CN1148936A - Concentration of Thuricide - Google Patents

Concentration of Thuricide Download PDF

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Publication number
CN1148936A
CN1148936A CN 96109494 CN96109494A CN1148936A CN 1148936 A CN1148936 A CN 1148936A CN 96109494 CN96109494 CN 96109494 CN 96109494 A CN96109494 A CN 96109494A CN 1148936 A CN1148936 A CN 1148936A
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China
Prior art keywords
feed liquid
concentration
ultrafilter
filtered solution
concentrate
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CN 96109494
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CN1066915C (en
Inventor
任东伟
李建中
刘忠洲
李书申
孙庆
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Research Center for Eco Environmental Sciences of CAS
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Research Center for Eco Environmental Sciences of CAS
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Publication of CN1066915C publication Critical patent/CN1066915C/en
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Abstract

A process for concentrating bacillus thuringiesis insecticide as biologic agricultural chemical features use of ultrafiltration in semipermeable membrane separation to intercept the active components in the said insecticide. It includes such steps as pre-filtering fermented liquid of bacillus thuringiesis, storing it in cyclic tank, ultrafiltrating to concentrate the liquid material to a certain concentration, addition of stabilizer and regulation of pH value in buffer, and pouring it in containers. The filtered liquid is used to wash the filter membrane. The intercepted rate of bacillus thuringiesis is up to 100% without damage to their activity.

