction, wash with DMF, After drying in an oven at 100°C, the temperature was raised to 200°C and baked for 4 hours to obtain nitrophthalocyanine iron supported on sepiolite.

[0021] Utilize above-mentioned sepiolite-loaded metal phthalocyanine heterogeneous catalyst to catalyze the method for preparing humic acid by oxidizing weathered coal, as follows:

[0022] After the weathered coal is crushed and passed through an 80-mesh sieve, 10 g (accurate to 0.1 g) of the deashed coal sample and 0.08 g ...

Embodiment 2

[0024] Example 2 Preparation of sepiolite-supported alkoxy-substituted manganese phthalocyanine

[0025] Methods as below:

[0026] (1) Immerse sepiolite in 6mol / L hydrochloric acid, the volume ratio of the two is 1:9, after soaking for 72, suction filter, wash, dry, grind to 80 mesh particles, and set aside.

[0027] (2) Take 10.0 g of the above-mentioned pretreated sepiolite, 200 mg of alkoxy-substituted manganese phthalocyanine, and 40 mL of chloroform, put them in a flask, stir for 20 hours, filter with suction, wash with chloroform, and dry in an oven at 100 ° C. Raise the temperature to 200°C and bake for 4 hours to obtain manganese phthalocyanine supported on sepiolite.

[0028] Utilize above-mentioned sepiolite-loaded metal phthalocyanine heterogeneous catalyst to catalyze the method for preparing humic acid by oxidizing weathered coal, as follows:

[0029] After the weathered coal is crushed and passed through an 80-mesh sieve, 10 g (accurate to 0.1 g) of the deashe...

Embodiment 3

[0031] Example 3 Preparation of sepiolite-supported sulfonated cobalt phthalocyanine

[0032] Methods as below:

[0033] (1) Immerse sepiolite in 3mol / L nitric acid solution, the volume ratio of the two is 1:9, after soaking for 60°C, filter with suction, wash, dry, grind to 80 mesh particles, and set aside.

[0034] (2) Take 10.0 g of the above-mentioned pretreated sepiolite, 100 mg of sulfonated cobalt phthalocyanine, and 30 mL of water, put them in a flask, stir for 20 hours, filter with suction, wash with water, dry in an oven at 100 ° C, and heat up to Bake at 200°C for 4 hours to obtain sulfonated cobalt phthalocyanine supported on sepiolite.

[0035] Utilize above-mentioned sepiolite-loaded metal phthalocyanine heterogeneous catalyst to catalyze the method for preparing humic acid by oxidizing weathered coal, as follows:

[0036] After the weathered coal is crushed and passed through an 80-mesh sieve, 10 g of the deashed coal sample (accurate to 0.1 g) and 0.10 g of c...

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Abstract

The invention discloses a sepiolite loaded metal phthalocyanine catalyst. A preparation method comprises following steps: (1) pretreatment of sepiolite; and (2) preparation of sepiolite loaded metal phthalocyanine, wherein sepiolite obtained via pretreatment, metal phthalocyanine, and water or DMF or chloroform or dichloromethane are mixed, and an obtained mixture is subjected to stirring reaction, suction filtration, washing, and drying so as to obtain sepiolite loaded metal phthalocyanine, the metal phthalocyanine is selected from sulfonated phthalocyanin iron, sulfonated cobalt phthalocyanine, sulfonated phthalocyanine manganese, nitrated phthalocyanine iron, nitrated cobalt phthalocyanine, nitrated phthalocyanine manganese, alkoxy substituted phthalocyanine iron, alkoxy substituted cobalt phthalocyanine, or alkoxy substituted phthalocyanine manganese. The sepiolite loaded metal phthalocyanine catalyst can be used for preparing humic acid via catalytic oxidation of weathered coal. Catalyst using amount is less; reaction time is short; humic acid content of an obtained product is high; and application value of the sepiolite loaded metal phthalocyanine catalyst in industrial production is high.

Description

technical field [0001] The invention relates to a sepiolite-loaded metal phthalocyanine catalyst and the application of the catalyst in preparing humic acid by catalyzing the oxidation of weathered coal. Background technique [0002] In recent years, metallophthalocyanine (MPc) has been widely used in the fields of chemical catalysis, optics, electricity, and medicine due to its large conjugated system, stable chemical structure, and its excellent properties in optics, electricity, and magnetism. However, as a homogeneous catalyst, metal phthalocyanines have disadvantages such as easy dimer formation, poor oxidation resistance, difficult recycling and easy to cause secondary pollution. Therefore, supported metal phthalocyanines have become a research hotspot in recent years. The loading of metal phthalocyanine includes impregnation method, blending method, bonding method, in situ synthesis method, axial coordination method and so on. Yao et al. used the impregnation method ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/26C08H99/00
CPCB01J31/183B01J31/22B01J31/26C08H99/00
Inventor 马盼吕亮
Owner 济南市农业科学研究院
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