摘要：【中文】本发明涉及化工领域，公开了一种合成噁二嗪的方法，包括以下步骤：反应釜中加入多聚甲醛、清水和催化剂，反应釜升温至80℃反应，多聚甲醛水解为甲醛，保温2h，保温2h结束后，加入甲胍继续保温反应15h，保温反应结束后，将反应釜温度降至10℃，将反应釜中的反应结束的物料取出进行过滤，过滤出噁二嗪固体，将噁二嗪固体用清水洗涤，将洗涤干净的噁二嗪固体烘干，得到成品噁二嗪，将滤液进行浓缩，进行回收利用。本发明的有益效果：多聚甲醛和甲胍在对甲苯磺酸的催化下合成的噁二嗪，经过滤、洗涤和干燥，得到的噁二嗪的纯度提高，噁二嗪的产率也提高了，使得催化剂和多聚甲醛的回收率提高，合成方法安全，适用于工业生产。 【EN】The invention relates to the field of chemical industry, and discloses a method for synthesizing oxadiazine, which comprises the following steps: polyformaldehyde, clear water and a catalyst are added into a reaction kettle, the reaction kettle is heated to 80 ℃ for reaction, paraformaldehyde is hydrolyzed into formaldehyde, the heat is preserved for 2 hours, after the heat preservation for 2 hours is finished, methylguanidine is added to continue the heat preservation reaction for 15 hours, after the heat preservation reaction is finished, the temperature of the reaction kettle is reduced to 10 ℃, materials after the reaction in the reaction kettle is finished are taken out for filtering, an oxadiazine solid is filtered out, the oxadiazine solid is washed by the clear water, the washed oxadiazine solid is dried to obtain a finished product of oxadiazine, and the filtrate is concentrated and recycled. The invention has the beneficial effects that: the purity of the obtained oxadiazine is improved and the yield of the oxadiazine is also improved through filtering, washing and drying the oxadiazine synthesized by paraformaldehyde and methylguanidine under the catalysis of p-toluenesulfonic acid, so that the recovery rate of the catalyst and paraformaldehyde is improved, and the synthesis method is safe and suitable for industrial production.

摘要：【中文】本发明涉及一种粒径小于4.0um的超细硝基胍的合成方法，该合成方法的具体步骤如下：S1：反应釜中加入硫酸，分批次投入硝酸胍，过程控制温度稳定在40～45℃之间，制得硝基胍粗胍；S2：水解釜中准备清水，使硝基胍与水之间满足一定的重量比例，打开釜夹套冷冻，降温至≤10℃，投入前一步反应产物硝基胍粗胍，制得硝基胍物料；S3：硝基胍物料通过分布器，带机真空脱水，清水漂洗；S4：将清水漂洗后的物料进打浆槽，与离心母液和蒸发水混合打浆，去离心，得到目标产品，送样检测，合格后打包入库。本发明的优点在于：本发明制备方法安全、环保，适用于工业生产，通过本发明合成方法合成的超细硝基胍粒径达到4.0um以下，超细硝基胍收率达到80%左右。 【EN】The invention relates to a method for synthesizing superfine nitroguanidine with a particle size of less than 4.0um, which comprises the following steps: s1: adding sulfuric acid into a reaction kettle, adding guanidine nitrate in batches, and stabilizing the process control temperature at 40-45 ℃ to prepare coarse nitroguanidine; s2: preparing clear water in a hydrolysis kettle to enable nitroguanidine and water to meet a certain weight ratio, opening a kettle jacket for freezing, cooling to be less than or equal to 10 ℃, and adding a reaction product nitroguanidine crude guanidine in the previous step to prepare a nitroguanidine material; s3: the nitroguanidine material passes through a distributor and a belt machine for vacuum dehydration and rinsing by clear water; s4: and (3) feeding the material rinsed with clear water into a pulping tank, mixing with centrifugal mother liquor and evaporated water for pulping, centrifuging to obtain a target product, sending the target product to a sample for detection, and packaging and warehousing after the target product is qualified. The invention has the advantages that: the preparation method is safe and environment-friendly, and is suitable for industrial production, the particle size of the superfine nitroguanidine synthesized by the synthesis method reaches below 4.0um, and the yield of the superfine nitroguanidine reaches about 80%.

