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1, phosphomolybdic acid
Phosphomolybdic acid is a catalyst for the ammoxidation of propylene to produce acrylonitrile. It plays an important role in the processing of synthetic fibers. It is also a raw material for silk and leather weighting agents, organic pigments, and analytical reagents.
The phosphomolybdic acid has a molecular formula of H 3 PO 4 ·12MoO 3 ·30H 2 O, and is soluble in water, ethanol, and diethyl ether. The density was 2.53 g/cm 3 and the melting point was 78 °C. It is yellow to orange crystal.
Main raw materials: molybdenum trioxide and phosphoric acid. The reaction formula is:
12MoO 3 +H 3 PO 4 +xH 2 O
boiled
H 3 PO 4 ·12MoO 3 ·xH 2 O
→
Production process: according to MoO 3 : water = 1:10 solid-liquid ratio is evenly stirred, adding 85% phosphoric acid, the amount of addition is calculated according to MoO 3 : H 3 PO 4 = 12: lmol number. Steam is introduced to boil the solution for 3 hours. When heating, the steam pressure should be controlled to make the solution boil smoothly. Do not bump. Also continue to replenish the water to maintain the initial liquid level. Before the reaction, the solution was milky white of MoO 3 , the reaction initially turned golden yellow, and later turned green, and the pH was 1.0 at the end of the reaction. Separation of liquid and solid, discarding filter residue (for recycling). The filtrate was firstly added with 30% hydrogen peroxide, and the color of the solution turned from green to yellow. The concentrated solution was evaporated (temperature 106 ° C), and the solution was cooled and crystallized to obtain a product flow as shown in FIG.
Figure 1 Phosphomolybdic acid production process
2, cobalt -molybdenum catalyst
When using natural gas , oil gas, oil and gas, coke oven gas or light oil as raw materials to produce synthetic ammonia, the sulfur content in gas and oil is required to be <0.3ppm. In the desulfurization, the inorganic sulfur can be completely removed by the desulfurizing agent, and the removal of the organic sulfur is difficult. To this end, it is necessary to use a molybdenum-based catalyst to hydrogenate organic sulfur to inorganic sulfur (H 2 S) and then remove it. The reaction formula is:
CS 2 +4H 2 →CH 4 +2H 2 S
COS+4H 2 →CH 4 +H 2 S+H 2 O
C 2 H 5 SH+H 2 →C 2 H 6 +H 2 S
Hydrodesulfurization catalyst based molybdenum, cobalt, nickel, iron, vanadium cocatalyst, an aluminum oxide as carrier. The application was originally cobalt-molybdenum. Iron-molybdenum or nickel-molybdenum is also useful now. Its composition changes and its structure is complicated. According to Richardson's research, the catalyst active is MoS 2 activated by active Co x , and Co x /Mo=0.18 is preferred. The form of the combination of the catalyst components, regardless of the form, must be sufficiently pre-vulcanized prior to hydrodesulfurization. [next]
There are three production processes for hydrodesulfurization of cobalt-molybdenum or nickel-molybdenum catalysts:
(1) Dry mixing method: Mix ammonium molybdate, cobalt nitrate or nickel nitrate with dry г-Al 2 O 3 or Al 2 O 3 ·3H 2 O in a ball mill (dry method), add binder or lubricate The agent and a certain amount of water are formed by pelletizing (extrusion or tableting), and the calcination causes the salt to decompose and leave the oxide. The process is shown in Figure 2.
Figure 2 dry mixing process
(2) Precipitation method: aluminum hydroxide gel, ammonium ammonia solution of ammonium molybdate and cobalt nitrate or nickel nitrate solution by addition, reverse addition or addition, neutralizing precipitation to form CoMoO 4 or NiMoO 4 , precipitated in aluminum hydroxide On the gel. After being stirred, aged, filtered, dried, formed, and finally calcined and decomposed, the process is shown in FIG.
Figure 3 Precipitation process
(3) Impregnation method: an alumina carrier and a solution reacted with molybdenum, cobalt (or nickel) salts, respectively, were prepared. The alumina support is immersed in a solution, filtered, dried, calcined and decomposed, and sieved into a final product. The process is shown in Figure 4.
Figure 4 Impregnation process