Description

Concentration of Thuricide
Concentration of Thuricide of the present invention is the filtering technique that utilizes in the semipermeable membrane isolation technics, holds back effective ingredient in this insecticide, reaches the purpose of concentrate pesticidal, belongs to the technical field of general physical separating method.
Biopesticide is compared with chemical pesticide, have harmless to people and animals' thing, insect is difficult for developing immunity to drugs, insecticidal effect is stablized advantages such as lasting, is one of main means of biological control crop pests.The biopesticide of China is used area and is lower than world average level, not as good as 0.5% of total control area.Therefore, greatly develop biopesticide, it is studied, develop that biopesticide is significant for China's agricultural production efficiently.
Bacillus thuringiensis (Bacillus thuringiensis sp.) insecticide has very strong insecticidal effect for many crops.The inventor adopts the strongest bacterial strain of the present virus killing power of bacillus thuringiensis in the world to prepare the feed liquid that is rich in bacillus thuringiensis under new technological condition for fermentation, need carry out concentration for these fermentation materials and tire, be convenient to transportation and storage simultaneously with raising.
For the method for concentration of bacillus thuringiensis fermented feed liquid,, do not see the report that adopts ultrafiltration to concentrate so far from the reported in literature and the domestic and international Searches of Patent Literature.At present mostly the method that adopts of prior art is centrifugal and concentrates, ebullated bed concentrates, vacuum filtration concentrates, expandedly concentrate, thin film evaporation concentrates etc.Some method, though reach concentrated purpose as centrifugal separation, concentrated effect is not good enough, and efficient is low, and loss of effective components is bigger; As the ebullated bed concentration method, by Steam Heating, water evaporates in the material is reached concentrated purpose, yet bacillus thuringiensis loses activity easily owing to the temperature height in concentration process, and also complicated operation, the energy consumption height.Relevant domestic and international patent documentation has: JP05023194 (1991), JP05211876 (1991), JP05260982 (1992), SU1792613 (1989), JP04265126 (1991), CN1068368 (1992), CN1061437 (1991), CN1064502A etc.
The various shortcoming and the weak point that in above-mentioned concentration process, produce for the fermentation product feed liquid that overcomes thuringiensis cladosporioides bacillus insecticide, technical scheme of the present invention should keep active unlikely infringement of this bacterium, advantage such as improve output capacity again as far as possible and cut down the consumption of energy.
The object of the present invention is to provide a kind of method of concentrated bacillus thuringiensis fermented feed liquid, make the essentially no loss of active ingredient of insecticide, and save the energy.
The present invention adopts hyperfiltration technique, because ultrafiltration is a kind of physical process purely, the biopesticide of bacillus thuringiensis preparation does not have chemical reaction in ultra-filtration process, no phase transformation, and normal-temperature operation is not so can damage this bacterium in whole process.Because the molecular size of bacillus thuringiensis is about about 1 μ, thalline is kept in the concentrate simultaneously, can cause the loss of this bacterium, tire thereby increase substantially so specific milipore filter can reach hundred-percent rejection to it.
Method for concentration of the present invention is realized by following equipment and step.
The bacillus thuringiensis zymotic fluid enters through prefilter and treats the concentrate feed liquid bath, and again through coarse filtration, circulating storage groove is gone in storage.Feed liquid is input into ultrafilter from circulating storage groove, and bacillus thuringiensis is stopped because of not seeing through milipore filter, realizes that solid-liquid separates, and water and small-molecule substance then see through film and flow into the filtered solution storage tank.A filtered solution part is used for the anti-cleaning to milipore filter, and all the other then efflux.Flow into circulating storage groove through the isolated once concentration feed liquid that contains bacillus thuringiensis of ultrafilter again by valve and pipeline, can enter ultrafilter once more and carry out secondary concentration, so circulation repeatedly, bacillus thuringiensis reaches predetermined concentration and transports to surge tank then in concentrate, add stabilizing agent, carry out the finished product can after the adjustment pH value.
It is inner pressed single skin hollow-fibre membrane that the present invention adopts milipore filter, also can adopt flat sheet membrane or rolled film.The hollow-fibre membrane inwall is a separating layer, and outer wall is an open-celled structure, makes through the water of internal layer and small-molecule substance is unlikely is stopped by outer wall.Along with the continuous concentration process of feed liquid, milipore filter will produce contamination and plugging descends percolate flux.In order to address this problem, in this technological process, the filtered solution in the filtered solution storage tank can be used for cleaning to milipore filter is counter, promptly clean to inwall from the milipore filter outer wall, remove the gel layer that sticks on the film inwall, make milipore filter keep stable performance.
The invention provides a width of cloth accompanying drawing, Biotrol BTV concentrator and block diagram are among the figure: 1 prefilter; 2 treat the concentrate feed liquid bath; 3 coarse filters; 4 circulating storage grooves; 5 ultrafilters; 6 cooling systems; 7 surge tanks; 8 filtered solution storage tanks.
The invention will be further described below in conjunction with accompanying drawing.
