公开(公告)号：US4376113A

公开(公告)日：1983-03-08

申请号：US181359

申请日：1980-08-26

Applicant: Jean-Claude Suglia ,  Colette Meinard

Inventor： Jean-Claude Suglia ,  Colette Meinard

IPC: A61K9/64 ,  A01N25/28 ,  A61K9/50 ,  A61K39/12 ,  B01J13/02 ,  B01J13/10 ,  C12N11/04 ,  A61K9/34

CPC classification number: C12N11/04 ,  A01N25/28 ,  A61K9/5047 ,  A61K9/5057 ,  B01J13/10 ,  C12N2710/14051 ,  Y10T428/2984

Abstract: A process for the preparation of stable suspensions and powders of stable microcapsules containing at least one active material having a variable porosity comprising preparing a colloidal solution of equal parts by weight of gelatin and acacia gum with a total concentration of 4 to 6% by weight of the final emulsion, preparing an oil solution, suspension or emulsion of the active material at a concentration of 1 to 5% by weight of the final emulsion and containing a variable amount of organosoluble ethyl hydroxyethylcellulose, mixing the said two compositions with stirring at a temperature near 50.degree. C. in the presence of an emulsifying agent to form an "oil in water" emulsion, effecting consecutively coacervation and microencapsulation of the emulsified droplets containing the active material by adjusting the pH to 4.2 to 4.4 by addition of an acid and then cooling the mixture to about 20.degree. C. with stirring, reticulating the walls of the formed microcapsules by reaction with glutaric aldehyde and tannin with stirring at about 20.degree. C. and either forming a concentrated suspension of microcapsules by slow addition at 20.degree. C. of a water soluble ethyl hydroxyethylcellulose to the eticulated microcapsules or adding an antiagglomeration agent with stirring to the reticulated microcapsules at 20.degree. C. and drying the resulting powder and the microcapsules produced thereby which are stable with respect to physico chemical influences and to exterior elements generally, such as sunlight and temperature changes so that the encapsulated active material maintains its activity.

Abstract translation: 制备稳定的悬浮液和稳定的微胶囊的粉末的方法，所述稳定的微胶囊含有至少一种具有可变孔隙率的活性物质，包括制备等份重量的明胶和阿拉伯树胶的胶体溶液，其总浓度为4至6重量％ 最终乳液，以最终乳液的1至5重量％的浓度制备活性物质的油溶液，悬浮液或乳液，并含有可变量的有机溶剂乙基羟乙基纤维素，在搅拌下将所述两种组合物在温度 在乳化剂存在下接近50℃以形成“水包油”乳液，通过加入酸将pH调节至4.2至4.4，从而连续地凝聚和微囊化包含活性物质的乳化液滴，然后 在搅拌下将混合物冷却至约20℃，通过与戊二烯反应将形成的微胶囊的壁网状化 在约20℃搅拌下，通过在20℃下缓慢加入水溶性乙基羟乙基纤维素形成微胶囊的浓缩悬浮液，并在搅拌下向搅拌下加入抗凝聚剂至网状微胶囊 干燥得到的粉末和由此产生的微胶囊，其相对于物理化学影响是稳定的，并且通常包括阳光和温度变化，从而使包封的活性材料保持其活性。

公开(公告)号：US4253877A

公开(公告)日：1981-03-03

申请号：US62985

申请日：1979-08-02

Applicant: John B. Miale ,  August Miale, Jr. ,  Raymond P. Porter

Inventor： John B. Miale ,  August Miale, Jr. ,  Raymond P. Porter

IPC: A01N25/28 ,  B01J13/10 ,  C09D5/08 ,  C09D5/16

CPC classification number: B01J13/10 ,  C09D5/1631 ,  Y10T428/2984 ,  Y10T428/2989

Abstract: A process for microencapsulating water-immiscible chemicals is disclosed which comprises mixing a colloidal solution of gelatin Type A and gum acacia with an emulsion or slurry of the water-immiscible chemical, both of which are prepared and mixed at a temperature above about 50.degree. C., and allowing the mixture to cool so that the droplets or particles of water-immiscible chemical are encapsulated with a macromolecular membrane of a complex coacervate of gelatin and gum acacia. Anti-fouling marine paints capable of sustained release of anti-fouling agent are prepared by adding microcapsules of anti-fouling agents to a marine paint vehicle.

