RO133615A2 - Process for preparing foliar bio-fertilizers together with component essential oil micro-capsules and foliar bio-fertilizer compositions - Google Patents

Process for preparing foliar bio-fertilizers together with component essential oil micro-capsules and foliar bio-fertilizer compositions Download PDF

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RO133615A2
RO133615A2 ROA201800167A RO201800167A RO133615A2 RO 133615 A2 RO133615 A2 RO 133615A2 RO A201800167 A ROA201800167 A RO A201800167A RO 201800167 A RO201800167 A RO 201800167A RO 133615 A2 RO133615 A2 RO 133615A2
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suspension
weight
taken
proportion
biofertilizer
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ROA201800167A
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Romanian (ro)
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Emil Stepan
Cristina Emanuela Enăşcuţă
Sanda Velea
Elena Radu
Elena Emilia Oprescu
Adrian Radu
Carmen Cornelia Gaidău
Doru-Gabriel Epure
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Institutul Naţional De Cercetare-Dezvoltare Pentru Chimie Şi Petrochimie - Icechim
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Priority to ROA201800167A priority Critical patent/RO133615A2/en
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A40/00Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
    • Y02A40/10Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in agriculture
    • Y02A40/20Fertilizers of biological origin, e.g. guano or fertilizers made from animal corpses

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  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The invention relates to a foliar bio-fertilizer composition and to a process for preparing the same. According to the invention, the composition consists of 14.31...19.41% hydrolised proteins with average molecular mass of 320...750 Da, 0.24...0.68% leaves adherence enhancing agent, 0.2...0.3% thickening agent, 0.73...2.70% hydrolised keratin, 6.50...8.25% micro-capsules with essential oil content having an oil release rate of 40.3...48.2% at 120 h, 4.04...5.96% non-ionic surfactants, 0.66...0.92% mixture of Cu, Zn, Fe, Mo, Mn, Mg salts of the ethylenediaminetetraacetic acid, as well as water, for the remainder, the percentage being expressed by mass. According to the invention, the process consists in manufacturing the micro-capsules with essential oil to be added into a mixture comprising hydrolised proteins, usual agents and hydrolised keratin, with intense stirring for 30 min, after which the surfactants and the aqueous solution comprising the salt mixture are added, to result in an aqueous suspension of fertilizer having a stability of >6 months.

Description

Invenția se refera la un procedeu pentru obținerea biofertilizantilor foliari împreuna cu microcapsulele cu uleiuri esențiale componente si compoziții de biofertilizanti foliari, conținând aceste microcapsule împreuna cu componenti in majoritate de proveniența naturala.The invention relates to a process for obtaining foliar biofertilizers together with microcapsules with essential oil components and compositions of foliar biofertilizers, containing these microcapsules together with components of mostly natural origin.

Sunt cunoscute numeroase procedee pentru obținerea microcapsulelor cu continui de uleiuri esențiale, avand utilizări in industria alimentara si textila.Numerous processes are known for obtaining microcapsules with continuous essential oils, having uses in the food and textile industry.

Un astfel de procedeu constă in incorporarea unei soluții de ulei esențial si etanol in hidrolizatul de colagen, omogenizarea acestuia, ajustarea pH-ului la 7,4 cu hidroxid de sodiu, adaugarea apei distilate pana când compoziția finala ajunge la 1,5 ... 10% colagen ca materie uscata, urmata de reticulare si uscarea microcapsulelor prin liofilizare sau atomizare (RO130962). Sunt prezentate compoziții de microcapsule cu uleiuri esențiale si colagen, sub forma de pulberi sferice cu diametre de 2-30 pm, utilizate la functionalizarea unor structuri textile (ex. ciorapi).Such a process consists of incorporating a solution of essential oil and ethanol into collagen hydrolyzate, homogenizing it, adjusting the pH to 7.4 with sodium hydroxide, adding distilled water until the final composition reaches 1.5 ... 10% collagen as dry matter, followed by cross-linking and microcapsule drying by lyophilization or atomization (RO130962). There are presented microcapsule compositions with essential oils and collagen, in the form of spherical powders with diameters of 2-30 pm, used for the functionalization of textile structures (eg socks).

Invenția prezintă dezavantaje legate de conducerea simplista a procesului de microincapsulare, uscarea prin atomizare a microcapsulelor poate determina degradarea acestora datorita temperaturilor ridicate (ex. 230°C), iar uscarea prin liofilizare implica un consum energetic semnificativ legat de vaporizarea unei cantitati mari de apa.The invention has disadvantages related to the simplistic conduct of the micro-encapsulation process, drying by atomization of microcapsules can cause their degradation due to high temperatures (eg 230 ° C), and drying by lyophilization implies a significant energy consumption related to the vaporization of a large amount of water.

O invenție se refera la un sistem integrat si la un procedeu de obținere a unor extracte cu rol de biofertilizant / bioinsecticid foliar in agricultura ecologica (RO131209). Procedeul consta in extracția substanțelor active din materialul vegetal la o temperatura de 37°C, cu cinci cicluri de extracție, timp de 600 s, la o presiune ridicata de 8,7 bar si cinci cicluri de presiune joasa de 1,25 bar, cu cate cinci cicluri cvasidinamice, fiecare timp de 520 s, cu circularea in contracurent a solventului pe parcursul ciclurilor de înalta presiune.An invention relates to an integrated system and a process for obtaining extracts with the role of foliar biofertilizer / bioinsecticide in organic farming (RO131209). The process consisted of the extraction of the active substances from the plant material at a temperature of 37 ° C, with five cycles of extraction, for 600 s, at a high pressure of 8.7 bar and five cycles of low pressure of 1.25 bar, with each five quasi-dynamic cycles, each for 520 s, with the countercurrent circulating the solvent during high pressure cycles.

Invenția prezintă dezavantaje legate de tipurile de biofertilizanti / bioinsecticide foliare care se pot obține prin aplicarea invenției.The invention has disadvantages related to the types of foliar biofertilizers / bioinsecticides that can be obtained by applying the invention.

O compoziție de biofertilizant foliar utilizat in culturile posibile sa fie afectate de fitotoxicitate si efecte nocive ale mediului are drept componente principale microorganisme si metabolitii lor, extracte marine, oligoelemente si fitohormoni (CN 104341218). Materiile prime si proporțiile utilizate la realizarea compozițiilor respective sunt: 15-35% extract lichid de Bacillus, 10-30% extracte din alge; 5-25% aminoacizi; 0,05-0,5% fitohormon de tip a 2018 00167A composition of foliar biofertilizer used in cultures that can be affected by phytotoxicity and harmful effects of the environment has as main components microorganisms and their metabolites, marine extracts, trace elements and phytohormones (CN 104341218). The raw materials and proportions used to make the respective compositions are: 15-35% liquid Bacillus extract, 10-30% algae extracts; 5-25% amino acids; 0.05-0.5% Phytohormone Type A 2018 00167

08/03/201803/08/2018

brassinolid, 0,2-1,5% sulfat de zinc, 0,2-1,5% sulfat feros, 0,5-3,5% sulfat de magneziu, 0,52,5% acid boric, 0,01-0,3% molibdat de amoniu si apa suplimentată la 100%.brassinolid, 0.2-1.5% zinc sulphate, 0.2-1.5% ferrous sulphate, 0.5-3.5% magnesium sulphate, 0.52.5% boric acid, 0.01- 0.3% ammonium molybdate and water supplemented to 100%.

Invenția prezintă dezavantaje legate de utilizarea unor componenti costisitori si relativ dificil de obtinut.The invention presents disadvantages related to the use of expensive and relatively difficult to obtain components.

