摘要：【中文】本发明公开了一种从三嗪环制备3‑巯基‑5‑甲基‑1,2,4‑三氮唑的方法，依次包括下列步骤：（1）取三嗪环溶解在水中得到三嗪环溶液；（2）向三嗪环溶液中加酸调节溶液pH值至2‑3；（3）升温回流；（4）回流结束后，降温固液分离得滤液；（5）滤液进行减压蒸馏，蒸馏至出现白色固体；（6）降温固液分离，得固体料；（7）烘干得3‑巯基‑5‑甲基‑1,2,4‑三氮唑。本发明以三嗪环为原料通过转化制备3‑巯基‑5‑甲基‑1,2,4‑三氮唑，其工艺流程简单，收率高，产生的三废少，对环境污染小，是一种高效安全的制备新方法。 【EN】The invention discloses a method for preparing 3-mercapto-5-methyl-1, 2, 4-triazole from triazine ring, which comprises the following steps in sequence: (1) dissolving triazine ring in water to obtain a triazine ring solution; (2) adding acid into the triazine ring solution to adjust the pH value of the solution to 2-3; (3) heating and refluxing; (4) after the reflux is finished, cooling and carrying out solid-liquid separation to obtain filtrate; (5) carrying out reduced pressure distillation on the filtrate until white solid appears; (6) cooling, carrying out solid-liquid separation to obtain a solid material; (7) drying to obtain the 3-mercapto-5-methyl-1, 2, 4-triazole. The method takes triazine ring as a raw material to prepare the 3-mercapto-5-methyl-1, 2, 4-triazole through conversion, has simple process flow, high yield, less three wastes and little environmental pollution, and is a novel, efficient and safe preparation method.

摘要：【中文】本发明公开了一种合成2‑甲基氨基硫脲的方法，按照一定比例向四口瓶内加入硫氰酸铵、甲基肼水溶液，负压升温，60‑70℃出现回流，80℃开始8:1采氨水；温度升至100‑102℃时，向四口瓶内滴加一定量甲苯，通过回流管路，甲苯回四口瓶内，氨水进中间瓶，滴加完毕后继续升温至108‑110℃保温2h，然后减压蒸甲苯，将四口瓶内甲苯蒸干，然后加入一定量纯净水，进行精制，升温至90℃，保温0.5h，然后降温至30℃抽滤、烘干得2‑甲基氨基硫脲。采用本发明的方法，甲基肼的转化率高，2‑甲基氨基硫脲收率高达95％以上，比传统工艺提高6‑8％。 【EN】The invention discloses a method for synthesizing 2-methyl thiosemicarbazide, which comprises the steps of adding ammonium thiocyanate and methyl hydrazine aqueous solution into a four-mouth bottle according to a certain proportion, heating under negative pressure, refluxing at 60-70 ℃, and collecting ammonia water at the temperature of 80 ℃ in a ratio of 8: 1; when the temperature is raised to 100-. By adopting the method, the conversion rate of the methylhydrazine is high, and the yield of the 2-methyl thiosemicarbazide is up to more than 95 percent, which is improved by 6 to 8 percent compared with the traditional process.

摘要：【中文】本发明公开了一种三嗪环残渣分解回收甲基肼的方法，向反应瓶中加入三嗪环残渣、水和铜盐，开启搅拌，升温至80‑130℃反应2‑5h，随着反应进行，从反应瓶中蒸馏采出馏分，馏分加入碱后进行蒸馏，蒸出成分为甲基肼和水的混合物。本发明将副产物三嗪环残渣水解回收甲基肼并用于合成2‑甲基氨基硫脲的合成，进一步合成三嗪环，废物资源化利用，解决三嗪环残渣工业化难处理的问题，实现三嗪环残渣到甲基肼再到三嗪环循环再生。不使用溶剂，免去了有机溶剂易燃易爆、成本高的缺点；原材料只有三嗪环残渣和水反应，铜盐作为催化剂，回收产出甲基肼，并将三嗪环残渣水解为小分子盐，易于处理，安全环保，成本低，适合工业化生产。 【EN】The invention discloses a method for decomposing and recycling methyl hydrazine in triazine ring residues, which comprises the steps of adding the triazine ring residues, water and copper salt into a reaction bottle, starting stirring, heating to 80-130 ℃ for reaction for 2-5h, distilling a fraction from the reaction bottle along with the reaction, adding alkali into the fraction, and distilling to obtain a mixture of methyl hydrazine and water. According to the method, the by-product triazine ring residue is hydrolyzed to recover the methyl hydrazine and is used for synthesizing the 2-methyl thiosemicarbazide, so that the triazine ring is further synthesized, the waste is recycled, the problem that the industrial treatment of the triazine ring residue is difficult is solved, and the cyclic regeneration of the triazine ring residue from the methyl hydrazine to the triazine ring is realized. No solvent is used, so that the defects of flammability and explosiveness and high cost of an organic solvent are avoided; the raw materials only react with water in the triazine ring residue, copper salt is used as a catalyst, methyl hydrazine is recovered and produced, and the triazine ring residue is hydrolyzed into small molecular salt, so that the method is easy to treat, safe, environment-friendly, low in cost and suitable for industrial production.