CN102217591A - Environmentally-friendly abamectin ointment production process - Google Patents
Environmentally-friendly abamectin ointment production process Download PDFInfo
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- CN102217591A CN102217591A CN2011101046583A CN201110104658A CN102217591A CN 102217591 A CN102217591 A CN 102217591A CN 2011101046583 A CN2011101046583 A CN 2011101046583A CN 201110104658 A CN201110104658 A CN 201110104658A CN 102217591 A CN102217591 A CN 102217591A
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Abstract
The invention relates to an environmentally-friendly abamectin ointment production process. The environmentally-friendly abamectin ointment production process comprises the following steps of: A, fermenting abamectin; B, filtering and drying a fermentation solution; C, extracting with secbutyl acetate, washing and filtering; D, concentrating the extract into paste to obtain an environmentally-friendly abamectin ointment product; and E, continuously extracting, dissolving and repeatedly crystallizing the concentrate to obtain a fine abamectin powder product. The environmentally-friendly nontoxic secbutyl acetate solvent is used for substituting a toxic toluene solvent to produce the abamectin ointment product, so that secondary pollution of the toxic solvent to a farmland is reduced, the harm of the toxic solvent to a user is reduced, and precious petroleum resources are saved.
Description
Technical field
The present invention relates to a kind of environment-friendly type Avermectin ointment production technology.
Technical background
Avermectin is a kind of low toxicity, efficient, high selection, green, environment-friendly type, biogenic insecticide, it has solved fully that traditional agricultural chemicals exists high poison, resistance and to the problem that environment exerts an influence, has been the key research projects of China's " the Seventh Five-Year Plan ", " eight or five ", " 95 ", " 15 " and Eleventh Five-Year Plan.Along with the popularizing and promoting of Avermectin and downstream product in recent years, not only driven greatly developing of China's agricultural, livestock breeding, and promoted farming and animal husbandry production to change to green, innoxious direction.
As the present Avermectin of one of effective insecticidal agent the most in the world, usage amount was about about 2500 tons in domestic year, became the main product in the agricultural chemical insecticide.Avermectin product commonly used mainly contains two kinds of the smart powder of Avermectin and Avermectin ointment on agricultural chemicals, and the Avermectin ointment is the accessory after the smart powder of Avermectin refines, and is the xylene soluble creamy, and content is between 3-7%.Because the Avermectin ointment is easy to dispose corresponding abamectin emulsifiable concentrate and microemulsion product, therefore be subjected to the extensive welcome of pesticidal preparations production firm, its consumption accounts for more than 70% of Avermectin product sales volume.The smart powder of Avermectin also has certain consumption, but consumption is less, and general and Avermectin ointment is used for the high-load abamectin emulsifiable concentrate simultaneously.
The extraction process flow process that Avermectin is general is that zymotic fluid is collected filter cake behind plate-frame filtering, divide the immersion filter cake 3 times with 5～6 times methyl alcohol or ethanol, merge leaching liquor, and concentrating under reduced pressure, use twice of toluene, the xylene extraction of 2 times of volumes then, behind 1% activated carbon decolorizing, concentrating under reduced pressure obtains yellow oil and is the Avermectin ointment.Use the drawback of this Avermectin ointment to be that organic solvents such as toluene, dimethylbenzene cause the pollution of farmland and plant easily.
Summary of the invention
In order to overcome the deficiencies in the prior art, the invention provides environment-friendly type Avermectin ointment production technology, the present invention replaces toxic solvent toluene to come production Avermectin ointment product with environment-friendly type innoxious solvent 2-butyl acetate, reduced the secondary pollution of toxic solvent to the farmland, reduced the harm of toxic solvent, saved valuable petroleum resources the user.
The technical solution adopted in the present invention is: this environment-friendly type Avermectin ointment production technology, and its processing step is as follows: the fermentation of A, Avermectin; B, filtering fermentation liquor, drying; C, 2-butyl acetate lixiviate, washing, filtration; D, be condensed into paste and get environment-friendly type Avermectin ointment product; E, concentrate continued extraction, dissolving and repeated crystallization and the smart powder product of Avermectin.Innovation of the present invention is that C selects for use 2-butyl acetate to carry out the lixiviate of active ingredient in the step, directly obtains novel environment-friendly Avermectin ointment product without extraction at D in the step.