Problema tehnica pe care urmărește sa o rezolve invenția, este creșterea producției si a calitatii fructelor si/sau a semințelor plantelor si respectiv protecția mediului, prin realizarea unor biofertilizanti foliari conținând microcapsule cu uleiuri esențiale, împreuna cu nutrienti cu azot organic si respectiv cu sulf organic, care pe langa nutriția plantelor asigura si protecția acestora împotriva unor microoganisme patogene, a unor fungi sau insecte, in condițiile eliberării controlate a biopesticidelor respective.The technical problem that the invention seeks to solve is to increase the production and quality of fruits and / or seeds of plants and respectively the protection of the environment, by making foliar biofertilizers containing microcapsules with essential oils, together with nutrients with organic nitrogen and organic sulfur, respectively. , which besides the nutrition of the plants also ensures their protection against pathogenic micro-organisms, fungi or insects, under the conditions of the controlled release of the respective biopesticides.

Procedeul pentru obținerea biofertilizantilor foliari împreuna cu microcapsulele cu uleiuri esențiale componente conform invenției înlătură dezavantajele menționate anterior prin aceea ca, proteinele hidrolizate avand masa moleculara medie de 50.000-60.000 Da, provenite din deșeuri de la prelucrarea pieilor de ovine, bovine, porcine, deșeuri din industria piscicola, deșeuri de la abatoare sau din industria alimentara (oase, cartilaje), luate in proporție de 1,172,28% in greutate fata de suspensia finala, se introduc peste apa luata in proporție de 20,41 65,54% in greutate fata de suspensia finala, încălzită la 60°C, soluția coloidala formata se răcește la 25°C, se adauga prin picurare sub agitare intensa ulei esențial, ales dintre uleiul de rozmarin, cimbru, coriandru, marar, cuisoare, scorțișoara, eucalipt, conifere, citrice, oregano, mirt, menta, usturoi, arbore de ceai, muscata, lavanda, anason, busuioc, singure sau in amestec, luat in proporție de 4,23-7,40% in greutate fata de suspensia finala, se pune in funcțiune baia cu ultrasunete iar emulsia formata se menține sub agitare intensa in câmp de ultrasunete la 20°C timp de 15 minute, separat se prepara o soluție formata dintr-un polimer anionic, de tip tripolifosfat de sodiu sau carboximetil celuloza sodica, luat in proporție de 1,09-2,28% in greutate fata de suspensia finala, din apa luata in proporție de 14,81-68,03% in greutate fata de suspensia finala si din dodecilbenzensulfonat de sodiu 50%, luat in proporție de 0,19-0,34% in greutate fata de suspensia finala, soluția rezultata se răcește la 1-2°C si se introduce prin picurare peste emulsia de ulei esențial anterior preparata, suspensia formata se răcește sub agitare intensa in câmp de microunde, mentinandu-se la 5°C timp de 15 minute, are loc procesul de coacervare complexa, microparticolele de ulei esențial fiind acoperite cu 2 straturi formate din polimerul cationic (proteina hidrolizata) si polimerul anionic, suspensia răcită la 5°C este tratata prin picurare cu o soluție formata din glutaraldehidă 50%, luata in proporție de 1,55-3,42% in greutate fata de suspensia finala si metanol, luat in proporție de a 2018 00167The process for obtaining foliar biofertilizers together with the microcapsules with essential oil components according to the invention removes the aforementioned disadvantages by the fact that, the hydrolysed proteins having an average molecular mass of 50,000-60,000 Da, derived from waste from the processing of sheep, from sheep, from poultry, sheep fish industry, waste from slaughterhouses or the food industry (bones, cartilage), taken in proportion of 1,172.28% by weight compared to the final suspension, is introduced over water taken in proportion of 20.41 65.54% by weight of the final suspension, heated to 60 ° C, the colloidal solution formed is cooled to 25 ° C, added by dripping under intense stirring the essential oil, chosen from the oil of rosemary, thyme, coriander, dill, cloves, cinnamon, eucalyptus, conifers, citrus, oregano, myrtle, mint, garlic, tea tree, nutmeg, lavender, anise, basil, alone or in mixture, taken in the proportion of 4.23-7.40 % by weight compared to the final suspension, the ultrasonic bath is put into operation and the emulsion formed is kept under intense stirring in the ultrasonic field at 20 ° C for 15 minutes, separately a solution consisting of an anionic polymer, of type sodium tripolyphosphate or carboxymethyl cellulose sodium, taken from 1.09-2.28% by weight against the final suspension, from water taken from 14.81-68.03% by weight against the final suspension and from dodecylbenzenesulfonate of 50% sodium, taken in the proportion of 0.19-0.34% by weight compared to the final suspension, the resulting solution is cooled to 1-2 ° C and introduced by dripping over the previously prepared essential oil emulsion, the suspension formed is cools under intense stirring in the microwave field, staying at 5 ° C for 15 minutes, the complex co-preservation process takes place, the essential oil microparticles being covered with 2 layers consisting of the cationic polymer (hydrolyzed protein) and the anionic polymer, the suspension cooled to 5 ° C is treated dropwise with a solution consisting of 50% glutaraldehyde, taken in the proportion of 1.55-3.42% by weight compared to the final suspension and methanol, taken in the proportion of 2018 00167

