CN111072522A - Preparation method of methyl nitroguanidine - Google Patents
Preparation method of methyl nitroguanidine Download PDFInfo
- Publication number
- CN111072522A CN111072522A CN201911298042.7A CN201911298042A CN111072522A CN 111072522 A CN111072522 A CN 111072522A CN 201911298042 A CN201911298042 A CN 201911298042A CN 111072522 A CN111072522 A CN 111072522A
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- Prior art keywords
- nitroguanidine
- methylamine
- methyl
- added
- water
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C277/00—Preparation of guanidine or its derivatives, i.e. compounds containing the group, the singly-bound nitrogen atoms not being part of nitro or nitroso groups
- C07C277/08—Preparation of guanidine or its derivatives, i.e. compounds containing the group, the singly-bound nitrogen atoms not being part of nitro or nitroso groups of substituted guanidines
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
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%.
Description
Technical Field
The invention belongs to the field of chemical industry, and particularly relates to a preparation method of methyl nitroguanidine.
Background
The methyl nitroguanidine is an important pesticide and medicine intermediate, is mainly used for nicotine pesticide intermediates, and has wide application in many fields, such as production of high-efficiency low-toxicity pesticides clothianidin, thiamethoxam, dinotefuran and the like. The requirements of the methylnitroguanidine in the production process are strict.
Therefore, the invention has profound significance for synthesizing the methyl nitroguanidine.
Disclosure of Invention
The invention aims to provide a method for preparing methyl nitroguanidine, which can improve the yield and productivity of the methyl nitroguanidine.
In order to solve the technical problems, the technical scheme of the invention is as follows: the preparation method of the methyl nitroguanidine has the innovation points that: the preparation method 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.
Further, the methylamine content in the S1 is 40 wt%.
Further, the aqueous methylamine solution in the S2 is added in a dropwise manner.
Further, the mass percentage concentration of the dilute sulfuric acid in the S2 is 60%.
The invention has the advantages that: the preparation method of the methyl nitroguanidine adopts the reaction of nitroguanidine, methylamine and sulfuric acid, is safe and environment-friendly, is suitable for industrial production, and the molar yield of the methyl nitroguanidine prepared by the method can reach more than 80%.
Detailed Description
The following examples are presented to enable one of ordinary skill in the art to more fully understand the present invention and are not intended to limit the scope of the embodiments described herein.
The preparation method of the methyl nitroguanidine 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.
As an example, a more specific embodiment is that the methylamine content in S1 is 40wt%, the methylamine water solution in S2 is added dropwise, and the dilute sulfuric acid concentration in S2 is 60 wt%.
The following will explain in detail the process for producing methylnitroguanidine according to the present invention by specific examples.
Examples
The embodiment discloses a preparation method of methyl nitroguanidine, which comprises the following steps of: sequentially adding water and methylamine into a 1000ml four-neck flask, adding methyl nitroguanidine in batches, stirring, dripping a methylamine water solution at 35 ℃ for 15 minutes, measuring the pH to be 12, continuing stirring for 10 minutes, slowly raising the temperature to 43 ℃, removing a neutralization kettle after the reaction is completed, reducing the temperature, dripping 60% dilute sulfuric acid, neutralizing to be neutral, and reducing the temperature to 25 ℃ after the reaction is finished; and (3) filtering and washing a product after reaction neutralization, adding a filter aid into the filtered and washed methyl nitroguanidine slurry, heating to 90 ℃, cooling to 25 ℃ under stirring, and centrifuging by using a centrifugal machine to obtain a refined methyl nitroguanidine tide product. And finally, drying to obtain a refined methyl nitroguanidine finished product with the molar yield of 83.7 percent.
The foregoing shows and describes the general principles and features of the present invention, together with the advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (4)
1. A method for preparing methyl nitroguanidine is characterized in that: the preparation method 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.
2. The method for preparing methylnitroguanidine according to claim 1, wherein: the methylamine content in the S1 is 40 wt%.
3. The method for preparing methylnitroguanidine according to claim 1, wherein: and the methylamine water solution in the S2 is added in a dropwise manner.
4. The method for preparing methylnitroguanidine according to claim 1, wherein: the mass percentage concentration of the dilute sulfuric acid in the S2 is 60%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911298042.7A CN111072522A (en) | 2019-12-17 | 2019-12-17 | Preparation method of methyl nitroguanidine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911298042.7A CN111072522A (en) | 2019-12-17 | 2019-12-17 | Preparation method of methyl nitroguanidine |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111072522A true CN111072522A (en) | 2020-04-28 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911298042.7A Withdrawn CN111072522A (en) | 2019-12-17 | 2019-12-17 | Preparation method of methyl nitroguanidine |
Country Status (1)
| Country | Link |
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| CN (1) | CN111072522A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111646959A (en) * | 2020-05-14 | 2020-09-11 | 广州海关技术中心 | Dinotefuran hapten, colloidal gold labeled dinotefuran monoclonal antibody and dinotefuran colloidal gold detection device |
-
2019
- 2019-12-17 CN CN201911298042.7A patent/CN111072522A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111646959A (en) * | 2020-05-14 | 2020-09-11 | 广州海关技术中心 | Dinotefuran hapten, colloidal gold labeled dinotefuran monoclonal antibody and dinotefuran colloidal gold detection device |
| CN111646959B (en) * | 2020-05-14 | 2022-07-15 | 广州海关技术中心 | Dinotefuran hapten, colloidal gold labeled dinotefuran monoclonal antibody and dinotefuran colloidal gold detection device |
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| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20200428 |
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| WW01 | Invention patent application withdrawn after publication |