HRP20180151T1 - Postupak za dobivanje mikrokapsula - Google Patents

Postupak za dobivanje mikrokapsula Download PDF

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Publication number
HRP20180151T1
HRP20180151T1 HRP20180151TT HRP20180151T HRP20180151T1 HR P20180151 T1 HRP20180151 T1 HR P20180151T1 HR P20180151T T HRP20180151T T HR P20180151TT HR P20180151 T HRP20180151 T HR P20180151T HR P20180151 T1 HRP20180151 T1 HR P20180151T1
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HR
Croatia
Prior art keywords
solution
monomeric component
reactor
sodium
microcapsules
Prior art date
Application number
HRP20180151TT
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English (en)
Inventor
Marco Bernardini
Francesca Borgo
Giorgio Freschi
Edoardo Russo
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Sipcam S.P.A.
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Publication date
Application filed by Sipcam S.P.A. filed Critical Sipcam S.P.A.
Publication of HRP20180151T1 publication Critical patent/HRP20180151T1/hr

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/02Making microcapsules or microballoons
    • B01J13/06Making microcapsules or microballoons by phase separation
    • B01J13/14Polymerisation; cross-linking
    • B01J13/16Interfacial polymerisation
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/26Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests in coated particulate form
    • A01N25/28Microcapsules or nanocapsules
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K31/00Medicinal preparations containing organic active ingredients
    • A61K31/16Amides, e.g. hydroxamic acids
    • A61K31/165Amides, e.g. hydroxamic acids having aromatic rings, e.g. colchicine, atenolol, progabide
    • A61K31/167Amides, e.g. hydroxamic acids having aromatic rings, e.g. colchicine, atenolol, progabide having the nitrogen of a carboxamide group directly attached to the aromatic ring, e.g. lidocaine, paracetamol
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/48Preparations in capsules, e.g. of gelatin, of chocolate
    • A61K9/50Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
    • A61K9/5089Processes

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Organic Chemistry (AREA)
  • Pest Control & Pesticides (AREA)
  • Plant Pathology (AREA)
  • Environmental Sciences (AREA)
  • Zoology (AREA)
  • Wood Science & Technology (AREA)
  • Dentistry (AREA)
  • Agronomy & Crop Science (AREA)
  • Engineering & Computer Science (AREA)
  • Toxicology (AREA)
  • Epidemiology (AREA)
  • Medicinal Chemistry (AREA)
  • Veterinary Medicine (AREA)
  • Public Health (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Animal Behavior & Ethology (AREA)
  • Dispersion Chemistry (AREA)
  • Pain & Pain Management (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Manufacturing Of Micro-Capsules (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Claims (18)