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3,11-6,83% in greutate fata de suspensia finala, fiind menținută sub agitare intensa in câmp de microunde la 5°C, inca 5 minute, se înlătură baia cu microunde, iar suspensia rezultata se menține sub agitare intensa la temperatura ambianta inca 180 minute, temperatura amestecului creste pana la 20-25°C din exotermicitatea procesului, se perfectează procesul de reticulare prin marirea temperaturii pana la 30-35°C, suspensia finala se filtrează sau centrifugheaza, separandu-se turta umeda cu continui de 22,44-24,11% microcapsule cu ulei esențial, de filtratul apos, care se poate reutiliza la șarjele ulterioare, eficienta microincapsularii fiind de 93,44-97,37%, separat se prepara un amestec format din proteine hidrolizate cu continui inițial de substanța proteica uscata de 28,83-41,33% si masa moleculara medie de 320-750 Da, provenite din deșeuri de la prelucrarea pieilor de ovine, bovine, porcine, deșeuri din industria piscicola, deșeuri de la abatoare sau din industria alimentara (oase, cartilaje), luate in proporție de 14,31-19,41% in greutate fata de suspensia de biofertilizant, din agent de îmbunătățire a aderentei pe frunze, selectat dintre proteinele hidrolizate cu masa moleculara medie de 50.000-60.000 Da, sau hidroxipropil metil celuloza, luat in proporție de 0,24-0,68% in greutate fata de suspensia de biofertilizant, din agent de ingrosare, de tipul gumei xanthan, a gumei guar, sau a gumei arabice, luat in proporție de 0,20-0,30% in greutate fata de suspensia de biofertilizant, se încălzește amestecul, mentinandu-se temperatura la 60°C timp de 15 minute, apoi se răcește la 25°C, se introduce sub agitare cheratina hidrolizata cu continui inițial de substanța proteica uscata de 8,1829,13%, provenita din deșeuri de lana, de pene, de par, de coame, sau de copite, luata in proporție de 0,73-2,70% in greutate fata de suspensia de biofertilizant si turta de la filtrare cu 22,44-24,11% microcapsule cu continui de ulei esențial ales dintre uleiul de rozmarin, cimbru, coriandru, marar, cuișoare, scorțișoara, eucalipt, conifere, citrice, oregano, mirt, menta, usturoi, arbore de ceai, muscata, lavanda, anason, busuioc, singure sau in amestec, microcapsulele fiind luate in proporție de 6,50-8,25% in greutate fata de suspensia de biofertilizant, se continua agitarea timp de 30 minute sau se trece amestecul printr-o moara coloidala, apoi se introduc surfactanti neionici luati in proporție de 4,04-5,96% in greutate fata de suspensia de biofertilizant si o soluție apoasa conținând un amestec de săruri de Cu, Zn, Fe, Mo, Mn, Mg ale acidului etilendiaminotetraacetic, sărurile fiind luate in proporție de 0,66-0,92% in greutate fata de suspensia de biofertilizant, se continua agitarea 15 minute, obtinandu-se biofertilizantul foliar sub forma de suspensie apoasa, compozițiile de biofertilizanti foliari conform invenției, înlătură dezavantajele menționate anterior prin aceea ca, sunt constituite din 14,31-19,41% in greutate proteine hidrolizate cu masa moleculara a 2018 001673.11-6.83% by weight compared to the final suspension, being kept under intense stirring in the microwave field at 5 ° C, for another 5 minutes, the microwave bath is removed, and the resulting suspension is kept under intense stirring at ambient temperature. another 180 minutes, the temperature of the mixture rises to 20-25 ° C from the exothermicity of the process, the cross-linking process is improved by increasing the temperature up to 30-35 ° C, the final suspension is filtered or centrifuged, separating the wet cake with continuous 22 , 44-24.11% microcapsules with essential oil, aqueous filtrate, which can be reused at subsequent batches, the efficiency of the micro-encapsulation being 93.44-97.37%, separately a mixture consisting of hydrolysed proteins with initial contents is prepared. dry protein substance of 28.83-41,33% and average molecular mass of 320-750 Yes, from waste from the processing of sheep, cattle, pigs, waste from the fishery, waste from slaughterhouses or from industry of food (bones, cartilage), taken in proportion of 14.31-19.41% by weight compared to the suspension of biofertilizer, from a leaf adhesion enhancing agent, selected from hydrolysed proteins with an average molecular weight of 50,000-60,000 Da , or hydroxypropyl methyl cellulose, taken in a proportion of 0.24-0.68% by weight compared to the suspension of biofertilizer, from a thickening agent, such as xanthan gum, guar gum, or arabic gum, taken at 0 , 20-0.30% by weight compared to the suspension of biofertilizer, the mixture is heated, maintaining the temperature at 60 ° C for 15 minutes, then cooling to 25 ° C, and the hydrolyzed keratin is hydrolyzed with an initial content of stirring. the dry protein substance of 8,1829.13%, coming from waste of wool, of feathers, of hair, of mane, or of hooves, taken in proportion of 0,73-2,70% by weight compared to the suspension of biofertilizer and filter cake with 22.44-24.11% microcapsules with essential oil content of es of rosemary oil, thyme, coriander, dill, cloves, cinnamon, eucalyptus, conifers, citrus, oregano, myrtle, mint, garlic, tea tree, nutmeg, lavender, anise, basil, alone or in mix, microcapsules being taken 6.50-8.25% by weight compared to the biofertilizer suspension, stirring is continued for 30 minutes or the mixture is passed through a colloidal mill, then non-ionic surfactants taken in proportion of 4.04-5 are introduced. , 96% by weight with respect to the biofertilizer suspension and an aqueous solution containing a mixture of Cu, Zn, Fe, Mo, Mn, Mg salts of ethylenediaminetetraacetic acid, the salts being taken from 0.66-0.92% in weight with respect to the biofertilizer suspension, stirring is continued for 15 minutes, obtaining the foliar biofertilizer in the form of aqueous suspension, the foliar biofertilizer compositions according to the invention, remove the aforementioned disadvantages by the fact that, they consist of 14.31-19 , 41% by weight hydrolysed proteins with molecular weight of 2018 00167

08/03/2018 medie de 320-750 Da, din 0,24-0,68% in greutate agent de îmbunătățire a aderentei pe frunze, din 0,20-0,30% in greutate agent de ingrosare, din 0,73-2,70% in greutate cheratina hidrolizata, din 6,50-8,25% in greutate microcapsule cu continui de ulei esențial, avand viteza de eliberare a uleiului din microcapsule la 120 ore de 40,30-48,20%, din 4,04-5,96% in greutate surfactanti neionici, din 0,66-0,92% in greutate un amestec de săruri de Cu, Zn, Fe, Mo, Mn, Mg ale acidului etilendiaminotetraacetic, si din 63,62-70,28% in greutate apa, stabilitatea suspensiei de biofertilizant fiind > 6 luni.08/03/2018 average of 320-750 Yes, from 0.24-0.68% by weight leaf enhancement agent, from 0.20-0.30% by weight thickening agent, from 0.73 -2.70% by weight hydrolyzed keratin, from 6.50-8.25% by weight microcapsules with essential oil contents, having the speed of release of oil from microcapsules at 120 hours of 40.30-48.20%, from 4.04-5.96% by weight nonionic surfactants, 0.66-0.92% by weight a mixture of Cu, Zn, Fe, Mo, Mn, Mg salts of ethylenediaminetetraacetic acid, and 63.62- 70.28% by weight of water, the stability of the biofertilizer suspension being> 6 months.

Invenția prezintă următoarele avantaje:The invention has the following advantages:

• Se imbunatateste eficienta microincapsularii uleiurilor esențiale si se realizează micșorarea dimensiunilor microparticolelor, prin conducerea procesului in câmp de ultrasunete • Utilizarea biofertilizantilor foliari contribuie la creșterea producției si a calitatii fructelor si/sau a semințelor plantelor, datorita microcapsulelor cu uleiuri esențiale si a nutrientilor cu azot organic si respectiv cu sulf organic, care pe langa nutriția plantelor asigura si proiecția acestora împotriva unor microoganisme patogene, a unor fungi sau insecte • Prezenta agentilor de îmbunătățire a aderentei pe frunze din componenta biofertilizantilor, asigura o eficienta sporita a asimilării acestora de către plante • Microcapsulele cu uleiuri esențiale din componenta biofertilizantilor conferă protecție sporita la depozitare, împotriva degradării unor componente (ex. proteine hidrolizate si cheratine hidrolizate) si inhiba mirosurile neplăcute datorita acestora • Microcapsulele avand eliberare controlata a uleiurilor esențiale asigura marirea duratei de proiecție conferita de acestea • Se asigura proiecția mediului prin utilizarea componentelor in majoritate de proveniența naturala• The efficiency of micro-encapsulation of essential oils is improved and the size of the microparticles is reduced, by conducting the process in ultrasound field. organic and respectively with organic sulfur, which in addition to plant nutrition also ensures their projection against pathogenic micro-organisms, fungi or insects • The presence of agents to improve the adherence on the leaves of the component of biofertilizers, ensures an increased efficiency of their assimilation by plants • Microcapsules with essential oils from the biofertilizers component provide increased protection during storage, against degradation of components (eg hydrolyzed proteins and hydrolyzed keratin) and inhibit unpleasant odors due to them • Microca psulules having controlled release of the essential oils ensures the increase of the projection duration conferred by them • The projection of the environment is ensured by using the components mainly from the natural origin.

Se dau in continuare 5 exemple de realizare a invenției:5 examples of the invention are given below:

Exemplul 1Example 1

Intr-un balon cu 4 gaturi prevăzut cu agitare actionata electric, pâlnie de picurare si termometru, balonul fiind amplasat intr-o baie cu ultrasunete cu posibilitate de răcire, se introduc sub agitare 36 g proteine hidrolizate din deșeuri de la prelucrarea pieilor de ovine avand masa moleculara medie de 50.000 Da, peste 1380 g apa încălzită la 60°C. Soluția coloidala formata se răcește la 25°C si se adauga prin picurare sub agitare intensa 90 g ulei de rozmarin. Se pune in funcțiune baia cu ultrasunete si emulsia formata se menține sub agitare intensa in câmp de ultrasunete la 20°C timp de 15 minute. Intr-o instalație similara, dar fara baie cu ultrasunete, se prepara sub agitare o soluție formata din 36 g tripolifosfat de sodiu a 2018 00167In a 4-necked flask equipped with electrically operated stirring, drip funnel and thermometer, the flask being placed in an ultrasonic bath with the possibility of cooling, 36 g hydrolysed proteins from waste from the processing of sheepskin having average molecular mass of 50,000 Da, over 1380 g of water heated to 60 ° C. The colloidal solution formed is cooled to 25 ° C and 90 g of rosemary oil is added dropwise under intense stirring. The ultrasonic bath is put into operation and the emulsion formed is kept under intense stirring in the ultrasonic field at 20 ° C for 15 minutes. In a similar installation, but without ultrasonic bath, a solution of 36 g sodium tripolyphosphate of 2018 00167 is prepared under stirring.

