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一、原料:1.三氯乙醛,2.三氯化磷,3.甲醇。二、器材:1.反应器,2.安气漏斗(不用也可),3.加料漏斗,4.冷凝管,5.百度表,6.五个带橡皮塞瓶子,7.橡皮管及玻璃按合管,8.搅拌器(土造竹板代替也可).三、制作步骤方法:1.将14.7份三氯乙醛放入干燥的反应器中,以冰盐水冷却到10℃左右,缓缓加入14.1份三氯化磷并边加搅拌,搅拌后仍保持温度10℃以下.2.自加料漏斗加入11份的甲醇,此时要越快越好。但要注意勿使反应温度超过2O℃。3.加甲醇时有大量盐酸及氯甲烷气体放出,利用导管经过安全瓶转到盐酸吸收器中(瓶内放水),使盐酸溶解于水,氯甲烷不溶于水,自排气
First, raw materials: 1. Chloral, 2. Phosphorus trichloride, 3. Methanol. Second, the equipment: 1. Reactor, 2. An air funnel (not available), 3. Adding funnel, 4. Condensing tube, 5. Baidu table, 6. Five with rubber stopper bottle, 7. Rubber tube and glass According to the co-pipe, 8. Stirrer (bamboo soil can also be replaced.) Third, the production steps and methods: 1. 14.7 parts of trichloroacetaldehyde into a dry reactor cooled to about 10 ℃ with ice brine, Slowly add 14.1 parts of phosphorus trichloride and stirring, stirring still keep the temperature below 10 ° C. Add 11 parts of methanol from the addition funnel, the faster the better. But be careful not to make the reaction temperature exceeds 2O ℃. 3. When adding methanol, a large amount of hydrochloric acid and methyl chloride gas release, the use of catheters through the safety bottle into the hydrochloric acid absorber (bottle water), so that hydrochloric acid dissolved in water, methyl chloride insoluble in water, since the exhaust