JPS58198533A - Acting substance-charged microporous powder and manufacture - Google Patents

Acting substance-charged microporous powder and manufacture

Info

Publication number
JPS58198533A
JPS58198533A JP6847483A JP6847483A JPS58198533A JP S58198533 A JPS58198533 A JP S58198533A JP 6847483 A JP6847483 A JP 6847483A JP 6847483 A JP6847483 A JP 6847483A JP S58198533 A JPS58198533 A JP S58198533A
Authority
JP
Japan
Prior art keywords
active substance
microporous
powder
loaded
polymer
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
JP6847483A
Other languages
Japanese (ja)
Inventor
クリストフ・ヨゼフイアク
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Akzo NV
Original Assignee
Akzo NV
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Akzo NV filed Critical Akzo NV
Publication of JPS58198533A publication Critical patent/JPS58198533A/en
Pending legal-status Critical Current

Links

Classifications

    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION 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
    • A01N25/00—Biocides, 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
    • A01N25/12—Powders or granules
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/0241—Containing particulates characterized by their shape and/or structure
    • A61K8/0279—Porous; Hollow
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/81—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
    • A61K8/8105—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • A61K8/8111—Homopolymers or copolymers of aliphatic olefines, e.g. polyethylene, polyisobutene; Compositions of derivatives of such polymers
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
    • A61K8/88—Polyamides
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00—Medicinal preparations characterised by special physical form
    • A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
    • A61K9/16—Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
    • A61K9/1605—Excipients; Inactive ingredients
    • A61K9/1617—Organic compounds, e.g. phospholipids, fats
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00—Medicinal preparations characterised by special physical form
    • A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
    • A61K9/16—Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
    • A61K9/1605—Excipients; Inactive ingredients
    • A61K9/1629—Organic macromolecular compounds
    • A61K9/1641—Organic macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polyethylene glycol, poloxamers
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00—Medicinal preparations characterised by special physical form
    • A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
    • A61K9/16—Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
    • A61K9/1605—Excipients; Inactive ingredients
    • A61K9/1629—Organic macromolecular compounds
    • A61K9/1641—Organic macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polyethylene glycol, poloxamers
    • A61K9/1647—Polyesters, e.g. poly(lactide-co-glycolide)
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L9/00—Disinfection, sterilisation or deodorisation of air
    • A61L9/015—Disinfection, sterilisation or deodorisation of air using gaseous or vaporous substances, e.g. ozone
    • A61L9/04—Disinfection, sterilisation or deodorisation of air using gaseous or vaporous substances, e.g. ozone using substances evaporated in the air without heating
    • A61L9/042—Disinfection, sterilisation or deodorisation of air using gaseous or vaporous substances, e.g. ozone using substances evaporated in the air without heating with the help of a macromolecular compound as a carrier or diluent
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00—Preparations for care of the skin
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/12—Powdering or granulating
    • C08J3/122—Pulverisation by spraying
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/41—Particular ingredients further characterized by their size
    • A61K2800/412—Microsized, i.e. having sizes between 0.1 and 100 microns
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/56—Compounds, absorbed onto or entrapped into a solid carrier, e.g. encapsulated perfumes, inclusion compounds, sustained release forms

Abstract

Microporous powder charged with an active substance for the controlled release thereof, is made by spraying into a gas a homogeneous solution of a polymer, an active substance and, optionally, an inert liquid. The microporous powder may comprise a thermoplastic polymer charged with the active substance and may have a porosity of from 60 to 80%, an outer skin of the thermoplastic polymer having a thickness of from 0.1 to 1 mu m and an opening content of from 2 to 20%, the openings in the outer skin having a diameter of up to 1 mu m. The microporous powders are particularly suitable for the controlled release of active substances over a prolonged period.

Description

【発明の詳細な説明】 本発明は、作用物質を制御放出するため作用物質が装荷
された微孔質粉末並びにその製造法に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a microporous powder loaded with an active substance for controlled release of an active substance and a process for its production.

多孔質ないしは微孔質である粉末状−または微粒子状粒
子を製造することは久しく公知である。また、特定の作
用物質を含有する微細な微孔質粒子の製造法が公知であ
る。It has been known for a long time to produce powdery or particulate particles that are porous or microporous. Also known are methods for producing fine microporous particles containing specific active substances.

従って、［クンストシュトノフエＪ　ｔ　（ＫＩＩｔＪ
ＳＴＳ’Ｉ’ＯＦ’ＦＥ　）第５５巻、第５号（１９６
５年）の３８９〜３９０頁には、土壌改良に使用される
ことができるプラスチックフオームが記載されている。Therefore, [Kunststnohue J t (KIItJ
STS'I'OF'FE) Volume 55, No. 5 (196
5), pages 389-390, describe plastic foams that can be used for soil improvement.