08/03/2018 (TPP), 420 g apa si 6 g dodecilbenzensulfonat de sodiu 50%. Soluția se răcește la 1-2°C si se introduce prin picurare peste emulsia de ulei de rozmarin anterior preparata. Suspensia formata se răcește sub agitare intensa in câmp de microunde, mentinandu-se la 5°Ctimp de 15 minute. Are loc procesul de coacervare complexa, microparticolele de ulei de rozmarin fiind acoperite cu 2 straturi formate dintr-un polimer cationic (proteina hidrolizata) si un polimer anionic (TPP). Suspensia răcită la 5°C este tratata prin picurare cu o soluție formata din 54 g glutaraldehida 50% si 108 g metanol, fiind menținută sub agitare intensa, in câmp de microunde la 5°C, inca 5 minute. Se înlătură baia cu microunde, iar suspensia rezultata se menține sub agitare intensa la temperatura ambianta inca 180 minute. Temperatura amestecului creste pana la 20-25°C din exotermicitatea procesului de reticulare a membranelor microcapsulelor. Spre sfârșitul perioadei de agitare, in scopul perfectării procesului de reticulare, se mărește temperatura suspensiei pana la 30°C. Suspensia finala in cantitate de 2130 g, se filtrează sau centrifugheaza, separandu-se 600 g turta umeda de microcapsule cu ulei de rozmarin, de filtratul apos, care se poate reutiliza la șarjele ulterioare. Turta are un continui de 23,17% microcapsule. Eficienta microincapsularii este de 96,28%. Vitezei de eliberare a uleiului la 120 ore este de 46,5%.08/03/2018 (TPP), 420 g of water and 6 g of 50% sodium dodecylbenzenesulfonate. The solution is cooled to 1-2 ° C and is introduced dropwise over the previously prepared rosemary oil emulsion. The suspension formed is cooled under intense stirring in the microwave field, maintaining at 5 ° C for 15 minutes. The complex co-preservation process takes place, the microparticles of rosemary oil being coated with 2 layers consisting of a cationic polymer (hydrolyzed protein) and an anionic polymer (TPP). The suspension cooled to 5 ° C is treated dropwise with a solution consisting of 54 g 50% glutaraldehyde and 108 g methanol, being kept under intense stirring, in the microwave field at 5 ° C, for another 5 minutes. The microwave bath is removed and the resulting suspension is kept under intense stirring at room temperature for another 180 minutes. The temperature of the mixture increases to 20-25 ° C from the exothermicity of the process of cross-linking the microcapsule membranes. Towards the end of the stirring period, in order to complete the cross-linking process, the suspension temperature is increased to 30 ° C. The final suspension in the amount of 2130 g, is filtered or centrifuged, separating 600 g moist microcapsule cake with rosemary oil, aqueous filtrate, which can be reused at subsequent batches. The cake has a continuum of 23.17% microcapsules. The efficiency of micro-encapsulation is 96.28%. The oil release rate at 120 hours is 46.5%.

Intr-un balon cu 4 gaturi prevăzut cu agitare actionata electric de tip turbina cu turatie mare, amplasat intr-o baie de apa cu posibilități de încălzire, răcire, se introduc 1000 g proteine hidrolizate din deșeuri de la prelucrarea pieilor de ovine avand continui de substanța proteica uscata de 28,83% si masa moleculara medie de 320 Da. Se pornește agitarea si încălzirea, apoi se introduc 9 g proteine hidrolizate din deșeuri de la prelucrarea pieilor de ovine avand masa moleculara medie de 50.000 Da si 6 g guma xanthan. Se menține temperatura amestecului la 60°C timp de 15 minute, apoi se răcește la 25°C. Se introduc sub agitare 200 g cheratina hidrolizata din pene, avand substanța proteica uscata de 10,14% si 600 g turta de la filtrare cu 23,17% microcapsule cu continui de ulei de rozmarin. Se continua agitarea timp de 30 minute, apoi se introduc 120 g surfactanti neionici si 80 g soluție apoasa conținând 20,25% un amestec de săruri de Cu, Zn, Fe, Mo, Mn, Mg ale acidului etilendiaminotetraacetic. Se continua agitarea 15 minute, obtinandu-se 2015 g biofertilizant foliar sub forma de suspensie apoasa. Stabilitatea suspensiei este > 6 luni.In a 4-necked flask equipped with high-speed turbine-type electrically operated shaking, placed in a water bath with heating, cooling possibilities, 1000 g of hydrolysed proteins from waste from the processing of sheep's skins are kept having continuous the dry protein substance of 28.83% and the average molecular mass of 320 Da. Stirring and heating is started, then 9 g of hydrolyzed protein from waste from the processing of sheep skins with an average molecular weight of 50,000 Da and 6 g of xanthan gum is introduced. Keep the temperature of the mixture at 60 ° C for 15 minutes, then cool to 25 ° C. 200 g hydrolyzed keratin from the feathers were stirred, having the dry protein substance of 10.14% and 600 g of the filter cake with 23.17% microcapsules containing rosemary oil. Stirring is continued for 30 minutes, then 120 g of nonionic surfactants and 80 g of aqueous solution containing 20.25% of a mixture of Cu, Zn, Fe, Mo, Mn, Mg of ethylenediaminetetraacetic acid are introduced. Stirring is continued for 15 minutes, yielding 2015 g of foliar biofertilizer in the form of aqueous suspension. The stability of the suspension is> 6 months.

Exemplul 2Example 2

Intr-un balon cu 4 gaturi prevăzut cu agitare actionata electric, pâlnie de picurare si termometru, balonul fiind amplasat intr-o baie cu ultrasunete cu posibilitate de răcire, se introduc sub agitare 24 g proteine hidrolizate din deșeuri de sorici din industria alimentara a2018 00167In a 4-necked flask equipped with electrically operated stirring, drip funnel and thermometer, the flask being placed in an ultrasonic bath with cooling possibility, 24 g hydrolyzed proteins from mice waste from the food industry a2018 00167 are introduced under stirring.