Contain the feed liquid of Dipel through some bigger particles of prefilter 1 filtering, pre-filter medium choosing Use nylon cloth, its advantage is inexpensive, easily change, but Reusability after the cleaning. Pre-filtrate entering treated dense Contracting feed liquid storage tank 2 enters circulating storage groove 4 by coarse filter 3. The medium of coarse filter is selected closeer Nylon cloth is further removed particle in some feed liquids alleviating the obstruction to ultrafilter, prolongs ultrafilter Service life. Feed liquid flows out laggardly to enter ultrafilter 5 and carry out concentration from circulating slot 4. Milipore filter is saturating The liquid of crossing enters filtered solution storage tank 8, and wherein a part of filtered solution is prepared against the usefulness of the anti-cleaning of film, its Besides arrange. Feed liquid is transported to surge tank when circulation is concentrated to predefined concentration in circulating slot 4 7, at surge tank 7 interior adding stabilizing agents, regulate the pH value, pass through then canning line can Cheng Suyun gold The finished product of bacillus pesticide. In addition, in ultra-filtration process, for avoiding feed temperature too high, also be equipped with cold But system 6 lowers the temperature to feed liquid.
Ultrafilter 5 is the most important equipment of whole feed liquid concentration technology, and the Main Function of ultrafilter is to use Milipore filter is held back bacillus thuringiensis in the feed liquid, and some small-molecule substances and water then see through film. By Have different apertures in milipore filter, usually come the big of secondary indication aperture by the size of molecular cut off Little. In order effectively to hold back Dipel, it is 60,000 dalton that the present invention has made molecular cut off Milipore filter, its rejection to bacillus thuringiensis can reach 100%. Because feed liquid is at normal temperature The lower operation in ultrafilter mainly is physical process, so through bacillus thuringiensis after the hyperfiltration treatment Active ingredient is trapped within the concentrate, and the small-molecule substances such as water then see through film. So, concentrate The concentration of middle active ingredient increases substantially, and tiring is improved. When reaching required concentration, dense The feed liquid of contracting enters surge tank 7 from circulating storage groove 4, adds stabilizing agent in tank, adjusts the pH value, namely But can finished product.
Feed liquid is being carried out in the continuous ultra-filtration process, and milipore filter will produce inevitably to pollute and cause film Flux descend, thickening efficiency reduces. For solving these difficult problems, what the present invention selected is anti-pollution Film is selected rational operating parameter and operating procedure in operation simultaneously. What the present invention selected is hydrophilic The polymeric material A that property is good or the polymeric material B after the modification or polymer A, B bi-material The film that blend is made makes film both have the good hydrophily of materials A, has again the anti-of material B Pollution capacity. The A material is polysulfones, polyether sulfone, phenolphthalein side group etc.; The B material be polyvinyl alcohol, SPSF, acetate fiber etc.
The kit form of milipore filter has Flat Membrane, rolled film, middle chamber tunica fibrosa. The present invention adopts hollow The fiber film component form also can adopt Flat Membrane or rolled film. Hollow-fibre membrane has several forms, Such as single skin, two cortexes etc. The present invention adopts inner pressed single skin hollow-fibre membrane, and its inwall is for dividing Absciss layer, outer wall is open-celled structure, makes through the small-molecule substance of internal layer can not held back by outer wall.
Along with the ultrafiltration prolongation of running time, feed concentration improves constantly, and face will pollute, very Extremely dense feed liquid can stick to the film surface, forms the layer of gel layer permeable amount is sharply reduced, serious shadow Ring the performance of film. The present invention adopts the membrane module of ultrafilter 5 to import and export exchange method and anti-cleaning side Method, namely when normal operation, the liquor inlet of ultrafilter 5 membrane modules intermittently exchanges with outlet, like this Can effectively control feed liquid and form gel layer at face, thereby the life-span of film is prolonged significantly. Work as film Permeable amount when dropping to a certain degree, can also adopt the method for anti-cleaning, backwash liquor is directly from filter Cross in the liquid storage tank 8 and obtain. The present invention adopts full automatic working technology, and the material liquid entrance of membrane module is mutual Change, instead clean and all take automatic control, ultrafilter 5 can be moved steadily in the long term.
Compare with prior biological agricultural chemicals method for concentration, the present invention concentrates biopesticide, and technology is simple, and the rejection of agricultural chemicals is high and preserve biologically active fully, and the basic free of losses of drug effect is energy-conservation, and the filtered solution discharging does not pollute environment.
An embodiment below is provided.
Concentrating and treating system according to technical scheme design of the present invention experimentizes in certain biopesticide factory, and its operation such as accompanying drawing are shown in Figure 1.From the zymotic fluid in the fermentation tank, promptly feed liquid is gone into ultrafilter 5 and is carried out ultrafiltration and concentration through the two-stage pre-flock is laggard, the about 1,000,000,000/m1 of bacillus thuringiensis concentration in the zymotic fluid, and the ultrafilter inlet pressure is 0.2MPa, outlet pressure is 0.03MPa.After the process loop ultrafiltration concentrated, this cell concentration reached the about 10,000,000,000/m1 that requires in advance.This concentration technology experimentizes at the scene, and operation conditions is good, and particularly ultrafilter 5 ultrafiltration membrane permeate rate variation in the long-play process is little, remains on 10L/m always 2About h.Bacillus thuringiensis is through behind the ultrafiltration and concentration, and thalline 100% is trapped in and concentrates in the feed liquid, does not have any loss, and filtered solution is some low molecule fermentation product and water.
With method of the present invention 6 tons of zymotic fluids being carried out ultrafiltration and concentration only needed 2 hours can reach concentrated requirement.
Concentrate shows that through biological analysis and microscopy and actual spray test concentrate is tired and increased substantially.Method concentrated biological agricultural chemicals of the present invention is compared with centrifugal concentration method, evaporation concentration method, and energy consumption greatly reduces, and has saved production cost.

