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氨基磺酸的合成方法!
来源:http://www.jnjrh.com 日期:2019-04-10 发布人:admin
  1.氨基磺酸的生产方法很多,有二氧化硫与羟胺或丙酮肟为原料的羟胺法,亚硫酸或硫酸盐与液氨为原料的氨化法,尿素与氯磺酸为原料的氯磺化法,以发烟硫酸和尿素为原料的发烟硫酸法,尿素、三氧化硫和硫酸为原料的硫酸法和发烟硫酸法(又称液相法)和液氨经气化与三氧化硫在气相条件下反应的气相法等。国内外具有工业意义的工艺为发烟硫酸法以及三氧化硫与氨直接合成的氨化法两种。由尿素与发烟硫酸在40-70℃下进行磺化生成氨基磺酸粗品,然后加水进行结晶制得氨基磺酸成品。原料消耗定额:尿素2000kg/t、发烟硫酸1500kg/t。
  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, sulfuric acid method with urea, sulfur trioxide and sulfuric acid as raw materials and fuming sulfuric acid method (also called liquid phase method) and liquid method. The reaction of ammonia with sulphur trioxide in gas phase is studied by gas phase method. The industrial processes at home and abroad are fuming sulfuric acid process and ammoniation process of direct synthesis of sulfur trioxide and ammonia. Sulfonated urea and fuming sulfuric acid at 40-70 ~C to produce crude sulfamic acid, then added water to crystallize to produce sulfamic acid products. Material consumption quota: urea 2000 kg/t, fuming sulfuric acid 1500 kg/t.
  2.其合成方法主要有气相法和液相法两种。气相法操作条件苛刻,设备材质要求高。副产品多,且氨基酸易粘附在反应器内壁需经常清理。生产成本高。优点是产品纯度高。厂家采用的多为液相法。
  2. The main synthetic methods are gas-phase method and liquid-phase method. The operation conditions of gas phase method are harsh and the material requirements of equipment are high. There are many by-products, and amino acids are easy to adhere to the inner wall of the reactor and need to be cleaned regularly. The production cost is high. The advantage is that the product has high purity. Most of the methods used by manufacturers are liquid phase method.
  3.将过量的发烟硫酸加入反应釜中,搅拌降温至20~40 ℃,开始加入按比例混合好的硫酸和尿素。加料结束后,在20 ℃左右搅拌8 h。再逐渐升温至70~90 ℃,蒸出三氧化硫,冷却析晶。固液分享后得粗氨基磺酸,用水重结晶,脱水干燥得高纯度精品氨基磺酸。
  3. Adding excessive fuming sulfuric acid to the reactor, stirring and cooling to 20-40 C, then adding proportionally mixed sulfuric acid and urea. After feeding, stir for 8 hours at 20 C. Then the temperature gradually rises to 70-90 C. Sulfur trioxide is evaporated and cooled to crystallize. After solid-liquid sharing, crude aminosulfonic acid was obtained, recrystallized with water and dehydrated to obtain high-purity and high-quality aminosulfonic acid.
氨基磺酸
  4.氨基磺酸是强Lewis酸SO3与强Lewis碱NH3的加合物,制取少量纯度要求高的氨基磺酸时,可在完全无水的条件下,直接用高纯度的SO3与氨反应。若用量较大时可用尿素与发烟硫酸反应来制取。将带有机械搅拌装置的圆底烧瓶置于流水浴中,向其中加入560g 100%的硫酸,在强烈搅拌下将100g尿素分多次(约45min加完)慢慢加入到硫酸中,注意不要使温度超过40℃。然后向其中加入309g发烟硫酸(含65%游离SO3),并在42~45℃的温度下放置16h。用玻璃砂芯漏斗过滤反应混合物,先用纯硫酸洗涤,再用50%的硫酸洗涤,最后用冷的甲醇洗涤。
  4. Aminosulfonic acid is the adduct of strong Lewis acid SO3 and strong Lewis base NH3. When a small amount of high purity sulfonic acid is prepared, it can react directly with ammonia with high purity SO3 under completely anhydrous conditions. When the dosage is large, urea can be prepared by reacting with fuming sulfuric acid. Put the round bottom flask with mechanical stirring device in the running water bath, add 560g 100% sulfuric acid to it, add 100g urea into sulfuric acid several times (about 45 minutes) under strong stirring, and take care not to make the temperature exceed 40 C. Then 309g fuming sulfuric acid (containing 65% free SO3) was added to the mixture and placed for 16 hours at 42-45 C. The reaction mixture was filtered by a glass sand funnel. First, the mixture was washed with pure sulfuric acid, then with 50% sulfuric acid, and finally with cold methanol.
  5.将20%的发烟硫酸加热至30℃,慢慢加入尿素,温度控制在60~65℃,加完后保温3H,然后升温至80~85℃,保温2h,反应结束后,冷却至5℃,过滤,所得结晶离心甩干后,用5%乙醇洗涤,滤干后用蒸馏水重结晶精制,得氨基磺酸纯品。
  5. Heating 20% fuming sulfuric acid to 30 C, adding urea slowly, controlling the temperature at 60-65 C, holding for 3H after adding, then heating to 80-85 C, holding for 2h. After reaction, cooling to 5 C, filtering, the obtained crystals were centrifugally dried, washed with 5% ethanol, recrystallized with distilled water, and refined to obtain amino sulfonic acid.