この場合、粒径４〜１２朋のフレーク状ポリスチロール
粒子または尿素−ホルｌ、−ｒルデヒドフォームが挙げ
られる。これら粒子は、土壌な砕解性とすることができ
かつ、ある程ＩＷにまで水をも吸着しかつその後の時点
で土壌が少雨のため再び乾燥した場合に再び放出する状
態にあり、従ってこれらは、排水成分として作用しかつ
、とくに乾燥地帯の土壌の水分代謝を制御することがで
きる。しかしながら、このような粒子は、その後に環境
へ制御放出される作用物質がはじめから装荷されるには
不適当である。In this case, flaky polystyrene particles or urea-forml,-rdehyde foams with a particle size of 4 to 12 mm may be mentioned. These particles can be disintegrated into the soil and are also in a state of adsorbing water to a certain extent to the IW and releasing it again if the soil dries out again due to light rainfall at a later point in time, so they can act as a drainage component and control water metabolism in soils, especially in arid regions. However, such particles are unsuitable for initial loading with active substances for subsequent controlled release into the environment.

十だ、西］５イツ国特許公開明細書第１６９４７１３号
には、種々の活性剤用の封入物質また（↑Ｖ−ヤリャと
して使用される連続気泡の粒状）十−ノ、が記載されて
いる。しかしながらこの明細書には、有利な方法−で作
用物質が装荷され、制御された長時間放出に適当である
粒子の製造に関する理論が示唆されていない。5 Italian Patent Publication No. 1,694,713 describes encapsulating materials for various active agents (open-celled granules used as ↑ V-Yaya) . However, this document does not suggest any theory for the production of particles that are loaded with active substances in an advantageous manner and are suitable for controlled, long-term release.

西ドイツ国特許明細書第２０３５６０１号には、粒径最
高５００〜最低０．０２ｔｔｍを有しかり、干物直径最
低２００μｍを有する最低１つ、有利に多数の空間を有
する微孔質のポリマー粒子・が記載されている。またこ
のポリマー粒子は、作用物質の制御された長期間放出に
とくに適当ではない。West German Patent Specification No. 2035601 describes microporous polymer particles having a particle size of at most 500 to at least 0.02 ttm and having at least one, preferably multiple, spaces with a dry diameter of at least 200 μm. has been done. These polymer particles are also not particularly suitable for controlled long-term release of active substances.

最後に、オランダ国特許公開明細書７５１００８７３号
には、また粒子または粉末に磨砕されることができるポ
リオレフィンより成る帯電防止剤が記載されている。し
かしながら、これに記載された粒子は、とくに制御され
た長間放出に実際に不適当であり、むしろ、いわゆる゛
７スター・２ノチとして使用される他の、１５　ＩＩ　
−７コン・ξランドに添加され、かつ、帯電防止性を維
持すべきポリマー中の帯電防止剤の分配を改善するため
使用される。Finally, NL 75100873 also describes antistatic agents consisting of polyolefins which can be ground into particles or powders. However, the particles described therein are actually unsuitable, especially for controlled long-term release, and are rather used as the so-called "7 star 2 knots", such as 15 II
-7 con-ξ land and used to improve the distribution of the antistatic agent in the polymer that is to maintain antistatic properties.

また、作用物質を含有する粉末または多孔質粒子に含浸
剤を施こすことが公知である。従うて、例えば欧州特許
明細書第５３０２号には、粒子に作用物質を施こしかつ
化学的に反応させることにより、気泡を密閉するポリウ
レタン被覆を形成する方法が記載されている。このよう
な方法は複雑かつ煩雑である。It is also known to apply impregnating agents to powders or porous particles containing active substances. Thus, for example, European Patent Specification No. 5302 describes a method for forming a polyurethane coating that seals air bubbles by applying active substances to the particles and chemically reacting them. Such methods are complex and cumbersome.

すでに、作用物質の吸収および放出に適当である１連の
微孔質粉末が公知ではあるが、なお、作用物質を長期間
にわたり環境へ放出することが可能である微孔質粉末が
要求される。また、このような微孔質粉末を製造するた
めの、経済的にかつ簡単に作動する改良法が要求される
。Although a series of microporous powders are already known that are suitable for the absorption and release of active substances, there is still a need for microporous powders that are capable of releasing active substances into the environment over long periods of time. . There is also a need for an improved method for producing such microporous powders that is both economical and easily operated.

従って、本発明の課題は、作用物質が装荷さ才１かり、
作用物質を長期間にわたり制御しかつ均質に放出する微
孔質の粉末をうろことである。It is therefore an object of the present invention to ensure that the active substance is loaded with
It is a microporous powder that provides a controlled and homogeneous release of the active substance over a long period of time.

さらに、本発明の課題は、多量の作用物質が装荷される
ことができ、その特別な構造により、初期作用物質分量
が大きい場合でもはじめに多量の作用物質を放出せず、
従ってその放出量が迅速に低減することのない微孔質粉
末をうろことである。Furthermore, it is an object of the present invention that large amounts of active substance can be loaded and that, due to its special structure, it does not initially release large amounts of active substance even with large initial active substance quantities;
Therefore, it is a microporous powder whose release amount does not decrease rapidly.

さらに、本発明の課題は、前記せる種類の微孔質粉末が
簡単かつ経済的に入手可能である方法をうろことである
。Furthermore, it is an object of the present invention to provide a method by which microporous powders of the type described above can be obtained simply and economically.