08/03/2018 avand masa moleculara medie de 60.000 Da, peste 420 g apa încălzită la 60°C. Soluția coloidala formata se răcește la 25°C si se adauga prin picurare sub agitare intensa 90 g ulei de cimbru. Se pune in funcțiune baia cu ultrasunete si emulsia formata se menține sub agitare intensa in câmp de ultrasunete la 20°C timp de 15 minute. Intr-o instalație similara, dar fara baie cu ultrasunete, se prepara sub agitare o soluție formata din 24 g carboximetil celuloza sodica (CMC-Na), 1400 g apa si 4 g dodecilbenzensulfonat de sodiu 50%. Soluția se răcește la 1-2°C si se introduce prin picurare peste emulsia de ulei de rozmarin anterior preparata. Suspensia formata se răcește sub agitare intensa in câmp de microunde, mentinandu-se la 5°C timp de 15 minute. Are loc procesul de coacervare complexa, microparticolele de ulei de cimbru fiind acoperite cu 2 straturi formate dintr-un polimer cationic (proteina hidrolizata) si un polimer anionic (CMC-Na). Suspensia răcită la 5°C este tratata prin picurare cu o soluție formata din 32 g glutaraldehida 50% si 64 g metanol, fiind menținută sub agitare intensa, in câmp de microunde la 5°C, inca 5 minute. Se înlătură baia cu microunde, iar suspensia rezultata se menține sub agitare intensa la temperatura ambianta inca 180 minute. Temperatura amestecului creste pana la 20-25°C din exotermicitatea procesului de reticulare a membranelor microcapsulelor. Spre sfârșitul perioadei de agitare, in scopul perfectării procesului de reticulare, se mărește temperatura suspensiei pana la 30°C. Suspensia finala in cantitate de 2058 g, se filtrează sau centrifugheaza, separandu-se 508 g turta umeda de microcapsule cu ulei de rozmarin, de filtratul apos, care se poate reutiliza la șarjele ulterioare. Turta are un continui de 22,44% microcapsule. Eficienta microincapsularii este de 93,44%. Vitezei de eliberare a uleiului la 120 ore este de 48,20%.08/03/2018 having an average molecular mass of 60,000 Da, over 420 g of water heated to 60 ° C. The colloidal solution formed is cooled to 25 ° C and 90 g of thyme oil is added dropwise under intense stirring. The ultrasonic bath is put into operation and the emulsion formed is kept under intense stirring in the ultrasonic field at 20 ° C for 15 minutes. In a similar installation, but without an ultrasonic bath, a solution consisting of 24 g carboxymethyl cellulose sodium (CMC-Na), 1400 g water and 4 g sodium dodecylbenzene sulphonate 50% is prepared under stirring. The solution is cooled to 1-2 ° C and is introduced dropwise over the previously prepared rosemary oil emulsion. The suspension formed is cooled under intense stirring in the microwave field, maintaining at 5 ° C for 15 minutes. The complex co-preservation process takes place, the microparticles of thyme oil being covered with 2 layers consisting of a cationic polymer (hydrolyzed protein) and an anionic polymer (CMC-Na). The suspension cooled to 5 ° C is treated dropwise with a solution of 32 g of 50% glutaraldehyde and 64 g of methanol, being kept under intense stirring, in the microwave field at 5 ° C, for another 5 minutes. The microwave bath is removed and the resulting suspension is kept under intense stirring at room temperature for another 180 minutes. The temperature of the mixture increases to 20-25 ° C from the exothermicity of the process of cross-linking the microcapsule membranes. Towards the end of the stirring period, in order to complete the cross-linking process, the suspension temperature is increased to 30 ° C. The final suspension in the amount of 2058 g, is filtered or centrifuged, separating 508 g moist microcapsule cake with rosemary oil, aqueous filtrate, which can be reused at subsequent batches. The cake has a continuum of 22.44% microcapsules. The efficiency of micro-encapsulation is 93.44%. The oil release rate at 120 hours is 48.20%.

Intr-un balon cu 4 gaturi prevăzut cu agitare actionata electric de tip turbina cu turatie mare, amplasat intr-o baie de apa cu posibilități de încălzire, răcire, se introduc 900 g proteine hidrolizate din deșeuri de la prelucrarea pieilor de bovine avand continui de substanța proteica uscata de 35,14% si masa moleculara medie de 750 Da. Se pornește agitarea si încălzirea, apoi se introduc 9 g proteine hidrolizate din deșeuri deșeuri de sorici avand masa moleculara medie de 60.000 Da si 6 g guma guar. Se menține temperatura amestecului la 60°C timp de 15 minute, apoi se răcește la 25°C. Se introduc sub agitare 150 g cheratina hidrolizata din lana, avand substanța proteica uscata de 29,13% si 508 g turta de la filtrare cu 22,44% microcapsule cu continui de ulei de cimbru. Se continua agitarea timp de 30 minute, apoi se introduc 100 g surfactanti neionici si 80 g soluție apoasa conținând 20,25% un amestec de săruri de Cu, Zn, Fe, Mo, Mn, Mg ale acidului etilendiaminotetraacetic. Se continua agitarea a 2018 00167In a 4-necked flask equipped with high-speed turbine-type electrically operated shaking, placed in a water bath with heating, cooling possibilities, 900 g of hydrolyzed protein from waste from the processing of bovine skins containing continents is introduced. the dry protein substance of 35.14% and the average molecular mass of 750 Da. Stirring and heating are started, then 9 g of hydrolyzed protein from waste wastes of mice having an average molecular weight of 60,000 Da and 6 g of guar gum. Keep the temperature of the mixture at 60 ° C for 15 minutes, then cool to 25 ° C. 150 g hydrolyzed keratin from wool is introduced with stirring, having the dry protein substance of 29.13% and 508 g of the cake filtered with 22.44% microcapsules containing cinnamon oil. Stirring is continued for 30 minutes, then 100 g of nonionic surfactants and 80 g of aqueous solution containing 20.25% of a mixture of Cu, Zn, Fe, Mo, Mn, Mg of ethylenediaminetetraacetic acid are introduced. The stirring of 2018 00167 continues

08/03/2018 minute, obtinandu-se 1755 g biofertilizant foliar sub forma de suspensie apoasa. Stabilitatea suspensiei este > 6 luni.08/03/2018 minutes, yielding 1755 g of foliar biofertilizer in the form of aqueous suspension. The stability of the suspension is> 6 months.

Exemplul 3Example 3

Intr-un balon cu 4 gaturi prevăzut cu agitare actionata electric, pâlnie de picurare si termometru, balonul fiind amplasat intr-o baie cu ultrasunete cu posibilitate de răcire, se introduc sub agitare 36 g proteine hidrolizate din deșeuri de la prelucrarea pieilor de bovine avand masa moleculara medie de 50.000 Da, peste 1200 g apa încălzită la 60°C. Soluția coloidala formata se răcește la 25 °C si se adauga prin picurare sub agitare intensa 120 g amestec de ulei de cuisoare si scorțișoara in raport gravimetric de 1:1. Se pune in funcțiune baia cu ultrasunete si emulsia formata se menține sub agitare intensa in câmp de ultrasunete la 20°C timp de 15 minute. Intr-o instalație similara, dar fara baie cu ultrasunete, se prepara sub agitare o soluție formata din 20 g tripolifosfat de sodiu (TPP), 300 g apa si 5 g dodecilbenzensulfonat de sodiu 50%. Soluția se răcește la 1-2°C si se introduce prin picurare peste emulsia de ulei de cuisoare si scorțișoara anterior preparata. Suspensia formata se răcește sub agitare intensa in câmp de microunde, mentinandu-se la 5°C timp de 15 minute. Are loc procesul de coacervare complexa, microparticolele de ulei de cuisoare si scorțișoara fiind acoperite cu 2 straturi formate dintr-un polimer cationic (proteina hidrolizata) si un polimer anionic (TPP). Suspensia răcită la 5°C este tratata prin picurare cu o soluție formata din 50 g glutaraldehida 50% si 100 g metanol, fiind menținută sub agitare intensa, in câmp de microunde la 5°C, inca 5 minute. Se inlatura baia cu microunde, iar suspensia rezultata se menține sub agitare intensa la temperatura ambianta inca 180 minute. Temperatura amestecului creste pana la 20-25°C din exotermicitatea procesului de reticulare a membranelor microcapsulelor. Spre sfârșitul perioadei de agitare, in scopul perfectării procesului de reticulare, se mărește temperatura suspensiei pana la 30°C. Suspensia finala in cantitate de 1831 g, se filtrează sau centrifugheaza, separandu-se 672 g turta umeda de microcapsule cu ulei de cuisoare si scorțișoara, de filtratul apos, care se poate reutiliza la șarjele ulterioare. Turta are un continui de 24,11% microcapsule. Eficienta microincapsularii este de 94,42%. Vitezei de eliberare a uleiului la 120 ore este de 40,30%.In a 4-necked flask fitted with electrically operated stirring, drip funnel and thermometer, the flask being placed in an ultrasonic bath with the possibility of cooling, 36 g hydrolysed proteins from waste from the processing of bovine hides having been introduced under stirring. average molecular mass of 50,000 Da, over 1200 g of water heated to 60 ° C. The colloidal solution formed is cooled to 25 ° C and 120 g of oil of cinnamon and cinnamon are added dropwise under intense stirring in a gravimetric ratio of 1: 1. The ultrasonic bath is put into operation and the emulsion formed is kept under intense stirring in the ultrasonic field at 20 ° C for 15 minutes. In a similar installation, but without an ultrasonic bath, a solution consisting of 20 g sodium tripolyphosphate (TPP), 300 g water and 5 g sodium dodecylbenzenesulfonate 50% is prepared under stirring. The solution is cooled to 1-2 ° C and is introduced by drip over the previously prepared oil of cinnamon and cinnamon oil. The suspension formed is cooled under intense stirring in the microwave field, maintaining at 5 ° C for 15 minutes. The complex co-preservation process takes place, the microparticles of cinnamon and cinnamon oil being covered with 2 layers consisting of a cationic polymer (hydrolyzed protein) and an anionic polymer (TPP). The suspension cooled to 5 ° C is treated dropwise with a solution consisting of 50 g glutaraldehyde 50% and 100 g methanol, being kept under intense stirring, in the microwave field at 5 ° C, for another 5 minutes. The microwave bath is removed and the resulting suspension is kept under intense stirring at room temperature for another 180 minutes. The temperature of the mixture increases to 20-25 ° C from the exothermicity of the process of cross-linking the microcapsule membranes. Towards the end of the stirring period, in order to complete the cross-linking process, the suspension temperature is increased to 30 ° C. The final suspension in the amount of 1831 g, is filtered or centrifuged, separating 672 g wet microcapsule cake with cinnamon and cinnamon oil, aqueous filtrate, which can be reused at subsequent batches. The cake has a continuum of 24.11% microcapsules. The efficiency of micro-encapsulation is 94.42%. The oil release rate at 120 hours is 40.30%.

