JPH01293128A - Granulating method - Google Patents
Granulating methodInfo
- Publication number
- JPH01293128A JPH01293128A JP12290588A JP12290588A JPH01293128A JP H01293128 A JPH01293128 A JP H01293128A JP 12290588 A JP12290588 A JP 12290588A JP 12290588 A JP12290588 A JP 12290588A JP H01293128 A JPH01293128 A JP H01293128A
- Authority
- JP
- Japan
- Prior art keywords
- freeze
- soln
- liquid
- granulated
- nonhydrated
- 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
Links
- 238000000034 method Methods 0.000 title claims description 18
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 239000011230 binding agent Substances 0.000 claims abstract description 10
- 238000005469 granulation Methods 0.000 claims abstract description 9
- 230000003179 granulation Effects 0.000 claims abstract description 9
- 239000008187 granular material Substances 0.000 claims description 25
- 239000004615 ingredient Substances 0.000 claims description 13
- 239000007864 aqueous solution Substances 0.000 claims description 11
- 239000000546 pharmaceutical excipient Substances 0.000 claims description 9
- 238000009777 vacuum freeze-drying Methods 0.000 claims description 8
- 238000007710 freezing Methods 0.000 claims description 2
- 230000008014 freezing Effects 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 18
- 239000000203 mixture Substances 0.000 abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 12
- 239000000126 substance Substances 0.000 abstract description 9
- 229920002472 Starch Polymers 0.000 abstract description 4
- 238000009472 formulation Methods 0.000 abstract description 4
- 239000008107 starch Substances 0.000 abstract description 4
- 235000019698 starch Nutrition 0.000 abstract description 4
- 239000003905 agrochemical Substances 0.000 abstract description 3
- 239000000284 extract Substances 0.000 abstract description 3
- 238000004040 coloring Methods 0.000 abstract description 2
- 239000003350 kerosene Substances 0.000 abstract description 2
- 239000004094 surface-active agent Substances 0.000 abstract description 2
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 238000004108 freeze drying Methods 0.000 abstract 1
- 238000007493 shaping process Methods 0.000 abstract 1
- -1 alkalis Substances 0.000 description 9
- 239000000843 powder Substances 0.000 description 9
- 239000004375 Dextrin Substances 0.000 description 6
- 229920001353 Dextrin Polymers 0.000 description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 6
- 244000269722 Thea sinensis Species 0.000 description 5
- 235000019425 dextrin Nutrition 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000007796 conventional method Methods 0.000 description 4
- 239000003921 oil Substances 0.000 description 4
- 235000019198 oils Nutrition 0.000 description 4
- 244000215068 Acacia senegal Species 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 229920000084 Gum arabic Polymers 0.000 description 3
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 235000010489 acacia gum Nutrition 0.000 description 3
- 239000000205 acacia gum Substances 0.000 description 3
- 238000009835 boiling Methods 0.000 description 3
- 239000001913 cellulose Substances 0.000 description 3
- 229920002678 cellulose Polymers 0.000 description 3
- 235000010980 cellulose Nutrition 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 235000013616 tea Nutrition 0.000 description 3
- MIDXCONKKJTLDX-UHFFFAOYSA-N 3,5-dimethylcyclopentane-1,2-dione Chemical compound CC1CC(C)C(=O)C1=O MIDXCONKKJTLDX-UHFFFAOYSA-N 0.000 description 2
- 239000005995 Aluminium silicate Substances 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- 241001465754 Metazoa Species 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- 235000006468 Thea sinensis Nutrition 0.000 description 2
- FPIPGXGPPPQFEQ-OVSJKPMPSA-N all-trans-retinol Chemical compound OC\C=C(/C)\C=C\C=C(/C)\C=C\C1=C(C)CCCC1(C)C FPIPGXGPPPQFEQ-OVSJKPMPSA-N 0.000 description 2
- 235000012211 aluminium silicate Nutrition 0.000 description 2
- 239000010775 animal oil Substances 0.000 description 2
- 235000020279 black tea Nutrition 0.000 description 2
- DIKBFYAXUHHXCS-UHFFFAOYSA-N bromoform Chemical compound BrC(Br)Br DIKBFYAXUHHXCS-UHFFFAOYSA-N 0.000 description 2
- 235000013736 caramel Nutrition 0.000 description 2
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 239000003086 colorant Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- 230000002265 prevention Effects 0.000 description 2