さらに、本発明の課題は、微孔質粉末が、長期間放出を
改善するため他の材料より成る２次的薄膜を有せざる微
孔質粉末およびその製造法をうろことである。Furthermore, it is an object of the present invention to provide a microporous powder and a process for its production, which do not have a secondary film of other materials in order to improve long-term release.

この課題は、作用物質を制御放出する熱可塑性、＋９　
リマーより成る粉末において、多孔率６０〜８０％を有
し、熱可塑性ポリマーより成る厚さ約０．１〜１μｍお
よび開口率約２〜２０％を有する外皮を有し、その場合
外皮の開口が直径ｌｌＬｍ　までを有することな特徴と
する作用物質が装荷された微孔質粉末により解決される
・本発明によれば、作用物質が装荷され、作用物質を制
御放出するこのような微孔質粉末を製造するに当り、ポ
リマーおよび作用物質より成り、場合により付加的な不
活性液体を含有する均質な溶液をガス中へ噴霧すること
を特徴とする方法が得られる。この場合、有利に気孔形
成性の作用物質が使用されろ。不活性液体を付加的に共
用する場合、このものが気孔形成性であることができる
。The challenge is to develop thermoplastics with controlled release of active substances, +9
The powder made of reamer has a porosity of 60 to 80% and a skin made of a thermoplastic polymer having a thickness of about 0.1 to 1 μm and an aperture ratio of about 2 to 20%, in which case the apertures of the skin are According to the invention, such a microporous powder loaded with an active substance and with a controlled release of the active substance is solved by a microporous powder loaded with an active substance, characterized in that it has a diameter of up to A process is obtained which is characterized in that a homogeneous solution of polymer and active ingredient, optionally containing an additional inert liquid, is sprayed into the gas. In this case, preference is given to using pore-forming active substances. If an inert liquid is additionally used, this can be pore-forming.

本発明による方法の殊に有利な実施例にお（・て、液状
の凝集状態で完全混合の範囲よ、５よび混合欠陥を有す
る範囲を有する２成分混合物を形成する、ポリマーおよ
び作用物質より成る均質な溶液を使用し、その場合、凝
離温度を上廻る温度を有する溶液を、凝離温度を上廻る
温度を有するガス中へ噴霧する。In a particularly advantageous embodiment of the process according to the invention, the polymer and the active substance form a two-component mixture in the liquid agglomerated state that has a range of complete mixing, a range of 5 and a range of mixed defects. A homogeneous solution is used, in which case a solution with a temperature above the separation temperature is sprayed into a gas with a temperature above the separation temperature.

不活性液体は、使用せるポリマーに苅する不溶剤であれ
ばよい。有利に、溶液を形成するた１〜））、作用物質
約２０〜７０％および不活性液体約３０〜８０％が使用
される・殊にこのよりな組成は、作用物質自体が気孔形
成性でない場合に有利である。The inert liquid may be any insoluble agent that is compatible with the polymer used. Advantageously, to form a solution, about 20-70% of active substance and about 30-80% of inert liquid are used; in particular, this higher composition is advantageous if the active substance itself is not pore-forming. advantageous in some cases.

本発明による方法のもう１つの殊に有利な実施例におい
て、噴霧後の粉末が洗浄される。In another particularly advantageous embodiment of the method according to the invention, the powder after spraying is washed.

ボ゛リマーとして、とりわけポリアミド−６が極めて適
当であり、その場合付加的な不活性液体としてとくにγ
−プチロラクトノを使用することができる。Polyamide-6 is particularly suitable as polymer, in which case as additional inert liquid especially γ
- Petitrolactono can be used.

有利に本発明で使用可能である熱可塑性ポリ゛７−は、
この場合とくに引用する西ドイツ国特許公開明細書第２
７３７７４５号に記載されて（・る。また、この公開明
細書には、その中でしばしば官能性液体と呼称される全
ての系列の作用物質が挙げられ、これらは熱可塑性ポリ
マーと一緒になって本発明に王る微孔質粉末に加工され
ることができる。従って、前記引用の西ドイツ国特許公
開明細書第２７３７７４５号の第８９頁第２節および第
９０頁第１節に記載されたような、動物駆逐剤、放香剤
、駆虫剤、医薬、芳香加良剤、殺菌剤、香料等として作
１１１する官能性液体が本発明により使用されろことが
できる。Thermoplastic polymers 7- which can advantageously be used in the present invention are:
West German Patent Publication Specification No. 2, which is specifically cited in this case.
No. 737,745 (1999). This publication also mentions a whole series of active substances, often referred to therein as functional liquids, which together with thermoplastic polymers According to the present invention, the microporous powder can be processed into a microporous powder as described in the above-cited West German Patent Publication No. 2737745, page 89, section 2 and page 90, section 1. Sensory liquids which can be used as animal repellents, fragrance agents, anthelmintic agents, medicines, fragrance enhancers, disinfectants, fragrances, etc. can be used in accordance with the present invention.

前記特許公開明細書の実施例および表中に、全系列の官
能性液体が使用可能なポリマーとともに列挙されている
。本発明の範囲内で、前記特許公開明細書の記載が挙げ
られる。In the examples and tables of said patent publication, a whole series of functional liquids are listed along with the polymers that can be used. Within the scope of the present invention, reference may be made to the descriptions of the aforementioned patent publications.

