CN115403513A - 一种n-甲基氯化吡啶连续化合成工艺 - Google Patents
一种n-甲基氯化吡啶连续化合成工艺 Download PDFInfo
- Publication number
- CN115403513A CN115403513A CN202211067688.6A CN202211067688A CN115403513A CN 115403513 A CN115403513 A CN 115403513A CN 202211067688 A CN202211067688 A CN 202211067688A CN 115403513 A CN115403513 A CN 115403513A
- Authority
- CN
- China
- Prior art keywords
- methanol
- pyridine
- synthesis process
- chloride
- methylpyridine
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- IARCGBCZSPZLGK-UHFFFAOYSA-N 1-methyl-1,2-dihydropyridin-1-ium;chloride Chemical compound Cl.CN1CC=CC=C1 IARCGBCZSPZLGK-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims abstract description 22
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 17
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 17
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 87
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims abstract description 50
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 claims abstract description 44
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 229940050176 methyl chloride Drugs 0.000 claims abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 238000001291 vacuum drying Methods 0.000 claims abstract description 7
- 239000011259 mixed solution Substances 0.000 claims abstract description 6
- 238000004321 preservation Methods 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 230000035484 reaction time Effects 0.000 claims abstract description 4
- 238000002309 gasification Methods 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 claims description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 11
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 238000005086 pumping Methods 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 2
- 239000002904 solvent Substances 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 238000010924 continuous production Methods 0.000 abstract description 5
- 238000012824 chemical production Methods 0.000 abstract description 2
- 238000005260 corrosion Methods 0.000 abstract description 2
- 230000007797 corrosion Effects 0.000 abstract description 2
- 238000007599 discharging Methods 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 238000011049 filling Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- QAIGYXWRIHZZAA-UHFFFAOYSA-M 1-methylpyridin-1-ium;chloride Chemical compound [Cl-].C[N+]1=CC=CC=C1 QAIGYXWRIHZZAA-UHFFFAOYSA-M 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 238000005804 alkylation reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- FIKAKWIAUPDISJ-UHFFFAOYSA-L paraquat dichloride Chemical compound [Cl-].[Cl-].C1=C[N+](C)=CC=C1C1=CC=[N+](C)C=C1 FIKAKWIAUPDISJ-UHFFFAOYSA-L 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 150000003222 pyridines Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
