A preparation method and quality detection method of composite spherical particles for adsorption and removal of active phosphate in organic solvent

A technology of spherical particles and organic solvents, applied in the chemical industry, can solve problems such as catalyst poisoning and deactivation, and achieve the effects of promoting adsorption capacity, improving adsorption capacity, and increasing adsorption surface area

Active Publication Date: 2022-07-15
SHANDONG CHENYANG NEW CARBON MATERIAL CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] As can be seen from the above, in the catalytic hydrogenation reaction of phthalic anhydride, the active phosphate contained in the raw material will cause the poisoning and deactivation of the catalyst. research topic

Method used

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  • A preparation method and quality detection method of composite spherical particles for adsorption and removal of active phosphate in organic solvent
  • A preparation method and quality detection method of composite spherical particles for adsorption and removal of active phosphate in organic solvent

Examples

Experimental program
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Embodiment 1

[0033] Embodiment 1, a preparation method of composite spherical particles for adsorption and removal of active phosphates in organic solvents.

[0034] a) Raw material activation:

[0035] Pulverize the clay and pass it through a 100-mesh sieve, pass the industrial diatomite powder through a 150mm sieve, take the material under the sieve, weigh 900g of the clay powder and 600g of the diatomite powder and mix thoroughly, soak in 4000mL of 1mol / L hydrochloric acid solution, and ultrasonically acidify for 1 ~2h, negative pressure filtration and washing with ultrapure water to neutrality. It was dried at 120 °C, then placed in a muffle furnace, calcined at 700 °C for 5 h, taken out and cooled to room temperature, and ground through a 150-mesh sieve to obtain activated powder.

[0036] b) Impregnation modification:

[0037] Weigh 1000g of the activated mixed powder, put it in 2500g of 3mol / L calcium nitrate solution, mix it thoroughly, conduct magnetic stirring, supersaturate im...

Embodiment 2

[0046] Embodiment 2, a preparation method of composite spherical particles for adsorption and removal of active phosphates in organic solvents.

[0047] Compared with Example 1, the difference is that the concentration of the calcium nitrate solution in the step b) is changed to 5mol / L, the immersion time is changed to 18h, and other conditions are the same as those of Example 1. The effect of impregnant concentration on the adsorption capacity of spherical particles was mainly investigated.

Embodiment 3

[0048] Embodiment 3, a preparation method of composite spherical particles for adsorption and removal of active phosphates in organic solvents.

[0049] Compared with Example 1, the difference is that the calcium nitrate solution in the step b) replaces the calcium chloride solution. Other conditions are the same as in Example 1. The effect of the type of impregnating agent on the adsorption capacity of spherical particles was mainly investigated.

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Abstract

The invention relates to a preparation method of composite spherical particles for adsorption and removal of active phosphates in organic solvents, comprising the following steps: step a), activation of raw materials; step b), impregnation modification; step c), granulation, roasting and molding; Step d), particle organic modification. The invention also discloses a quality detection method for the composite spherical particles for adsorbing and removing active phosphates in organic solvents. The beneficial effects of the invention are as follows: the composite material is granulated and formed, and the pore-forming agent is added to obtain porous composite spherical particles with different pore sizes and excellent performance, which can realize the dynamic adsorption of organic solvents and is more suitable for industrial production. The surface of the spherical particles is hydrophilic, and a stable hydrophilic film is formed on the surface of the particles, which promotes the adsorption capacity of the spherical particles to the active phosphate, and makes it quickly desorb from the organic solvent, so that the composite material can absorb the organic active phosphate. Better performance.

Description

technical field [0001] The invention belongs to the field of chemical industry, and relates to a preparation method and a quality detection method of composite spherical particles for adsorbing and removing active phosphate in an organic solvent. Background technique [0002] Catalytic hydrogenation of phthalic anhydride is a method in which phthalic anhydride is dissolved in a solvent in the presence of a catalyst, and phthalic anhydride is reduced to phthalide or hexahydrophthalic anhydride under the action of a certain concentration of reactants, temperature and pressure. The catalytic hydrogenation of phthalic anhydride has higher requirements on catalysts. The general hydrogenation catalyst is a precious metal or composite metal catalyst as the core of the hydrogenation reaction, and the catalyst activity becomes a key factor determining the operating cost of the entire hydrogenation reaction system. However, active phosphate impurities in the feedstock are common pois...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/26B01J20/28B01J20/30G01N30/96
CPCB01J20/14B01J20/12B01J20/041B01J20/2803B01J20/28004B01J20/28019B01J20/261G01N30/96
Inventor 余萍胡燕红车忠敏张海霞胡春燕王方丽闫桂林
Owner SHANDONG CHENYANG NEW CARBON MATERIAL CO LTD
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