有利に、使用されたポリマーおよび作用物質が、液状の
凝集状態で完全混合性ｐ）範囲および混合欠陥を有する
範囲を有する混合物を形成する。噴霧されるのが、唯一
の液相として存在する溶液である。このことは、溶液が
、混合物の凝離温度を上廻る温度を有する必要のあるこ
とを表わす。Preferably, the polymers and active substances used form a mixture in the liquid agglomerated state which has a fully miscible p) range and a range with mixing defects. What is sprayed is a solution present as the only liquid phase. This means that the solution must have a temperature above the separation temperature of the mixture.

この溶液が、凝離温度を上廻る温度を有するガス中へ噴
霧される。凝離温度を上廻ると混合物が２相になり、す
なわち差当って一般に２−）の液相が相互に形成される
。This solution is sprayed into a gas having a temperature above the separation temperature. Above the separation temperature, the mixture becomes biphasic, ie generally 2-) liquid phases are initially formed with each other.

殊に有利なのは、均質な溶液を、宰温を有す７、　ｉｆ
ガス中噴霧することである。Particularly advantageous is the homogeneous solution having a temperature of 7, if
It is sprayed in gas.

ガスとして空気が使用されてもよいが；しか［７また可
能なのは、例えば窒素または希ガスのような他のガス１
作業することである。Air may be used as gas; however, it is also possible to use other gases, such as nitrogen or noble gases.
It's about working.

殊に有利なのが、使用された混合物が液状の凝集状態で
混合欠陥を有する場合であり；この方法で、微孔質粉末
には殊に有利な気孔−な（・し７は微孔組織が得られる
。作用物質とともに１種またはそれ以上の不活性液体が
一緒に使用されることができ；この場合、不活性液体、
作用物質およびポリマーが同じく一緒に均質な溶液を形
成する。It is particularly advantageous if the mixture used has mixing defects in the liquid agglomerated state; in this way, the microporous powder has a particularly advantageous pore structure. One or more inert liquids can be used together with the active substance; in this case, an inert liquid,
The active substance and the polymer also form a homogeneous solution together.

相応する不活性液体を添加することにより、液状の凝集
状態で混合欠陥を有せざるポリマー）６よび作用物質よ
り成る混合物が、液状の凝集状態で混合欠陥を有する混
合物へ変換されることができる。従って、不活性液体を
添加することにより、もっばらはじめに混合欠陥が形成
されることができるか、ないしはまた混合欠陥を増大さ
せることが可能！あり、それにより太き（・効果が得ら
れる。By adding a corresponding inert liquid, a mixture consisting of a polymer (6) and an active ingredient which is free of mixing defects in the liquid agglomerated state can be converted into a mixture which has mixing defects in the liquid agglomerated state. . Therefore, by adding an inert liquid, mixing defects can be formed at the outset or even be increased! Yes, it makes it thicker (・effect can be obtained).

噴霧すべき溶液の温度および、溶液が噴霧されるガスの
温度間の温度差を選択することにより、粉末の特性を変
更することが１１能である。By selecting the temperature difference between the temperature of the solution to be atomized and the temperature of the gas onto which the solution is atomized, it is possible to change the properties of the powder.

なかんずく温度を選択することにより、粉末の形状、気
泡容積の種類等が制御されることができる。温度差がわ
ずかな場合、生じる粉末の形状が球形の方へ変動する。By selecting the temperature, among other things, the shape of the powder, the type of bubble volume, etc. can be controlled. If the temperature difference is small, the shape of the resulting powder shifts towards a spherical shape.

有利なのは、溶液およびガス間の温度差ができるだけ大
きい場合であり；従って有利に、室温を有するガス中へ
噴霧させる。It is advantageous if the temperature difference between solution and gas is as large as possible; it is therefore advantageous to atomize into a gas having room temperature.

凝固に際し、粉末が、冷却特性に応じ程度の差こそあれ
不規則な形状で生じる。さらにこの粉末は、外側にも作
用物質より成る薄膜を有し、それによりこれが一定の粘
着性を生じることがある。しかしながらこの粘着性は、
これによりそれぞれの粒子の分離が不可能になる程度に
犬ではない。さらに、この方法で？（＋もれた粉末は、
一般に極めて容易に、例えば他の液体中ハ、分離するこ
とによるかあるいはまた機械的方法で分散することがで
きるＯ 殊に有利なのが、凝固後の粉末に洗浄を施こした場合↑
あり、それにより殊に流動性の粒子が（１）られ、この
ものは乾燥した粉末、粒子または顆粒のように取扱われ
ることができる。洗浄に役立つのは、アルコール等のよ
うな適当な溶剤または洗浄剤を使用する簡単な短時間の
処理である。Upon solidification, the powder forms with a more or less irregular shape depending on the cooling characteristics. Furthermore, the powder also has a thin film of active substance on the outside, which can result in a certain stickiness. However, this stickiness
This is not dog-like to the extent that it is impossible to separate the individual particles. Moreover, in this way? (+Leaked powder is
In general, it can be dispersed very easily, for example in other liquids, by separation or also by mechanical methods. It is particularly advantageous if the powder is washed after solidification.
Thereby, in particular flowable particles (1) are obtained, which can be handled like dry powders, particles or granules. Cleaning is aided by a simple, short-term treatment using a suitable solvent or cleaning agent such as alcohol or the like.