- C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
- C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D213/06—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom containing only hydrogen and carbon atoms in addition to the ring nitrogen atom
- C07D213/16—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom containing only hydrogen and carbon atoms in addition to the ring nitrogen atom containing only one pyridine ring
- C07D213/20—Quaternary compounds thereof
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
- C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
- C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D213/06—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom containing only hydrogen and carbon atoms in addition to the ring nitrogen atom
- C07D213/127—Preparation from compounds containing pyridine rings
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Pyridine Compounds (AREA)
Abstract
本发明涉及一种N‑甲基氯化吡啶连续化合成工艺，属于化工生产技术领域，包括如下步骤：步骤一、将吡啶和甲醇混合，通入混合器进行预热，得到甲醇和吡啶的混合液；步骤二、将氯甲烷通入预热器预热气化；步骤三、在管式反应器进口通入甲醇和吡啶的混合液以及氯甲烷气体，进行保温、保压反应，反应结束后，用接收罐保温收料；步骤四、真空干燥。本发明中的合成工艺原理简单，工业化方便，实现了N‑甲基氯化吡啶的连续化生产，产量稳定，产物纯度高；合成工艺中使用甲醇作为溶剂，对生产设备腐蚀性小；减少了溶剂甲醇的用量，降低了生产成本；且甲醇与N‑甲基氯化吡啶分离的过程操作简单；采用连续化生产，缩短反应时间，提高生产效率。
Description
技术领域
本发明属于化工生产技术领域，具体地，涉及一种N-甲基氯化吡啶连续化合成工艺。
背景技术
N-甲基氯化吡啶，又名1-甲基氯化吡啶，英文名N～Methylpyridiniumchloride，简称MPC，分子式：C6H8ClN，是一种重要的吡啶衍生物。纯净的N-甲基氯化吡啶为无色至百色粉末状结晶，具有较强的吸湿性，易溶于水，微溶于乙醇、丙酮，不溶于苯、甲苯、环己烷等多数有机溶剂，其溶解性类似于无机盐。N-甲基氯化吡啶的合成方法主要以吡啶、氯甲烷为反应原料，以甲醇或乙醇或水为溶剂，经烷基化反应制得。
目前N-甲基氯化吡啶合成主要是以反应釜为容器阶段性生产，因此产量较低，且操作较多。
实用新型专利CN208732975U公开了一种连续生产N-甲基氯化吡啶的系统，该方法可有效提高产量并减少人工操作，但是由于使用了水为溶剂，产生氯化氢对设备有一定腐蚀，且由于N-甲基氯化吡啶的吸水性，后续水分处理难度大。
中国发明专利CN101875628A公开了一种百草枯氯化物的制备方法，其采用甲醇为溶剂合成N-甲基氯化吡啶，该方法工艺简单，但产量较小。
发明内容
为了解决背景技术中提到的技术问题，本发明提供一种N-甲基氯化吡啶连续化合成工艺。
本发明的目的可以通过以下技术方案实现：
一种N-甲基氯化吡啶连续化合成工艺，包括如下步骤：
步骤一、将吡啶和甲醇按照质量比1：0.1～0.3混合，通入混合器进行预热，得到甲醇和吡啶的混合液；采用连续化合成过程，可以减少甲醇的用量，降低生产成本；溶剂甲醇的使用量过多会导致回收困难，增加处理成本，溶剂甲醇的使用量过少会导致产品结晶，堵塞反应管，影响反应进行；
步骤二、将氯甲烷通入预热器预热气化；
步骤三、在管式反应器进口通入甲醇和吡啶的混合液以及氯甲烷气体，吡啶和氯甲烷的摩尔比为1：1.1～1.25，进行保温、保压反应，反应结束后，用接收罐保温收料；管式反应器为横向放置；
步骤四、真空干燥。
进一步地，混合器预热温度为60～65℃。
进一步地，氯甲烷预热温度为35～55℃。
进一步地，保压反应温度为75～85℃；保压反应压力为0.4～0.6MPa；保压反应时间为2～4h。
进一步地，干燥温度50～60℃；干燥压力为-0.08～-0.1MPa；干燥时间为4～6h。
进一步地，停止抽真空后填充氮气。
本发明的有益效果：
本发明提供了一种N-甲基氯化吡啶连续化合成工艺，原理简单，工业化方便，实现了N-甲基氯化吡啶的连续化生产，产量稳定，产物纯度高；合成工艺中使用甲醇作为溶剂，对生产设备腐蚀性小；减少了溶剂甲醇的用量，降低了生产成本；且甲醇与N-甲基氯化吡啶分离的过程操作简单；采用连续化生产，缩短反应时间，提高生产效率。
