CN102489043B - Recovery technology of methylamino avermectin benzoate amination solvent - Google Patents
Recovery technology of methylamino avermectin benzoate amination solvent Download PDFInfo
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- CN102489043B CN102489043B CN 201110429462 CN201110429462A CN102489043B CN 102489043 B CN102489043 B CN 102489043B CN 201110429462 CN201110429462 CN 201110429462 CN 201110429462 A CN201110429462 A CN 201110429462A CN 102489043 B CN102489043 B CN 102489043B
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Abstract
The invention relates to a recovery technology of methylamino avermectin benzoate amination solvent. Sodium carbonate aqueous solution is utilized to separate dichloromethane and methanol in the amination solvent, and contents of water and methanol in separated and purified dichloromethane solvent accord with requirements of methylamino avermectin benzoate amination workshop section on amination solvent quality; and separated dichloromethane solvent can be used indiscriminately in the methylamino avermectin benzoate amination workshop section, and the methanol solution can be used indiscriminately in methylamino avermectin benzoate amination workshop section. The invention not only solves a treatment problem of the amination solvent but also reuses resource, so as to satisfy national energy saving, emission reduction and environmental protection idea.
Description
Technical field
The invention belongs to resource recycling and environmental protection field, be specifically related to a kind of emamection benaoate amination solvent recovery new technology.This technology can be separated the carrene in the amination solvent with methyl alcohol, and the content of moisture and methyl alcohol meets the requirement of emamection benaoate amination workshop section to the amination solvent quality in the dichloromethane solvent of separation and purification.Therefore the dichloromethane solvent after separating can overlap and be used in emamection benaoate amination workshop section, and methanol solution can overlap and be used in the emamection benaoate preparation.The present invention has not only solved the handling problem of amination solvent, and it is recycling that resource has been obtained, and meets national energy-saving and emission-reduction and environmental protection concept.
Background technology
First dimension salt full name emamection benaoate is a kind of higher effective and lower toxic pesticide.Safer to crop, be effective substitute of organophosphor and other high poison, high residue pesticide.Emamection benaoate has the incomparable activity of other agricultural chemicals to a lot of insects, especially to Lepidoptera, Diptera, the thrips class ultra high efficiency of crops such as vegetables, cotton, paddy rice, tobacco.
The technology of domestic production emamection benaoate mainly is to be raw material with the AVM now, its protection, oxidation, amination, deprotection, salify is total to five-step approach produces emamection benaoate.It need be solvent with the carrene that protection, oxidation, amination, four steps of deprotection are arranged in this five-step approach, and the solvent use amount is very big.Particularly produced the dichloromethane solution that contains methyl alcohol 10%-15% in a large number in amination workshop section.Because amination workshop section is strict to dichloromethane solvent, require that carrene content is higher than 99.4% in its solvent, methanol content is lower than 0.1%, and moisture is lower than 0.1%.And methanol content is higher in the amination solvent, can't overlap without separation and purification to be used in amination workshop section.At present, domestic major part is produced emamection benaoate enterprise by this method, and the amination solvent great majority that its amination workshop section produces are by applying mechanically after the rectification and purification.This process energy consumption height, cost height, equipment investment are big.
Summary of the invention
The objective of the invention is to overcome the shortcoming that rectificating method energy consumption height, cost height and azeotropic mixture are difficult to separate, a kind of emamection benaoate amination solvent recovery new technology is provided, reduce wastewater flow rate, cut down the consumption of energy, simplify the operation, reduce cost under the qualified condition of moisture and methanol content guaranteeing.
The inventive method comprises the steps:
(1) the amination solvent suction washing still that emamection benaoate amination workshop section is produced is opened then and is stirred, and adds the sodium carbonate liquor that the quality percentage composition is 3%-5% again, treats to leave standstill behind the material mixing, layering;
(2) collect lower floor's organic facies and be used as the aminating reaction solvent;
(3) upper water heat phase distillation, condensate liquid are reclaimed the back cover and are used in the emamection benaoate preparation; Raffinate discharging after the sewage plant processing is qualified;
Above-mentioned amination solvent contains carrene and two components of methyl alcohol, and wherein the content of carrene is 85%-90%; The content of methyl alcohol is 10%-15%.
Must be during above-mentioned steps (1) washing with amination solvent and the abundant mixing of water lotion; Must keep the enough time during standing demix, guarantee that organic facies thoroughly separates with water.The volume ratio of preferred amination solvent of this process and water lotion is 1:0.5-2, and preferred volume ratio is 1:1.2-1.5, and best water lotion is the sodium carbonate liquor of 3%-5%.