1. Kontinuirani postupak pripreme mikrokapsula s učinkovitošću inkapsulacije ≥96% aktivnog sastojka, te mikrokapsule pokazuju omjer b)/a), pri čemu da b) je prosječni promjer određen na 90% mikrokapsula i a) je prosječni promjer određen na 50% mikrokapsula, koji se nalazi između 1.5 i 2.5 dok je prosječni promjer 90% mikrokapsula manji od 15 µm, i inkapsulira water aktivne sastojke netopljive u vodi koji se koriste u farmaceutskom i agrokemijskom području, naznačen time da postupak obuhvaća: (1) pripremanje u prvom reaktoru uz miješanje vodene otopine koja sadrži jedan ili više surfaktanata, (2) pripremanje u drugom reaktoru uz miješanje otopine koja sadrži aktivni sastojak koji se ne miješa u vodenoj fazi i prve monomerne komponente, istodobno dovođenje u cijevni reaktor struje vodene otopine (1) i struje otopine (2), koja je omjer struja otopine (2)/struja otopine (1) u rasponu između 0.5 i 2.0, struje (1) i (2) su pod turbulentnim uvjetima strujanja u reaktoru, zatim, ulaz u reaktor pod turbulentnim uvjetima strujanja struje (3) koja sadrži drugu monomernu komponentu, a ekvivalentni omjer između prve monomerne komponente i druge monomerne komponente se nalazi između 0.9 i 1.1, struje (1), (2) i (3) se kontinuirano dovode u cijevni reaktor, struje (1), (2) i (3) imaju odvojene ulaze u cijevni reaktor.
2. Postupak prema zahtjevu 1 naznačen time da se koriste struje (1), (2) i (3).
3. Postupak prema zahtjevima 1-2 naznačen time da se kao prva monomerna komponenta koristi smjesa izocijanata.
4. Postupak prema zahtjevima 1-3 naznačen time da se otopina (1) i otopina (2) aktivnog sastojka i prve monomerne komponente uvode u reaktor kod temperature u rasponu od 10°C sve do 60°C.
5. Postupak prema zahtjevima 1-4 naznačen time da se otopina (2) priprema miješanjem otopine (2a) koja sadrži aktivni sastojak i proizvoljno organsko otapalo, te otopine (2b) koja sadrži prvu monomernu komponentu, proizvoljno otopljenu u organskom otapalu, (2a) i (2b) te se kontinuirano prethodno miješa i zatim se puni u cijevni reaktor.
6. Postupak prema zahtjevima 1-5 naznačen time da viskoznost otopine (2), koja je proizvoljno razrijeđena organskim otapalom, je u rasponu 4X10-1 Pa.s (400 cps) i 1 Pa.s (1000 cps).
7. Postupak prema zahtjevima 1-6 naznačen time da su surfaktanti otopine (1) odabrani od anionskih i neionskih surfaktanata.
8. Postupak prema zahtjevu 7 naznačen time da su anionski surfaktanti odabrani iz skupine koju čine natrijevi ligninsulfonati, kalcijevi ligninsulfonati i natrijevi polikarboksilati, a neionski surfaktanti su odabrani od blok kopolimera nastalih s etoksiliranim i propoksiliranim jedinicama.
9. Postupak prema zahtjevima 1-8 naznačen time da su aktivni sastojci odabrani od herbicida, akaricida, insekticida, fungicida, biocida, regulatora rasta biljaka i insekata, antidota.
10. Postupak prema zahtjevu 9, naznačen time da su aktivni sastojci odabrani iz slijedećih razreda: herbicidi, odabrani iz sljedećih razreda: dinitroanilini; kloracetamidi; karbamati; difenileteri; akaricidi razreda METI; insekticidi, odabrani od onih koji pripadaju sljedećim razredima: piretroidi; fosfororganski spojevi; neonikotinoidi; karbamati; fungicidi, odabrani od onih koji pripadaju razredu imidazola, triazola, anilinopirimidina.
11. Postupak prema zahtjevu 10 naznačen time da herbicid je pendimetalin.
12. Postupak prema zahtjevima 1-11 naznačen time da polimerna ovojnica mikrokapsule se može dobiti reakcijom prve monomerne komponente s drugom monomernom komponentom interfacijalnom polimerizacijom pomoću polikondenzacije ili reakcijom druge monomerne komponente nastale in situ s prvom monomernom komponentom.
13. Postupak prema zahtjevu 12 naznačen time da je polimerna ovojnica odabrana iz skupine koju čine poliamidi, poliesteri, poliuretani, poliuree.
14. Postupak prema zahtjevima 12-13 naznačen time da polimer je poliurea ili poliuretan i prva monomerna komponenta je odabrana između di- i tri-izocijanata pri čemu su izocijanatne skupine vezane na alifatsku ili aromatsku skupinu i druga komponenta je alifatski diamin koji ima C2-C7 ugljikovih atoma.
15. Postupak prema zahtjevima 1-14 naznačen time da se tijekom pripremanja mikrokapsule ili nakon nastajanja mikrokapsule dodaju, soli anorganskih alkalnih metala odabrane od litijevog klorida, natrijevog klorida, kalijevog klorida, litijevog nitrata, natrijevog nitrata, kalijevog nitrata, litijevog sulfata, natrijevog sulfata, kalijevog sulfata, natrijevog monohidrogenfosfata, kalijevog monohidrogenfosfata, natrijevog dihidrogenfosfata, kalijevog dihidrogenfosfata; soli zemno alkalijskih metala odabrane od magnezijevog klorida, kalcijevog klorida, magnezijevog nitrata, kalcijevog nitrata, magnezijevog sulfata; amonijeve soli odabrane od amonijevog klorida, amonijevog sulfata, amonijevog monohidrogen fosfata, amonijevog dihidrogen fosfata; soli alkalijskih metala octene kiseline.
16. Postupak prema zahtjevu 15 naznačen time da sol je kalcijev nitrat.
17. Postupak prema zahtjevu 10 naznačen time da su u razredu herbicida: dinitroanilini su odabrani od pendimetalina i trifluralina, kloroacetamidi su odabrani od alaklora, acetoklora, dimetenamida, metolaklora, pethoksamida, pretilaklora, karbamati su odabrani od molinata, trialata, EPTC, difenileteri su odabrani od oksifluorfena, flurokloridona, klomazona, diklobenila, akaricidi METI razreda su odabrani od fenazakvina, piridabena, heksitiazoksa; u razredu insekticida: piretroidi su odabrani od bifentrina, α-cipermetrina, cipermetrina, deltametrina, imiprotrina, λ-cihalotrina, praletrina, tetrametrina, poželjno od bifentrina, α-cipermetrina, deltametrina, λ-cihalotrina, etofenproksa, fosfoorganski spojevi su odabrani od fosmeta, klorpirifosa, naleda, fenitrotiona, neonikotinoidi su odabrani od imidakloprida, acetamiprida, karbamati su odabrani od karbosulfana, pirimikarba, aldikarba, tiodikarba, karbofurana i propoksura, poželjno od karbosulfana.
18. Postupak prema zahtjevu 1 naznačen time da je prosječni promjer 90% mikrokapsula manji od 12 μm.
HRP20180151TT 2011-05-09 2018-01-26 Postupak za dobivanje mikrokapsula HRP20180151T1 (hr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
IT000784A ITMI20110784A1 (it) 2011-05-09 2011-05-09 Processo per l'ottenimento di microcapsule
EP12166778.6A EP2522421B1 (en) 2011-05-09 2012-05-04 A process for obtaining microcapsules

