CN1191013C - Novel pesticide of monosultap ammonium and productive technology thereof - Google Patents
Novel pesticide of monosultap ammonium and productive technology thereof Download PDFInfo
- Publication number
- CN1191013C CN1191013C CNB001106937A CN00110693A CN1191013C CN 1191013 C CN1191013 C CN 1191013C CN B001106937 A CNB001106937 A CN B001106937A CN 00110693 A CN00110693 A CN 00110693A CN 1191013 C CN1191013 C CN 1191013C
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- ammonium
- monosultap
- chloride
- methanol
- reduced
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Abstract
The present invention discloses a new pesticide of monosultap ammonium and a production technology. Achloride hydrochloride is used as raw material, methanol is used as a solvent, and alkaline substances are added to the chloride hydrochloride and the methanol to be neutralized to 15 to 20%, and are heated to 40 to 45 DEG C. The temperature is naturally raised to the return temperature of the water methanol. The methanol is removed, the temperature is reduced, and ammonium chloride is filtered and separated. Hydrochloric acid is added, the temperature is reduced to 0 DEG C, the solution is crystallized, and then the pesticide monosultap ammonium and a small amount of ammonium chloride are prepared. As the neutralization degree is small, the addition amount of alkaline substances is reduced, the ammonium chloride is little generated, and the putting amount of the hydrochloric acid is reduced. As the methanol is used as the solvent, the sulfonation reaction is the homogeneous reaction, the crystallization rate of the pesticide monosultap ammonium is favorably enhanced, and the production cost is reduced.
Description
The present invention relates to the fertile economic benefits and social benefits novel pesticide of a kind of medicine, definite saying so discloses a kind of novel pesticide of monosultap ammonium and production technology, belongs to nereistoxin line biomimetic insecticide technical field.
Existing agricultural insecticide list, dimehypo in process of production, yield is lower, and produces a large amount of sodium chloride by products, because this by product has the desinsection toxic component, all can not directly use in the industrial or agricultural, and become the residue contamination environment; No. the 96116850.1st, the application for a patent for invention of " Chinese patent communique ", a kind of solution to the problems described above is disclosed, but this method exists following weak point: big with the raw material ammonia water consumption in during reaction, the generation intermediate product is many, makes the dimehypo ammonium is being changed in the process of monosultap ammonium, needs a large amount of sulfuric acid, it is also many to produce ammonium sulfate simultaneously, therefore, must just can produce qualified products, improve production cost greatly through crystallization repeatedly.
The present invention discloses a kind of novel pesticide of monosultap ammonium production technology, and purpose is intended to overcome the shortcoming and defect that above-mentioned process exists.
The object of the present invention is achieved like this: with intermediate--chloride hydrochloride (1-N, the N dimethylamine base-2 of dimehypo production, 3-dichloropropane hydrochloride) be primary raw material, in the methanol solvate of input 75%, add alkaline matter and be neutralized to pH=6.5～6.7, described alkaline matter comprises ammoniacal liquor, ammonia, carbon ammonia etc., degree of neutralization is 15～25%, and reaction equation is:
Add ATS (Ammonium thiosulphate) again, its charge ratio is (molecular proportion):
Chloride hydrochloride: alkaline matter: ATS (Ammonium thiosulphate)=1: (0.15～0.25): heating was 40～45 ℃ after (2.1～2.2) fed intake, allow it be warming up to the methanol aqueous solution reflux temperature naturally, after reflux temperature reacts 1 hour, slough methyl alcohol, cooling isolated by filtration by product ammonium chloride, feed liquid is evacuated to crystallization kettle, and the product that this sulfonating reaction is produced is monosultap ammonium and dimehypo ammonium
Under agitation be cooled to 40 ℃, add hydrochloric acid (0.17～0.20 molecular proportion), make the part dimehypo ammonium after the sulfonation further be converted into monosultap ammonium, and generate with ammonium chloride, continue to stir and be cooled to about 0 ℃, the insulation crystallization was got rid of filter after 8 hours, obtained monosultap ammonium and a small amount of ammonium chloride.
Good effect of the present invention is:
1, chloride hydrochloride neutralizes with alkaline matter before sulfonation, degree of neutralization is 15～25%, guaranteed to have reduced on the basis of acid sulfonation not the addition of alkaline matter, by product ammonium chloride is generated on a small quantity, and the product after the sulfonation more than 80% to be monosultap ammonium, for acidifying before the crystallization has reduced the input amount of hydrochloric acid, also reduced the generation of by product ammonium chloride.
2, owing to chloride hydrochloride generates free chlorated liquid with in the ammoniacal liquor and back, be oily liquids, proportion is little, and boiling point is low, with the thiosulfuric acid aqueous ammonium generation two phase reaction in the sulfonation.For improving sulphonation recovery, employing methyl alcohol is solvent, and making sulfonating reaction is homogeneous reaction, has not only improved sulphonation recovery, and helps the raising of monosultap ammonium percent crystallization in massecuite.