- 239000012798 spherical particle Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000011550 stock solution Substances 0.000 description 2
- 235000015112 vegetable and seed oil Nutrition 0.000 description 2
- 239000008158 vegetable oil Substances 0.000 description 2
- 238000009423 ventilation Methods 0.000 description 2
- SCYULBFZEHDVBN-UHFFFAOYSA-N 1,1-Dichloroethane Chemical compound CC(Cl)Cl SCYULBFZEHDVBN-UHFFFAOYSA-N 0.000 description 1
- HMUNWXXNJPVALC-UHFFFAOYSA-N 1-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical group C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)C(CN1CC2=C(CC1)NN=N2)=O HMUNWXXNJPVALC-UHFFFAOYSA-N 0.000 description 1
- RZRNAYUHWVFMIP-KTKRTIGZSA-N 1-oleoylglycerol Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OCC(O)CO RZRNAYUHWVFMIP-KTKRTIGZSA-N 0.000 description 1
- IIZPXYDJLKNOIY-JXPKJXOSSA-N 1-palmitoyl-2-arachidonoyl-sn-glycero-3-phosphocholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCC\C=C/C\C=C/C\C=C/C\C=C/CCCCC IIZPXYDJLKNOIY-JXPKJXOSSA-N 0.000 description 1
- FHVDTGUDJYJELY-UHFFFAOYSA-N 6-{[2-carboxy-4,5-dihydroxy-6-(phosphanyloxy)oxan-3-yl]oxy}-4,5-dihydroxy-3-phosphanyloxane-2-carboxylic acid Chemical compound O1C(C(O)=O)C(P)C(O)C(O)C1OC1C(C(O)=O)OC(OP)C(O)C1O FHVDTGUDJYJELY-UHFFFAOYSA-N 0.000 description 1
- 229920001817 Agar Polymers 0.000 description 1
- WSVLPVUVIUVCRA-KPKNDVKVSA-N Alpha-lactose monohydrate Chemical compound O.O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H](CO)O[C@H](O)[C@H](O)[C@H]1O WSVLPVUVIUVCRA-KPKNDVKVSA-N 0.000 description 1
- 229920001342 Bakelite® Polymers 0.000 description 1
- 239000004604 Blowing Agent Substances 0.000 description 1
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 1
- 102000011632 Caseins Human genes 0.000 description 1
- 108010076119 Caseins Proteins 0.000 description 1
- 244000302899 Cassia mimosoides Species 0.000 description 1
- 235000014112 Cassia mimosoides Nutrition 0.000 description 1
- 229920002101 Chitin Polymers 0.000 description 1
- 229920001661 Chitosan Polymers 0.000 description 1
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 description 1
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 1
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- 240000002989 Euphorbia neriifolia Species 0.000 description 1
- 108010010803 Gelatin Proteins 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 229920002907 Guar gum Polymers 0.000 description 1
- 240000005979 Hordeum vulgare Species 0.000 description 1
- 235000007340 Hordeum vulgare Nutrition 0.000 description 1
- 241000519695 Ilex integra Species 0.000 description 1
- GUBGYTABKSRVRQ-QKKXKWKRSA-N Lactose Natural products OC[C@H]1O[C@@H](O[C@H]2[C@H](O)[C@@H](O)C(O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@H]1O GUBGYTABKSRVRQ-QKKXKWKRSA-N 0.000 description 1
- 229920000161 Locust bean gum Polymers 0.000 description 1
- CYTYCFOTNPOANT-UHFFFAOYSA-N Perchloroethylene Chemical group ClC(Cl)=C(Cl)Cl CYTYCFOTNPOANT-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- 240000004584 Tamarindus indica Species 0.000 description 1
- 235000004298 Tamarindus indica Nutrition 0.000 description 1
- 235000009470 Theobroma cacao Nutrition 0.000 description 1
- 244000299461 Theobroma cacao Species 0.000 description 1
- 229920001615 Tragacanth Polymers 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000008272 agar Substances 0.000 description 1
- 229940023476 agar Drugs 0.000 description 1
- 235000010419 agar Nutrition 0.000 description 1
- 229940072056 alginate Drugs 0.000 description 1
- 235000010443 alginic acid Nutrition 0.000 description 1
- 229920000615 alginic acid Polymers 0.000 description 1
- 239000011717 all-trans-retinol Substances 0.000 description 1
- 235000019169 all-trans-retinol Nutrition 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 239000000305 astragalus gummifer gum Substances 0.000 description 1
- 239000004637 bakelite Substances 0.000 description 1
- 239000000440 bentonite Substances 0.000 description 1
- 229910000278 bentonite Inorganic materials 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 229950005228 bromoform Drugs 0.000 description 1
- 239000001273 butane Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 235000010418 carrageenan Nutrition 0.000 description 1
- 239000000679 carrageenan Substances 0.000 description 1
- 229920001525 carrageenan Polymers 0.000 description 1
- 229940113118 carrageenan Drugs 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 235000008504 concentrate Nutrition 0.000 description 1