Publications (1)

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HRP20180151T1 true HRP20180151T1 (hr) 2018-03-23

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HRP20211499TT HRP20211499T1 (hr) 2011-05-09 2012-05-04 Postupak za dobivanje mikrokapsula
HRP20180151TT HRP20180151T1 (hr) 2011-05-09 2018-01-26 Postupak za dobivanje mikrokapsula

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Country Status (16)

Country Link
US (1) US9764302B2 (hr)
EP (2) EP2522421B1 (hr)
CY (1) CY1119922T1 (hr)
DK (1) DK2522421T3 (hr)
ES (2) ES2659742T3 (hr)
HR (2) HRP20211499T1 (hr)
HU (2) HUE036386T2 (hr)
IL (1) IL219622A (hr)
IT (1) ITMI20110784A1 (hr)
JO (1) JO3801B1 (hr)
LT (1) LT2522421T (hr)
NO (1) NO2522421T3 (hr)
PL (2) PL2522421T3 (hr)
PT (2) PT3300795T (hr)
RS (2) RS56800B1 (hr)
SI (1) SI2522421T1 (hr)

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Publication number Priority date Publication date Assignee Title
UA121876C2 (uk) 2015-01-06 2020-08-10 Монсанто Текнолоджи Ллс Модуляція швидкості вивільнення з мікроінкапсульованих пестицидів
CN109197869B (zh) * 2018-10-25 2021-07-06 湖南人文科技学院 一种丙草胺微囊悬浮剂及其制备方法
CN109717187A (zh) * 2018-12-21 2019-05-07 江苏艾津农化有限责任公司 一种氯乙酰胺类除草剂微囊悬浮剂及其制备方法
CN112138669B (zh) * 2020-09-30 2022-08-19 广东石油化工学院 一种连续化制备铜锌铝催化剂的方法

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US3577515A (en) 1963-12-13 1971-05-04 Pennwalt Corp Encapsulation by interfacial polycondensation
DE3020781C2 (de) * 1980-05-31 1982-11-18 Hoechst Ag, 6000 Frankfurt Druckbeständige Mikrokapseln mit einer Polyamid-Außenhülle und einer durch Polyurethan-Polyharnstoff oder Polyharnstoff strukturierten Innenmasse und Verfahren zu ihrer Herstellung
US4454083A (en) * 1981-12-21 1984-06-12 Appleton Papers Inc. Continuous microencapsulation
US4936901A (en) * 1986-07-09 1990-06-26 Monsanto Company Formulations of water-dispersible granules and process for preparation thereof
US5925464A (en) * 1995-01-19 1999-07-20 Dow Agrosciences Llc Microencapsulation process and product
US5705174A (en) 1995-06-07 1998-01-06 American Cyanamid Company Process for the preparation of microcapsule compositions
US6001312A (en) * 1996-04-17 1999-12-14 Wang; Taylor G. Reactor for making uniform capsules
DE19925311B4 (de) 1999-05-27 2004-06-09 Schering Ag Mehrstufen-Verfahren zur Herstellung von gasgefüllten Mikrokapseln
ES2764971T3 (es) * 2009-12-22 2020-06-05 Evonik Corp Proceso basado en emulsión para la preparación de micropartículas y conjunto de cabezal de trabajo para su uso con el mismo

Also Published As

Publication number Publication date
SI2522421T1 (en) 2018-03-30
PL3300795T3 (pl) 2021-12-20
US20120286438A1 (en) 2012-11-15
RS62378B1 (sr) 2021-10-29
RS56800B1 (sr) 2018-04-30
NO2522421T3 (hr) 2018-04-21
JO3801B1 (ar) 2021-01-31
ES2890048T3 (es) 2022-01-17
DK2522421T3 (da) 2018-01-29
PT3300795T (pt) 2021-09-13
LT2522421T (lt) 2018-03-12
EP3300795B1 (en) 2021-06-30
US9764302B2 (en) 2017-09-19
PT2522421T (pt) 2018-02-23
IL219622A0 (en) 2012-07-31
IL219622A (en) 2017-05-29
HRP20211499T1 (hr) 2021-12-24
EP2522421A1 (en) 2012-11-14
HUE056468T2 (hu) 2022-02-28
PL2522421T3 (pl) 2018-04-30
ES2659742T3 (es) 2018-03-19
HUE036386T2 (hu) 2018-07-30
ITMI20110784A1 (it) 2012-11-10
EP2522421B1 (en) 2017-11-22
EP3300795A1 (en) 2018-04-04
CY1119922T1 (el) 2018-12-12

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