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Sulfydryl cellulose type straw adsorbent and preparation method thereof as well as recycling of noble metal silver

A technology of cellulose and adsorbent, which is applied in the field of green adsorbent preparation and precious metal extraction, can solve the problems of long process, high operating cost, complicated operation, etc., and achieve the effects of reduced processing cost, wide application range and simple preparation

Active Publication Date: 2015-02-25
LIAONING UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The separation methods of precious metals mainly include precipitation method, extraction method, ion exchange method, electrolysis method and selective volatilization method, etc. The most prominent shortcomings of these methods are that when treating low-concentration metal wastewater, the operation is cumbersome, the operation cost is high, and the energy consumption is large. , and easily cause secondary pollution
Before the 1970s, the classic refining process based on selective precipitation was used to separate and purify precious metals. The process was long, the cycle was long, the plant area was large, the operation was complicated, and the direct recovery rate was low. Some precious metals were stranded in the production process. Economic benefits are affected
[0004] At the same time, the straw waste generated every year in our country is not only brought great pollution to the environment but also causes a waste of resources through burning. If these wastes can be effectively used, it will not only reduce environmental pollution but also alleviate the energy crisis.

Method used

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  • Sulfydryl cellulose type straw adsorbent and preparation method thereof as well as recycling of noble metal silver
  • Sulfydryl cellulose type straw adsorbent and preparation method thereof as well as recycling of noble metal silver
  • Sulfydryl cellulose type straw adsorbent and preparation method thereof as well as recycling of noble metal silver

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Example 1 A mercaptocellulose-based straw adsorbent

[0025] Its preparation method is as follows:

[0026] 1) Take the straw, wash it with deionized water, put it in a constant temperature drying box, dry it at 50°C, take it out and pulverize it into powder, then take 20g of straw powder, add 80mL of concentrated sulfuric acid, heat in a water bath, and control the temperature at At about 80°C, stir for 12 hours and filter, then use 0.1mol / L NaHCO 3 Washing, and then washing with deionized water until neutral, filtering again, and drying at 60°C for 24 hours to obtain product A, which was ground and sieved. Then add 30mL ammonia water and 100mL epichlorohydrin to a 500mL round bottom flask, react at a constant temperature of 60°C for 4h, then add product A, 1gNaOH, react at a constant temperature of 110°C for 8h, filter, wash with water until neutral, and dry at 55°C to obtain product B.

[0027] 2) Add 9.114g (0.1mol) thiosemicarbazide to a 500mL round bottom flask,...

Embodiment 2

[0029] Example 2 The effect of a mercaptocellulose-based straw adsorbent on the separation of silver in high-concentration copper-nickel solutions at different acidities

[0030] Take Cu 10g·L -1 , Ni 10g L -1 , and Ag(I) 15mg / L solution 50mL, the acidity of hydrochloric acid in the solution is 0.1mol L -1 , 0.3mol·L -1 , 0.5mol·L -1 , 0.8mol·L -1 , 1mol L -1 , 2mol L -1 and 3mol L -1 , and then add 100 mg of mercaptocellulose-based straw adsorbent respectively, and measure the concentration of each ion in the solution after shaking for 2 hours. Such as figure 2 Shown, at 0.1mol·L -1 , 0.3mol·L -1 , 0.5mol·L -1 Under the condition of acidity, the adsorption rate of the adsorbent to the high-concentration copper-nickel solution is not much different, and the highest adsorption rate reaches 92%, indicating that the acidity is less than 0.5mol L -1 At high concentrations of Cu 2+ and Ni 2+ Under the influence of the sorbent, the adsorbent still has a high adsorptio...

Embodiment 3

[0031] Example 3 Separation of silver by a mercaptocellulose-based straw adsorbent in different coexisting ion solutions

[0032] Prepare solution Cu 10g·L respectively -1 and Ag(I) 15mg / L; Ni 10g·L -1 And Ag(I) 15mg / L, Cu 10g·L -1 , Ni 10g L -1 and Ag(I) 15mg / L three solutions 50mL, the acidity of hydrochloric acid in the solution is 0.5mol L -1 , then add 100mg of mercaptocellulose straw adsorbent respectively, shake for 1h, 2h, 3h, 4h, 5h, 8h, 12h, 24h and track the concentration of silver ions in the solution as image 3 shown by image 3It can be seen that there is no competitive adsorption when there are only nickel and silver in the system, but when there is a high concentration of copper ions in the solution, copper ions will compete with silver ions for adsorption after 2 hours of reaction, resulting in a decrease in the adsorption rate of silver. Therefore, the preferred adsorption time of the mercaptocellulose straw adsorbent is 0.5-2h.

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Abstract

The invention discloses a sulfydryl cellulose type straw adsorbent. A preparation method comprises the following steps: (1) taking straws and washing; drying at 50 DEG C; adding concentrated sulfuric acid and heating; filtering after stirring; washing to be neutral; filtering again and drying at 60 DEG C for 24 hours to obtain a product A; putting ammonia water and epoxy chloropropane into a reaction container I and reacting at 60 DEG C for 4 hours; adding the product A into the reaction container I and adding NaOH; reacting at 110 DEG C for 8 hours; after the reaction, filtering and washing the product to be neutral; drying at 55 DEG C to obtain a product B; and (2) dissolving thiosemicarbazide into a reaction container II and adding the product B and glutaraldehyde; reacting at 90 DEG C for 5 hours; filtering and washing; and drying at 55 DEG C to obtain a target product. The preparation method is simple, has no pollution and has low cost; the prepared straw adsorbent has high separation and enriching efficiency and trace silver can be separated and enriched from a high-concentration copper-nickel solution; and the preparation method has no energy consumption, is energy-saving and environmentally friendly, has a wide applicable range, and has actual applicability.

Description

technical field [0001] The invention belongs to the technical field of preparation of green adsorbents and extraction of precious metals, and in particular relates to the preparation of a mercaptocellulose-based straw adsorbent and the recovery of precious metal silver. Background technique [0002] Precious metals include 8 elements including gold, silver, platinum, palladium, nails, rhodium, osmium and iridium. Due to their special properties, they are widely used in aerospace, electronics and petrochemical industries. The content of silver in the earth's crust is very small, accounting for only 1×10 -5 %, elemental natural silver exists in nature, but it is mainly produced in the form of compounds. Pure silver is silvery white, with a melting point of 960.8°C, a boiling point of 2210°C, and a density of 10.49 g / cm 3 . Silver is a face-centered cubic lattice with good plasticity and ductility second only to gold, but when it contains a small amount of arsenic, antimony,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/24B01J20/30C22B11/00C22B3/24
CPCB01J20/24B01J20/3085B01J2220/4825C22B11/042Y02P10/20
Inventor 熊英万丽娄振宁单炜军
Owner LIAONING UNIVERSITY
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