Synthesis of nickel sulfamate (non cyanide alkali copper)

2018-01-29 1851

1. There are many production methods of aminosulfonic acid, including hydroxylamine method with sulfur dioxide and hydroxylamine or acetone oxime as raw materials, ammoniation method with sulfite or sulfate and liquid ammonia as raw materials, chlorosulfonation method with urea and chlorosulfonic acid as raw materials, fuming sulfuric acid method with fuming sulfuric acid and urea as raw materials, urine Sulfuric acid method and fuming sulfuric acid method (also known as liquid phase method) using sulfur trioxide and sulfuric acid as raw materials, and gas phase method in which liquid ammonia reacts with sulfur trioxide under gas phase conditions through gasification. The processes with industrial significance at home and abroad include fuming sulfuric acid method and ammoniation method of direct synthesis of sulfur trioxide and ammonia. The crude sulfamic acid is produced by sulfonation of urea and fuming sulfuric acid at 40-70 ℃, and then water is added to crystallize to obtain sulfamic acid products. Material consumption quota: urea 2000kg / T, fuming sulfuric acid 1500kg / T.

2. Its synthesis methods mainly include gas phase method and liquid phase method. The operation conditions of gas phase method are strict and the requirements for equipment and raw materials are high. There are many by-products and amino acids are easy to adhere to the inner wall of the reactor, which needs to be cleaned frequently. The production cost is high. The advantage is the high purity of the product. The liquid phase method is mostly used by the manufacturer.
3.将过量的发烟硫酸加入反应釜中,拌和降温至20~40 ℃,开端加入按份额混合好的硫酸和尿素。加料结束后,在20 ℃左右拌和8 h。再逐步升温至70~90 ℃,蒸出三氧化硫,冷却析晶。固液共享后得粗氨基磺酸,用水重结晶,脱水枯燥得高纯度精品氨基磺酸。

4. Aminosulfonic acid is the adduct of strong Lewis acid SO3 and strong Lewis base NH3. When preparing a few aminosulfonic acids with high purity requirements, high purity SO3 can be directly reacted with ammonia under the condition of complete anhydrous. If the dosage is large, it can be prepared by reacting urea with fuming sulfuric acid. Place the round bottom flask with mechanical mixing equipment in the running water bath, add 560g of 100% sulfuric acid to it, and gradually add 100g of urea into the sulfuric acid repeatedly (about 45min) under intense mixing. Be careful not to make the temperature exceed 40 ℃. Then, 309 g of fuming sulfuric acid (containing 65% free SO3) was added thereto and placed at a temperature of 42 to 45. D egree. C. for 16 hours. Filter the reaction mixture with a glass sand core funnel, wash it with pure sulfuric acid, then with 50% sulfuric acid, and finally with cold methanol.

5. Heat 20% fuming sulfuric acid to 30 ° C, gradually add urea, control the temperature at 60-65 ° C, keep it warm for 3h after adding, then heat it to 80-85 ° C and keep it warm for 2h. After the reaction is completed, cool it to 5 ° C and filter it. After the obtained crystals are centrifugally dried, wash them with 5% ethanol, and then re crystallize and refine them with distilled water to obtain pure sulfamic acid.

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