- CYKLGTUKGYURDP-UHFFFAOYSA-L copper;hydrogen sulfate;hydroxide Chemical compound O.[Cu+2].[O-]S([O-])(=O)=O CYKLGTUKGYURDP-UHFFFAOYSA-L 0.000 description 1
- 238000004925 denaturation Methods 0.000 description 1
- 230000036425 denaturation Effects 0.000 description 1
- 150000005690 diesters Chemical class 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000003925 fat Substances 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 210000003746 feather Anatomy 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 230000037406 food intake Effects 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 238000009483 freeze granulation Methods 0.000 description 1
- 235000011389 fruit/vegetable juice Nutrition 0.000 description 1
- 230000000855 fungicidal effect Effects 0.000 description 1
- 239000000417 fungicide Substances 0.000 description 1
- 239000008273 gelatin Substances 0.000 description 1
- 229920000159 gelatin Polymers 0.000 description 1
- 235000019322 gelatine Nutrition 0.000 description 1
- 235000011852 gelatine desserts Nutrition 0.000 description 1
- 235000020710 ginseng extract Nutrition 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 235000009569 green tea Nutrition 0.000 description 1
- 235000010417 guar gum Nutrition 0.000 description 1
- 239000000665 guar gum Substances 0.000 description 1
- 229960002154 guar gum Drugs 0.000 description 1
- 150000005826 halohydrocarbons Chemical class 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000008101 lactose Substances 0.000 description 1
- 229960001375 lactose Drugs 0.000 description 1
- 229960001021 lactose monohydrate Drugs 0.000 description 1
- 235000010445 lecithin Nutrition 0.000 description 1
- 239000000787 lecithin Substances 0.000 description 1
- 229940067606 lecithin Drugs 0.000 description 1
- 235000021388 linseed oil Nutrition 0.000 description 1
- 239000000944 linseed oil Substances 0.000 description 1
- 239000003915 liquefied petroleum gas Substances 0.000 description 1
- 235000010420 locust bean gum Nutrition 0.000 description 1
- 239000000711 locust bean gum Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- 235000014593 oils and fats Nutrition 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000000825 pharmaceutical preparation Substances 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 229940088417 precipitated calcium carbonate Drugs 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 229940080237 sodium caseinate Drugs 0.000 description 1
- 235000014214 soft drink Nutrition 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000600 sorbitol Substances 0.000 description 1
- 235000010356 sorbitol Nutrition 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- 235000000346 sugar Nutrition 0.000 description 1
- 150000008163 sugars Chemical class 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 239000006188 syrup Substances 0.000 description 1
- 235000020357 syrup Nutrition 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 239000003784 tall oil Substances 0.000 description 1
- 235000010491 tara gum Nutrition 0.000 description 1
- 239000000213 tara gum Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 150000003626 triacylglycerols Chemical class 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 239000000341 volatile oil Substances 0.000 description 1
- 239000001993 wax Substances 0.000 description 1
- 229920001285 xanthan gum Polymers 0.000 description 1
- 235000010493 xanthan gum Nutrition 0.000 description 1
- 239000000230 xanthan gum Substances 0.000 description 1
- 229940082509 xanthan gum Drugs 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
- 150000003751 zinc Chemical class 0.000 description 1
- UHVMMEOXYDMDKI-JKYCWFKZSA-L zinc;1-(5-cyanopyridin-2-yl)-3-[(1s,2s)-2-(6-fluoro-2-hydroxy-3-propanoylphenyl)cyclopropyl]urea;diacetate Chemical compound [Zn+2].CC([O-])=O.CC([O-])=O.CCC(=O)C1=CC=C(F)C([C@H]2[C@H](C2)NC(=O)NC=2N=CC(=CC=2)C#N)=C1O UHVMMEOXYDMDKI-JKYCWFKZSA-L 0.000 description 1
Abstract
Description
【発明の詳細な説明】
イ８発明の利用分野
本発明は、医薬、農薬、各種の化成品の製剤分野、なら
びに食品の製剤分野において利用しうる。DETAILED DESCRIPTION OF THE INVENTION A.8 Field of Application of the Invention The present invention can be utilized in the field of pharmaceutical, agrochemical, and various chemical product formulations, as well as the food formulation field.
口、従来の技術
従来、有用成分を含む製剤の粒状物の造粒方法にはいく
つかのものが知られている。BACKGROUND OF THE INVENTION Conventionally, several methods are known for granulating granules of pharmaceutical preparations containing useful ingredients.
