Preparation method and quality detection method of composite spherical particles for adsorbing and removing active phosphate in organic solvent
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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: 2021-07-02
山东晨阳新型碳材料研究院有限公司
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[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
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Embodiment 1
[0033] Example 1, a method for preparing composite spherical particles that adsorb and remove active phosphate in organic solvents.
[0034] a) Raw material activation:
[0035] Crush clay through a 100-mesh sieve, pass industrial diatomite powder through a 150mm sieve, take the undersieve, weigh 900g of clay powder and 600g of diatomite powder, mix thoroughly, soak in 4000mL 1mol / L hydrochloric acid solution, and ultrasonically acidify for 1 ~2h, filter with negative pressure and wash with ultrapure water until neutral. Dry it at 120°C, put it into a muffle furnace, bake it at 700°C for 5 hours, take it out and cool it to room temperature, and grind it through a 150-mesh sieve to obtain an activated powder.
[0036] b) Impregnation modification:
[0037] Weigh 1000g of the activated mixed powder, put it into 2500g 3mol / L calcium nitrate solution, mix thoroughly, carry out magnetic stirring, supersaturated impregnation, after impregnation for 10h, let stand and age for 24h, ...
Embodiment 2
[0046] Example 2, a method for preparing composite spherical particles that adsorb and remove active phosphate 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 5 mol / L, the immersion time is changed to 18 hours, and other conditions are the same as in Example 1. The effect of impregnating agent concentration on the adsorption capacity of spherical particles was mainly investigated.
Embodiment 3
[0048] Example 3, a method for preparing composite spherical particles that adsorb and remove active phosphate 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 identical with embodiment 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 adsorbing and removing active phosphate in an organic solvent. The preparation method comprises the following steps: step a, activating raw materials; step b, conducting dipping modification; step c, conducting granulating, roasting and forming; and step d, organically modifying the particles. The invention further discloses a quality detection method of the composite spherical particles for adsorbing and removing the active phosphate in the organic solvent. The preparation method has the beneficial effects that the composite material is granulated and molded, the porous composite spherical particles with different pore diameters and excellent performance can be prepared by adding the pore-forming agent, the dynamic adsorption of an organic solvent can be realized, and the preparation method is more suitable for industrial production. The surfaces of the spherical particles are hydrophilic, a layer of stable hydrophilic film is formed on the surfaces of the particles, the adsorption capacity of the spherical particles to active phosphate is promoted, the spherical particles are rapidly desorbed from the organic solvent, and the absorption performance of the composite material to the organic matter active phosphate is more excellent.
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 organic solvents. 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 the phthalic anhydride is reduced to phthalide or hexahydrophthalic anhydride under certain reactant concentration, temperature and pressure. The catalytic hydrogenation reaction of phthalic anhydride has higher requirements on the catalyst. The general hydrogenation catalyst is a noble 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 raw materials are common poisons in hy...
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