Intr-un balon cu 4 gaturi prevăzut cu agitare actionata electric de tip turbina cu turatie mare, amplasat intr-o baie de apa cu posibilități de încălzire, răcire, se introduc 900 g proteine hidrolizate din deșeuri din industria piscicola avand continui de substanța proteica uscata de 41,33% si masa moleculara medie de 400 Da. Se pornește agitarea si încălzirea, apoi se introduc 7 g proteine hidrolizate din deșeuri de la prelucrarea pieilor de bovine avand masa a 2018 00167In a 4-necked flask fitted with high-speed turbine-type electrically driven agitation, placed in a water bath with heating, cooling possibilities, 900 g hydrolysed proteins from waste from the fishery industry are introduced having the dry protein substance of 41.33% and the average molecular mass of 400 Da. Start stirring and heating, then introduce 7 g hydrolysed proteins from waste from the processing of bovine skins having the mass of 2018 00167

08/03/2018 moleculara medie de 50.000 Da si 4 g guma arabica. Se menține temperatura amestecului la 60°C timp de 15 minute, apoi se răcește la 25°C. Se introduc sub agitare 200 g cheratina hidrolizata din par, avand substanța proteica uscata de 26,50% si 672 g turta de la filtrare cu 24,11% microcapsule cu continui de ulei de cuisoare si scorțișoara. Se continua agitarea timp de 30 minute, apoi se introduc 100 g surfactanti neionici si 80 g soluție apoasa conținând 20,25% un amestec de săruri de Cu, Zn, Fe, Mo, Mn, Mg ale acidului etilendiaminotetraacetic. Se continua agitarea 15 minute, obtinandu-se 1963 g biofertilizant foliar sub forma de suspensie apoasa. Stabilitatea suspensiei este > 6 luni.03/03/2018 Molecular average of 50,000 Yes and 4 g of gum arabic. Keep the temperature of the mixture at 60 ° C for 15 minutes, then cool to 25 ° C. 200 g hydrolyzed keratin from the hair is stirred, having the dry protein substance of 26.50% and 672 g of the filter cake with 24.11% microcapsules with continuous oil of cinnamon and cinnamon. Stirring is continued for 30 minutes, then 100 g of nonionic surfactants and 80 g of aqueous solution containing 20.25% of a mixture of Cu, Zn, Fe, Mo, Mn, Mg of ethylenediaminetetraacetic acid are introduced. Stirring continued for 15 minutes, yielding 1963 g of foliar biofertilizer in the form of aqueous suspension. The stability of the suspension is> 6 months.

Exemplul 4Example 4

Intr-un balon cu 4 gaturi prevăzut cu agitare actionata electric, pâlnie de picurare si termometru, balonul fiind amplasat intr-o baie cu ultrasunete cu posibilitate de răcire, se introduc sub agitare 40 g proteine hidrolizate din deșeuri de la abatoare sau din industria alimentara (oase, cartilaje) avand masa moleculara medie de 60.000 Da, peste 1100 g apa încălzită la 60°C. Soluția coloidala formata se răcește la 25°C si se adauga prin picurare sub agitare intensa 130 g ulei de coriandru. Se pune in funcțiune baia cu ultrasunete si emulsia formata se menține sub agitare intensa in câmp de ultrasunete la 20°C timp de 15 minute. Intro instalație similara, dar fara baie cu ultrasunete, se prepara sub agitare o soluție formata din 36 g trîpolifosfat de sodiu (TPP), 260 g apa si 6 g dodecilbenzensulfonat de sodiu 50%. Soluția se răcește la 1-2°C si se introduce prin picurare peste emulsia de ulei de rozmarin anterior preparata. Suspensia formata se răcește sub agitare intensa in câmp de microunde, mentinandu-se la 5°C timp de 15 minute. Are loc procesul de coacervare complexa, microparticolele de ulei de rozmarin fiind acoperite cu 2 straturi formate dintr-un polimer cationic (proteina hidrolizata) si un polimer anionic (TPP). Suspensia răcită la 5°C este tratata prin picurare cu o soluție formata din 60 g glutaraldehida 50% si 120 g metanol, fiind menținută sub agitare intensa, in câmp de microunde la 5°C, inca 5 minute. Se înlătură baia cu microunde, iar suspensia rezultata se menține sub agitare intensa la temperatura ambianta inca 180 minute. Temperatura amestecului creste pana la 20-25°C din exotermicitatea procesului de reticulare a membranelor microcapsulelor. Spre sfârșitul perioadei de agitare, in scopul perfectării procesului de reticulare, se mărește temperatura suspensiei pana la 30°C. Suspensia finala in cantitate de 1756 g, se filtrează sau centrifugheaza, separandu-se 762 g turta umeda de microcapsule cu ulei de coriandru, de filtratul apos, care se poate reutiliza la șarjele ulterioare. Turta are un continui de 23,88% microcapsule. Eficienta microincapsularii este de 97,37%. Vitezei de eliberare a uleiului la 120 ore este de 44,30%.In a 4-necked flask fitted with electrically operated stirring, drip funnel and thermometer, the balloon being placed in an ultrasonic bath with cooling possibility, 40 g hydrolysed proteins from waste from slaughterhouses or food industry are introduced under stirring. (bones, cartilage) having an average molecular mass of 60,000 Da, over 1100 g of water heated to 60 ° C. The colloidal solution formed is cooled to 25 ° C and 130 g of coriander oil is added dropwise under intense stirring. The ultrasonic bath is put into operation and the emulsion formed is kept under intense stirring in the ultrasonic field at 20 ° C for 15 minutes. In a similar installation, but without an ultrasonic bath, a solution consisting of 36 g sodium triphosphate (TPP), 260 g water and 6 g sodium dodecylbenzenesulfonate 50% is prepared under stirring. The solution is cooled to 1-2 ° C and is introduced dropwise over the previously prepared rosemary oil emulsion. The suspension formed is cooled under intense stirring in the microwave field, maintaining at 5 ° C for 15 minutes. The complex co-preservation process takes place, the microparticles of rosemary oil being coated with 2 layers consisting of a cationic polymer (hydrolyzed protein) and an anionic polymer (TPP). The suspension cooled to 5 ° C is treated dropwise with a solution consisting of 60 g of 50% glutaraldehyde and 120 g of methanol, being kept under intense stirring, in the microwave field at 5 ° C, for another 5 minutes. The microwave bath is removed and the resulting suspension is kept under intense stirring at room temperature for another 180 minutes. The temperature of the mixture increases to 20-25 ° C from the exothermicity of the process of cross-linking the microcapsule membranes. Towards the end of the stirring period, in order to complete the cross-linking process, the suspension temperature is increased to 30 ° C. The final suspension in the amount of 1756 g, is filtered or centrifuged, separating 762 g of moist microcapsule cake with coriander oil, from the aqueous filtrate, which can be reused for subsequent batches. The cake has a continuum of 23.88% microcapsules. The efficiency of micro-encapsulation is 97.37%. The oil release rate at 120 hours is 44.30%.