■湿式不定形造粒乾燥法
有用成分と賦形剤もしくは結着剤の粉状混合物に水等の
溶媒を散布しつつ１通風しながら乾燥し。■Wet amorphous granulation drying method A powder mixture of useful ingredients and excipients or binders is sprayed with a solvent such as water and dried with ventilation.
湿潤状態で凝集した小塊を転勤状態下で造粒する方法で
ある。This is a method in which small agglomerated agglomerates in a wet state are granulated under transfer conditions.
この場合には生成粒子の形状は不定形であるとともに、
かなり広い粒度分布を有する。In this case, the shape of the generated particles is amorphous, and
It has a fairly wide particle size distribution.
（５）噴霧乾燥造粒法
有用成分と賦形剤もしくは結着剤を含む水溶液を熱風中
に噴霧して乾燥造粒する方法である。(5) Spray-drying granulation method This is a method in which an aqueous solution containing useful ingredients and excipients or binders is sprayed into hot air and dried and granulated.
生成する粒子は０．２羽以下の微粒子であり、広範囲の
粒度分布を有する。The particles produced are fine particles of 0.2 feathers or less and have a wide range of particle size distribution.
０凍結解砕−真空凍結乾燥法
有用成分と賦形剤もしくは結着剤を含む塊状の凍結物を
解砕し、所望の大きさの粒状物を分級して収集し、真空
凍結乾燥する方法である。0 Freeze-Thaw - Vacuum Freeze-Drying A method in which frozen blocks containing useful ingredients and excipients or binders are thawed, granules of desired size are classified and collected, and then vacuum freeze-dried. be.
生成する粒子は不定形である。The particles produced are amorphous.
（ＩＩＰ（Ｃ）の変法であり、型中に原液を型中に流し
こみ。(This is a modified method of IIP (C), in which the stock solution is poured into a mold.
凍結成形してから真空凍結乾燥する方法である。This method involves freeze-molding and then vacuum freeze-drying.
生成する粒子は定形であるが２多数の型を用意する必要
があり、型の製作、清掃等にコストが多くかかり、能率
的な方法とは言い難い。また１球状物を得ることは困難
である。Although the particles produced are of regular shape, it is necessary to prepare two molds, and the manufacturing and cleaning of the molds is costly, so it cannot be said to be an efficient method. Moreover, it is difficult to obtain a single spherical object.
■押し出し造粒法
有用成分、賦形材もしくは結着剤を含む高粘度の溶液、
もしくは線状物を細いノズルより押し出し、一定長さに
切断して通風乾燥して成形する方法である。■Extrusion granulation method A high viscosity solution containing useful ingredients, excipients or binders,
Alternatively, a linear material is extruded through a thin nozzle, cut to a certain length, and dried through ventilation to form the material.
生成する粒子はベレット状であり、生成する粒子は即溶
性に乏しい。The particles produced are pellet-shaped and have poor immediate solubility.
［Ｆ］打錠法
有用成分、賦形剤もしくは結着剤の混合粉体を型中に入
れて高圧にて打錠成形するものである。[F] Tableting method A mixed powder of useful ingredients, excipients, or binders is placed in a mold and compressed into tablets under high pressure.
本性では型が多数必要であること、生成する粒状物は高
密度で即溶性に乏しい等の難点がある。In nature, there are drawbacks such as the need for a large number of molds, and the granules produced are highly dense and have poor immediate solubility.
％ｉ′発明の解決すべき課題
本発明の目的は、型を用いることなく、能率的に、一定
の形状を有し、かつ、高い即溶性を有する粒状物を製造
する方法を提供せんとするものである。%i' Problems to be Solved by the Invention An object of the present invention is to provide a method for efficiently producing granules having a constant shape and high immediate solubility without using a mold. It is something.
今日２造粒による製剤化は医薬、農薬、各種化成品２食
品の分野において。Today, formulations using granulation are used in the fields of pharmaceuticals, agrochemicals, and various chemical products.
■取り扱い性（計量、吸湿防止、流動性、包装性溶解時
のまま粉発生防止等）の向上。■Improved handling (measurement, prevention of moisture absorption, fluidity, packaging ability, prevention of powder generation during dissolution, etc.).
の）外観の向上。) Improved appearance.
（ｑ使用時の溶解性の調整。(Adjustment of solubility when using q.
等を目的として広く利用されている。It is widely used for such purposes.
本発明者は球状、もしくはそれに近似する一定の粒度（
形状と粒径）の分布のそろった゛、即溶性を有する粒状
物を能率よく製造する方法を探索。The present inventor has determined that the particle size is spherical or has a certain particle size (approximately spherical).
