CN1046079C - Process for preparing soluble powder of polythiaane - Google Patents
Process for preparing soluble powder of polythiaane Download PDFInfo
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- CN1046079C CN1046079C CN93118875A CN93118875A CN1046079C CN 1046079 C CN1046079 C CN 1046079C CN 93118875 A CN93118875 A CN 93118875A CN 93118875 A CN93118875 A CN 93118875A CN 1046079 C CN1046079 C CN 1046079C
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- carrier
- polythiane
- preparation
- polythialan
- soluble powder
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Abstract
The present invention relates to a preparation method for the soluble powder of polythialan, which belongs to a preparation method for a sulfur heterocyclic compound salt. The present invention aims to provide a preparation method for soluble powder, which can reserve the pest killing performance of polythialan, improve the physical characteristics of polythialan and can be effectively used for industrial production and agricultural application. In the preparation method, one carrier is added in the process of preparing polythialan hydrochloride, and thus, the generated salt is absorbed on carrier micropores and the surface; common light calcium carbonate, light magnesium carbonate, white carbon black, and the like., are used as the carrier. The soluble powder prepared by the preparation method is the powder with optimal comprehensive performance in various processed polythialan preparations and has the advantages of good medicinal effect, safe and convenient storage and safe and convenient transportation.
Description
Method of the present invention is relevant with the processing of heterocyclic compound, particularly, belongs to the formulation processing method of the heterocyclic compound salt that contains a plurality of sulphur atoms.
Polythiane is the active component of a kind of insecticide in the neires toxin chemical pesticide, and its method for making has been documented among the application documents of Chinese patent CN85102251A.But polythiane itself is a kind of oily liquids, and transportation is all not very convenient with use, and production cost is also high.At these shortcomings, Guizhou Provincial Inst. of Chemical Technology has developed the production technology of polythiane salts, and has proposed the application for a patent for invention of " preparation method of polythiane salts ".Polythiane salts has improved the physics sex character of polythiane effectively, has kept its toxic action to insect.Yet in two kinds of salt of the polythiane of developing at present, solvent consumption was big when the preparation binoxalate prepared, and was difficult for reclaiming, and relative cost is higher; Though preparation hydrochloride cost is lower, it is too strong to exist hygroscopicity, is difficult for the deadly defect of producing, processing and storing.These weakness have directly limited the production and the use of polythiane agricultural chemicals.
Purpose of the present invention just is to provide a kind of can overcome above-mentioned shortcoming, can be used for the preparation method of the soluble powder of polythiaane that industrial production and agricultural use cost-effectively.
For reaching this purpose, method provided by the invention is: add a kind of carrier in the preparation process of polythiane hydrochloride, the polythiane hydrochloride is adsorbed on the micropore and surface of carrier, make its soluble powder.
The inventor considers, should have the big characteristics of economy, light weight, specific surface area and have inertia as the material of carrier, promptly not with the character of polythiane and salt thereof, solvent generation chemical reaction.The material that can be used as carrier is a lot, the mixture mutually formed in proportion of ash, chimney soot, high grade kaolinite, bentonite, diatomite, precipitated calcium carbonate, light magnesium carbonate, lightweight hydrated SiO 2, anhydrous sodium sulfate, phosphoric acid salt, A type molecular sieve etc. and these materials for example, wherein, be the best with the carrier that is mixed with precipitated calcium carbonate, light magnesium carbonate, lightweight hydrated SiO 2 and these materials and an amount of anhydrous sodium sulfate, phosphate etc.
The adding of carrier is to carry out feed dry hydrogen chloride in the organic solution of institute's polythiane before, and its addition is 2/3～4/5 of a theoretical amount of calculation.
Polythiane solution feeds when dry hydrogen chloride prepares the polythiane hydrochloride and wants strong agitation, and the hydrochloride of generation is adsorbed on the carrier equably.Reach behind the terminal point through abundant mixing, sample analysis, adding behind an amount of stabilizing agent by making content is that the requirement of 40%～50% soluble powder of polythiaane is added carrier and made filler again.Stabilizing agent commonly used is an oxalic acid.
With the soluble powder of polythiaane that the inventive method makes, its insecticidal spectrum and preventing efficiency and 25% the former powder basically identical of polythiane emulsion, polythiane, the desinsection that had both kept polythiane is renderd a service, and has improved its physics sex character again.Selected carrier is inertia to its various components, when using corps leaf surface is not had poisoning yet, and rain-out promptly falls.Facts have proved that soluble powder of polythiaane is the most excellent a kind of of combination property in the processing of the multiple formulation of polythiane, both economy, safety, transportation, use, storage is all convenient, drug effect is good.To be polythiane from laboratory research move towards the industrialization method of the present invention produces and the key problem in technology of high volume applications.