噴霧すべき溶液の粘度は広い範囲内で変更することがで
きるが；但し有利なのは、粘度が５１”ａ　！：を」二
廻らない場合である。相応する粘度は１、ｌ：’　ＩＪ
ママ一度の調節、ポリマー分子量の選択、温度、および
また作用物質および場合により付加的に使用される液体
の選択により調節される、二とができる。The viscosity of the solution to be sprayed can be varied within wide limits; however, it is advantageous if the viscosity does not exceed 51". The corresponding viscosity is 1, l:' IJ
Two adjustments can be made, one by one, the selection of the polymer molecular weight, the temperature, and also the selection of the active substances and optionally additionally used liquids.

自体明白なのは、粘度を噴霧時に有利な価に調節するこ
とであるが、この価がしばしばまた噴霧法、例えば使用
されるガスの噴霧ノズルの選択、ガスの淵反等に関連す
る。It is obvious in itself that the viscosity should be adjusted to an advantageous value during atomization, but this value is often also related to the atomization method, for example the selection of the atomization nozzle of the gas used, the gas flow, etc.

とくにポリマー。して、約４００００　）’ルトン（Ｄ
ａｌｔｏｎ　）までの分子量を有する低分子−子ＩＪマ
マ−使用される。Especially polymers. (approximately 40,000)'Luton (D
A small molecule with a molecular weight up to (alton) is used.

不活性液体を一緒に使用する場合、殊に有利なのは、西
ドイツ国特許出願明細書第３２０５２８９号に記載され
たような液体が使用される場合である。とりわけ、この
特許出願明細書中に挙げられた食用油および食用脂は多
数の用途に極めて適当である、それというのもこの場合
、種々の用途で必要とされろ無毒、無害な物質が挙げら
れているからである。If inert liquids are used together, it is particularly advantageous if liquids such as those described in German Patent Application No. 3,205,289 are used. In particular, the edible oils and edible fats mentioned in this patent application are highly suitable for a large number of applications, since in this case non-toxic and harmless substances may be mentioned as required in various applications. This is because

溶液が本発明により噴霧されるガスは標準的な圧縮比を
有してよく；または減圧下に作動することが可能である
が；しかしこのことは一般に不必要である。The gas with which the solution is atomized according to the invention may have a standard compression ratio; or it is possible to operate under reduced pressure; however, this is generally unnecessary.

殊に意外だったのは、本発明により、作用物質を制御し
て、すなわち長時間にわたり同じ量で放出する状態にあ
る、作用物質の装荷された粉末を製造することが可能で
あることである。What was particularly surprising was that, according to the invention, it was possible to produce active substance-loaded powders that released the active substance in a controlled manner, ie in the same amount over a long period of time. .

本発明は、極めて多方面に使用可能でありかつすでに前
記せる用途とともに、またとりわけホルモン、動物−お
よび人体医療用の種々の医薬の長期投与、林業および農
業等に使用されることができる０ さらに有利なのは、噴射工程が極めて簡単な方法で実施
されうろことである。この場合、噴射ないしは噴霧する
ため、操作技術から公知の常用の装置が使用されること
ができ、これらは例えばウルマンの１工業化学事典１　
（Ｕ、Ｌ　ｌ　ｍａｎｒ＋ｓ　。The present invention is extremely versatile and can be used in addition to the applications already mentioned above, as well as in the long-term administration of various pharmaceuticals for hormones, veterinary and human medicine, forestry and agriculture, etc. It is advantageous that the injection process can be carried out in a very simple manner. In this case, for the injection or atomization, conventional devices known from the operating technology can be used, such as, for example, Ullmann 1 Encyclopedia of Industrial Chemistry 1
(U,L lmanr+s.

１弓ｎｚｙｋ１．ａｐａｄｉｅ　ｄｅｒ　’ｒｅｃｈｎ
ｉＳｃｈｅｎ　Ｃｂｅｍｉｅ　）第１を（第３版、１９
５１年発行）７２８〜７３１貞または同事典第２巻（第
４版、１９７２年発行）２５４〜２５８頁に記載されて
いる。1 bow nzyk1. apadie der 'rechn
iSchen Cbemie) 1st (3rd edition, 19
It is described in 728-731 Sada (published in 1951) or pages 254-258 of the same dictionary, Volume 2 (4th edition, published in 1972).

作用物質の装荷された微孔質粉末の製造は、極めて簡単
かつ経済的な方法で実施されることができる。この場合
、例えばポリアミド−６のよ５なポリマーおよび、例え
ばメチルノニルケトンおよびｒ−プチロラクトノのよう
な、不活性気孔形成剤としての作用物質から、加熱する
ことにより溶液を製造する、その際場合により攪拌され
ることができる。この場合、最高５Ｐｔａ−８の粘度を
有する溶液を製造するのが不利である。The production of microporous powders loaded with active substances can be carried out in a very simple and economical manner. In this case, a solution is prepared by heating from a polymer such as, for example, polyamide-6 and an active substance as an inert pore-forming agent, such as, for example, methyl nonyl ketone and r-butyrolactone. Can be stirred. In this case, it is a disadvantage to produce solutions with a viscosity of up to 5 Pta-8.