摘要：【中文】本发明涉及农药中间体制备技术领域，具体公开了一种合成咪唑烷的方法，向反应釜中加入硝基胍和70％硫酸后升温，同时滴加乙二胺；升温反应后抽负压；过滤得到产品咪唑烷。本发明合成咪唑烷的方法操作简单，而且安全、环保，制作过程中采用硝基胍和硫酸滴，滴加乙二胺进行反应后抽负压得到产品，提高反应速率和产品纯度，降低了生产成本，适用于工业生产。 【EN】The invention relates to the technical field of pesticide intermediate preparation, and particularly discloses a method for synthesizing imidazolidine, wherein nitroguanidine and 70% sulfuric acid are added into a reaction kettle, the temperature is raised, and ethylenediamine is added dropwise; heating for reaction, and then pumping negative pressure; and filtering to obtain the product imidazolidine. The method for synthesizing the imidazolidine is simple to operate, safe and environment-friendly, nitroguanidine and sulfuric acid are adopted in the preparation process, ethylenediamine is dropwise added to react, and then negative pressure is pumped to obtain the product, so that the reaction rate and the product purity are improved, the production cost is reduced, and the method is suitable for industrial production.

摘要：【中文】本发明涉及一种硝酸胍的精制方法，所述精制方法采用93%硝酸胍、自来水、25%氨水和活性炭溶解吸附过滤，具体步骤如下：S1：在反应容器中加入自来水和93%硝酸胍，搅拌均匀，并用25%氨水调PH=8；S2：升温到85‑90℃加入活性炭吸附杂质，继续升温至95‑100℃；S3：在负压条件下热过滤，除去析出物；S4：滤液搅拌降温至≤25℃，析出硝酸胍过滤得潮品硝酸胍去烘干；S5：母液用硝酸调PH=7过滤除去析出物，母液继续循环套用。本发明的优点在于：本发明硝酸胍的精制方法，使用的原料，过程简单、用量少，处理过程用时短，设备利用率高，处理后的水，可继续循环使用，处理后的硝酸胍摩尔收率90%，含量达到99.3%，且制备方法安全、环保，适用于工业生产。 【EN】The invention relates to a method for refining guanidine nitrate, which adopts 93 percent of guanidine nitrate, tap water, 25 percent of ammonia water and activated carbon to dissolve, adsorb and filter, and comprises the following steps: s1: adding tap water and 93% guanidine nitrate into a reaction container, uniformly stirring, and adjusting the pH value to be =8 by using 25% ammonia water; s2: heating to 85-90 deg.C, adding active carbon to adsorb impurities, and heating to 95-100 deg.C; s3: hot filtering under negative pressure to remove precipitate; s4: stirring the filtrate, cooling to less than or equal to 25 ℃, separating out guanidine nitrate, filtering to obtain a damp product guanidine nitrate, and drying; s5: adjusting the pH of the mother liquor to =7 by using nitric acid, filtering to remove precipitates, and continuously recycling the mother liquor. The invention has the advantages that: the method for refining guanidine nitrate has the advantages of simple process, less consumption, short treatment process, high equipment utilization rate, capability of continuously recycling treated water, 90 percent of molar yield of the treated guanidine nitrate and 99.3 percent of content of the treated guanidine nitrate, safe and environment-friendly preparation method and suitability for industrial production.

