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Heavy metal adsorbent suitable for menthol and preparation method thereof

A heavy metal and adsorbent technology, applied in non-metallic elements, alkali metal compounds, chemical instruments and methods, etc., can solve the problems of time-consuming and laborious, and achieve the effect of increasing adsorption capacity, wide adaptability, and not easy to block

Active Publication Date: 2020-11-06
HUANGSHAN TIANMU MINT PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to overcome the time-consuming and labor-intensive problem of the existing menthol heavy metal removal process, the present invention provides a heavy metal adsorbent suitable for menthol and a preparation method thereof. The heavy metal adsorbent is added before the menthol freezing and crystallization step to absorb heavy metals, and the heavy metals are adsorbed The agent has two layers of MCM-48 molecular sieves with different pore sizes, which can adsorb different heavy metals in menthol in a targeted manner, and the adsorption effect is good. seperate

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  • Heavy metal adsorbent suitable for menthol and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] A kind of preparation method applicable to the heavy metal adsorbent of menthol:

[0022] (1) Surface modification of ferric oxide: disperse ferric ferric oxide micro-particles with a particle size of 30 μm in distilled water to form a solution with a concentration of 4 mg / L, add 1.6 mL of citric acid for ultrasonic dispersion treatment, and obtain carboxyl-modified ferric oxide on the surface. Iron oxide;

[0023] (2) Preparation of thiol-modified MCM-48: Dissolve CTAB and NaOH in deionized water, add TEOS, the molar ratio of CTAB, NaOH, TEOS and deionized water is 1:1:3.5:110, stir for 0.5h, Crystallize at 90°C for 2 days, cool to room temperature and adjust the pH to 8 with hydrochloric acid, then crystallize at 90°C for 2 days, filter, wash, and dry in the air, and roast at 550°C for 6 hours to obtain MCM-48 molecular sieve; mercaptopropyltrimethoxysilane Dissolved in toluene, added to the MCM-48 molecular sieve, the mass of mercaptopropyltrimethoxysilane is 1% of ...

Embodiment 2

[0028] (1) Ferric oxide surface modification: Disperse ferric oxide microparticles with a particle size of 10 μm in distilled water to form a solution with a concentration of 5 mg / L, add 1 mL of citric acid for ultrasonic dispersion treatment, and obtain carboxyl-modified ferric oxide on the surface. Ferric oxide;

[0029] (2) Preparation of thiol-modified MCM-48: Dissolve CTAB and NaOH in deionized water, add TEOS, the molar ratio of CTAB, NaOH, TEOS and deionized water is 1:1:4:100, stir for 1 h, and Crystallize at 100°C for 2 days, cool to room temperature and adjust the pH to 8 with hydrochloric acid, then crystallize at 90°C for 2 days, filter, wash, and dry in the air, and roast at 530°C for 7 hours to obtain MCM-48 molecular sieve; Add toluene to the MCM-48 molecular sieve, the quality of mercaptopropyltrimethoxysilane is 0.5% of the MCM-48 molecular sieve, reflux for 22 hours, centrifuge the product, wash and dry to obtain the mercapto-modified MCM-48 molecular sieve ...

Embodiment 3

[0033] (1) Ferric oxide surface modification: Disperse ferric oxide microparticles with a particle size of 50 μm in distilled water to form a solution with a concentration of 6 mg / L, add 2 mL of citric acid for ultrasonic dispersion treatment, and obtain carboxyl-modified ferric oxide on the surface. Ferric oxide;

[0034] (2) Preparation of thiol-modified MCM-48: Dissolve CTAB and NaOH in deionized water, add TEOS, the molar ratio of CTAB, NaOH, TEOS and deionized water is 1:1:6:105, stir for 0.8h, Crystallize at 90°C for 1 day, cool to room temperature and adjust the pH to 8 with hydrochloric acid, then crystallize at 90°C for 2 days, filter, wash, and dry in the air, and roast at 500°C for 8 hours to obtain MCM-48 molecular sieve; mercaptopropyltrimethoxysilane Dissolved in toluene, added to the MCM-48 molecular sieve, the quality of mercaptopropyltrimethoxysilane is 2% of the MCM-48 molecular sieve, refluxed for 20h, the product was centrifuged, washed and dried to obtain ...

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Abstract

The invention relates to a menthol production process. Aiming at the problem that an existing menthol heavy metal removal process wastes time and labor, provided is a heavy metal adsorbent suitable for menthol; ferroferric oxide micron particles serve as a core, the outer sides of the ferroferric oxide micron particles are coated with two layers of MCM-48 molecular sieves, and the pore diameter ofthe MCM-48 molecular sieve on the outer layer is larger than that of the MCM-48 molecular sieve on the inner layer. The heavy metal adsorbent disclosed by the invention takes ferroferric oxide as thecore, and the outer side of ferroferric oxide is coated with the MCM-48 molecular sieve; ferroferric oxide particles have quite strong magnetic responsiveness, so the heavy metal adsorbent can be rapidly separated from menthol by adopting a magnetic separation method,; the outer side of ferroferric oxide is coated with two layers of MCM-48 molecular sieves with different pore diameters, so that not only is the adsorption capacity increased, but also the adaptability is wider compared with that of a product with a single pore diameter. The invention also provides a preparation method of the heavy metal adsorbent.

Description

technical field [0001] The invention relates to a menthol production process, in particular to a heavy metal adsorbent suitable for menthol and a preparation method thereof. Background technique [0002] Heavy metals in Chinese herbal medicines have become one of the issues of special concern to the export of Chinese traditional medicines in the world, and their safety evaluation has become a research hotspot; Safety in use, so inventing a method for reducing the content of heavy metal elements in menthol is a problem to be solved urgently at present. [0003] For example, Chinese Patent Publication No. CN109293479A discloses a method for extracting menthol that reduces the content of heavy metal elements in menthol, which specifically includes the following steps: (1) fresh mint is subjected to microwave heat treatment, crushed, added ethanol solution, heated with a slow fire, and kept stirring , filter to obtain ethanol extract one and filter residue one; (2) add ethanol ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/16B01J20/28B01J20/30C07C29/76C07C35/12
CPCB01J20/16B01J20/28009B01J20/28016B01J20/3085B01J20/3078C07C29/76C07C2601/14C07C35/12Y02A50/30
Inventor 方胜汪莉萍任移生李友谊
Owner HUANGSHAN TIANMU MINT PHARMA