空気ないしはガス中への噴霧は、技術的難点のない極め
て簡単な工程である。Spraying into air or gas is a very simple process without any technical difficulties.

さらに、ウルフ／の事典に記載さ才またノズルとともに
、中空繊維の製造で公知であるノズルが適当である。こ
れらのいわゆる２つ孔ノズルの場合、内側の孔が溶液の
押出しに使用され；外側の環状孔により、圧力下にある
ガスが導かれることができ、その場合噴霧効果が格別に
改善される。Furthermore, nozzles known for the production of hollow fibers are suitable, as well as the nozzles described in the Wolff Dictionary. In the case of these so-called two-bore nozzles, the inner bore is used for extrusion of the solution; the outer annular bore allows gas under pressure to be conducted, in which case the atomization effect is significantly improved.

殊に意外だったのは、本発明による方法で製造された粉
末が、作用物質の貯蔵さ才１ろ犬き（・内部有効気孔率
を有しかつさらに相対的に密閉された表面を有し、この
表面が、作用物質が長時間にわたり不変の微小配量で環
境へ放出されるように配慮することである。この方法で
、抜群の長期作用が得られる。It was particularly surprising that the powders produced by the process according to the invention have an excellent internal effective porosity and also have a relatively closed surface, which makes it possible to store active substances. This surface ensures that the active substance is released into the environment in constant, minute doses over a long period of time.In this way, an outstanding long-term action is obtained.

本発明による方法で形成された粉末の表面ないしは表皮
は相対的に密閉され、従って作用物ｒｉｆｊが、早期に
かつ、放出の開始時に高濃度で放出されることがないが
、但しこれは、作用物質の装荷された粉末から外方へ脱
出することが作用物質にとって可能であるような十分な
孔を有−１″ろ〇 以下に、本発明を実施例につき詳説する。The surface or epidermis of the powder formed in the method according to the invention is relatively sealed, so that the active substance rifj is not released early and in high concentrations at the onset of release, although this The invention will now be explained in more detail with reference to examples.

例１ 約１９０℃で、ポリアミド−６（溶液粘度２５）１０％
、γ−ブチロラクトン８０％およびメチルノニルケトン
ｌＯ％（作用物質）より成る溶液を製造し、かつ２００
℃で、圧搾空気をｆ＝Ｊｕ用し２つ孔ノズルを経て、室
温に調節された大形捕集容器中へ噴霧した。得られた粉
末は、粉末を抽出した後に水銀多孔爪針により測定した
気孔容積率６２チを有する。Example 1 At about 190°C, 10% polyamide-6 (solution viscosity 25)
, a solution consisting of 80% γ-butyrolactone and 10% methylnonylketone (active substance) and 200%
℃, compressed air with f=Ju was sprayed through a two-hole nozzle into a large collection vessel maintained at room temperature. The resulting powder has a pore volume fraction of 62, measured with a mercury porous needle after extraction of the powder.

例２ ；１′■ノゾロピレン１０％、ひまし油２７係およびイ
ノプロピルミリステート６３係より成る溶液を、２５０
°Ｃで空気中へ噴霧する。得られたポリゾロピレン粉末
は、気孔容積率約７０チを有する。Example 2; 1'■ A solution consisting of 10% nozolopyrene, 27 parts castor oil and 63 parts inopropyl myristate was mixed with 250 parts
Spray into the air at °C. The resulting polyzolopyrene powder has a pore volume fraction of about 70 inches.

これら２つの実施例において、直径１５；。In these two examples, the diameter is 15;

９および０．６５　ｍｍを有する常用構造の中空繊維ノ
ズルを使用した。Hollow fiber nozzles of conventional construction with 9 and 0.65 mm were used.

Claims (1)