Abstract translation: 公开了一种用于微胶囊化与水不混溶的化学品的方法，其包括将A型明胶和阿拉伯树胶的胶体溶液与水不混溶化学品的乳液或浆料混合，两者均在约50℃以上的温度下制备和混合 并且使混合物冷却，使得与水不混溶的化学物质的微滴或颗粒用明胶和阿拉伯树胶复合凝聚层的大分子膜包封。 通过向海洋涂料载体中加入防污剂微胶囊制备能够持续释放防污剂的防污水性油漆。

公开(公告)号：US4222891A

公开(公告)日：1980-09-16

申请号：US892318

申请日：1978-03-31

Applicant: Tomoyuki Okimoto ,  Tomoharu Shiozaki ,  Makoto Miyake

Inventor： Tomoyuki Okimoto ,  Tomoharu Shiozaki ,  Makoto Miyake

IPC: B01J13/10 ,  B41M5/165 ,  B01J13/02

CPC classification number: B41M5/165 ,  B01J13/10 ,  Y10S428/914 ,  Y10T428/2984 ,  Y10T428/2987

Abstract: The method of making oil-containing microcapsules comprises the step of (1) preparing an aqueous system comprising an aqueous solution of gelatin and at least one anionic colloid material and oil droplets dispersed in said solution (2) causing coacervation in said aqueous system at a temperature above the gelation point of said gelatin to form a coacervate suspension in which each of said oil droplets is surrounded by a coacervate and (3) cooling said coacervate suspension to a temperature below the gelation points of said gelatin to form multi-nucleus capsules. During the step of cooling the coacervate suspension, aggregation of particles of oil droplets each having a coacervate therearound is controlled by an agitation flow so as to allow formation of multi-nucleus microcapsules having an average diameter within the range of 3 to 20 microns. The gelatin has an average viscosity not larger than 35 millipoise in terms of the value measured by the bloom type pipette method at 40.degree..+-.0.5.degree. C. according to Japan Industrial Standard K 6503 with respect to a 62/3% aqueous solution of said gelatin at the pH of 4.5 and at least 5% by weight of said gelatin has a viscosity not larger than 25 millipoise in said terms and/or the anionic colloid material is a carboxymethylcellulose having a viscosity within the range of 2 to 500 centipoise measured by the Brookfield viscometer with a 60 r.p.m. No. 1 rotor with respect to a 2% aqueous solution of said carboxymethylcellulose at 25.degree. C.

Abstract translation: 制备含油微胶囊的方法包括以下步骤：（1）制备包含明胶水溶液和至少一种阴离子胶体材料的水性体系和分散在所述溶液（2）中的油滴的水性体系，使所述水性体系中的凝聚在 温度高于所述明胶的凝胶化点以形成凝聚层悬浮液，其中每个所述油滴被凝聚层包围，和（3）将所述凝聚层悬浮液冷却至低于所述明胶凝胶点的温度以形成多核胶囊。 在冷却凝聚物悬浮液的步骤期间，通过搅拌流控制每个具有凝聚层的油滴颗粒的聚集，以便形成平均直径在3至20微米范围内的多核微胶囊。 根据日本工业标准K 6503相对于62/3％的水溶液，明胶的平均粘度根据通过花式吸移管法在40℃+/- 0.5℃测量的值不大于35毫泊 的所述明胶，并且所述明胶的至少5重量％的所述明胶具有不大于25毫泊的粘度，和/或阴离子胶体材料是粘度在2至500厘泊范围内的羧甲基纤维素 由Brookfield粘度计用60rpm测量 相对于25℃下所述羧甲基纤维素的2％水溶液为1转子

公开(公告)号：US4115315A

公开(公告)日：1978-09-19

申请号：US769296

申请日：1977-02-16

Applicant: Nicola Marinelli

Inventor： Nicola Marinelli

IPC: A61K9/50 ,  B01J13/10 ,  B01J13/02

CPC classification number: A61K9/50 ,  B01J13/10 ,  Y10T428/2984

Abstract: Minute capsules having a pearlescent effect are obtained by incorporating inorganic pearlescent particles in the capsule walls during the manufacture thereof. Pearlescent particles of mica coated with titanium dioxide are initially dispersed in an oily internal phase material and then flushed into the aqueous coacervation phase upon addition of the internal phase to an encapsulation medium. The pearlescent particles remain embedded in the capsule wall material and provide the pearlescent effect to the finished capsules.

Abstract translation: 通过在其制造过程中将无机珠光颗粒结合在胶囊壁中，获得具有珠光效果的分钟胶囊。 首先将涂覆有二氧化钛的云母颗粒分散在油性内相材料中，然后在将内相加入到包封介质中后冲洗入水凝胶相。 珠光颗粒保持嵌入胶囊壁材料中，并为成品胶囊提供珠光效果。

公开(公告)号：US4010038A

公开(公告)日：1977-03-01

申请号：US563974

申请日：1975-04-01

Applicant: Hiroshi Iwasaki ,  Shunsuke Shioi ,  Jujiro Kouno

Inventor： Hiroshi Iwasaki ,  Shunsuke Shioi ,  Jujiro Kouno

IPC: A01N25/28 ,  A61K49/04 ,  B01J13/10 ,  B41M5/165 ,  C11B9/00 ,  G03C1/00 ,  B01J13/02 ,  C09D11/00

CPC classification number: B01J13/10 ,  B41M5/165 ,  Y10T428/2984 ,  Y10T428/2989

