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A kind of preparation method and application of mercapto silk adsorbent

A technology of adsorbent and silk, which is applied in the preparation and application field of mercapto silk adsorbent, and achieves the effects of low production cost, high adsorption capacity and good desorption performance

Inactive Publication Date: 2016-03-02
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The patent with the application number: 201110276212.9 discloses the preparation method and application of mercapto-flax. It is characterized in that: in a corked Erlenmeyer flask, it is added according to the following composition mass percentage, thioglycolic acid: 45-52%, tetrahydrofuran: 35-40% , degummed flax: 23~30%, glacial acetic acid: 1~1.5%, concentrated sulfuric acid: 0.15~0.3%, stoppered, at 50~60℃, reflux under stirring for 4~6h, then wash with deionized water and filter with suction , until the filtrate is neutral, after washing with a small amount of ethanol, put it in a 35°C oven and dry to obtain mercapto flax, which has a strong effect on Cd 2+ The adsorption capacity can be as high as 282mg / g, and the highest adsorption rate can reach 99.6%. 2+ The maximum adsorption capacity is 519mg / g, for Cu 2+ The maximum adsorption capacity is 160mg / g; there is no report on the chemical modification and adsorption performance of silk at home and abroad.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] (1) Silk pretreatment: wash the silkworm cocoons with water to remove impurities and silkworm chrysalis, put them in a container and soak them in water for 1 day, cut the silkworm chrysalis into small pieces, wash them with clean water, dry them in vacuum, crush them, and sieve them through a 40-mesh sieve to obtain the silkworm chrysalis. processing silk;

[0019] (2) Preparation of degummed silk: Pretreated silk with a solid-to-liquid ratio of 1:20mL, soaked in 3% sodium carbonate aqueous solution for 8h, boiled for 40min, washed with deionized water until neutral after cooling, dried at 65°C after suction filtration Dry to get degummed silk;

[0020] (3) Preparation of mercapto silk adsorbent: In the reactor, add 40mL thioglycolic acid, 32mL tetrahydrofurfuryl alcohol, 27g degummed silk, 0.5mL concentrated sulfuric acid, keep the temperature at 65°C, stir, reflux for 5h, and then use deionized Wash with water, filter with suction until the filtrate is neutral, wash ...

Embodiment 2

[0022] (1) Silk pretreatment: wash the silkworm cocoons with water to remove impurities and silkworm chrysalis, put them in a container and soak them in water for 2 days, cut the silkworm chrysalis into small pieces, wash them with clean water, dry them in vacuum, crush them, and sieve them through a 40-mesh sieve to obtain the pre-treated silkworm silk. processing silk;

[0023] (2) Preparation of degummed silk: Pretreated silk with a solid-to-liquid ratio of 1:15mL, soaked in 4% sodium carbonate aqueous solution for 7h, boiled for 30min, washed with deionized water until neutral after cooling, dried at 65°C after suction filtration Dry to get degummed silk;

[0024] (3) Preparation of mercapto silk adsorbent: In the reactor, add 50mL thioglycolic acid, 30mL tetrahydrofurfuryl alcohol, 20g degummed silk, 0.1mL concentrated sulfuric acid, keep the temperature at 60°C, stir, reflux for 6h, and then use deionized Wash with water, filter with suction until the filtrate is neutra...

Embodiment 3

[0026] (1) Silk pretreatment: wash the silkworm cocoons with water to remove impurities and silkworm chrysalis, put them in a container and soak them in water for 1.5 days, cut the silkworm chrysalis into small pieces, wash them with clean water, dry them in vacuum, crush them, and sieve them through a 40-mesh sieve to obtain the pre-treated silkworm silk. processing silk;

[0027] (2) Preparation of degummed silk: Pretreated silk with a solid-to-liquid ratio of 1:25mL, soaked in 5% sodium carbonate aqueous solution for 6h, boiled for 50min, washed with deionized water until neutral after cooling, dried at 65°C after suction filtration Dry to get degummed silk;

[0028] (3) Preparation of mercapto silk adsorbent: In the reactor, add 35mL thioglycolic acid, 42mL tetrahydrofurfuryl alcohol, 22g degummed silk, 0.4mL concentrated sulfuric acid, keep the temperature at 70°C, stir, reflux for 4h, and then use deionized Wash with water, filter with suction until the filtrate is neut...

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Abstract

The invention discloses a preparation method and an application technique of a sulfydryl silk adsorbent. The preparation method of the sulfydryl silk adsorbent is characterized by comprising the following steps: adding the following components in percentage by weight concentration: 35-50% of mercaptoacetic acid, 30-55% of tetrahydrofurfuryl alcohol, 8-27% of degumming silk, 0.15-1.0% of concentrated sulfuric acid in a reactor, stirring the components at constant temperature of 60-70 DEG C, carrying out reflux reaction for 4-6 hours, then washing by deionized water, performing suction filtration until filtrate is neutral, washing by a small amount of ethyl alcohol, putting into a baking oven at 45 DEG C, and drying so as to obtain the sulfydryl silk adsorbent. The sulfydryl silk adsorbent is high in adsorption quantity to metal ions, has a sulfydryl characteristic, can directly adsorb and dilute various metal ions in a water body, is high in adsorption efficiency, is high in adsorption speed, has the favorable physical, chemical and mechanical stability, not only is low in cost, but also has the environmental-friendly effect.

Description

technical field [0001] The invention relates to a preparation method and application technology of an adsorbent for metal ions in a water system, in particular to a preparation method of a mercapto silk adsorbent and an application technology for adsorbing metal ions in water. Background technique [0002] Silk (silk) is a continuous long fiber that is coagulated by the silk liquid secreted by cooked silkworms when they cocoon. It is also called natural silk and is a natural fiber. One of the earliest animal fibers used by human beings. Silk is the lightest, softest and thinnest natural fiber in nature. It can be easily restored to its original shape after the removal of external force. Warm, warm but not dry. Mulberry silk is mainly composed of animal protein, rich in 18 kinds of amino acids necessary for the human body, can promote the vitality of skin cells, and is known as "the second skin of the human body" and "the queen of fiber". The silk fibers of silkworm cocoons...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/24B01J20/30C02F1/28C02F1/58C02F1/62
Inventor 李慧芝王英姿陈艳晶
Owner UNIV OF JINAN
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