Name : Sulfamic acid
English Name : ACETO ACID; AMIDOSULFONIC ACID; AMIDOSULFURIC ACID; AMINOSULFONIC ACID; BETZ 0254; SULFAMIDIC ACID; SULFAMINIC ACID; SULPHAMIC ACID; aminosulfuricacid; Imidosulfonic acid; Jumbo; Kyselina amidosulfonova; Kyselina sulfaminova; kyselinaamidosulfonova; kyselinaamidosulfonova (czech); kyselinasulfaminova; kyselinasulfaminova (czech); sulfamic; sulphamidic acid
Grade : AR
CAS No. :5329 -14-6 [ 1 ]
Formula : H3NO3S
Weight: 97.09
supplies: http://www.lubonchem.com
No. MDL: MFCD00011603
EC Number: 226-218-8
2 Products
Raw materials : urea, fuming sulfuric acid, chlorosulfonic acid
Preparation Products : cobalt sulfamate , nickel sulfamate , Acid Green 20 , cyclamate, detergents, alkali superplasticizer , affinity of the toner , ammonium sulfamate , strong detergents , cleaning agents
Characters
Colorless or white crystals , soluble in water, slightly soluble in ethanol and methanol, slightly soluble in acetone, ether insoluble in aqueous solution gradually break down into ammonium bisulfate , water solubility :. 146.8 g / l (20 ℃)
Physical parameters
Melting point : 215-225 ℃
Storage and transportation
Sealed dry place.
Instructions for use
Standard amount of the base titration , complexation masking agents , organic trace analysis of nitrogen and sulfur determination criteria .
Hazard statement
Dangerous code : Xi
Hazard Class : R36/38- R52/53
Security Level : S26-S28-S61
3 Synthetic Method
An amino acid produced in many ways, sulfur dioxide or acetone oxime with hydroxylamine as raw material hydroxylamine , sulfite or sulfate and ammonia as raw materials ammoniting , urea and chlorine acid as raw materials sulfochlorination law , fuming sulfuric acid and urea as raw fuming sulfuric acid , urea , sulfur trioxide and sulfuric acid as raw materials and fuming sulfuric acid method (also known as liquid phase ) and ammonia via gasification and sulfur trioxide in Gas under vapor phase reaction conditions and the like. Domestic and industrial significance of the process has to send two amination with ammonia and direct synthesis of sulfur trioxide fuming sulfuric acid method. Urea is sulfonated with fuming sulfuric acid to form an amino acid in the crude 40-70 ℃, and then water was added for crystallization to obtain the amino acid product. Consumption of raw materials fixed: Urea 2000kg / t, oleum 1500kg / t.
2 , there are two main methods synthesis gas and liquid method. Fumed harsh operating conditions , equipment material requirements . Byproducts and more easily adhere to the amino acids and the reactor wall need regular cleaning. High production costs . The advantage is the high product purity. Manufacturers use mostly liquid phase .
3 excess fuming sulfuric acid in the reaction vessel , cooled with stirring to 20 ~ 40 ℃, start adding the mixed proportion of urea and sulfuric acid . After completion of the addition , stirring at about 20 ℃ 8 h. Then gradually warmed to 70 ~ 90 ℃, distilled sulfur trioxide , cooling crystallization . The crude obtained after the solid-liquid share amino acid, and recrystallized from water , dehydrated and dried to obtain a high-purity quality amino acid.
Four amino acid is a strong Lewis acid and a strong Lewis base NH3 SO3 adduct , prepared a small amount of high purity when the amino acid , in a completely anhydrous conditions , with high purity directly by reaction with ammonia SO3 . If a larger amount of urea is available with fuming sulfuric acid reaction to the system. The round bottom flask equipped with a mechanical stirrer was placed in the water bath , to which was added 560g 100% sulfuric acid under vigorous stirring to 100g of urea times ( about 45min plus End ) was slowly added to sulfuric acid , being careful not the temperature exceed 40 ℃. Then thereto was added 309g of fuming sulfuric acid ( containing 65 % free SO3), and 16h is placed at a temperature of 42 ~ 45 ℃ . Filtered through a glass frit funnel the reaction mixture was washed first with pure sulfuric acid , washed with 50% sulfuric acid , washed with cold methanol and finally with .
5 heating oleum 20% to 30 ℃, urea was slowly added , the temperature controlled at 60 ~ 65 ℃, after adding heat 3H, then warmed to 80 ~ 85 ℃, incubated 2h, after the reaction was cooled to 5 ℃, filtration, drying the obtained crystals by centrifugation , washed with 5% ethanol and recrystallized with distilled water and drained after purification to obtain pure amino acid .