Hydrothermal Synthesis Tungsten Trioxide

Hydrothermal methodHydrothermal method was invented by the geologist simulating the natural mineralization in mid-19th century and later turned to study functional materials. Currently hydrothermal method has prepared hundreds of kinds of crystals. Hydrothermal method, also known as hydrothermal method, is the scope of liquid chemical method. It means in a sealed pressure vessel, carriing out at high temperature and pressure conditions of the chemical reaction. Hydrothermal reaction depends on the type of reaction and it can be divided into hydrothermal oxidation, water and heat reduction, hydrothermal precipitation, hydrothermal synthesis, water hot solution, hydrothermal crystallization.

The Main Steps:
1. Dissolving the 3.5gNa2WO4•2H20 in 20ml of distilled water, dubbed the solution;
2. Exchanging resin column to produce hydrated tungstate sol by the solution that was hydrated;
3. Stirring constantly the dropped sol with a volume of 70ml glass barrel;
4. Adding to the resulting sol, and mixing well under 4.84g of citric acid.

Conclusions:
Preparing quadrature phase WO3 nano-sized rectangular sheets by hydrothermal synthesis with citric acid as a controlling agent, which shows there is a great relationship between the structure of product and the reaction temperature. X-ray diffraction results show that the reaction product is a WO3 • H2O and a small amount of monoclinic WO3 (γ- WO3); with the reaction temperature, the product of the following occurs transition: WO3 • H2O → WO3. SEM results showed that the product obtained are rectangular sheet structure at the reaction temperature. They are less than the surface area, between 8 ~ 9 m2 • g-1. We can control the product's composition, morphology and specific surface area by adjusting the citric acid and the amount of substance ratio (nCit / nTA). When nCitn / TA = 0, the product of h-WO3 and WO3 • 1 / 3H2O is composition; when nCit / nTA = 0.5 and nCit / nTA = 1, the product is γ-WO3 morphology rectangular sheet. In the case of citric acid was added, than the surface area of the product decreases with an increase of nCit / nTA.

 

Waste Tungsten-Nickel Catalyst Preparing Sodium Tungstate 2/2

Nickel, is a kind of approximate silvery white, hard, malleable and ferromagnetic metal element. It can be highly polished and is of corrosion resistance. Tungsten is important strategic metal resource and is also one of China's traditional export minerals. With the continuously exploitation, tungsten resources are decreasing gradually and the waste is very serious. To make up for the original tungsten resource shortage, the recycling of waste tungsten becomes one of the important measures.
 
Sodium tungstate was prepared by roasting plus sodium-leaching-ion exrhange and with waste tungsten-nickel hydrogenation catalyst as the raw material. We can draw the following conclusions: 
1. The influence of the waste catalyst grinding particle size: waste catalyst grinding particle size has a certain influence on leaching rate of tungsten. Tungsten leaching rate after grinding increases by 10%. Grinding to 0.15 mm is the best process condition of experiments.
2. The influence of the dosage of sodium carbonate: As the dosage of sodium carbonate increasing from 0.46 to 0.69, tungsten leaching rate increases by 30%. The effect is very obvious. However, when the dosage of sodium carbonate ratio increases continuously, it has no significant effect on the experimental results. So the most appropriate dosage ratio of sodium carbonate is 0.69.
3. The influence of water temperature and time: Leaching temperature from 80 ℃ to 90 ℃, the leaching rate of tungsten increases by 2%. Leaching time has a small influence on the leaching effect of tungsten. Leaching it in 1 h and 90 ℃, the leaching rate of tungsten can reach nearly 99%.
4. The influence of the adsorption process of ion exchange: String column adsorption method can make each resin to saturated exchange capacity, which greatly improves the production capacity of ion exchange column. Using 2 mol/L NaCl and NaOH 1 mol/L mixture liquid as desorption, tungsten desorption rate can reach 98.2%.
5. Mix and heat the desorbed liquid. By evaporation, crystallization and recrystallization white crystal can be got. The purity of sodium tungstate products can reach more than 99%.
 
In conclusion, the method of using waste tungsten - nickel hydrogenation catalyst as raw material, using roasting plus sodium-leaching-ion exrhange to prepare sodium tungstate has the advantages of simple steps, mild conditions, easy operation, high recovery rate and low production cost. It can meet the requirements of circular economy and environmental protection.

 

Sodium Tungstate Spectrophotometry Determining Gingko Flavonoids

Gingko Flavonoid is the Ginkgo biloba extract. It can increase CBF and improve the function of cerebral circulation. It also can protect brain cells, expand coronary artery, prevent angina and myocardial infarction, prevent thrombosis, and enhance the body's immune ability. It’s good for the patients with coronary heart disease, angina pectoris, cerebral arteriosclerosis, senile dementia and hypertension. The methods of determination are derivatives-gas chromatography, reversed-phase high performance liquid chromatography (HPLC), colorimetric method and so on.
 