Embodiment 1: adds sulfuric acid in the laboratory with sodium chloride by well-established law and prepares gas chlorination hydrogen, and with concentrated sulfuric acid drying.With add in the 1000ml there-necked flask of agitator, breather pipe and tail gas absorption tube through super-dry contain 15.40% polythiane toluene solution 159.3g (0.1mol), dispersant ethylene glycol 1ml, toluene 300g, light magnesium carbonate 12g, under strong agitation, feed dry hydrogen chloride.Control salify endpoint pH 3～4.5.Stop to feed hydrogen chloride, take out the material vacuum filtration, in 70～80 ℃ of oven dry, pulverizing makes it by 40 mesh sieves, and making content is 55,81% polythiane hydrochloric acid soluble powder product 48.35g.Add oxalic acid 0.5g and carrier light magnesium carbonate 4.5g again, finally make content and be 50.43% product 53.3g.
Embodiment 2: experimental provision is with embodiment 1, take by weighing the 15.40% polythiane toluene solution 190.9g (0.12mol) that contains of drying, add toluene 356g, ethylene glycol 1.5ml, light magnesium carbonate 15g, precipitated calcium carbonate 5g feeds dry hydrogen chloride under strong agitation.Control salify endpoint pH is 3～4.5.Afterwards with embodiment 1 filter, oven dry, crushing screening, make the soluble powder of polythiaane product 69.0g of content 45.72%.Add 0.7g oxalic acid, 6.7g light magnesium carbonate, the 1.5g precipitated calcium carbonate makes the product 77.4g of content 40.43%.
Embodiment 3: experimental provision is with embodiment 1, in the there-necked flask of 3000ml, add dry cross contain 17.59% polythiane toluene solution 557.0g (0.4mol), toluene 1800g, hydrated SiO 2 (white carbon) 100g.Following steps filter, dry, pulverize, make content with embodiment 2, logical hydrogen chloride, behind the terminal point be 50.9% soluble powder of polythiaane product 216g, adds the 218g that 2g oxalic acid is mixed with the product of content 50.42%.
Claims (4)
1. the preparation method of soluble powder of polythiaane is characterized in that adding a kind of carrier in the preparation process of polythiane hydrochloride, and the polythiane hydrochloride is adsorbed on the micropore of carrier.
2. in accordance with the method for claim 1, it is characterized in that used carrier is precipitated calcium carbonate, light magnesium carbonate, lightweight hydrated SiO 2, anhydrous sodium sulfate, phosphate, A type molecular sieve, high grade kaolinite, bentonite, diatomite etc. or their mixture.
3. in accordance with the method for claim 1, it is characterized in that carrier is to add feed dry hydrogen chloride in the organic solution of institute's polythiane before, its addition is 2/3～4/5 of a theoretical amount of calculation.
4. in accordance with the method for claim 1, it is characterized in that wanting when the dry hydrogen chloride of polythiane solution feeding prepares the polythiane hydrochloride strong agitation, reach behind the terminal point through abundant mixing, sample analysis is added an amount of stabilizing agent oxalic acid and is added carrier by the product content requirement again and make filler.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN93118875A CN1046079C (en) | 1993-10-21 | 1993-10-21 | Process for preparing soluble powder of polythiaane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN93118875A CN1046079C (en) | 1993-10-21 | 1993-10-21 | Process for preparing soluble powder of polythiaane |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1101792A CN1101792A (en) | 1995-04-26 |
| CN1046079C true CN1046079C (en) | 1999-11-03 |
Family
ID=4992691
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN93118875A Expired - Fee Related CN1046079C (en) | 1993-10-21 | 1993-10-21 | Process for preparing soluble powder of polythiaane |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1046079C (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101372943B1 (en) * | 2012-06-26 | 2014-03-12 | 주식회사경농 | Method for preparing emulsifiable solid agrochemical composition comprising an inorganic salt |
| US20240041028A1 (en) * | 2021-01-04 | 2024-02-08 | Omya International Ag | Delivery system for plant protection |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85102251A (en) * | 1985-04-01 | 1986-09-24 | 贵州省化工研究所 | The preparation method of polythiane |
-
1993
- 1993-10-21 CN CN93118875A patent/CN1046079C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85102251A (en) * | 1985-04-01 | 1986-09-24 | 贵州省化工研究所 | The preparation method of polythiane |
Non-Patent Citations (1)
| Title |
|---|
| 农药学会第五届年会论文集中国化式学会农药学会 1989.10.1 《多噻烷合成及其结构鉴定》郭文松等 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1101792A (en) | 1995-04-26 |
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| C06 | Publication | ||
| PB01 | Publication | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |