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Production of super-macroporous intermediate-pressure-resisting spherical cellulose grain and adsorbent

A cellulose and ultra-large pore technology, applied in chemical instruments and methods, and other chemical processes, can solve the problems of wide distribution of pore size, slow solution mass transfer speed, difficult diffusion of macromolecular substances, etc., and achieve the effect of simple preparation method

Inactive Publication Date: 2007-06-20
EAST CHINA UNIV OF SCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The preparation and application of cellulose particles and their adsorbents started as early as the early 1950s. At that time, due to the limited preparation methods, most of the commercial cellulose particles and their adsorbents had two main defects: 1. The appearance was mostly Powdery, fibrous or amorphous particulate, the hydraulic properties of the column are not good, which will easily cause the defects of slowing down the bed flow rate and increasing the column pressure; 2. There is no macroporous structure, resulting in slow solution mass transfer rate and large volume The disadvantage that molecular substances are difficult to diffuse into the pores
However, these spherical cellulose particles often have cracks on the outer surface or inside, and the pore size distribution is very wide, which is not suitable for industrial chromatography operations.

Method used

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  • Production of super-macroporous intermediate-pressure-resisting spherical cellulose grain and adsorbent
  • Production of super-macroporous intermediate-pressure-resisting spherical cellulose grain and adsorbent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) Preparation of viscose

[0031] Soak 500g of ordinary cotton in 10kg of 18% sodium hydroxide aqueous solution for 2 hours, then take out the cotton, squeeze it dry, and age it for 3 days. Put in an airtight container, then add 250g CS 2 , shake at room temperature for 3 hours, put in an ice-water bath, add 5kg of 5.5% sodium hydroxide aqueous solution, and stir for 7 hours to obtain cellulose yellow acid viscose.

[0032] (2) "Hot sol phase inversion" ball making method

[0033] Mix oil phase 1500mL chlorobenzene with dispersant 37g (30g calcium carbonate, 2g potassium oleate and 5g span85), water phase 500g cellulose yellow acid viscose and mixed porogen 235g (20g benzene, 200g average molecular weight 10,000 polyphenylene Ethylene, 15g Tween80) were mixed evenly, and then the water phase was added to the oil phase, stirred at 200rpm for half an hour, rapidly heated to 70°C, and kept for half an hour. The oil phase was decanted to obtain spherical cellulose xant...

Embodiment 2

[0039] (1) Preparation of viscose

[0040] Operate by the same operation steps as in Example 1.

[0041] (2) "Hot sol phase inversion" ball making method

[0042] Mix the oil phase 1500mL vacuum pump oil with dispersant 47g (30g calcium carbonate, 2g potassium oleate and 15g span85) evenly, and then mix the water phase with 500g cellulose yellow acid viscose and 275g porogen (20g isopropanol , 250g of polyvinyl alcohol with an average molecular weight of 10,000, and 5g of Tween60) were evenly mixed and added to the oil phase, stirred at 200rpm for half an hour, rapidly heated to 70°C, and kept for half an hour. The oil phase was decanted to obtain spherical cellulose xanthate particles containing porogen.

[0043] (3) post-processing

[0044] Follow the same steps as in Example 1.

[0045] It has been determined that the ultra-large-porous medium-pressure-resistant spherical cellulose particles prepared by this method have a spherical or ellipsoidal appearance, 75% of whic...

Embodiment 3

[0047] (1) Preparation of viscose

[0048] Follow the same steps as in Example 1.

[0049] (2) "Hot sol phase inversion" ball making method

[0050] Mix 1500mL transformer oil in the oil phase with 62g of dispersant (30g calcium carbonate, 2g potassium oleate and 30g span85), and then mix 500g of cellulose yellow acid viscose liquid in the water phase and 258g of mixed porogen (3g cyclohexylamine, 250g of polyoxyethylene with an average molecular weight of 10,000 and 5g of polyoxyethylene castor oil) were mixed evenly and added to the oil phase, stirred at 200rpm for half an hour, rapidly heated to 70°C, and kept for half an hour. The oil phase was decanted to obtain spherical cellulose xanthate particles containing porogen.

[0051] (3) post-processing

[0052] Follow the same steps as in Example 1.

[0053] It has been determined that the ultra-large-porous medium-pressure-resistant spherical cellulose particles prepared by this method have a spherical or ellipsoidal app...

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Abstract

A medium pressure (5-7 bar) resistant macroreticular spherical cellulose particle is prepared from cotton through alkalizing, ageing, xanthating to obtain cellulose xanthate viscose, mixing it with pore-forming agent, dispersing the mixture in oil phase, phase transfer of hot sol to obtain shperical cellulose xanthate porticles, regenerating by acid, desulfurizing by alkali, and cross-linking. An adsorbent is prepared from said spherical cellulose particles through activating by alkali and reacting respectively on alkyl halide salt, alkyl halide, or aglucone to obtain different kinds of adsorbent.

Description

technical field [0001] The invention belongs to the field of functional polymer materials, and in particular relates to a preparation method of super-macroporous medium-pressure-resistant spherical cellulose particles and an adsorbent. Background technique [0002] Cellulose and cellulose sorbents have been widely used as chromatographic supports. In chromatography, it can be used for both analytical chromatography and preparative chromatography; it is widely used in several main chromatography techniques such as gel chromatography, ion chromatography, hydrophobic chromatography, and affinity chromatography. [0003] The preparation and application of cellulose particles and their adsorbents started as early as the early 1950s. At that time, due to the limited preparation methods, most of the commercial cellulose particles and their adsorbents had two main defects: 1. The appearance was mostly Powdery, fibrous or amorphous particulate, the hydraulic properties of the column...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/285B01J20/30
Inventor 寇正福刘坐镇江邦和王玉恒陈玲
Owner EAST CHINA UNIV OF SCI & TECH
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