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安基磺酸的合成方法!
来源:http://www.jnjrh.com 日期:2019-03-05 发布人:admin
1.氨基磺酸的生产办法许多,有二氧化硫与羟胺或丙酮肟为质料的羟胺法,亚硫酸或硫酸盐与液氨为质料的氨化法,尿素与为质料的氯磺化法。
1. There are many production methods of aminosulfonic acid, such as hydroxylamine method with sulfur dioxide and hydroxylamine or acetone oxime as the material, ammoniation method with sulfite or sulfate and liquid ammonia as the material, and chlorosulfonation method with urea and chlorosulfonic acid as the material.
以发烟硫酸和尿素为质料的发烟硫酸法,尿素、三氧化硫和硫酸为质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。
The fuming sulfuric acid method with fuming sulfuric acid and urea as materials, the sulfuric acid method with urea, sulfur trioxide and sulfuric acid as materials, the fuming sulfuric acid method (also called liquid phase method), and the gas phase method with gasification of liquid ammonia and reaction of sulfur trioxide under gas phase conditions, etc.
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组成的氨化法两种。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制品。质料消耗定额:尿素2000kg/t、发烟硫酸1500kg/t。
There are two processes of industrial significance at home and abroad: fuming sulfuric acid process and ammoniation process, which is directly composed of sulfur trioxide and ammonia. Sulfonated urea and fuming sulfuric acid at 40-70 C to produce crude aminosulfonic acid, then added water to crystallize to produce aminosulfonic acid products. Material consumption quota: urea 2000 kg/t, fuming sulfuric acid 1500kg/t.
2.其组成办法首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响器内壁需常常整理。生产成本高。长处是产品纯度高。厂家选用的多为液相法。
2. Gas phase method and liquid phase method are the main methods of its composition. 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. The production cost is high. The advantage is that the product is of high purity. The liquid phase method is mostly used by manufacturers.
3.将过量的发烟硫酸参加反响釜中,拌和降温至20~40 ℃,开端参加按比例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。
3. Adding excessive fuming sulfuric acid to the reactor, mixing and cooling to 20-40 C, and starting with the proportionally mixed sulfuric acid and urea. After feeding, mix at 20 C for 8 hours. 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,制取少数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。将带有机械拌和设备的圆底烧瓶置于流水浴中。
4. Aminosulfonic acid is the adduct of strong Lewis acid SO3 and strong Lewis base NH3. When preparing a few high purity amino sulfonic acid, it can react directly with ammonia with high purity SO3 under absolutely anhydrous conditions. If the dosage is large, the reaction between urea and fuming sulfuric acid can be used. Place the round bottom flask with mechanical mixing equipment in the running water bath.
向其间参加560g 100%的硫酸,在强烈拌和下将100g尿素分屡次(约45min加完)渐渐参加到硫酸中,注意不要使温度超过40℃。然后向其间参加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,先用纯硫酸洗刷,再用50%的硫酸洗刷,最后用冷的甲醇洗刷。
Participate in 560g 100% sulphuric acid, mix 100g urea several times (about 45 minutes) and gradually participate in sulphuric acid. 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,反响结束后,冷却至5℃,过滤,所得结晶离心甩干后,用5%乙醇洗刷,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 and gradually participating in urea, the temperature is controlled at 60-65 and holding for 3H after adding, then heating to 80-85 and holding for 2h. After reaction, cooling to 5 and filtering, the obtained crystals are centrifugally dried, washed with 5% ethanol, recrystallized with distilled water, and refined to obtain amino sulfonic acid.