Abstract: In a process for producing microcapsules of complex hydrophilic colloid material enclosing fine particles of a hydrophobic substance, the improvement characterized in that:An acid-treated gelatin and at least one of carboxy-modified cellulose derivatives are used as the hydrophilic colloid materials, the amount of the cellulose derivative being 1/7 to 1/40 the amount of the gelatin by weight, the cellulose derivative having an average polymerization degree of 50 to 1,000 and a carboxyl substitution degree of 0.4 to 1.5, andThe coacervation of the colloid material solution is effected at a pH of 4.8 to 6.0.

Abstract translation: 在生产包含疏水性物质的细颗粒的复合亲水胶体材料微胶囊的方法中，其改进之处在于：

公开(公告)号：US3970585A

公开(公告)日：1976-07-20

申请号：US354050

申请日：1973-04-24

Applicant: Hiroharu Matsukawa ,  Shizuo Katayama ,  Masataka Kiritani

Inventor： Hiroharu Matsukawa ,  Shizuo Katayama ,  Masataka Kiritani

IPC: B01J13/10 ,  B01J13/02

CPC classification number: B01J13/10 ,  Y10T428/2984 ,  Y10T428/2987

Abstract: In a process for preparing oil-containing microcapsules comprising cooling a coacervate dispersion of a gelatin-containing colloid deposited around individual oil droplets to cause gelation of the colloid and subsequently hardening the gelled colloid by adding to the dispersion a hardening agent and adjusting the pH to the alkaline region, the improvement which comprises adding to the dispersion, after gelation but prior to hardening, an aqueous solution of an anionic high molecular weight electrolyte and an aqueous solution of an anionic surface active agent. Specific electrolytes and specific surface active agents are disclosed.

Abstract translation: 在制备含油微胶囊的方法中，包括冷却沉积在各个油滴周围的含凝胶胶体的凝聚分散体，引起胶体凝胶化，随后通过向分散体中加入硬化剂并调节pH至 碱性区域的改进，其包括在凝胶化之后但在硬化之前向阴离子高分子量电解质的水溶液和阴离子表面活性剂的水溶液中加入分散体。 公开了特定的电解质和比表面活性剂。

公开(公告)号：US3803045A

公开(公告)日：1974-04-09

申请号：US16656371

申请日：1971-07-27

Applicant: FUJI PHOTO FILM CO LTD

IPC: A61K8/11 ,  A61K9/50 ,  A61Q13/00 ,  B01J13/10 ,  B01J13/02 ,  B44D1/44

CPC classification number: A61K8/11 ,  A61K9/50 ,  A61K2800/412 ,  A61Q13/00 ,  B01J13/10 ,  Y10T428/2984 ,  Y10T428/2987

Abstract: In a process for producing oil-containing microcapsules by coacervation comprising A. INTRODUCING A FINE POWDER OR HYDROPHOBIC LIQUID INTO A HIGH MOLECULAR WEIGHT ELECTROLYTIC WALL-FORMING COLLOID; B. COACERVATING THE RESULTING DISPERSION OR EMULSION; C. COOLING THE RESULTING COACERVATE TO GEL IT AND FORM THE WALL OF SAID MICROCAPSULES; AND D. HARDENING SAID WALL OF SAID MICROCAPSULES; THE IMPROVEMENT WHICH COMPRISES ADDING A PHENOLIC COMPOUND TO THE SYSTEM AT A TEMPERATURE ABOVE 8* C., during steps B) and C), said phenolic compound being present in an amount ranging from 1/500 to 3/4 parts by weight based on one part by weight of colloid used to form the capsule wall.