摘要：【中文】本发明涉及一种柠檬醛的制备方法，该制备方法包括如下步骤：S1：在圆底烧瓶中依次加量溶剂、催化剂和异戊烯醇；S2：开启搅拌使S1中物料搅拌均匀并升温至≥75℃；S3：缓慢滴加异戊烯醛于反应体系中，控制温度不高于75℃；S4：异戊烯醛滴加完毕后，控制反应温度75‑85℃保温8‑10h；S5：保温反应过程中，用溶剂不断将水带出；S6、保温反应结束后，减压蒸出异戊烯醇、异戊烯醛与溶剂；S7：向圆底烧瓶中继续加入碳酸铵，减压升温蒸出轻组分；S8：轻组分蒸出后，将反应液升温≥130℃，反应1‑2h后得到产品柠檬醛。本发明的优点在于：通过本发明制备的柠檬醛产品纯度高、杂质含量少、摩尔收率高，柠檬醛的收率≥95.0%，含量达到98.0%以上，取得了良好的经济效益。 【EN】The invention relates to a preparation method of citral, which comprises the following steps: s1: sequentially adding a solvent, a catalyst and isoamylol into a round-bottom flask; s2: starting stirring to uniformly stir the material in the S1 and heating to more than or equal to 75 ℃; s3: slowly dripping the isoamylene aldehyde into a reaction system, and controlling the temperature to be not higher than 75 ℃; s4: after the dripping of the isopropenylaldehyde is finished, controlling the reaction temperature to be 75-85 ℃ and preserving the heat for 8-10 h; s5: in the process of heat preservation reaction, continuously taking out water by using a solvent; s6, after the heat preservation reaction is finished, decompressing and steaming out the isopentenol, the isopentenal and the solvent; s7: continuously adding ammonium carbonate into the round-bottom flask, and heating under reduced pressure to evaporate light components; s8: after the light components are evaporated, the temperature of the reaction liquid is increased to be more than or equal to 130 ℃, and the citral product is obtained after the reaction is carried out for 1-2 h. The invention has the advantages that: the citral product prepared by the method has high purity, less impurity content and high molar yield, the citral yield is more than or equal to 95.0%, the citral content reaches more than 98.0%, and good economic benefit is obtained.

摘要：【中文】本发明涉及一种1‑氯‑3‑甲基‑2‑丁烯的连续化生产工艺，该连续化生产工艺包括如下步骤：1)原料异戊二烯、浓盐酸及干燥的氯化氢气体经流量计计量后连续送入一级反应釜进行反应；2）一级反应后的反应物料通过釜侧上部溢流管到二级、三级反应釜继续反应；3）三级反应釜溢流至分相器，进行连续分层，上层为氯化液去成品槽，即为1‑氯‑3‑甲基‑2‑丁烯产品，下层为盐酸层，返回反应釜继续套用。本发明的优点在于：本发明通过多级釜式串联反应，实现连续化生产，自动化程度和安全性大大提高，无需使用有机溶剂和催化剂，较现有工艺相比，生产流程大大缩短，设备投资成本低，生产周期短，产品质量稳定等特点。 【EN】The invention relates to a continuous production process of 1-chloro-3-methyl-2-butene, which comprises the following steps: 1) metering isoprene, concentrated hydrochloric acid and dry hydrogen chloride gas by a flowmeter, and continuously feeding into a first-stage reaction kettle for reaction; 2) the reaction materials after the first-stage reaction are continuously reacted through an overflow pipe at the upper part of the side of the kettle to a second-stage reaction kettle and a third-stage reaction kettle; 3) and overflowing the third-stage reaction kettle to a phase separator for continuous layering, wherein the upper layer is chlorinated liquid and is fed to a finished product tank to obtain the 1-chloro-3-methyl-2-butene product, and the lower layer is a hydrochloric acid layer and is returned to the reaction kettle for continuous application. The invention has the advantages that: the invention realizes continuous production through multi-stage kettle type series reaction, greatly improves the automation degree and safety, does not need to use organic solvent and catalyst, and has the characteristics of greatly shortened production flow, low equipment investment cost, short production period, stable product quality and the like compared with the prior art.