We are exploring ways to efficiently produce granular materials with a uniform distribution (shape and particle size) and immediate solubility.
検討し本発明に到達した。After much research, we arrived at the present invention.
二１発明の構成 本発明は以下の工程を結合して構成されるものである。21 Composition of the invention The present invention is constructed by combining the following steps.
■有用成分と、必要ならば賦形剤あるいは結着剤を含む
水溶液を、その水溶液が凍結固化するに充分な低温に保
持されｔ：非水和性の液体ｌ１ｌｌｌｉこ滴化し。(2) An aqueous solution containing the useful ingredients and, if necessary, an excipient or binder, is kept at a low enough temperature to freeze and solidify the aqueous solution, and the aqueous solution is reduced to a non-hydratable liquid.
凍結造粒する工程。Freeze granulation process.
■かくして得られた凍結造粒物を非水和性の液体より分
別する工程。■The step of separating the thus obtained frozen granules from non-hydratable liquids.
（Ｃ）分別された凍結造粒物を真空凍結乾燥する工程。(C) A step of vacuum freeze-drying the separated frozen granules.
以下に、（８）、＠、（Ｃ）の各工程を詳説したい。Below, I would like to explain each step (8), @, and (C) in detail.
■滴下・凍結造粒工程
有用成分としては２例えば医薬（合成品、天然抽出品）
、農薬、各種の化成品２種々のエキス類。■Dripping/freezing granulation process Useful ingredients include 2, such as pharmaceuticals (synthetic products, natural extracts)
, pesticides, various chemical products, 2 various extracts.
色素類、飲料（コーヒー、茶類（日本茶（緑茶。Colors, beverages (coffee, teas (Japanese tea (green tea).
番茶、麦茶、はうじ茶等）、紅茶、プアール茶。(bancha, barley tea, haujicha, etc.), black tea, puerh tea.
ココア、ジュース類２清涼飲料類等）等の種々のものを
あげうる。Cocoa, juices, soft drinks, etc.).
有用成分としては人体への摂取を目的とするもののみな
らず、屋内、屋外への散布、化成品製品の使用時に添加
等を目的として使用されるものをも含む。Useful ingredients include not only those intended for ingestion into the human body, but also those used for purposes such as spraying indoors and outdoors, and adding when using chemical products.
有用成分は必ずしも水に溶解するものである必要はなく
、不溶性のものでも懸濁、ないしは乳化の状態で本発明
に供することができる。The useful components do not necessarily have to be soluble in water, and even insoluble components can be used in the present invention in a suspended or emulsified state.
有用成分を水溶液（場合により懸濁、あるいは乳化）と
する際に、溶解助剤（例えば界面性剤。A solubilizing agent (for example, a surfactant) is used when useful ingredients are made into an aqueous solution (suspended or emulsified as the case may be).
酸、アルカリ、キレート剤、塩類、ＰＨ調整剤等）。acids, alkalis, chelating agents, salts, PH adjusters, etc.).
香料２色部、賦形剤（例えば鉱物粉末（ベントナイト、
ケイソウ上、カオリン、タルク、ゼオライト、シリカゲ
ル等）２合成樹脂床（ポリスチレン。Fragrance two colors, excipients (e.g. mineral powders (bentonite,
2 synthetic resin beds (polystyrene, kaolin, talc, zeolite, silica gel, etc.)
ポリエチレン、ポリプロピレン、ベークライト等）天然
高分子（キトサン、キチン、でん粉、ゼラチン、セルロ
ーズ、パルプ、多糖類（アラビアガム。polyethylene, polypropylene, Bakelite, etc.) natural polymers (chitosan, chitin, starch, gelatin, cellulose, pulp, polysaccharides (gum arabic).
キサンタンガム、グアガム、タラガム、寒天、アルギネ
ート、トラガントガム、フルセラン、カラギナン、ロー
カストビーンガム、タマリンドガム等）））、 結着剤
（ポリビニアルコールとその誘導体。xanthan gum, guar gum, tara gum, agar, alginate, tragacanth gum, furceran, carrageenan, locust bean gum, tamarind gum, etc.)), binders (polyvinyl alcohol and its derivatives).
セルロースのカルボキシアルキルエーテル類、各種のガ
ム類、カゼインナトリウム等、糖類（乳糖２デキストリ
ン、可溶性でんぷん、水あめ、グルコース等））等を添
加することができる。Carboxyalkyl ethers of cellulose, various gums, sodium caseinate, sugars (lactose 2-dextrin, soluble starch, starch syrup, glucose, etc.), etc. can be added.