【特許請求の範囲】 １、熱可塑性ポリマーより成り、作用物質を制御放出す
る粉末において、多孔率６０〜８０チを有し、熱可塑性
ポリマーより成る厚さ０゜１〜１μｍおよび開口率２〜
２０％の外皮を有し、その場合外皮の開口が１μｍまで
の直径を有することを特徴とする作用物質の装荷された
微孔質粉末。 ２　熱可塑性ポリマーより成り、多孔度６０〜８０％を
有し、熱可塑性ポリマーより成る厚さ０．１〜１μｍお
よび開口率２〜３０％の外皮を有し、その場合外皮の開
口が１μｍまでの直径を有する、作用物質を制御放出す
る粉末を製造するに当り、ポリマーおよび作用物質より
成。す、場合により付加的に不活性液体を含有する均質
な溶液をガス中へ噴霧することを特徴とする作用物質の
装荷された微孔質粉末の製造法。 ３、気孔形成性の作用物質を使用することを特徴とする
特許請求の範囲第２項記載の作用物質の装荷された微孔
質粉末の製造法。 ４、気孔形成性の不活性液体を使用することを特徴とす
る特許請求の範囲第２および第３項のいずれかに記載の
作用物質の装荷された微孔質粉末の製造法。 ５　ポリマーおよび作用物質より成り、液状の凝集状態
で完全混合の範囲と混合欠陥を有する範囲とを有する均
質な溶液を使用し、かつ凝離温度を下廻る温度を有する
この溶液を、凝離温度を１廻る温度を有するガス中へ噴
霧することを特徴とする特許請求の範囲第２〜第４項の
いずれかに記載の作用物質の装荷された微孔質粉末の製
造法。 ６、それ自体が使用ポリマーの不溶剤である不活性液体
を使用することを特徴とする特許を請求の範囲第２〜第
５項のいずれかに記載の作用物質の装荷された微孔質粉
末の製造法。 ７　作用物質２０〜７０％および不活性液体３０〜８０
チを含有する溶液を使用することを特徴とする特許請求
の範囲第２〜第６項のいずれかに記載の作用物質の装荷
された微孔質粉末の製造法。 ８　噴霧後の粉末を洗浄することを特徴とする特許請求
の範囲第２〜第７項のいずれかに記載の作用物質の装荷
された微孔質粉末の製造法・ ９、　ポリマーとしてポリアミド（を使用することを特
徴とする特許請求の範囲域２〜第８項のいずれかに記載
の作用物質の装荷された微孔質粉末の製造法。 １０　　付加的な不活性液体としてγ−ブチロラクトン
を使用することを特徴とする特許請求の範囲第９項記載
の作用物質の装荷された微孔質粉末の製造法。[Claims] 1. Powder made of a thermoplastic polymer for controlled release of an active substance, having a porosity of 60 to 80 mm, a thickness of 0°1 to 1 μm and an aperture ratio of 2 to 1 μm, made of a thermoplastic polymer.
Microporous powder loaded with active substance, characterized in that it has a 20% shell, the openings of the shell having a diameter of up to 1 μm. 2. It is made of a thermoplastic polymer and has a porosity of 60 to 80%, and has an outer skin made of a thermoplastic polymer with a thickness of 0.1 to 1 μm and an open area of 2 to 30%, in which case the opening of the outer skin is up to 1 μm. of a polymer and an active substance for the production of a powder with a controlled release of an active substance, having a diameter of . A process for the preparation of microporous powders loaded with active substances, characterized in that a homogeneous solution optionally additionally containing an inert liquid is sprayed into a gas. 3. Process for producing a microporous powder loaded with an active substance according to claim 2, characterized in that a pore-forming active substance is used. 4. Process for producing microporous powders loaded with active substances according to any of claims 2 and 3, characterized in that a pore-forming inert liquid is used. 5. Using a homogeneous solution of polymer and active substance, which has a range of complete mixing and a range of mixed defects in the liquid agglomerated state, and having a temperature below the separation temperature, 5. Process for producing a microporous powder loaded with an active substance according to any of claims 2 to 4, characterized in that the powder is sprayed into a gas having a temperature of about 1°C. 6. Microporous powder loaded with active substance according to any of claims 2 to 5, characterized in that an inert liquid is used which is itself an insolvent for the polymer used. manufacturing method. 7 20-70% active substance and 30-80% inert liquid
7. A process for producing microporous powders loaded with active substances according to any one of claims 2 to 6, characterized in that a solution containing H is used. 8. A method for producing a microporous powder loaded with an active substance according to any one of claims 2 to 7, characterized in that the powder is washed after spraying.9. Process for the production of a microporous powder loaded with an active substance according to any of claims 2 to 8, characterized in that: 10 using γ-butyrolactone as an additional inert liquid; A method for producing a microporous powder loaded with an active substance according to claim 9, characterized in that:
JP6847483A 1982-04-23 1983-04-20 Acting substance-charged microporous powder and manufacture Pending JPS58198533A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE32152116 1982-04-23
DE19823215211 DE3215211A1 (en) 1982-04-23 1982-04-23 MICROPOROISIS POWDER LOADED WITH ACTIVE SUBSTANCES

Publications (1)

Publication Number Publication Date
JPS58198533A true JPS58198533A (en) 1983-11-18

Family

ID=6161767

Family Applications (1)

Application Number Title Priority Date Filing Date
JP6847483A Pending JPS58198533A (en) 1982-04-23 1983-04-20 Acting substance-charged microporous powder and manufacture

Country Status (4)

Country Link
JP (1) JPS58198533A (en)
DE (1) DE3215211A1 (en)
FR (1) FR2525492A1 (en)
GB (1) GB2118945B (en)

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB8333053D0 (en) * 1983-12-12 1984-01-18 Lilly Industries Ltd Pharmaceutical and veterinary formulations
JPS6310701A (en) * 1986-07-02 1988-01-18 Meiji Seika Kaisha Ltd Production of granular agricultural chemical
DE3824940C2 (en) * 1988-07-22 2002-06-27 Ipac Haushalt & Technik Gmbh E Process for the manufacture of a material for dispensing aromas or essences
DE4308282C2 (en) * 1993-03-16 1994-12-22 Beiersdorf Ag Galenic matrices preferably in the form of microspheres
TWI405804B (en) * 2010-04-19 2013-08-21 Geonano Environmental Technology Inc Polymeric complex supporter for controlling gas-releasing substances and manufacturing thereof
JP2021134233A (en) * 2020-02-21 2021-09-13 パナソニックＩｐマネジメント株式会社 Resin composition