2-butyl acetate is a sec-butyl acetate, also claims butyl acetate-sec, molecular formula CH
3COO (CH
3) CHCH
2CH
3, molecular weight 116.16 is one of four kinds of isomer of butyl acetate.2-butyl acetate is colourless liquid with fruit flavor.2-butyl acetate is generally at industrial promotion component or reaction dissolvent etc. as spices, solvent, drug absorption.2-butyl acetate have that solvent nature is strong, evaporation rate is moderate when the extractant, little, the residual advantage such as few of extraction yield height, toxicity.
The invention has the beneficial effects as follows: the present invention will utilize 2-butyl acetate to replace used ethanol, toluene, dimethylbenzene in the Avermectin extraction process, and environmental protection and shortening separation and purification flow process, simplification separate purification step, improve product purity, reduce production costs.
Embodiment:
The invention will be further described below in conjunction with embodiment:
This environment-friendly type Avermectin ointment production technology, its processing step is as follows:
Embodiment 1:
A, Avermectin is produced bacterial classification A Foman streptomycete at first in the indoor natural separation of carrying out of bacterial classification, be coated with two dish medium, constant temperature (28.0 ± 0.5 ℃) was cultivated after 7 days, choose single bacterium colony and go into eggplant bottle inclined-plane constant temperature (28.0 ± 0.5 ℃) cultivation 10 days, filter out the slant strains that height is tired by shaking the bottle investigation, this is produced the spore or the mycelia of bacterial classification, under aseptic situation, insert in the seeding tank, in seed culture medium, after cultivating 45 hours under the suitable culture condition, treat that seed liquor concentration reaches more than 28%, mycelia becomes net that balling trend is arranged, and changes fermentation tank over to.In fermentation medium, after cultivating 300 hours under the suitable culture condition, treat that total reducing sugar is depleted to below 2%, reducing sugar is depleted to below 0.8%, and the mycelia microscopy has tangible autolysis, and PH is judged to be when rise trend is arranged and sends out a jar terminal point, finishes fermentation.
B, zymotic fluid is heated to 85 ℃ after, zymotic fluid is squeezed into plate and frame filter press filters, collect filter cake, guarantee that the Avermectin content of filtrate is lower than 20ug/ml.Moisture content behind the plate-frame filtering is carried out drying at 60%～80% filter cake, obtain water capacity after the drying and be the dried mycelium below 10%.
C, the ratio of dried mycelium according to 1:3 is immersed in the 2-butyl acetate, stirred the normal temperature lixiviate 8 hours, carry out plate-frame filtering, collect mycelium and carry out the secondary lixiviate, the ratio of mycelium and 2-butyl acetate is 1:3, stirs the back soak at room temperature 6 hours, carry out plate-frame filtering once more, collect mycelium and carry out three lixiviates, the ratio of mycelium and 2-butyl acetate is 1:2, stirs the back soak at room temperature 4 hours.Collect the above leaching liquor that three times lixiviate produced, add water, stir after 20 minutes under 55～60 ℃ the condition, static 20 minutes, water is got rid of according to the ratio of 5:2.Repeat above-mentioned washing operation 2 times.
D, leaching liquor is distilled, concentrates.In the still-process, the destilling tower liquid level is controlled at 50%～60%, 80～85 ℃ of column bottom temperature controls, 50～55 ℃ of distillate temperature controls.The preliminary back leaching liquor that concentrates continues into concentrating under reduced pressure in the concentration kettle, reach needed Avermectin concentration after, stop to concentrate.Filtration, centrifugal removal mechanical admixture obtain dark red brown paste and are novel Avermectin ointment product.
E, in D step 2-butyl acetate is all steamed, add dissolve with ethanol according to the ratio of 1:6 and stirred 30 minutes, carry out nature cooling 10 hours, primary crystallization is carried out in temperature≤15 ℃, filters after the crystallization, and wet-milling is weighed; Add ethanol according to the ratio of 1:10,2% active carbon, 0.05% glacial acetic acid, 70～80 ℃ of dissolvings of temperature were stirred 30 minutes, lowered the temperature 8 hours naturally, and secondary crystallization is carried out in temperature≤15 ℃, filters after the crystallization, and wet-milling is weighed; Add ethanol according to the ratio of 1:13,1% active carbon, 0.1% glacial acetic acid, 70～80 ℃ of dissolvings of temperature were stirred 30 minutes, lowered the temperature 8 hours naturally, and three crystallizations are carried out in temperature≤15 ℃.Filter after the crystallization, dig with cold ethanol and wash, the constant temperature water bath oven dry is the smart powder product of Avermectin.