摘要：【中文】本发明涉及一种甲基硝基胍的制备方法，该制备方法包括如下步骤：S1：将硝基胍投至已加入水和甲胺的投料釜中；S2：在35‑40℃下，在15‑20min内加入甲胺水溶液，保温结束后，中和，滴加稀硫酸，进行中和；S3：中和结束过滤，粗品与水打浆；S4：甲基硝基胍浆料进入到已加入助滤剂硅藻土的加热溶解釜中，加热，溶解完全后热过滤，滤液在搅拌下冷却、离心得到精制甲基硝基胍潮品，干燥后，得到合格品。本发明的优点在于：本发明采用硝基胍、甲胺、硫酸反应，制备方法安全、环保，适用于工业生产，且通过本发明方法制备得的甲基硝基胍摩尔收率能达80%以上。 【EN】The invention relates to a preparation method of methyl nitroguanidine, which comprises the following steps: s1: adding nitroguanidine into a feeding kettle in which water and methylamine are added; s2: adding methylamine water solution at 35-40 deg.C within 15-20min, keeping the temperature, neutralizing, and dropwise adding dilute sulfuric acid for neutralization; s3: filtering after neutralization, and pulping the crude product with water; s4: and (3) putting the methyl nitroguanidine slurry into a heating and dissolving kettle added with filter aid diatomite, heating, carrying out heat filtration after complete dissolution, cooling and centrifuging the filtrate under stirring to obtain a refined methyl nitroguanidine tide product, and drying to obtain a qualified product. The invention has the advantages that: the method adopts nitroguanidine, methylamine and sulfuric acid for reaction, the preparation method is safe and environment-friendly, and is suitable for industrial production, and the molar yield of the methyl nitroguanidine prepared by the method can reach more than 80%.

摘要：【中文】本发明涉及一种氰基乙酯的制备方法，该制备方法采用钛酸异丙酯作催化剂，使氰基甲酯与乙醇反应得到氰基乙酯，具体包括如下步骤：S1：在精馏塔釜中依次加入氰基甲酯、乙醇和钛酸异丙酯；S2、加热升温使S1中物料反应并继续缓慢加入乙醇；S3、在反应有氰基乙酯生成后，及时采集低于68℃的馏分；S4、定期取精馏塔釜中物料进行气相色谱分析，至氰基甲酯含量为≤2%时，停止反应；S5、反应结束后，塔釜中物料减压蒸馏，回收甲醇与乙醇；S6、将S3中采集的馏分减压蒸馏，分离出低沸物和氰基乙酯成品。本发明的优点在于：本发明制备的氰基乙酯产品纯度高、杂质含量少、摩尔收率高，取得了良好的经济效益。 【EN】The invention relates to a preparation method of cyanoethyl ester, which adopts isopropyl titanate as a catalyst to react methyl cyanoester with ethanol to obtain the cyanoethyl ester, and specifically comprises the following steps: s1: sequentially adding methyl cyanoester, ethanol and isopropyl titanate into a rectifying tower kettle; s2, heating to increase the temperature to enable the materials in the S1 to react, and continuously and slowly adding ethanol; s3, collecting fractions at a temperature lower than 68 ℃ in time after the cyanoethyl ester is generated in the reaction; s4, periodically taking the material in the rectifying tower kettle for gas chromatography analysis, and stopping the reaction until the content of cyanomethyl ester is less than or equal to 2%; s5, after the reaction is finished, carrying out reduced pressure distillation on the materials in the tower kettle, and recovering methanol and ethanol; s6, distilling the fraction collected in S3 under reduced pressure, and separating out low-boiling-point substances and a finished product of cyanoethyl ester. The invention has the advantages that: the cyanoethyl ester product prepared by the method has high purity, less impurity content and high molar yield, and obtains good economic benefit.