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氨基磺酸在制作合成的过程中应该注重哪些配比?
来源:http://www.jnjrh.com 日期:2019-08-12 发布人:admin
1.氨基磺酸的消费办法很多,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响的气相法等。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℃下停止磺化生成氨基磺酸粗品,然后加水停止结晶制得氨基磺酸废品。原料耗费定额:尿素2000kg/t、发烟硫酸1500kg/t。
1. There are many ways to consume aminosulfonic acid, such as 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. The method includes fuming sulfuric acid method (also known as liquid phase method) and gas phase method in which liquid ammonia is gasified and sulfur trioxide reacts under gas phase conditions. The industrial processes at home and abroad are fuming sulfuric acid process and ammoniation process of direct synthesis of sulfur trioxide and ammonia. The sulfonation of urea and fuming sulfuric acid stopped at 40-70 (?) C to produce crude sulfamic acid, and then stopped crystallizing with water to produce sulfamic acid waste. Material consumption quota: urea 2000 kg/t, fuming sulfuric acid 1500kg/t.
工业硫酸
Industrial sulphuric acid
2.其合成办法主要有气相法和液相法两种。气相法操作条件苛刻,设备材质请求高。副产品多,且氨基酸易粘附在反响器内壁需经常清算。消费本钱高。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 the amino acids are easy to adhere to the inner wall of the reactor and need to be cleared frequently. Consumption costs are high. The advantage is that the product has high purity. Most of the methods used by manufacturers are liquid phase method.
3.将过量的发烟硫酸参加反响釜中,搅拌降温至20~40 ℃,开端参加按比例混合好的硫酸和尿素。加料完毕后,在20 ℃左右搅拌8 h。再逐步升温至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,脱水枯燥得高纯度精品氨基磺酸。
氨基磺酸
3. Participate excessive fuming sulfuric acid in the reactor, stirring and cooling to 20-40 C, and start to participate in proportionally mixed sulfuric acid and urea. After the feeding is finished, stir for 8 hours at 20 C. Then the temperature is gradually raised to 70-90 C, sulfur trioxide is evaporated, and crystallization is cooled. After solid-liquid sharing, crude aminosulfonic acid was obtained, recrystallized with water, and dehydrated to obtain high-purity high-quality aminosulfonic acid.
4.氨基磺酸是强Lewis酸SO3与强Lewis碱NH3的加合物,制取少量纯度请求高的氨基磺酸时,可在完整无水的条件下,直接用高纯度的SO3与氨反响。若用量较大时可用尿素与发烟硫酸反响来制取。将带有机械搅拌安装的圆底烧瓶置于流水浴中,向其中参加560g 100%的硫酸,在激烈搅拌下将100g尿素分屡次(约45min加完)渐渐参加到硫酸中,留意不要使温度超越40℃。然后向其中参加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响混合物,先用纯硫酸洗濯,再用50%的硫酸洗濯,后用冷的甲醇洗濯。
4. Aminosulfonic acid is the adduct of strong Lewis acid SO3 and strong Lewis base NH3. When a small amount of ammonia sulfonic acid with high purity is prepared, it can react directly with ammonia with high purity SO3 under complete anhydrous condition. If the dosage is large, the reaction between urea and fuming sulfuric acid can be used. Put the round bottom flask with mechanical stirring installation in the running water bath. Participate 560g 100% sulfuric acid in the flask. Under intense stirring, add 100g urea fraction (about 45 minutes) to the sulfuric acid gradually. Be careful not to make the temperature exceed 40 C. Then, 309g fuming sulfuric acid (containing 65% free SO3) was added and placed for 16 hours at 42-45 C. The reaction mixture is filtered by glass sand funnel. First, it is 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℃,渐渐参加尿素,温度控制在60~65℃,加完后保温3H,然后升温至80~85℃,保温2h,反响完毕后,冷却至5℃,过滤,所得结晶离心甩干后,用5%乙醇洗濯,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, gradually participating in urea, the temperature is controlled at 60-65 C, after adding, the temperature is kept for 3H, then rising to 80-85 C, holding for 2h. After the reaction is completed, the crystals are cooled to 5 C and filtered. After centrifugal drying, the crystals are washed with 5% ethanol, and recrystallized with distilled water to purify amino sulfonic acid. Product.
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