具体实施方式
下面将结合本发明实施例，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其它实施例，都属于本发明保护的范围。
实施例1
步骤一、取300g吡啶加入30g甲醇混合均匀后加热至60℃，以0.5g/min泵至管式反应器；
步骤二、氯甲烷预热至55℃控制流量0.28g/min通入四个串联管式反应器，吡啶、氯甲烷的摩尔比为1：1.1；
步骤三、管式反应器总体积为180mL，尾部装背压阀，调节压力至0.4MPa，控制温度为75℃，2h后开始出料；
步骤四、出料半小时后调整至接收罐，接收罐50℃保温，收料4h后停止反应；
步骤五、对接收罐进行真空干燥，干燥温度为50℃、真空度为-0.1MPa，干燥4h后填充氮气。
步骤五、干燥完成后检测：吡啶含量未检出，甲醇含量为0.4％。
实施例2
步骤一、取300g吡啶加入90g甲醇混合均匀后加热至65℃，以0.5g/min泵至管式反应器；
步骤二、氯甲烷预热至35℃控制流量0.28g/min通入四个串联管式反应器，吡啶、氯甲烷的摩尔比为1：1.25；
步骤三、管式反应器总体积为180mL，尾部装背压阀，调节压力至0.6MPa，控制温度为85℃，4h后开始出料；
步骤四、出料半小时后调整至接收罐，接收罐50℃保温，收料4h后停止反应；
步骤五、对接收罐进行真空干燥，干燥温度为60℃、真空度为-0.1MPa，干燥6h后填充氮气。
步骤五、干燥完成后检测：吡啶含量未检出，甲醇含量为0.5％。
实施例3
步骤一、取300g吡啶加入60g甲醇混合均匀后加热至65℃，以0.5g/min泵至管式反应器；
步骤二、氯甲烷预热至35℃控制流量0.28g/min通入四个串联管式反应器，吡啶、氯甲烷的摩尔比为1：1.1；
步骤三、管式反应器总体积为180mL，尾部装背压阀，调节压力至0.5MPa，控制温度为80℃，3.5h后开始出料；
步骤四、出料半小时后调整至接收罐，接收罐50℃保温，收料4h后停止反应；
步骤五、对接收罐进行真空干燥，干燥温度为50℃、真空度为-0.1MPa，干燥4h后填充氮气。
步骤五、干燥完成后检测：吡啶含量未检出，甲醇含量为0.3％。
实施例4
步骤一、取600g吡啶加入120g甲醇混合均匀后加热至65℃，以0.5g/min泵至管式反应器。
步骤二、氯甲烷预热至35℃控制流量0.3g/min通入四个串联管式反应器；吡啶、氯甲烷的摩尔比为1：1.25；
步骤三、管式反应器总体积为180mL，尾部装背压阀，调节压力至0.5MPa，控制温度为80℃，3.5h后开始出料；
步骤四、出料半小时后调整至接收罐A，接收罐50℃保温；收料4h后切换至另一接收罐B；收料4h后停止反应。
步骤五、对两个接收罐进行真空干燥，干燥温度为50℃、真空度为-0.08MPa，干燥4h后填充氮气。
干燥完成检测接检测：收罐A吡啶含量未检出，甲醇含量为0.38％；接收罐B吡啶含量未检出，甲醇含量为0.55％。
在说明书的描述中，参考术语“一个实施例”、“示例”、“具体示例”等的描述意指结合该实施例或示例描述的具体特征、结构、材料或者特点包含于本发明的至少一个实施例或示例中。在本说明书中，对上述术语的示意性表述不一定指的是相同的实施例或示例。而且，描述的具体特征、结构、材料或者特点可以在任何的一个或多个实施例或示例中以合适的方式结合。
以上内容仅仅是对本发明所作的举例和说明，所属本技术领域的技术人员对所描述的具体实施例做各种各样的修改或补充或采用类似的方式替代，只要不偏离发明或者超越本权利要求书所定义的范围，均应属于本发明的保护范围。
Claims (6)
1.一种N-甲基氯化吡啶连续化合成工艺，其特征在于，包括如下步骤：
步骤一、将吡啶和甲醇按照质量比1：0.1～0.3混合，通入混合器进行预热，得到甲醇和吡啶的混合液；
步骤二、将氯甲烷通入预热器预热气化；
步骤三、在管式反应器进口通入甲醇和吡啶的混合液以及氯甲烷气体，吡啶和氯甲烷的摩尔比为1：1.1～1.25，进行保温、保压反应，反应结束后，用接收罐保温收料；
步骤四、真空干燥。
2.根据权利要求1所述的一种N-甲基氯化吡啶连续化合成工艺，其特征在于，混合器预热温度为60～65℃。
3.根据权利要求1所述的一种N-甲基氯化吡啶连续化合成工艺，其特征在于，氯甲烷预热温度为35～55℃。
4.根据权利要求1所述的一种N-甲基氯化吡啶连续化合成工艺，其特征在于，保压反应温度为75～85℃；保压反应压力为0.4～0.6MPa；保压反应时间为2～4h。
5.根据权利要求1所述的一种N-甲基氯化吡啶连续化合成工艺，其特征在于，干燥温度50～60℃；干燥压力为-0.08～-0.1MPa；干燥时间为4～6h。
6.根据权利要求1所述的一种N-甲基氯化吡啶连续化合成工艺，其特征在于，停止抽真空后填充氮气。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211067688.6A CN115403513A (zh) | 2022-09-01 | 2022-09-01 | 一种n-甲基氯化吡啶连续化合成工艺 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211067688.6A CN115403513A (zh) | 2022-09-01 | 2022-09-01 | 一种n-甲基氯化吡啶连续化合成工艺 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115403513A true CN115403513A (zh) | 2022-11-29 |
Family
ID=84162857