a 2018 00167to 2018 00167

08/03/201803/08/2018

Intr-un balon cu 4 gaturi prevăzut cu agitare actionata electric de tip turbina cu turatie mare, amplasat intr-o baie de apa cu posibilități de încălzire, răcire, se introduc 1300 g proteine hidrolizate din deșeuri de la prelucrarea pieilor de ovine avand continui de substanța proteica uscata de 36,92% si masa moleculara medie de 430 Da. Se pornește agitarea si încălzirea, apoi se introduc 6 g hidroxipropil metil celuloza si 6 g guma xanthan. Se menține temperatura amestecului la 60°C timp de 15 minute, apoi se răcește la 25°C. Se introduc sub agitare 220 g cheratina hidrolizata din coame si copite, avand substanța proteica uscata de 8,18% si 762 g turta de la filtrare cu 23,88% microcapsule cu continui de ulei de coriandru. Se continua agitarea timp de 30 minute, apoi se introduc 100 g surfactanti neionici si 80 g soluție apoasa conținând 20,25% un amestec de săruri de Cu, Zn, Fe, Mo, Mn, Mg ale acidului etilendiaminotetraacetic. Se continua agitarea 15 minute, obtinandu-se 2473 g biofertilizant foliar sub forma de suspensie apoasa. Stabilitatea suspensiei este > 6 luni.In a 4-necked flask equipped with high-speed turbine-type electrically operated shaking, placed in a water bath with heating, cooling possibilities, 1300 g hydrolysed proteins from waste from the processing of sheep's skins were added. the dry protein substance of 36.92% and the average molecular mass of 430 Da. Stirring and heating are started, then 6 g of hydroxypropyl methyl cellulose and 6 g of xanthan gum are introduced. Keep the temperature of the mixture at 60 ° C for 15 minutes, then cool to 25 ° C. 220 g hydrolyzed keratin from the ridge and hooves are introduced with stirring, having the dry protein substance of 8.18% and 762 g of the filter cake with 23.88% microcapsules containing coriander oil. Stirring is continued for 30 minutes, then 100 g of nonionic surfactants and 80 g of aqueous solution containing 20.25% of a mixture of Cu, Zn, Fe, Mo, Mn, Mg of ethylenediaminetetraacetic acid are introduced. Stirring is continued for 15 minutes, yielding 2473 g of foliar biofertilizer in the form of aqueous suspension. The stability of the suspension is> 6 months.

Exemplul 5Example 5

Se respecta procedeul descris in exemplul 1, inlocuindu-se uleiul de rozmarin cu ulei de marar, eucalipt, conifere, citrice, oregano, mirt, menta, usturoi, arbore de ceai, muscata, lavanda, anason, sau busuioc, singure sau in amestec. Eficienta microincapsularii, viteza de eliberare a uleiului din microcapsule si stabilitatea suspensiei se incadreaza in limitele valorilor prezentate in exemplele de mai sus.Follow the procedure described in example 1, replacing rosemary oil with dill oil, eucalyptus, conifers, citrus, oregano, myrtle, mint, garlic, tea tree, nutmeg, lavender, anise, or basil, alone or in mixture. . The efficiency of the micro-encapsulation, the speed of release of the oil from the microcapsules and the stability of the suspension are within the limits of the values presented in the examples above.

Claims (3)