Above-mentioned steps (2) is not put into organic facies with water when collecting lower floor's organic facies, and will notice that the intermediate layer between water and the organic facies can not put into organic facies.
The temperature that above-mentioned steps (3) adds thermal distillation is not higher than 90 ℃.
The present invention adopts extraction and separation technology with carrene in the amination solvent and methyl alcohol two component separation and purification.Whole recovery process energy consumption is low, cost is low, equipment investment is few, simple to operate, thoroughly solved rectification method and separated amination solvent cost height, problem that energy consumption is high, meet national energy-saving and emission-reduction theory.
Description of drawings
Accompanying drawing is an emamection benaoate amination solvent recovery process flow chart of the present invention.
Illustration is as follows.
| Device numbering | Device name |
| V1 | Amination solvent measuring tank |
| V2 | The water lotion measuring tank |
| V3 | Receiving tank |
| E | Condenser |
| R1 | The washing still |
| R2 | Distillation still |
| P1 | Washing still stirring motor |
| P2 | The distillation still stirring motor |
The specific embodiment
Below by embodiment content of the present invention is further specified, but the present invention is not limited to these embodiment.
Embodiment 1
500mL amination solvent is added washing still (its carrene content is 89.8%, and methanol content is 10.2%), open and stir, add the 250mL mass content again and be 3% sodium carbonate water lotion.Stir after 20 minutes static layering 2 hours.Collect lower floor's organic facies, be weighed as 449g, carrene content is 99.44% in the gas chromatographic detection organic facies, and moisture is 0.09%, and methanol content is 0.04%; The inorganic water in upper strata distilled 2 hours down at 85 ℃, obtained the 52.2g condensate liquid, and methanol content is 88% in the condensate liquid after testing, and moisture is 12%.Press emamection benaoate amination workshop section synthesis technique, the carrene and the technical grade carrene that reclaim are compared as the synthetic amide of amination solvent, with reclaiming the synthetic amination owner content of carrene is 77.65%, the amination owner content synthetic with the technical grade carrene is 77.8%, and correction data shows: the carrene that reclaims by this technic index is used in emamection benaoate amination workshop section as amination solvent cover does not influence ammonification owner content.
Embodiment 2
500mL amination solvent is added washing still (its carrene content is 89.1%, and methanol content is 10.9%), open and stir, add the 500mL mass content again and be 3% sodium carbonate water lotion.Stir after 30 minutes static layering 2 hours.Collect lower floor's organic facies, be weighed as 446g, carrene content is 99.47% in the vapor detection organic facies, and moisture is 0.1%, and methanol content is 0.02%; The inorganic water in upper strata distilled 3 hours down at 85 ℃, obtained the 54.5g condensate liquid, and methanol content is 90% in the condensate liquid after testing, and moisture is 10%.Press emamection benaoate amination workshop section synthesis technique, the carrene and the technical grade carrene that reclaim are compared as the synthetic amide of amination solvent, with reclaiming the synthetic amination owner content of carrene is 79.30%, the amination owner content synthetic with the technical grade carrene is 77.8%, and correction data shows: the carrene that reclaims by this technic index is used in emamection benaoate amination workshop section as amination solvent cover does not influence ammonification owner content.
Embodiment 3
500mL amination solvent is added washing still (its carrene content is 89.5%, and methanol content is 10.5%), open and stir, add the 1000mL mass content again and be 3% sodium carbonate water lotion.Stir after 30 minutes static layering 4 hours.Collect lower floor's organic facies, be weighed as 447g, carrene content is 99.44% in the vapor detection organic facies, and moisture is 0.07%, and methanol content is 0.09%; The inorganic water in upper strata distilled 5 hours down at 85 ℃, obtained the 52.5g condensate liquid, and methanol content is 88.3% in the condensate liquid after testing, and moisture is 11.7%.Press emamection benaoate amination workshop section synthesis technique, the carrene and the technical grade carrene that reclaim are compared as the synthetic amide of amination solvent, with reclaiming the synthetic amination owner content of carrene is 77.2%, the amination owner content synthetic with the technical grade carrene is 77.8%, and correction data shows: the carrene that reclaims by this technic index is used in emamection benaoate amination workshop section as amination solvent cover does not influence ammonification owner content.