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211067688.6A Pending CN115403513A (zh) | 2022-09-01 | 2022-09-01 | 一种n-甲基氯化吡啶连续化合成工艺 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115403513A (zh) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4115390A (en) * | 1977-08-19 | 1978-09-19 | Nardi John C | Method for the preparation of 1-alkyl pyridinium chlorides |
| CN101875628A (zh) * | 2009-04-28 | 2010-11-03 | 苏州佳辉化工有限公司 | 一种百草枯氯化物的制备方法 |
| CN103254123A (zh) * | 2013-05-17 | 2013-08-21 | 孟宪锋 | 一种氰氨法合成百草枯的工艺方法 |
| CN106883196A (zh) * | 2017-03-15 | 2017-06-23 | 安阳市小康农药有限责任公司 | 一种甲哌鎓原药的合成方法 |
| CN208732975U (zh) * | 2018-06-25 | 2019-04-12 | 河北临港化工有限公司 | 一种用于连续生产n-甲基氯化吡啶的系统 |
| CN109705026A (zh) * | 2019-02-25 | 2019-05-03 | 安徽国星生物化学有限公司 | 一种百草枯中间体连续化生产装置及生产方法 |
-
2022
- 2022-09-01 CN CN202211067688.6A patent/CN115403513A/zh active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4115390A (en) * | 1977-08-19 | 1978-09-19 | Nardi John C | Method for the preparation of 1-alkyl pyridinium chlorides |
| CN101875628A (zh) * | 2009-04-28 | 2010-11-03 | 苏州佳辉化工有限公司 | 一种百草枯氯化物的制备方法 |
| CN103254123A (zh) * | 2013-05-17 | 2013-08-21 | 孟宪锋 | 一种氰氨法合成百草枯的工艺方法 |
| CN106883196A (zh) * | 2017-03-15 | 2017-06-23 | 安阳市小康农药有限责任公司 | 一种甲哌鎓原药的合成方法 |
| CN208732975U (zh) * | 2018-06-25 | 2019-04-12 | 河北临港化工有限公司 | 一种用于连续生产n-甲基氯化吡啶的系统 |
| CN109705026A (zh) * | 2019-02-25 | 2019-05-03 | 安徽国星生物化学有限公司 | 一种百草枯中间体连续化生产装置及生产方法 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US20220119330A1 (en) | Method for preparing resorcinol through micro-channel reaction | |
| CN108558607B (zh) | 一种邻氟苯酚的高效合成方法 | |
| CN102115444B (zh) | 一种连续化生产三醋酸甘油酯的工艺及装置 | |
| CN107365279A (zh) | 乙螨唑的合成工艺 | |
| CN115403513A (zh) | 一种n-甲基氯化吡啶连续化合成工艺 | |
| CN101921191B (zh) | 一种莰烯与乙酸酯化合成乙酸异龙脑酯的制备方法 | |
| CN102030625B (zh) | 一种香兰素合成的方法 | |
| CN113105379A (zh) | 一种以吊白块为还原剂制备硒代胱氨酸的方法及装置 | |
| CN110627754B (zh) | 一种利用连续流微通道反应器制备2-氧代-2-呋喃基乙酸的方法 | |
| CN1426981A (zh) | 复方长效尿素生产工艺及专用设备 | |
| CN109646977B (zh) | 一种反应精馏耦合塔及其在制备甲酸中的应用 | |
| CN209848872U (zh) | 一种合成草酰胺的生产装置 | |
| CN113214258A (zh) | 一种敌草快二氯盐合成方法及装置 | |
| CN110117259B (zh) | 一种利用离子液体催化制备2,5-脱氧果糖嗪的方法 | |
| CN106748841A (zh) | 一种天冬氨酸甲酯的生产方法 | |
| CN112694407A (zh) | 一种2-甲基-4-异丙基苯胺生产制备方法 | |
| CN220835569U (zh) | 一种连续化合成(E)-2-甲基-α-羟亚胺基苯乙酸的装置 | |
| CN106699723B (zh) | 一种15-冠醚-5的制备方法 | |
| CN111675607A (zh) | 一种微分环流连续化生产原乙酸三甲酯的方法 | |
| CN116617971B (zh) | 一种格列齐特中间体的连续化生产方法 | |
| CN113717025B (zh) | 一种氯代特戊烷的合成方法 | |
| CN219721935U (zh) | 一种变压精馏分离2-甲基吡啶-水的装置 | |
| CN113563230B (zh) | 一种霜霉威盐酸盐原药的制备方法 | |
| CN220386510U (zh) | 一种连续化生产叔丁醇钠的装置 | |
| CN220257997U (zh) | 一种锂盐合成装置 |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20221129 |