有用成分単体でも真空凍結乾燥後の粒状物の保形性を維
持しうる場合もあるが（例えば後の実施例４に示したカ
ラメル）、多くの場合粒状構造を使用時までの取扱いに
おいて維持するためには賦形剤もしくは結着剤の添加が
必要なことが多い。Although there are cases where the useful ingredient alone can maintain the shape retention of granules after vacuum freeze-drying (for example, the caramel shown in Example 4 below), in many cases the granular structure is maintained during handling until use. This often requires the addition of excipients or binders.
粒状物の溶解性を調整するために油脂類（各種の動植物
油類、レシチン類、グリセリン七）、あるいはジエステ
ル類、ワックス類、トール油、硫酸化油類等）２発泡剤
（炭酸塩類９重炭酸塩類等）。To adjust the solubility of granules, oils (various animal and vegetable oils, lecithin, glycerin), diesters, waxes, tall oil, sulfated oils, etc.), blowing agents (carbonates, etc.) carbonates, etc.).
結晶性セルロースの微粉等を添加してもよい。Fine powder of crystalline cellulose or the like may be added.
水溶液を調製するにあたっては適宜、加熱、かる場合に
は適宜に加温して用いることもできる。When preparing an aqueous solution, it can be heated as appropriate, and in some cases, it can be heated appropriately before use.
非水和性の液体としては１例えば炭化水素類（灯油、軽
油、揮発油、ｎ−ヘキサン、ペンタン、ブタン、液化石
油ガス、トルエン等）、ハロ炭化水素類（クロロホルム
、ブロモホルム、ジクロルメタン、ジクロルエタン、パ
ークロルエチレン、フロン類等）、エーテル類、エステ
ル類、ケトン類。Examples of non-hydratable liquids include hydrocarbons (kerosene, light oil, volatile oil, n-hexane, pentane, butane, liquefied petroleum gas, toluene, etc.), halohydrocarbons (chloroform, bromoform, dichloromethane, dichloroethane, perchloroethylene, fluorocarbons, etc.), ethers, esters, ketones.
油脂類（動植物油２合成トリグリセリド類）、液化ガス
類（液化チッ素、液化エタン、液体空気。Oils and fats (animal and vegetable oils, 2 synthetic triglycerides), liquefied gases (liquefied nitrogen, liquefied ethane, liquid air).
液体炭酸ガス等）等の単一、あるいは任意の混合溶媒を
用いればよい。A single solvent such as liquid carbon dioxide gas, etc., or any mixed solvent may be used.
非水相性の液体は滴下する水溶液の固化温度よりも低く
保持し、所望によってはゆるくがくはんしておく。The non-aqueous liquid is maintained at a temperature lower than the solidification temperature of the aqueous solution to be added dropwise, and is slightly stirred if desired.
滴下された水溶液は表面張力によって球状に近い形状に
成形されるが、非水和性の溶媒の温度が極端に低い場合
には成形の行なわれる前に凍結固化するので、液体の深
さに応じて温度匂配を持たせ、上層はやや高い温度にし
ておくこともできる。The dropped aqueous solution is formed into a nearly spherical shape due to surface tension, but if the temperature of the non-hydratable solvent is extremely low, it freezes and solidifies before forming. It is also possible to create a temperature gradient by keeping the upper layer at a slightly higher temperature.
滴下はノズルより吐出することにより行なわれ。Dripping is performed by discharging from a nozzle.
ノズルの口径、形状、水溶液の粘度を変えることにより
粒状物の粒径を変えることができる。The particle size of the granular material can be changed by changing the diameter and shape of the nozzle and the viscosity of the aqueous solution.
■凍結粒状物と非水和性の液体との分別工程口過、ある
いは非水相性の液体を蒸発させることにより容易に両者
を分別しうろ。非水和性の液体が高沸点の場合には１口
過後、凍結粒状物を低沸点の溶媒にて洗えばよい。■Separation process of frozen granules and non-hydratable liquid The two can be easily separated by filtration or by evaporating the non-aqueous liquid. If the non-hydratable liquid has a high boiling point, the frozen granules may be washed with a low boiling point solvent after one sip.
０真空凍結乾燥工程
凍結粒状物を常法に従って回分式、あるいは連続式の真
空凍結乾燥に付する。すなわち、 １Ｔｏｒｒ以下、好
ましくは０．５ Ｔｏｒｒ以下の高真空下に数時間〜数
十時間程度、適宜たな加熱を行ないつつ。0 Vacuum freeze-drying process The frozen granules are subjected to batch or continuous vacuum freeze-drying according to a conventional method. That is, while performing appropriate heating under a high vacuum of 1 Torr or less, preferably 0.5 Torr or less, for several hours to several tens of hours.