The prepared Avermectin ointment of said method is experimentized:
Experiment 1:
In conjunction with the strong characteristics of 2-butyl acetate solubility property, select for use 2-butyl acetate to carry out the lixiviate of active ingredient in the dried mycelia, reduce solvent consumption.And the extracting effect of 2-butyl acetate is significantly better than conventional methyl alcohol or the ethanol that uses in the present production.
The normal temperature lixiviate contrast table 1 of identical dried mycelia, same equal time, different solvents
Experiment 2:
Each 500 kilograms of the dried mycelia of Avermectin that obtains through step B carry out three lixiviates respectively with 2-butyl acetate and ethanol.Obtain the 2-butyl acetate leaching liquor and add up to 4 tons, obtain alcohol extract and add up to 9 tons.Distillation concentration process parameter and energy consumption situation see Table 2.
Table 2
Identical material is when lixiviate, and the leaching liquor volume of 2-butyl acetate is half of alcohol extract, although the 2-butyl acetate boiling point is higher, distillation needs higher temperature, has shortened operation hours, has saved power consumption and production cost.
Experiment 3:
500 kilograms of the dried mycelia that obtains through step B, after carrying out lixiviate three times with 2-butyl acetate, extraction time amounts to 18 hours, obtain leaching liquor and add up to 4000 kilograms, for the leaching liquor that obtains washing three times (because of ethanol and water dissolve each other, so the leaching liquor of ethanol can't be washed), add 1600 kilograms in water at every turn, stir after 20 minutes under 55 ℃ the condition, static 20 minutes, after getting rid of water, distill, concentrate, volume reaches 1500 kilograms, 1100 kilograms, 800 kilograms, 600 kilograms, stop to concentrate sampling filtering about 400 kilograms, centrifugal removal mechanical admixture, detecting respectively and obtaining content is 3.8%, 5.5%, 7.68%, 9.8%, 14.68% ointment product.0 ℃ of storage of the cold storage-stable of finished product 14 days, 54 ℃ of storages of heat storage stability 14 days.The results are shown in Table 3.
Table 3
Present embodiment is by utilizing the Avermectin in the 2-butyl acetate extraction thalline, and specific energy consumption, material consumption obviously reduce mutually with conventional ethanol lixiviate.The conventional leach extraction method of the mass ratio of ointment product leaching liquor carried out three washings, removed the partial impurities in the ointment, so will be got well.Every index of 2-butyl acetate ointment is significantly better than the ointment product of routine.The results are shown in Table 4.
Table 4
Present embodiment replaces used ethanol, toluene, dimethylbenzene in the Avermectin extraction process by utilizing 2-butyl acetate, shorten the separation and purification flow process, simplify and separate purification step, reduce production costs, improved product quality, the what is more important product conforms with the environmental protection code requirement.
Embodiment 2:
A, Avermectin is produced bacterial classification A Foman streptomycete at first in the indoor natural separation of carrying out of bacterial classification, be coated with two dish medium, constant temperature (28.0 ± 0.5 ℃) was cultivated after 7 days, choose single bacterium colony and go into eggplant bottle inclined-plane constant temperature (28.0 ± 0.5 ℃) cultivation 10 days, filter out the slant strains that height is tired by shaking the bottle investigation, this is produced the spore or the mycelia of bacterial classification, under aseptic situation, insert in the seeding tank, in seed culture medium, after cultivating 45 hours under the suitable culture condition, treat that seed liquor concentration reaches more than 28%, mycelia becomes net that balling trend is arranged, and changes fermentation tank over to.In fermentation medium, after cultivating 300 hours under the suitable culture condition, treat that total reducing sugar is depleted to below 2%, reducing sugar is depleted to below 0.8%, and the mycelia microscopy has tangible autolysis, and PH is judged to be when rise trend is arranged and sends out a jar terminal point, finishes fermentation.