Claims (6)

1. concentration of Thuricide is characterized in that the hyperfiltration technique that adopts the semipermeable membrane solid-liquid to separate, the ultrafilter feed liquid that contains bacillus thuringiensis for preparing of will ferment concentrates by following equipment and step:
(1) one or more prefilter or coarse filter are in order to remove larger particles in the fermented feed liquid;
Treat the concentrate feed liquid bath for (2) one, in order to store feed liquid through pre-flock;
(3) ultrafilters, in order to hold back the bacillus thuringiensis in the feed liquid, the liquor inlet of ultrafilter can intermittently exchange with outlet;
(4) circulating storage grooves concentrate in order to feed liquid is input into ultrafilter, and its concentrate is imported circulating storage groove again, and filtered solution is input into the filtered solution storage tank;
(5) surge tanks, in order to be stored in the circulating storage groove through ultrafiltration and concentration is to the feed liquid of predetermined concentration repeatedly, can is a finished product again;
(6) filtered solution storage tanks, filtered solution wherein is used for the anti-cleaning of milipore filter, effluxes then.
2. method for concentration according to claim 1 is characterized in that the milipore filter in the ultrafilter adopts inner pressed single skin hollow-fibre membrane to make, and also can adopt flat sheet membrane or rolled film to make.
3. method for concentration according to claim 1 and 2 is characterized in that milipore filter utilizes that filtered solution is counter to be cleaned.
4. method for concentration according to claim 1 is characterized in that prefilter or coarse filter, treats the concentrate feed liquid bath, connects with pipeline between the circulating slot, ultrafilter, surge tank, filtered solution storage tank, also is provided with valve therebetween.
5. method for concentration according to claim 1 is characterized in that being provided with in the circulating storage groove cooling system.
6. method for concentration according to claim 1, the filter medium that it is characterized in that prefilter or coarse filter adopts the nylon cloth of different densities.
CN96109494A 1996-09-02 1996-09-02 Concentration of Thuricide Expired - Fee Related CN1066915C (en)

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CN96109494A CN1066915C (en) 1996-09-02 1996-09-02 Concentration of Thuricide

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Application Number Priority Date Filing Date Title
CN96109494A CN1066915C (en) 1996-09-02 1996-09-02 Concentration of Thuricide

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CN1066915C CN1066915C (en) 2001-06-13

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100420737C (en) * 2005-05-11 2008-09-24 张婷丽 Preparation process of concentrating photosynthetic bacteria
CN103636604A (en) * 2013-11-27 2014-03-19 中国科学院武汉植物园 Biopesticide synergist
CN110615151A (en) * 2019-10-28 2019-12-27 河北省微生物研究所 Pasteurization filling equipment for filling bacillus agent and application thereof

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1064502A (en) * 1991-07-30 1992-09-16 北京农业大学 Process for concentrating liquid bacterial agent of yield increasing bacteria
JPH05260982A (en) * 1992-03-23 1993-10-12 Asahi Chem Ind Co Ltd Production of microorganismic product involving continuous membrane separation
CN1068368A (en) * 1992-08-03 1993-01-27 北京市营养源研究所 Filter culture technique and produce the colibacillary method of highly containing polynucleotide Starch phosphorylase
TW342346B (en) * 1996-01-25 1998-10-11 Nat Science Council Production of thuringiensin concentrates

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100420737C (en) * 2005-05-11 2008-09-24 张婷丽 Preparation process of concentrating photosynthetic bacteria
CN103636604A (en) * 2013-11-27 2014-03-19 中国科学院武汉植物园 Biopesticide synergist
CN110615151A (en) * 2019-10-28 2019-12-27 河北省微生物研究所 Pasteurization filling equipment for filling bacillus agent and application thereof
CN110615151B (en) * 2019-10-28 2021-10-08 河北省微生物研究所 Pasteurization filling equipment for filling bacillus agent and application thereof

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