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A preparation method of a magnetic field fluidized bed stationary phase for separating chiral substances

A fluidized bed, stationary phase technology, applied in separation methods, chemical instruments and methods, solid adsorbent liquid separation, etc., can solve problems such as low pressure of fixed particles, unusable separation columns, and magnetic particles escaping.

Active Publication Date: 2017-01-25
江苏汉峰数控科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, with the development of material science, the magnetic particles used are all nano-scale or micron-scale particles with large surface area, which makes it easy for magnetic particles to escape from the magnetic field fluidized bed.
Magnetically stabilized fluidized beds generally use electromagnetic coils to generate magnetic fields. In the practical application of magnetically stabilized fluidized beds, there are the following problems: a small amount of fine magnetic particle carrier / catalyst is entrained by liquid from the outlet of the reactor and flows out, resulting in separation medium loss; in order to prevent loss, the magnetic field strength is usually increased by increasing the voltage and current of the external electromagnetic coil. In the freezing zone, the magnetic adsorption carrier is in a chain shape, channeling occurs in the bed, and the fluid distribution is uneven, resulting in a decrease in mass transfer efficiency
[0007] At present, the difficulty of chiral separation also has the problem of difficulty in expanding the production scale. The separation column used in the laboratory cannot be used on an industrial scale. The small immobilized particles cause excessive pressure and low efficiency, and the loss of the stationary phase solution Live problem; In order to solve the above problems, the present invention utilizes magnetic field as external force and makes stationary phase form stable fluidization in separation column, has solved above-mentioned problem, can be applicable to industrialized production scale

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] (1), ferric trichloride is dissolved in the dilute hydrochloric acid aqueous solution, is mixed with the solution that concentration is 1% by weight, slowly drips the ammoniacal liquor that concentration is 10% until there is flocculent black precipitation to appear, until PH is 12, stand still For 48 hours, filter, wash until PH = 7, move the nanoparticles to absolute ethanol, stir and evaporate the resulting suspension at 90°C to obtain magnetic nanoparticles;

[0018] (2), adding a certain amount of aqueous dispersion of magnetic nanoparticles to the aqueous alcohol solution and mixing, adding sodium hydroxide solution and ethyl orthosilicate under stirring, the reaction temperature is 30 ° C, and the reaction time is 36 hours; The amount of particles added accounts for 1.0% of the weight of the entire system, alcohol accounts for 65%, alkali solution accounts for 2.0%, and alkyl orthosilicate accounts for 1.0%. Magnetic particles wrapped in silicon dioxide are obtain...

Embodiment 2

[0023] (1), ferric trichloride is dissolved in dilute hydrochloric acid aqueous solution, is mixed with the solution that concentration is 10% by weight, and slowly dripping concentration is the ammoniacal liquor of 1%-% to appear until flocculent black precipitation is arranged, until pH is 10, Stand still for 48 hours, filter, wash until PH = 7, move the nanoparticles to absolute ethanol, stir and evaporate the resulting suspension at 90°C to obtain magnetic nanoparticles;

[0024] (2) Add a certain amount of aqueous dispersion of magnetic nanoparticles to the aqueous alcohol solution and mix, add sodium hydroxide solution and butyl orthosilicate under stirring, the reaction temperature is 30°C, and the reaction time is 36 hours; The amount of particles added accounts for 1.0% of the weight of the entire system, alcohol accounts for 65%, alkali solution accounts for 2.0%, and alkyl orthosilicate accounts for 1.0%. Magnetic particles wrapped in silicon dioxide are obtained;

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Abstract

The invention relates to a preparation method of a stationary phase of a magnetic fluidized bed for separating chiral substances. The preparation method comprises the following steps: (1) dissolving ferric trichloride into a diluted hydrochloric acid aqueous solution, dropwise adding ammonia water until flocculent and black precipitates appear, filtering, washing and evaporating to obtain magnetic nano-particles; (2) adding an aqueous dispersion of the magnetic nano-particles into an alcohol aqueous solution, mixing, and adding a sodium hydroxide solution and alkyl orthosilicate to obtain silicon dioxide coated magnetic particles; (3) cleaning the magnetic particles obtained in the step (2), drying and adding a silane coupling agent; (4) collecting products in the step (3), washing the products with ethyl alcohol and water respectively, dispersing the products into deionized water to obtain a silane coupling agent modified magnetic nano-particle aqueous dispersion; and (5) dissolving N-isopropylacrylamide, cyclodextrin or bovine serum albumin, a polymer cross-linking agent and an initiator into the magnetic nano-particle aqueous dispersion obtained in the step (4), introducing nitrogen gas and stirring.

Description

technical field [0001] The invention relates to a preparation method of a magnetic field fluidized bed stationary phase used for separating chiral substances in the field of biomedicine. Background technique [0002] Due to their large surface area and high surface activity, superparamagnetic nano / micro particles are thermodynamically unstable and easily agglomerated into clusters. In order to prevent the coagulation between the magnetic particles and form a stable colloidal solution, the surface of the magnetic particles needs to be modified during the preparation process. The surface of the modified magnetic particles should have more active functional groups, such as -NH2 , -COOH, -OH and -CHO, etc., in order to couple biomolecules and affinity ligands to obtain suitable magnetic carriers for various applications. The magnetic particles contain magnetic particles inside, which have superparamagnetism. When there is an external magnetic field, they show better magnetic pr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/22B01J20/28B01J20/30B01D15/18B01D15/38
CPCB01D15/1807B01D15/38B01D15/3833B01D2215/02B01J20/0229B01J20/06B01J20/103B01J20/22B01J20/24B01J20/28009B01J2220/46B01J2220/4806B01J2220/4812
Inventor 华文蔚
Owner 江苏汉峰数控科技有限公司