水分率５％以下程度にまで乾燥する。Dry to a moisture content of 5% or less.
以上のような工程に従って本発明は実施されるが２所望
により、得られる粒状物に着色、コーティング、抗酸化
処理等をさらに施してもよい。The present invention is carried out according to the steps described above, but if desired, the resulting granules may be further subjected to coloring, coating, anti-oxidation treatment, etc.
ホ１発明の効果
本発明を実施する場合には、従来の造粒方法では得られ
なかった次のような効果が得られる。E1 Effects of the Invention When the present invention is carried out, the following effects that cannot be obtained with conventional granulation methods can be obtained.
（ハ）粒状物の形状２粒径がよくそろう。（計量性。(c) Shape of the granules: 2 particle sizes are well aligned. (Metricability.
流動性、包装性の制御が容易である。）■粒径の変更が
容易である。（粒径毎に多数の型を用意しなくてもよい
。）
０型を使用しなくてすむので、型の清掃、製作等に要す
る費用が不要である。）
◎真空凍結Ｉ乾燥により乾燥されるので得られる粒状物
は多孔質で水に対する即溶性があり、有用成分は熱変性
を受けない。Easy to control fluidity and packaging. )■ Particle size can be easily changed. (There is no need to prepare a large number of molds for each particle size.) Since it is not necessary to use mold 0, there is no need to spend money on mold cleaning, manufacturing, etc. ) Since it is dried by vacuum freeze-drying, the resulting granules are porous and immediately soluble in water, and the useful ingredients are not subject to thermal denaturation.
へ、実施例
実施例１１シ
せんぶり抽出液の濃縮物（９７，２）にデキストリン（
「パインデックス嵐１」（松谷化学工業■）１０°Ｃに
冷却し、内径３＋ｗ、外径５朋のガラス管より一３０°
Ｃ±３°Ｃに冷却した深さ５０αの静かにかくはんした
ｎ−ヘキサン中に静かに滴下し、 ５００ｇを造粒した
。Examples Example 11 Dextrin (
"Pindex Arashi 1" (Matsuya Chemical Industry ■) Cooled to 10°C, 130° from a glass tube with an inner diameter of 3 + W and an outer diameter of 5 mm.
It was gently dropped into gently stirred n-hexane cooled to ±3°C to a depth of 50α to granulate 500g.
造粒物を金網にて口取し、トレーもすして常法により回
分式の真空凍結乾燥し、 １０２ｇの直径３．０〜３
，３朋の略球状の造粒品を得た。The granules were taken out with a wire mesh, the tray was also drained, and the granules were vacuum freeze-dried in batches using a conventional method to obtain 102 g of 3.0-3.0 g in diameter.
, 3 approximately spherical granules were obtained.
実施例２６□
高麗人参抽出液の濃縮物（餅４．８ ）にシヨ糖脂肪酸
エステル帆４％を加え、デキストリン、乳糖１水和物、
アラビアガムの８：２１の混合物をｘ
加温かくはん下に溶解し、Ｅｍ１７．９とした。１０″
Ｃに冷却し、内径１ｍ、外径１．５＊＊のガラス管より
。Example 26□ 4% sucrose fatty acid ester was added to a concentrate of ginseng extract (Mochi 4.8), and dextrin, lactose monohydrate,
An 8:21 mixture of gum arabic was dissolved under x heating to give Em 17.9. 10″
from a glass tube with an inner diameter of 1 m and an outer diameter of 1.5**.
−３０°Ｃ±３°Ｃに冷却した酢酸エチル、ｎ−ヘキサ
ンの１”ｌ混合液中に滴下造粒した。The mixture was dropped and granulated into a 1"l mixture of ethyl acetate and n-hexane cooled to -30°C±3°C.
口取し、常法によって真空凍結乾燥し、直径１．８絹の
略球状の粒子を得た。原液１ｋｇより１５３ｇの粒状物
を得た。The sample was sampled and vacuum freeze-dried using a conventional method to obtain approximately spherical particles with a diameter of 1.8 silk. 153 g of granules were obtained from 1 kg of the stock solution.
このものは、実施例１の粒状物同様に６０°Ｃの水に対
し１０秒程度で溶解した。Like the granules in Example 1, this product dissolved in water at 60°C in about 10 seconds.