Embodiment 4
500mL amination solvent is added washing still (its carrene content is 89.8%, and methanol content is 10.2%), open and stir, add the 350mL mass content again and be 3% sodium carbonate water lotion.Stir after 20 minutes static layering 2 hours.Collect lower floor's organic facies, be weighed as 448g, carrene content is 99.4% in the vapor detection organic facies, and moisture is 0.09%, and methanol content is 0.04%; The inorganic water in upper strata distilled 2 hours down at 85 ℃, obtained the 52g condensate liquid, and methanol content is 89% in the condensate liquid after testing, and moisture is 11%.Press emamection benaoate amination workshop section synthesis technique, the carrene and the technical grade carrene that reclaim are compared as the synthetic amide of amination solvent, with reclaiming the synthetic amination owner content of carrene is 77.55%, the amination owner content synthetic with the technical grade carrene is 77.8%, and correction data shows: the carrene that reclaims by this technic index is used in emamection benaoate amination workshop section as amination solvent cover does not influence ammonification owner content.
Embodiment 5
500mL amination solvent is added washing still (its carrene content is 89.8%, and methanol content is 10.2%), open and stir, add the 250mL mass content again and be 5% sodium carbonate water lotion.Stir after 20 minutes static layering 2 hours.Collect lower floor's organic facies, be weighed as 449g, carrene content is 99.44% in the vapor detection organic facies, and moisture is 0.09%, and methanol content is 0.05%; The inorganic water in upper strata distilled 2 hours down at 85 ℃, obtained the 52.2g condensate liquid, and methanol content is 88% in the condensate liquid after testing, and moisture is 12%.Press emamection benaoate amination workshop section synthesis technique, the carrene and the technical grade carrene that reclaim are compared as the synthetic amide of amination solvent, with reclaiming the synthetic amination owner content of carrene is 77.43%, the amination owner content synthetic with the technical grade carrene is 77.8%, and correction data shows: the carrene that reclaims by this technic index is used in emamection benaoate amination workshop section as amination solvent cover does not influence ammonification owner content.
Embodiment 6
500mL amination solvent is added washing still (its carrene content is 89.8%, and methanol content is 10.2%), open and stir, add the 400mL mass content again and be 4% sodium carbonate water lotion.Stir after 40 minutes static layering 4 hours.Collect lower floor's organic facies, be weighed as 449g, carrene content is 99.47% in the vapor detection organic facies, and moisture is 0.09%, and methanol content is 0.01%; The inorganic water in upper strata distilled 2 hours down at 85 ℃, obtained the 52.0g condensate liquid, and methanol content is 89% in the condensate liquid after testing, and moisture is 11%.Press emamection benaoate amination workshop section synthesis technique, the carrene and the technical grade carrene that reclaim are compared as the synthetic amide of amination solvent, with reclaiming the synthetic amination owner content of carrene is 78.01%, the amination owner content synthetic with the technical grade carrene is 77.8%, and correction data shows: the carrene that reclaims by this technic index is used in emamection benaoate amination workshop section as amination solvent cover does not influence ammonification owner content.
500mL amination solvent is added washing still (its carrene content is 89.1%, and methanol content is 10.9%), open and stir, add the 200mL mass content again and be 4% sodium carbonate water lotion.Stir after 30 minutes static layering 2 hours.Collect lower floor's organic facies, be weighed as 428g, carrene content is 99% in the vapor detection organic facies, and moisture is 0.12%, and methanol content is 0.7%; The inorganic water in upper strata distilled 3 hours down at 85 ℃, obtained the 54.5g condensate liquid, and methanol content is 90% in the condensate liquid after testing, and moisture is 10%.Press emamection benaoate amination workshop section synthesis technique, the carrene and the technical grade carrene that reclaim are compared as the synthetic amide of amination solvent, with reclaiming the synthetic amination owner content of carrene is 65.8%, and the amination owner content synthetic with the technical grade carrene is 77.8%.Correction data shows: it is very big to ammonification owner content influence that the carrene that reclaims by this technic index is used in emamection benaoate amination workshop section as amination solvent cover.
Embodiment 8
500mL amination solvent is added washing still (its carrene content is 89.1%, and methanol content is 10.9%), open and stir, add the 200mL mass content again and be 4% sodium carbonate water lotion.Stir after 30 minutes static layering 2 hours.Collect lower floor's organic facies, be weighed as 430g, carrene content is 89.5% in the vapor detection organic facies, and moisture is 0.15%, and methanol content is 0.85%; The inorganic water in upper strata distilled 3 hours down at 85 ℃, obtained the 54g condensate liquid, and methanol content is 90% in the condensate liquid after testing, and moisture is 10%.Press emamection benaoate amination workshop section synthesis technique, the carrene and the technical grade carrene that reclaim are compared as the synthetic amide of amination solvent, with reclaiming the synthetic amination owner content of carrene is 64.96%, the amination owner content synthetic with the technical grade carrene is 77.8%, and correction data shows: it is very big to ammonification owner content influence that the carrene that reclaims by this technic index is used in emamection benaoate amination workshop section as amination solvent cover.