公开(公告)号：US3791987A

公开(公告)日：1974-02-12

申请号：US3791987D

申请日：1972-02-03

Applicant: NCR

Inventor： FANGER G

IPC: B01J13/10 ,  B01J13/02 ,  B44D1/02

CPC classification number: B01J13/10 ,  Y10T428/2984 ,  Y10T428/2989

Abstract: A PROCESS IS DISCLOSED FOR MANUFACTURING MINUTE CAPSULES, EN MASSE, WHEREIN THE CAPSULE WALLS COMPRISE A HARDENED SILICATE MATERIAL. THE PROCESS INCLUDES LIQUIDLIQUID PHASE SEPARATION OF THE WALL MATERIAL SILICATE FROM SOLUTION AS SILICIC ACID IN AN AQUEOUS CAPSUL MANUFACTURING VEHICLE BY MEANS OF A GLYCOL PHASE-SEPARATION-INDUCING MATERIAL. PREFERRED STARTING MATERIALS FOR THE PRESENT PROCESS INCLUDE ALKALI-METAL WATER GLASS AND POLYETHYLENE GLYCOL, THE PRESENT LIQUID-LIQUID PHASE SEPARATION CAN BE CONSIDERED TO BE SIMILAR TO SO-CALLED "COMPLEX COACERVATION" OF THE PRIOR ART IN THAT A COMPLEX OF TWO POLYMERIC MATERIALS ARE CONCENTRATED IN THE EMERGENT LIQUID PHASE. THE CAPSULE WALLS ARE SOLIDIFIED BY REACTING THE SILCEOUS CAPSULE WALL MATERIAL WITH AN INORGANIC SALT, VIZ, ALUMINUM SULFATE, CALCIUM CHLORIDE, MAGNESIUM SULFATE, IRON CHLORIDE OR MAGNESIUM BROMIDE.

公开(公告)号：US3712867A

公开(公告)日：1973-01-23

申请号：US3712867D

申请日：1971-02-17

Applicant: BAYER AG

Inventor： SCHON N ,  PAMPUS G ,  SCHNORING H ,  WITTE J

IPC: B01J13/10 ,  B01J13/02 ,  B44D1/02

CPC classification number: B01J13/10 ,  Y10T428/2987 ,  Y10T428/2989

Abstract: A PROCESS FOR THE PRODUCTION OF MICROCAPSULES WITH COACERVATES OF SYNTHETIC POLYMERS AS SHELL SUBSTANCES, WHEREIN THE SOLID OR LIQUID CORE MATERIAL TO BE ENCAPSULATED IS DISPERSED IN AN AQUOUS SOLUTION OF A THERMOREVERSIBLE COACERATIVE COPOLYMER OF 70 TO 30 MOL PERCENT OF THE ACRYLIC ACID AND 30 TO 70 MOL PERCENT OF ACRYLAMIDE AT A TEMPERATURE ABOVE THE COACERVATE TRANSITION TEMPERATURE, THE RESULTING DISPERSION IS COOLED TO BELOW THE COACERVATE TRANSITION TEMPERATURE, THE COACERVATE FORMED IS DEPOSITED ONTO THE DISPERSED PARTICLES, IS OPTIONALLY CHEMICALLY CROSSLINKED, AND THE MICROCAPSULES OBTAINED ARE SEPARATED OFF AND DRIED.

公开(公告)号：US3692690A

公开(公告)日：1972-09-19

申请号：US3692690D

申请日：1970-05-27

Applicant: NCR CO

Inventor： HORGER GEORG

IPC: A61K9/50 ,  B01J13/10 ,  A61K9/04 ,  B01J13/02 ,  B44D1/02

CPC classification number: B01J13/10 ,  A61K9/50 ,  Y10T428/2984 ,  Y10T428/2987 ,  Y10T428/2989

Abstract: A PROCESS IS DISCLOSED FOR MANUFACTURING CAPSULES, EN MASSE, BY USE OF A LIQUID-LIQUID PHASE SEPARATION WHICH INCLUDES POLYSILICATE INORGANIC MATERIAL AS A COMPLEXING, PHASE-SEPARATION-INDUCING, POLYMER. THE DISCLOSED PROCESS IN CONDUCTED IN AN AQUEOUS CAPSULE MANUFACTURING VEHICLE AND THE MATERIAL WHICH EMERGES AS A LIQUID PHASE IS AN AQUEOUS SOLUTION OF ORGANIC HYDROPHILIC POLYMERIC MATERIAL AND INORGANIC POLYSILICATE MATERIAL. THE LIQUID-LIQUID PHASE SEPARATION OF THIS INVENTION IS THE TYPE GENERALLY NAMED "COMPLEX" COACERVATION WHEREIN THE SEPARATED, EMERGENT, LIQUID PHASE INCLUDES A MAJOR PORTION OF BOTH, THE ORGANIC HYDROPHILIC POLYMERIC MATERIAL AND THE PHASESEPARATION-INDUCING MATERIAL;-IN THIS INVENTION POLYSILICATE POLYMERIC MATERIAL. THE ORGANIC POLYMERIC MATERIAL AND THE INORGANIC POLYMERIC MATERIAL ARE COMPLEXED TOGETHER BY VIRTUE OF OPPOSITE ELECTRICAL CHARGES, THE COMPLEX IS LEAST PARTIALLY IMMISCIBLE WITH THE MANUFACTURING VEHICLE, AND THE MANUFACTURING VEHICLE CONTAINS ONLY A MINOR AMOUNT OF EITHER POLYMERIC MATERIAL. PREFERRED MATERIALS FOR USE IN PRACTICING THE PRESENT INVENTION INCLUDE GELATIN AS THE ORGANIC HYDROPHILIC POLYMERIC MATERIAL AND POLYSILICATES AS THE INORGANIC POLYMERIC PHASE-SEPARATIONINDUCING MATERIAL.