1. Procedeu pentru obținerea biofertilizantilor foliari împreuna cu microcapsulele cu uleiuri esențiale componente, caracterizat prin aceea ca proteinele hidrolizate avand masa moleculara medie de 50.000-60.000 Da, luate in proporție de 1,17-2,28% in greutate fata de suspensia finala, se introduc peste apa luata in proporție de 20,41-65,54% in greutate fata de suspensia finala, încălzită la 60°C, soluția coloidala formata se răcește la 25°C, se adauga prin picurare sub agitare intensa ulei esențial luat in proporție de 4,23-7,40% in greutate fata de suspensia finala, se pune in funcțiune baia cu ultrasunete iar emulsia formata se menține sub agitare intensa in câmp de ultrasunete la 20°C timp de 15 minute, separat se prepara o soluție formata dintr-un polimer anionic luat in proporție de 1,09-2,28% in greutate fata de suspensia finala, din apa luata in proporție de 14,81-68,03% in greutate fata de suspensia finala si din dodecilbenzensulfonat de sodiu 50%, luat in proporție de 0,19-034% in greutate fata de suspensia finala, soluția rezultata se răcește la 1-2°C si se introduce prin picurare peste emulsia de ulei esențial anterior preparata, suspensia formata se răcește sub agitare intensa in câmp de microunde, mentinandu-se la 5°Ctimp de 15 minute, are loc procesul de coacervare complexa, microparticolele de ulei esențial fiind acoperite cu 2 straturi formate din polimerul cationic (proteina hidrolizata) si polimerul anionic, suspensia răcită la 5°C este tratata prin picurare cu o soluție formata din glutaraldehida 50%, luata in proporție de 1,55-3,42% in greutate fata de suspensia finala si metanol, luat in proporție de 3,11-6,83% in greutate fata de suspensia finala, fiind menținută sub agitare intensa in câmp de microunde la 5°C, inca 5 minute, se inlatura baia cu microunde, iar suspensia rezultata se menține sub agitare intensa la temperatura ambianta inca 180 minute, temperatura amestecului creste pana la 20-25°C din exotermicitatea procesului, se perfectează procesul de reticulare prin marirea temperaturii pana la 30-35°C, suspensia finala se filtrează sau centrifugheaza, separandu-se turta umeda cu continui de 22,44-24,11% microcapsule cu ulei esențial, de filtratul apos, care se poate reutiliza la șarjele ulterioare, eficienta microincapsularii fiind de 93,44-97,37%, separat se prepara un amestec format din proteine hidrolizate cu continui inițial de substanța proteica uscata de 28,83-41,33% si masa moleculara medie de 320-750 Da, luate in proporție de 14,31-19,41% in greutate fata de suspensia de biofertilizant, din agent de îmbunătățire a aderentei pe frunze luat in proporție de 0,24-0,68% in greutate fata de suspensia de biofertilizant, din agent de ingrosare, luat in proporție de 0,20-0,30% in greutate fata de suspensia de biofertilizant, se încălzește amestecul, mentinandu-se temperatura la 60°C timp de 15 minute, apoi se răcește la 25°C, se introduce sub agitare cheratina hidrolizata cu a 2018 001671. Process for obtaining foliar biofertilizers together with the microcapsules with component essential oils, characterized in that the hydrolysed proteins having an average molecular mass of 50,000-60,000 Da, taken in a proportion of 1.17-2.28% by weight compared to the final suspension, it is introduced over water taken in proportion of 20.41-65.54% by weight compared to the final suspension, heated to 60 ° C, the colloidal solution formed is cooled to 25 ° C, it is added dropwise under intense agitation the essential oil taken in ratio of 4.23-7.40% by weight compared to the final suspension, the ultrasonic bath is put into operation and the emulsion formed is kept under intense agitation in the ultrasonic field at 20 ° C for 15 minutes, separately a solution is prepared formed of an anionic polymer taken in proportion of 1.09-2.28% by weight compared to the final suspension, of water taken in proportion of 14.81-68.03% by weight compared to the final suspension and of sodium dodecylbenzenesulfonate 50%, taken in ratio of 0.19-034% by weight compared to the final suspension, the resulting solution is cooled to 1-2 ° C and introduced dropwise over the previously prepared essential oil emulsion, the formed suspension is cooled under intense stirring in the microwave field, maintaining at 5 ° C for 15 minutes, the complex co-preservation process takes place, the essential oil microparticles being coated with 2 layers consisting of the cationic polymer (hydrolyzed protein) and the anionic polymer, the suspension cooled to 5 ° C is treated by dripping with a solution consisting of 50% glutaraldehyde, taken in the proportion of 1.55-3.42% by weight compared to the final suspension and methanol, taken in the proportion of 3.11-6.83% by weight compared to the final suspension, being maintained under intense stirring in the microwave field at 5 ° C, for another 5 minutes, remove the microwave bath, and the resulting suspension is kept under intense stirring at room temperature for another 180 minutes, the temperature of the mixture increases to 20-25 ° C from exothermic process, perfect the cross-linking process by increasing the temperature up to 30-35 ° C, the final suspension is filtered or centrifuged, separating the moist cake with continuous 22.44-24.11% microcapsules with essential oil, aqueous filtrate , which can be reused for subsequent batches, the efficiency of the micro-encapsulation being 93.44-97.37%, separately a mixture consisting of hydrolysed proteins is prepared, containing initially the dry protein substance of 28.83-41,33% and the molecular mass average 320-750 Yes, taken in proportion of 14.31-19.41% by weight compared to the suspension of biofertilizer, from a leaf adhesion enhancement agent taken in a proportion of 0.24-0.68% by weight of the biofertilizer suspension, from the thickening agent, taken in a proportion of 0.20-0.30% by weight compared to the biofertilizer suspension, the mixture is heated, maintaining the temperature at 60 ° C for 15 minutes, then cooling. at 25 ° C, it is introduced under stirring chera hydrolyzed tub with 2018 00167 08/03/2018 continui inițial de substanța proteica uscata de 8,18-29,13%, luata in proporție de 0,73-2,70% in greutate fata de suspensia de biofertilizant si turta de la filtrare cu 22,44-24,11% microcapsule cu continui de ulei esențial, microcapsulele fiind luate in proporție de 6,508,25% in greutate fata de suspensia de biofertilizant, se continua agitarea timp de 30 minute sau se trece amestecul printr-o moara coloidala, apoi se introduc surfactanti neionici luati in proporție de 4,04-5,96% in greutate fata de suspensia de biofertilizant si o soluție apoasa conținând un amestec de săruri de Cu, Zn, Fe, Mo, Mn, Mg ale acidului etilendiaminotetraacetic, sărurile fiind luate in proporție de 0,66-0,92% in greutate fata de suspensia de biofertilizant, se continua agitarea 15 minute, obtinandu-se biofertilizantul foliar sub forma de suspensie apoasa.08/03/2018 Initially continue with the dry protein substance of 8.18-29.13%, taken in proportion of 0.73-2.70% by weight compared to the suspension of biofertilizer and the filter cake with 22.44- 24.11% microcapsules with essential oil contents, the microcapsules being taken in proportion of 6,508.25% by weight compared to the suspension of biofertilizer, continue stirring for 30 minutes or pass the mixture through a colloidal mill, then introduce surfactants nonionics taken in a proportion of 4.04-5.96% by weight compared to the biofertilizer suspension and an aqueous solution containing a mixture of Cu, Zn, Fe, Mo, Mn, Mg, Mg of ethylenediaminetetraacetic acid, the salts being taken in proportion of 0.66-0.92% by weight compared to the biofertilizer suspension, stirring is continued for 15 minutes, obtaining the foliar biofertilizer in the form of aqueous suspension. 2. Compoziții de biofertilizanti foliari sub forma de suspensie apoasa caracterizate prin aceea ca sunt constituite din 14,31-19,41% in greutate proteine hidrolizate cu masa moleculara medie de 320-750 Da, din 0,24-0,68% in greutate agent de îmbunătățire a aderentei pe frunze, din 0,20-0,30% in greutate agent de ingrosare, din 0,73-2,70% in greutate cheratina hidrolizata, din 6,50-8,25% in greutate microcapsule cu continui de ulei esențial, avand viteza de eliberare a uleiului din microcapsule la 120 ore de 40,30-48,20%, din 4,045,96% in greutate surfactanti neionici, din 0,66-0,92% in greutate un amestec de săruri de Cu, Zn, Fe, Mo, Mn, Mg ale acidului etilendiaminotetraacetic, si din 63,62-70,28% in greutate apa, stabilitatea suspensiei de biofertilizant fiind > 6 luni.2. Compositions of foliar biofertilizers in the form of aqueous suspension characterized in that they consist of 14.31-19.41% by weight hydrolysed proteins with an average molecular weight of 320-750 Da, from 0.24-0.68% in weight of leaf adhesion enhancing agent, from 0.20-0.30% by weight thickening agent, from 0.73-2.70% by weight hydrolyzed keratin, from 6.50-8.25% by weight microcapsules with essential oil contents, having the oil release rate from microcapsules at 120 hours of 40.30-48.20%, from 4,045.96% by weight nonionic surfactants, from 0.66-0.92% by weight a mixture of Cu, Zn, Fe, Mo, Mn, Mg salts of ethylenediaminetetraacetic acid, and from 63.62-70.28% by weight of water, the stability of the biofertilizer suspension being> 6 months. 3. Procedeu conform revendicării 1, caracterizat prin aceea ca proteinele hidrolizate avand masa moleculara medie de 50.000-60.000 Da, cat si proteinele hidrolizate avand masa moleculara medie de 320-750 Da provin din deșeuri de la prelucrarea pieilor de ovine, bovine, porcine, deșeuri din industria piscicola, deșeuri de la abatoare sau din industria alimentara (oase, cartilaje), uleiurile esențiale sunt alese dintre uleiul de rozmarin, cimbru, coriandru, marar, cuisoare, scorțișoara, eucalipt, conifere, citrice, oregano, mirt, menta, usturoi, arbore de ceai, muscata, lavanda, anason, busuioc, singure sau in amestec, polimerul anionic este de tip tripolifosfat de sodiu sau carboximetil celuloza sodica, agentul de îmbunătățire a aderentei pe frunze este selectat dintre proteinele hidrolizate cu masa moleculara medie de 50.000-60.000 Da, sau hidroxipropil metil celuloza, agentul de ingrosare este de tipul gumei xanthan, a gumei guar, sau a gumei arabice, iar cheratina hidrolizata provine din deșeuri de lana, de pene, de par, de coame, sau de copite.3. Process according to claim 1, characterized in that the hydrolysed proteins having an average molecular weight of 50,000-60,000 Da, as well as the hydrolysed proteins having an average molecular mass of 320-750 Da, come from waste from the processing of sheep, cattle, swine, wastes from the fish industry, waste from slaughterhouses or the food industry (bones, cartilage), essential oils are chosen from rosemary oil, thyme, coriander, dill, cloves, cinnamon, cinnamon, eucalyptus, conifers, citrus, oregano, myrtle, mint, garlic, tea tree, nutmeg, lavender, anise, basil, singly or in mixture, the anionic polymer is sodium tripolyphosphate or carboxymethyl cellulose sodium, the adhesion enhancing agent on the leaves is selected from hydrolysed proteins with an average molecular weight of 50,000 -60,000 Yes, or hydroxypropyl methyl cellulose, the thickening agent is of the type of xanthan gum, guar gum, or arabic gum, and keratin hydrolysis ata comes from waste of wool, feathers, hair, mane, or hooves.
ROA201800167A 2018-03-08 2018-03-08 Process for preparing foliar bio-fertilizers together with component essential oil micro-capsules and foliar bio-fertilizer compositions RO133615A2 (en)

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