The device uses chlorine gas and hydrogen gas as raw materials, and integrates hydrochloric acid synthesis, absorption and exhaust gas treatment into a four-in-one graphite synthesis furnace to produce high-purity hydrochloric acid.The device has the following features:
The gas synthesis section, the gas absorption section, the cooling acid producing section and the exhaust gas absorption section are stacked successively from the bottom to the top.Chlorine gas and hydrogen gas enter the furnace from the bottom, and generate hydrogen chloride in the form of a combustion reaction in the synthesis furnace.The flame central temperature is above 2500 ℃ , and the generated hydrogen chloride gas temperature is above 2000 ℃.In the high temperature synthesis furnace section, a steel water-cooled fireplace cylinder is used, and the pressure of the byproduct steam is 1.4 MPa.
The residue was taken up in 1000ml water, acidified by the addition of conc. HCl, and washed with 3×50ml DCM, basified with 25% NaOH, and extracted with 3×100ml DCM. The combined DCM extracts were dried over MgS04, filtered and the solvent distilled off. The residue was distilled twice under aspirator vacuum at 100-110°C to give 14.65g (67%) of methacrylamide freebase as a water-white oil. The hydrochloride salt can be prepared by dissolving the oil in 10× the volume of diethyl ether and gassing the solution with dry HCl gas until no more precipitate forms. The methacrylamide hydrochloride is filtered off with suction and washed with diethyl ether and air dried.
将残渣放置于1000ml水中，加入浓盐酸进行酸化。然后用3×50毫升二氯甲烷进行冲洗,再用25%氢氧化钠溶液碱化,然后用3×100毫升的二氯甲烷萃取。用MgS04干燥含有二氯甲烷的萃取物，过滤并蒸馏溶剂至蒸干。残渣需要蒸馏两次，真空吸引器的温度设定在100 - 110°C之间，提供14.65克(67%)的甲基丙烯酰胺游离碱作为水白油。盐酸盐可以由如下方法制备：将水白油溶解于10×体积的二乙醚中，然后通入干燥的盐酸气,直到没有更多的沉淀形成。将甲基丙烯酰胺盐酸盐抽吸过滤，乙醚洗涤，风干。