Family Cites Families (21)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1642340U (en) * 1952-05-12 1952-08-14 Gustav Thun Fa LEVER BRAKE FOR BICYCLES.
NL249420A (en) * 1959-03-17
DE1802684U (en) * 1959-10-15 1959-12-17 Pelz & Co G M B H W RECEPTION CONTAINER FOR COTTON.
AT228387B (en) * 1960-04-07 1963-07-10 Philips Nv Process for the production of dry, spreadable, air-stable preparations
US3154397A (en) * 1960-06-30 1964-10-27 Dow Chemical Co Herbicidal composition and method
DE1201824B (en) * 1961-10-31 1965-09-30 Warner Lambert Pharmaceutical Process for the production of mannitol with a specific, free-flowing, compressible structure
DE1294932B (en) * 1964-02-12 1969-05-14 Dunlop Rubber Co Manufacture of microcapsules
US3657446A (en) * 1966-09-15 1972-04-18 Georgia Pacific Corp Process for preparation of a pesticide in dry form
CH509748A (en) * 1968-07-25 1971-07-15 Ciba Geigy Ag Synthetic high polymer granulates with adsorbed - biologically active materials
AU439432B2 (en) * 1968-11-28 1972-08-15 Dulux Australia Ltd Polymer and coating composition
NL6909123A (en) * 1969-06-16 1970-12-18 Slow release of volatile materials into the - atmosphere
GB1390032A (en) * 1971-08-27 1975-04-09 Sterling Winthrop Group Ltd Pharmaceutical compositions
GB1443545A (en) * 1972-12-30 1976-07-21 Toyo Jozo Kk Molecular sieving particleland preparation thereof
AU1158276A (en) * 1975-03-03 1977-09-08 Airwick Ag A solid air odor-improving agent-releasing diffuser system
DK171108B1 (en) * 1976-08-30 1996-06-10 Akzo Nv Microporous polymer body and its preparation and use
US4223070A (en) * 1978-05-04 1980-09-16 Stauffer Chemical Company Impregnated porous granules with slow release pore membranes and process therefor
US4286020A (en) * 1978-07-05 1981-08-25 Environmental Chemicals, Inc. In-flight encapsulation of particles
IT1207172B (en) * 1979-02-15 1989-05-17 Anic Spa PROCESS FOR THE PREPARATION OF GLOBAL MICROPOROUS BODIES ONE OR MORE ACTIVE AGENTS.
CH639282A5 (en) 1979-06-26 1983-11-15 Firmenich & Cie DEVICE FOR SCENTING AMBIENT AIR.
JPS56167601A (en) * 1980-05-28 1981-12-23 Kao Corp Insecticidal and insect-expelling composition of aerosal type
DE3026688C2 (en) * 1980-07-15 1986-02-20 Akzo Gmbh, 5600 Wuppertal Process for the production of powdery, porous polymer particles

Also Published As

Publication number Publication date
DE3215211A1 (en) 1983-10-27
GB2118945A (en) 1983-11-09
GB2118945B (en) 1985-08-29
GB8310812D0 (en) 1983-05-25
FR2525492A1 (en) 1983-10-28

Similar Documents

Publication Publication Date Title
US4286754A (en) Controlled-rate liquid dispenser
RU2142792C1 (en) Method and device for preparation of hard molds with controllable release of active ingredient
JP2565781B2 (en) Time release protein
JP2764143B2 (en) Composition encapsulating adjuvant with antiperspirant and encapsulation method
JPS58194969A (en) Composite body for releasing effective substance long time
NO960232D0 (en) Method for coating droplets or nanoparticles
US5079005A (en) Time release protein
JPS58198533A (en) Acting substance-charged microporous powder and manufacture
DE4122591C1 (en) Producing microcapsules of water insoluble polymer and active agent - includes dissolving or dispersing active agent in aq. polymer contg. gellable assistants
DE60309965T2 (en) Controlled release of fragrances through non-woven bags
KR100837793B1 (en) Hybrid air freshener composition having constant and long exhalation property
US3576759A (en) Process for en masse production of spherules by desiccation
EP1033976B1 (en) Microsphere reservoirs for controlled release application
EP0209870A2 (en) Cosmetic composition with sustained release of vaporizable chemical
Pinto et al. A relationship between surface free energy and polarity data and some physical properties of spheroids
JPS608219A (en) Pasty composition containing material for controlling release of volatile and diffusible substance
JP2589257B2 (en) Bath composition
JPS6226214A (en) Solid bath composition slowly soluble in hot water
JPH0356403A (en) Controlled release device for active ingredient
DE1504012C (en) Body with incorporated active ingredient based on a solidified emulsion
JPH0665412A (en) Volatile chemical agent-containing porous cellulose and its production
JPS59186912A (en) Perfume-containing soluble film
JPS6016914A (en) Slow-releasing perfumery composition and its preparation
JPS6122584B2 (en)
DE1504012B2 (en) BODY WITH INCORPORATED INGREDIENT ON THE BASIS OF A SOLID EMULSION