3, be percent crystallization in massecuite that improves monosultap ammonium and the content that improves monosultap ammonium, must separate by product ammonium chloride earlier, technology of the present invention is exactly different with monosultap ammonium crystallization concentration according to the ammonium chloride under this concentration, adopt first high temperature separating ammonium chloride, the low temperature crystallization monosultap ammonium obtains the monosultap ammonium of high concentration.
4, for free from environmental pollution, it is commodity selling that the present invention adopts 60% monosultap ammonium, therefore, monosultap ammonium more than 90% is prepared 60% monosultap ammonium, do to add auxiliary agent with the by product ammonium chloride in producing, promptly can reduce factory cost, can increase the drug effect and the fertilizer efficiency of agricultural chemicals again.
Below be embodiments of the invention:
In the sulfonation still of 1500 liters, drop into 500 kilograms of chloride hydrochlorides (chlorated liquid content is 62.5%) earlier, at 75% methyl alcohol that adds 500 kilograms, behind 66.8 kilograms of the ammoniacal liquor of dropping 17% under the condition of normal temperature and pressure stirs, drop into 530 kilograms of ATS (Ammonium thiosulphate), seal heat temperature raising to 45 ℃, stop heating, treat that it is warmed up to about 76 ℃ of reflux temperature naturally, insulation reaction 1 hour begins to reclaim methyl alcohol, finishes to 92 ℃ of Methanol Recovery, be cooled to 65 ℃, blowing filters, elimination ammonium chloride, and feed liquid is sent crystallization kettle, be cooled to 40 ℃, 32.6 kilograms of dripping hydrochloric acid (30% concentration) continue to be cooled to 0 ℃, crystallization 8 hours, centrifugal get rid of filter the moist crystal of monosultap ammonium, content is more than 85%, and oven dry back content is more than 92%, and mother liquor is used to prepare 20% dimehypo water solution.
Claims (2)
1, a kind of production technology of novel pesticide of monosultap ammonium, finish by following process: intermediate--the chloride hydrochloride of producing with dimehypo: 1-N, N dimethylamine base-2,3-dichloropropane hydrochloride is a primary raw material, methyl alcohol is solvent, add alkaline matter and be neutralized to pH6.5～6.7, degree of neutralization is 15--20%, adds ATS (Ammonium thiosulphate) again, and it feeds intake and by the molecular proportion proportioning is:
Chloride hydrochloride: alkaline matter: ATS (Ammonium thiosulphate)=1: (0.15～0.25): (2.1～2.2)
40-45 ℃ of back heating feeds intake, allow it be warming up to the methanol aqueous solution reflux temperature naturally, after 1 hour, slough methyl alcohol in the reflux temperature reaction, cooling isolated by filtration by product ammonium chloride, feed liquid is evacuated to crystallization kettle, under agitation be cooled to 40 ℃, the hydrochloric acid of adding 0.17-0.20 molecular proportion makes the part dimehypo ammonium after the sulfonation further be converted into monosultap ammonium, and generates with ammonium chloride, continue to stir and be cooled to about 0 ℃, the insulation crystallization is got rid of filter and is obtained monosultap ammonium and a small amount of sal-ammoniac after 8 hours.
2, production technology according to claim 1 is characterized in that: alkaline matter comprises ammoniacal liquor, ammonia, carbon ammonia.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB001106937A CN1191013C (en) | 2000-07-21 | 2000-07-21 | Novel pesticide of monosultap ammonium and productive technology thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB001106937A CN1191013C (en) | 2000-07-21 | 2000-07-21 | Novel pesticide of monosultap ammonium and productive technology thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1285145A CN1285145A (en) | 2001-02-28 |
| CN1191013C true CN1191013C (en) | 2005-03-02 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB001106937A Expired - Fee Related CN1191013C (en) | 2000-07-21 | 2000-07-21 | Novel pesticide of monosultap ammonium and productive technology thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1191013C (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103086799B (en) * | 2013-02-04 | 2014-09-24 | 广西田园生化股份有限公司 | Fertilizer-mix pesticide |
| CN104447458B (en) * | 2014-12-11 | 2016-10-05 | 湖南国发精细化工科技有限公司 | The process for purification of Cupric sulfate in Cupric sulfate synthesis technique |
| CN104610120B (en) * | 2015-01-28 | 2017-02-22 | 湖南昊华化工有限责任公司 | Preparation method capable of increasing proportion of 1,3-bit normal compound in bisultap |
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2000
- 2000-07-21 CN CNB001106937A patent/CN1191013C/en not_active Expired - Fee Related
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| Publication number | Publication date |
|---|---|
| CN1285145A (en) | 2001-02-28 |
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Granted publication date: 20050302 |