Gingko-FlavonoidsThis article mainly introduces a new method-spectrophotometry. Spectrophotometry is determining absorbance of light or luminous intensity of the material tested at a particular wavelength or within a certain wavelength range to make the qualitative and quantitative analysis of the material. The method is based on gingko flavonoids reacting with sodium tungstate to generate yellow tungsten acid ester. This method is highly sensitive, simple, fast, and reliable. If it can be used for the determination of actual samples, a satisfactory result will be got.
Experimental Methods:
1. Respectively add 0.08 mol/L sodium tungstate solution 2 ml in two 25 ml colorimetric tube. Add a certain volume of gingko flavonoids standard using liquid and shake well to dilute to scale.
2. Another is added to scale directly. Put the former in sample pool, the latter in reference pool and determine its absorbance at 304 nm.
Experimental results:
1. The reaction product of tungsten acid ester has maximum absorption at 304 nm, so the experiment selects the wavelength as measuring wavelength.
2. The acidity of the solution has a big influence on the production of tungsten acid ester, so the experiment selects neutral conditions to reaction.
3. The amount of sodium tungstate has a certain influence on the formation of tungsten acid ester. With the increase of the dosage of sodium tungstate solution, absorbance also increases accordingly.
4. At 20 ℃, absorbance value of solution is maximum. 40 minutes later the absorbance value decreases gradually.
5. The linear range of the method is 4 ~ 120 mu g/ml. Through determining of samples, the recovery is 100.0% ~ 100.6%.
 
In conclusion, the spectrophotometry of rapidly determining gingko flavonoids in pharmaceutical preparations has the advantages of convenience, rapidness, wide linear range, high sensitivity, high accuracy, less reagent dosage, less interference and good reproducibility. It can be easily used in determining gingko flavonoids in pharmaceutical preparations.

Waste Tungsten-Nickel Catalyst Preparing Sodium Tungstate 1/2

Tungsten is a kind of infusible and rare metal. China’s tungsten resources have significant superiority in the world. Although China's tungsten reserves, production and foreign trade exports are the first in the world at present, the situation of China's tungsten resources can’t be blindly optimistic. Tungsten resources which are available for exploiting in China are sharply reducing. Tungsten resources are facing a severe situation.
 
For this problem, many experts have studied the countermeasures. Recycling and efficiently using tungsten secondary resources is one of the important measures to make up for a lack of original tungsten resources. Waste tungsten - nickel hydrogenation catalyst is a kind of important marketable secondary resources. Realizing valuable metals recycling of waste tungsten - nickel hydrogenation catalyst, not only can reduce environmental pollution, increase the recycling of resources, but also can reduce the production cost of enterprises and improve the economic benefit.
waste catalyst composition
This article introduces a kind of method of using waste tungsten - nickel catalyst to prepare sodium tungstate. Researchers using waste tungsten - nickel hydrogenation catalyst as raw materials, chemical metallurgy method, and according to the process principle of ion exchange method with leaching liquid, design the secondary resource recycling plan of tungsten to provide a reference for the industrial production practice. The process can be divided into the following steps:
1. Waste tungsten - nickel hydrogenation catalyst contains high sulfur and organic compounds, so it must be removed oil by oxidation to let the carbon and sulfur removal rate reach 99%.
2. Mix the waste catalyst with sodium carbonate. Leach with hot water after a period of time of sodium modifying and roasting. Most of the tungsten oxides go into solution after transforming sodium tungstate. Nickel, iron oxides remain in the residue.
3. After acid leaching, residue is removed nickel, iron and aluminum, then alkali leach by sodium carbonate. The filtrate merges into the main process and the silicon residue can be directly landfill at this time.
4. The leaching filtrate through ion exchange adsorption, desorption, the high concentration of sodium tungstate solution can be got. Sodium tungstate can be obtained by crystallization and recrystallization.

Gold And Tungsten Gold-plated "Rusty" Reasons

The glistening gold shops on the market everywhere sufficiently show the likability of a variety of people for gold products, but recent years, because of the problem of “rusty”, the quality of gold products was suspected by many people. They think the reason for affecting the quality of the gold products is the shorting purity of gold. But what is the real reason for the golden and brighten gold and gold-plated tungsten products were rusted? Is it the reason of gold purity that produces those rust?
 
It’s well known that the gold has weaken metal activity but high corrosion resistance, which makes its chemical properties steadily, and therefore it will not cause the problem of “rusty” when existed by the form of simple substance in nature. But the chemical affinity of gold and sulfide is strong, and therefore its stable chemical properties will be changed along with the adjunction of metals and the other problems produced in the production process when  manufacturing the gold into a wide variety of shapes, handicrafts and jewelries. These problems include: the improper cleaning of gold in the production process, dust or other impurities intake during production process, prolonged exposure to air and light and so on. As for the tungsten gold-plated products, the reasons for being rusted dues to the improper store of gold plating solution in the gold-plating process and the adjunction content of other metals in the gold plating solution. These problems will make the gold-plated tungsten products’ surface rust, thereby greatly reducing the aesthetic and ornamental of the products. Thus, the "Rusty" surface of gold and tungsten gold-plated production does not prove the view of shorting purity of gold. It reminds us that should pay more attention to maintain the gold and tungsten gold-plated products, for avoiding the generation of rust.
rusty gold products

 

 

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