CN101548682B - New method for synthesizing propamocarb hydrochloride of 722g/l - Google Patents
New method for synthesizing propamocarb hydrochloride of 722g/l Download PDFInfo
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- CN101548682B CN101548682B CN2009100220053A CN200910022005A CN101548682B CN 101548682 B CN101548682 B CN 101548682B CN 2009100220053 A CN2009100220053 A CN 2009100220053A CN 200910022005 A CN200910022005 A CN 200910022005A CN 101548682 B CN101548682 B CN 101548682B
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Abstract
The invention relates to a synthesizing method of propamocarb hydrochloride, including chloroformic acid propyl ester, polycarbodiimide, dimethyl propane diamine, emulsifier and water as solvent. The adding amount of the polycarbodiimide is 0.08 to 0.12% of the chloroformic acid propyl ester; the polycarbodiimide accounts for 0.033 to 0.045 % in weight, the chloroformic acid propyl ester accounts for 33 to 45% and the emulsifier accounts for 2 to 8%; and the balance is water. The mixture of polycarbodiimide and the chloroformic acid propyl ester are added by spraying and dripping. The invention synthesizes 722g/L of propamocarb hydrochloride saline solution by one step, improves reaction speed and yield which rises from 80% to 95%, does not produce any 'three waste', operates easily, and reduces production cost greatly. The product has high quality, little impurities, and the appearance thereof is colorless transparent liquid.
Description
Technical field the present invention relates to the synthetic method of propamocarb.
Background technology propamocarb: 3-(dimethylamino) propyl carbamic acid propyl ester hydrochloride.It is a kind of interior absorption carbamate fungicide of efficient, low toxicity.Can be used as cauline leaf processing, soil treatment and seed treatment; There is not cross resistance with the bactericide that produces resistance; The soilborne disease that can control be caused by pythium spp and phytophthora, and by the microbial leaf diseases of downy mildew has the better prevention effect to damping off, eqpidemic disease, the downy mildew of vegetables, and is especially more obvious to Phycomycetes fungi preventive effect.Be applicable to disease control, and can impel the crop high yield to increase income such as crops such as melon, tomato, grape, lupulus, Chinese cabbage, capsicum, eggplant, tobacco, lichee, lettuce, oranges and tangerines, bananas.
Chloro-carbonic acid n-propyl and dimethylated propyl diethylenetriamine are two important intermediates of preparation propamocarb.Because chloro-carbonic acid n-propyl poor stability, hydrolysis easily, traditional handicraft be with organic solvent as reaction dissolvent, reaction adds alkali and water after finishing, and generates the mixture of solvent and the former medicine of Propamocarb, the recovery solvent obtains the former medicine of Propamocarb; The waste water that generates need be handled.Former medicine of Propamocarb and hydrochloric acid reaction generate propamocarb; Add an amount of water and emulsifier op-10 then; Processing the propamocarb aqua of 722 grams per liters (annotates: 722 grams per liters; Be the widely used product of present home and overseas, as long as change the aqua that amount of water just can be made other content).
Traditional handicraft exists following a plurality of problem to solve: 1. do reaction dissolvent with organic solvent, solvent can not reclaim fully, and the partial solvent volatilization causes environmental pollution; 2. solvent for use is poisonous, inflammable and explosive solvent, has potential safety hazard in the production process; 3. there is waste water to produce, increased three wastes disposal cost; 4. yield low (below 80%), cost is high, inferior quality, outward appearance is a yellow transparent liquid, water-insoluble is more.
Summary of the invention the object of the invention, be to provide a kind of safe and reliable, technology is easy, the method for lower-cost synthetic 722 grams per liter propamocarbs.
The preparation method of the present invention's propamocarb is: chloro-carbonic acid n-propyl, dimethylated propyl diethylenetriamine, emulsifier are arranged, and polycarbodiimide (anti-hydrolysis stabilizer ABSK), water is cooked solvent; The polycarbodiimide addition is 0.08～0.12% of a chloro-carbonic acid n-propyl.The weight proportion of each component is that to account for percentage by weight be 0.033-0.045% to polycarbodiimide; It is 33-45% that the chloro-carbonic acid n-propyl accounts for percentage by weight; It is 27-38% that dimethylated propyl diethylenetriamine accounts for percentage by weight, and it is 2-8% that emulsifier accounts for percentage by weight, and surplus is a water.
The present invention is synthetic according to following step:
1) in agitated reactor, adds water, dimethylated propyl diethylenetriamine and the emulsifier op-10 that measures, stir;
2) under freezing 20-30 ℃ condition, stir on one side, spray drips the mixture of polycarbodiimide and chloro-carbonic acid n-propyl on one side, and the control reaction temperature is not more than 30 ℃;
3) control pH5-7 in, insulation reaction 4～6 hours promptly obtains 722 grams per liter propamocarb aquas.Reaction mechanism:
Technological process: in agitated reactor, add water, dimethylated propyl diethylenetriamine and the emulsifier op-10 (annotate: emulsifier is not participated in reaction, helps improving effect of drugs) that measure, stir; Under freezing 20-30 ℃ condition, stir on one side, spray drips the mixture of anti-hydrolysis stabilizer ABSK and chloro-carbonic acid n-propyl on one side; The control reaction temperature is not more than 30 ℃, middle control pH value, and pH5-7 reacts end; Insulation reaction 4-6 hour, just can directly obtain 722 grams per liter propamocarb aquas.Do complete analysis by standard, qualified back packing.
The propamocarb aqua that has synthesized 722 grams per liters of the present invention one step property has improved reaction velocity and yield, and yield brings up to 95% by original 80%.The present invention does not produce any " three wastes "; Easy and simple to handle, reduced production cost (per ton reduce cost 7000 yuan) significantly; Superior product quality, product impurity is few, and outward appearance is a colourless transparent liquid.
Description of drawings
Fig. 1. process chart
Embodiment is below in conjunction with three embodiments of the invention of accompanying drawing narration
The about 1000 kilogram of 722 grams per liter propamocarb of embodiment 1 preparation
Batching: dimethylated propyl diethylenetriamine 3l8 kilogram, 382 kilograms of chloro-carbonic acid n-propyls, 0.38 kilogram of polycarbodiimide, 50 kilograms of emulsifier, 249.62 kilograms in water.
Carry out with following step:
The preparation process: with dimethylated propyl diethylenetriamine, emulsifier op-10, water drop in the 2000L enamel reaction still; Open and stir, and open the chilled brine of reacting kettle jacketing; After cooling to 20 ℃, begin to spray the mixture that drips chloro-carbonic acid n-propyl and anti-hydrolysis stabilizer ABSK, the control reaction temperature is not more than 30 ℃; Spray dripped about 5 hours, and the limit spray drips, and frontier inspection is surveyed pH value, when the pH value stops the spray dropping during to 5-7; 20-30 ℃ of insulation reaction 5 hours; Do complete analysis, qualified back packing warehouse-in.
It below is the survey report of five batches of productions.
| Project | Index | Batch 1 | Batches 2 | Batches 3 | Batches 4 | Batches 5 |
| The propamocarb mass concentration, g/1 >= | 722 | 725 | 726 | 725 | 724 | 723 |
| The water-insoluble mass fraction, %<= | 0.3 | Do not detect | Do not detect | 0.1 | Do not detect | 0.1 |
| PH value scope | 5.0-7.0 | 6.1 | 6.0 | 6.0 | 5.9 | 6.0 |
| Dilution stability (20 times) | Qualified | Qualified | Qualified | Qualified | Qualified | Qualified |
| Low-temperature stability | Qualified | Qualified | Qualified | Qualified | Qualified | Qualified |
| Heat storage stability | Qualified | Qualified | Qualified | Qualified | Qualified | Qualified |
The gained finished product can satisfy standard-required fully through Instrumental Analysis such as HPLC.
The about 1000 kilogram of 722 grams per liter propamocarb of embodiment 2 preparations
Batching: 280 kilograms of dimethylated propyl diethylenetriamines, 430 kilograms of chloro-carbonic acid n-propyls, 0.35 kilogram of polycarbodiimide, 80 kilograms of emulsifier, 209.65 kilograms of excess waters.
Preparation technology: identical with embodiment 1.
The about 1000 kilogram of 722 grams per liter propamocarb of embodiment 3 preparations
Batching: 370 kilograms of dimethylated propyl diethylenetriamines, 350 kilograms of chloro-carbonic acid n-propyls, 0.42 kilogram of polycarbodiimide, 20 kilograms of emulsifier, 259.58 kilograms in water.
Preparation technology: identical with embodiment 1.
Claims (1)
1. the method for synthetic 722 grams per liter propamocarbs contains chloro-carbonic acid n-propyl, dimethylated propyl diethylenetriamine, emulsifier, and water is cooked solvent, it is characterized in that: polycarbodiimide is arranged, and its addition is 0.08～0.12% of a chloro-carbonic acid n-propyl; It is 0.033-0.045% that polycarbodiimide accounts for percentage by weight, and it is 33-45% that the chloro-carbonic acid n-propyl accounts for percentage by weight, and it is 27-38% that dimethylated propyl diethylenetriamine accounts for percentage by weight, and it is 2-8% that emulsifier accounts for percentage by weight; Surplus is a water; Said propamocarb is synthetic with following step:
1) in agitated reactor, adds water, dimethylated propyl diethylenetriamine and the emulsifier op-10 that measures, stir;
2) under freezing 20-30 ℃ condition, stir on one side, spray drips the mixture of polycarbodiimide and chloro-carbonic acid n-propyl on one side, and the control reaction temperature is not more than 30 ℃;
3) control pH5-7 in, insulation reaction 4～6 hours promptly obtains 722 grams per liter propamocarb aquas.
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| CN2009100220053A CN101548682B (en) | 2009-04-14 | 2009-04-14 | New method for synthesizing propamocarb hydrochloride of 722g/l |
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| CN2009100220053A CN101548682B (en) | 2009-04-14 | 2009-04-14 | New method for synthesizing propamocarb hydrochloride of 722g/l |
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| CN101548682B true CN101548682B (en) | 2012-07-25 |
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| CN103965080A (en) * | 2013-01-29 | 2014-08-06 | 浙江禾本科技有限公司 | Propamocarb hydrochloride and preparation method thereof |
| CN104397040A (en) * | 2014-11-17 | 2015-03-11 | 陕西恒田化工有限公司 | Bactericide composition containing artemisia capillaris thunb extractive and propamocarb hydrochloride as well as application of bactericide composition |
| CN113563230B (en) * | 2020-08-24 | 2023-04-11 | 江苏禾本生化有限公司 | Preparation method of propamocarb hydrochloride technical |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1507433A (en) * | 2001-05-03 | 2004-06-23 | �ݶ�ũ������˾ | Process for the preparation of alkyl-N-(3-dimethylamino) alkylcarbamates |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1507433A (en) * | 2001-05-03 | 2004-06-23 | �ݶ�ũ������˾ | Process for the preparation of alkyl-N-(3-dimethylamino) alkylcarbamates |
Non-Patent Citations (1)
| Title |
|---|
| 周玉昆等.霜霉威盐酸盐的研究.《中国化工学会农药专业委员会第九届年会》.1998,第435-437页. * |
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Address after: Weinan 714000 Weinan city of Shaanxi province Dali County National Agricultural Science and Technology Park core area of Dali Patentee after: Shaanxi Hengtian Biological Agriculture Co. Ltd. Address before: Weinan City, Shaanxi Province, the 727000 national agricultural science and Technology Park core area of Dali Patentee before: Shaanxi Hentian Chem-Tech Co., Ltd. |
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