Embodiment of the present invention only is the description that preferred implementation of the present invention is carried out; be not that design of the present invention and scope are limited; under the prerequisite that does not break away from design philosophy of the present invention; engineers and technicians make technical scheme of the present invention in this area various modification and improvement; all should fall into protection scope of the present invention; the technology contents that the present invention asks for protection all is documented in claims.
Claims (6)
1. emamection benaoate amination solvent recovery process, it is characterized in that amination solvent suction washing still with the generation of emamection benaoate amination workshop section, the sodium carbonate liquor that adds mass content 3%-5% then is as water lotion, open and stir, mixing time be leave standstill behind the abundant mixing of 20min-60min, layering, time of repose 〉=2h; Collect lower floor's organic facies and be used in emamection benaoate amination workshop section as amination solvent cover; Water condensate liquid cover after adding thermal distillation in upper strata is used in the emamection benaoate preparation, and remaining liq is discharging after sewage plant is handled.
2. emamection benaoate amination solvent recovery process according to claim 1 is characterized in that described amination solvent composition is carrene and methyl alcohol; Wherein the content of carrene is 85%-90%, and the content of methyl alcohol is 10%-15%.
3. emamection benaoate amination solvent recovery process according to claim 1 and 2, the volume ratio that it is characterized in that described amination solvent and water lotion is 1:0.5-2.
4. emamection benaoate amination solvent recovery process according to claim 3, the volume ratio that it is characterized in that described amination solvent and water lotion is 1:1.2-1.5.
5. emamection benaoate amination solvent recovery process according to claim 1 is characterized in that described lower floor organic solvent is a carrene, and wherein the content of carrene is higher than 99.4%; The content of water is lower than 0.1%; Methanol content is lower than 0.1%.
6. emamection benaoate amination solvent recovery process according to claim 1 is characterized in that 85-90 ℃ of described upper water heat phase vapo(u)rizing temperature; The condensate liquid component is the first alcohol and water, and its methanol content is 85%-90%, and moisture is 10%-15%.
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| CN 201110429462 CN102489043B (en) | 2011-12-20 | 2011-12-20 | Recovery technology of methylamino avermectin benzoate amination solvent |
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| CN 201110429462 CN102489043B (en) | 2011-12-20 | 2011-12-20 | Recovery technology of methylamino avermectin benzoate amination solvent |
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| CN102489043B true CN102489043B (en) | 2013-07-31 |
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| CN112979591A (en) * | 2021-03-01 | 2021-06-18 | 安徽金轩科技有限公司 | Oxidation extraction process for recycling dichloromethane in preparation of furan ammonium salt |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE10203551A1 (en) * | 2002-01-29 | 2003-08-07 | Metanomics Gmbh & Co Kgaa | Extracting components from organic material, useful e.g. in large-scale metabolic profiling, comprises using a single-phase mixture containing water and methanol |
| CN1644523A (en) * | 2004-12-21 | 2005-07-27 | 哈尔滨工程大学 | Recovery of alcohol diisopropylamine from waste liquid of pharmaceutical industry |
| CN101284857A (en) * | 2008-05-28 | 2008-10-15 | 山东美罗福农化有限公司 | Process for abstracting biological pesticide avermectin from biochemical wastes |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE10203551A1 (en) * | 2002-01-29 | 2003-08-07 | Metanomics Gmbh & Co Kgaa | Extracting components from organic material, useful e.g. in large-scale metabolic profiling, comprises using a single-phase mixture containing water and methanol |
| CN1644523A (en) * | 2004-12-21 | 2005-07-27 | 哈尔滨工程大学 | Recovery of alcohol diisopropylamine from waste liquid of pharmaceutical industry |
| CN101284857A (en) * | 2008-05-28 | 2008-10-15 | 山东美罗福农化有限公司 | Process for abstracting biological pesticide avermectin from biochemical wastes |
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Denomination of invention: A kind of methylamino abamectin benzoate amination solvent recovery process Effective date of registration: 20220801 Granted publication date: 20130731 Pledgee: Hunan Linxiang rural commercial bank Limited by Share Ltd. Pledgor: HUNAN GOFAR FINE CHEMICAL TECH. CO.,LTD. Registration number: Y2022980011705 |