B, zymotic fluid is heated to 85 ℃ after, zymotic fluid is squeezed into plate and frame filter press filters, collect filter cake, guarantee that the Avermectin content of filtrate is lower than 20ug/ml.Moisture content behind the plate-frame filtering is carried out drying at 60%～80% filter cake, obtain water capacity after the drying and be the dried mycelium below 10%.
C, the ratio of dried mycelium according to 1:5 is immersed in the 2-butyl acetate, stirred the normal temperature lixiviate 5 hours, carry out plate-frame filtering, collect mycelium and carry out the secondary lixiviate, the ratio of mycelium and 2-butyl acetate is 1:4, stirs the back soak at room temperature 4 hours, carry out plate-frame filtering once more, collect mycelium and carry out three lixiviates, the ratio of mycelium and 2-butyl acetate is 1:3, stirs the back soak at room temperature 4 hours.Collect the above leaching liquor that three times lixiviate produced, add water, stir after 20 minutes under 50～55 ℃ the condition, static 30 minutes, water is got rid of according to the ratio of 5:1.Repeat above-mentioned washing operation 2 times.
D, leaching liquor is distilled, concentrates.In the still-process, the destilling tower liquid level is controlled at 55%-65%, 85～90 ℃ of column bottom temperature controls, 55～60 ℃ of distillate temperature controls.The preliminary back leaching liquor that concentrates continues into concentrating under reduced pressure in the concentration kettle, reach needed Avermectin concentration after, stop to concentrate.Filtration, centrifugal removal mechanical admixture obtain dark red brown paste and are novel Avermectin ointment product.
E, in D step 2-butyl acetate is all steamed, add dissolve with ethanol according to the ratio of 1:6 and stirred 30 minutes, carry out nature cooling 10 hours, primary crystallization is carried out in temperature≤15 ℃, filters after the crystallization, and wet-milling is weighed; Add ethanol according to the ratio of 1:10,2% active carbon, 0.05% glacial acetic acid, 70～80 ℃ of dissolvings of temperature were stirred 30 minutes, lowered the temperature 8 hours naturally, and secondary crystallization is carried out in temperature≤15 ℃, filters after the crystallization, and wet-milling is weighed; Add ethanol according to the ratio of 1:13,1% active carbon, 0.1% glacial acetic acid, 70～80 ℃ of dissolvings of temperature were stirred 30 minutes, lowered the temperature 8 hours naturally, and three crystallizations are carried out in temperature≤15 ℃.Filter after the crystallization, dig with cold ethanol and wash, the constant temperature water bath oven dry is the smart powder product of Avermectin.
The prepared Avermectin ointment of said method is tested:
500 kilograms of the dried mycelia that obtains through step B, carry out lixiviate three times with 2-butyl acetate after, extraction time amounts to 12 hours, obtain leaching liquor and add up to 6000 kilograms,, add 1200 kilograms in water at every turn for the leaching liquor washing that obtains three times, stir after 20 minutes under 50～55 ℃ the condition, static 30 minutes, behind the eliminating water, distill, in the still-process, the destilling tower liquid level is controlled at 55%-65%, 85～90 ℃ of column bottom temperature controls, 55～60 ℃ of distillate temperature controls.The preliminary back leaching liquor that concentrates continues the into interior concentrating under reduced pressure of concentration kettle, volume reaches about 1500 kilograms, 1100 kilograms, 800 kilograms, 600 kilograms, 400 kilograms and stops to concentrate, sampling filtering, centrifugal removal mechanical admixture, detecting respectively and obtaining content is 4.0%, 5.42%, 7.53%, 10.2%, 15.25% ointment product.0 ℃ of storage of the cold storage-stable of finished product 14 days, 54 ℃ of storages of heat storage stability 14 days.The results are shown in Table 5.
Table 5
Present embodiment replaces used ethanol, toluene, dimethylbenzene in the Avermectin extraction process by utilizing 2-butyl acetate, shortens the separation and purification flow process, simplifies and separate purification step, has obtained qualified Avermectin ointment product.
Claims (3)
1. environment-friendly type Avermectin ointment production technology, its processing step is as follows: the fermentation of A, Avermectin; B, filtering fermentation liquor, drying; C, 2-butyl acetate lixiviate, washing, filtration; D, be condensed into paste and get environment-friendly type Avermectin ointment product; E, concentrate continued extraction, dissolving and repeated crystallization and the smart powder product of Avermectin.
2. environment-friendly type Avermectin ointment production technology according to claim 1 is characterized in that:
Step C: the dried mycelium that step B is obtained is immersed in the 2-butyl acetate according to the ratio of mass ratio 1:3～1:5, stirred the normal temperature lixiviate 5～8 hours, carry out plate-frame filtering, collect mycelium and carry out the secondary lixiviate, the mass ratio of mycelium and 2-butyl acetate is 1:3～1:4, stirred the back soak at room temperature 4～6 hours, carry out plate-frame filtering once more, collect mycelium and carry out three lixiviates, the mass ratio of mycelium and 2-butyl acetate is 1:2～1:3, stir back soak at room temperature 4 hours, collect the above leaching liquor that three times lixiviate produced, add water according to the mass ratio of 5:1～5:2, stir after 20 minutes under 50～60 ℃ the condition, static 20～30 minutes, water is got rid of, repeat above-mentioned washing operation 2 times.
3. environment-friendly type Avermectin ointment production technology according to claim 2, it is characterized in that: step D: step C leaching liquor is distilled, concentrates, in the still-process, the destilling tower liquid level is controlled at 50%～65%, 80～90 ℃ of column bottom temperature controls, 50～60 ℃ of distillate temperature controls, the preliminary back leaching liquor that concentrates continues the into interior concentrating under reduced pressure of concentration kettle, after reaching needed Avermectin concentration, stop to concentrate, filtration, centrifugal removal mechanical admixture obtain dark red brown paste and are Avermectin ointment product.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102613172A (en) * | 2012-02-29 | 2012-08-01 | 大庆志飞生物化工有限公司 | Novel methylamino abamectin benzoate ointment and production method thereof |
| CN102617668A (en) * | 2012-02-29 | 2012-08-01 | 大庆志飞生物化工有限公司 | Production process of high-purity abamectin fine powder |
| CN103333214A (en) * | 2013-07-03 | 2013-10-02 | 大庆志飞生物化工有限公司 | Preparation method of Avermectin B2a fine powder |
| CN103613624A (en) * | 2013-12-05 | 2014-03-05 | 宁夏启元药业有限公司 | Refining method of avermectin |
| CN104650167A (en) * | 2015-03-10 | 2015-05-27 | 齐鲁制药（内蒙古）有限公司 | Preparation method of high-purity abamectin B2a |
| CN108164576A (en) * | 2017-12-26 | 2018-06-15 | 宁夏泰益欣生物科技有限公司 | A kind of extracting method of avermectin |
| CN111387179A (en) * | 2020-04-29 | 2020-07-10 | 河北威远生物化工有限公司 | Avermectin B2a solvation solid and preparation method thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102613172A (en) * | 2012-02-29 | 2012-08-01 | 大庆志飞生物化工有限公司 | Novel methylamino abamectin benzoate ointment and production method thereof |
| CN102617668A (en) * | 2012-02-29 | 2012-08-01 | 大庆志飞生物化工有限公司 | Production process of high-purity abamectin fine powder |
| CN102617668B (en) * | 2012-02-29 | 2015-04-08 | 大庆志飞生物化工有限公司 | Production process of high-purity abamectin fine powder |
| CN103333214A (en) * | 2013-07-03 | 2013-10-02 | 大庆志飞生物化工有限公司 | Preparation method of Avermectin B2a fine powder |
| CN103333214B (en) * | 2013-07-03 | 2015-08-12 | 大庆志飞生物化工有限公司 | A kind of Avrmectin B 2athe preparation method of fine powder |
| CN103613624A (en) * | 2013-12-05 | 2014-03-05 | 宁夏启元药业有限公司 | Refining method of avermectin |
| CN103613624B (en) * | 2013-12-05 | 2016-06-15 | 宁夏启元药业有限公司 | The process for purification of a kind of Avrmectin |
| CN104650167A (en) * | 2015-03-10 | 2015-05-27 | 齐鲁制药（内蒙古）有限公司 | Preparation method of high-purity abamectin B2a |
| CN108164576A (en) * | 2017-12-26 | 2018-06-15 | 宁夏泰益欣生物科技有限公司 | A kind of extracting method of avermectin |
| CN111387179A (en) * | 2020-04-29 | 2020-07-10 | 河北威远生物化工有限公司 | Avermectin B2a solvation solid and preparation method thereof |
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Application publication date: 20111019 |