実施例３
ト１部を水２００部に加え、９０°Ｃ１か（はん下にデ
キストリン、アラビアガム、ソルビトールの３゜乞
１２の混合物３０部を加えて懸濁さ齢た。４０°Ｃに冷
却し、冷却分別した液状アマニ油を一１５°Ｃ±２°Ｃ
に冷却し、静かにかくはんした状態下に、内径１朋、外
径１．５朋のガラス管より滴下した。金網にて口取し、
冷却したベンジンにてよく洗い、常法にて真空凍結乾燥
し１粒径１．８ｇｍ程度の球状粒状物を得た。このもの
は９０°Ｃの熱湯中にて瞬時に崩壊。Example 3 1 part of dextrin was added to 200 parts of water, and 30 parts of a 30% mixture of dextrin, gum arabic, and sorbitol was added to 90°C and suspended. Cooled to 40°C. The cooled and fractionated liquid linseed oil was heated to 15°C ± 2°C.
The mixture was cooled to a temperature of 1.5 mm, and then dripped into a glass tube with an inner diameter of 1 mm and an outer diameter of 1.5 mm while being gently stirred. Take the mouth with a wire mesh,
The mixture was thoroughly washed with cooled benzene and freeze-dried under vacuum in a conventional manner to obtain spherical particles each having a particle size of about 1.8 gm. This material disintegrates instantly in boiling water at 90°C.
分散した。Dispersed.
実施例４
市販の粉末カラメル（［５ｓＪ（大野実業ｆａｔ））を
固形分３０％に熱湯にかくはん溶解した。２０″Ｃに冷
却し、実施例３と同様に造粒し乾燥した。本市は冷水に
投入すると２０秒程度で溶解した。Example 4 Commercially available powder caramel ([5sJ (Ohno Jitsugyo fat)) was dissolved in hot water by stirring to a solid content of 30%. The mixture was cooled to 20''C, granulated and dried in the same manner as in Example 3. When Motoichi was added to cold water, it dissolved in about 20 seconds.
実施例５
ジネブ（エチレンジアミンのビスジチオカルバメイトの
亜鉛塩）の微粉末１０部、カオリン微粉末２０部、沈降
性炭酸カルシウム末５部、硫酸銅水和物粉末２部、ポリ
エチレングリコール２部、トール油２部、グリセリンモ
ノオレエート１部、ポリビニルアルコール３部、デキス
トリン１５部を水１５０部に激しくかくはん混合し懸濁
した。２５°Ｃに冷却し、実施例２と同様に造粒、乾燥
し、水に即崩壊性の土壌殺菌剤を得た。Example 5 10 parts of fine powder of zineb (zinc salt of bisdithiocarbamate of ethylenediamine), 20 parts of fine kaolin powder, 5 parts of precipitated calcium carbonate powder, 2 parts of copper sulfate hydrate powder, 2 parts of polyethylene glycol, Thor 2 parts of oil, 1 part of glycerin monooleate, 3 parts of polyvinyl alcohol, and 15 parts of dextrin were mixed and suspended in 150 parts of water with vigorous stirring. The mixture was cooled to 25°C, granulated and dried in the same manner as in Example 2 to obtain a soil fungicide that disintegrates immediately in water.
実施例６ ２２．０になるまで溶解し１５°Ｃに冷却した。Example 6 It was dissolved until the temperature reached 22.0 and cooled to 15°C.
液体チッ素をデユワ−びんに深さ３０口に保持し。Liquid nitrogen is held in a dewar bottle at a depth of 30 openings.
市販の１ ｍｌのメスピペットより滴下造粒した。The mixture was granulated by dropping using a commercially available 1 ml measuring pipette.
粒状物を金網にて口取し、常法にて真空凍結乾燥して２
粒径２．８へ３．１１ｆｆ程度の水に即溶性の粒状イン
スタント紅茶を得た。The granules were collected using a wire mesh and vacuum freeze-dried using a conventional method.
A granular instant black tea immediately soluble in water with a particle size of about 2.8 to 3.11 ff was obtained.
、・・’、、！Ｙ ＼；−１・,...’,,! Y \;-1・
Claims (1)
含む水溶液を、その水溶液が凍結固化するに充分な低温
に保持された非水和性の液体中に滴下し、凍結造粒する
工程。 （Ｂ）かくして得られた凍結造粒物を非水和性の液体よ
り分別する工程。 （Ｃ）分別された凍結造粒物を真空凍結乾燥する工程。 以上、（Ａ）、（Ｂ）、（Ｃ）の三つの工程を結合して
なることを特徴とする造粒方法。[Scope of Claims] (A) An aqueous solution containing useful ingredients and, if necessary, an excipient or binder, in a non-hydratable liquid kept at a temperature sufficiently low to freeze and solidify the aqueous solution. Dripping and freezing granulation process. (B) A step of separating the thus obtained frozen granules from non-hydratable liquids. (C) A step of vacuum freeze-drying the separated frozen granules. A granulation method characterized by combining the three steps (A), (B), and (C) described above.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP12290588A JPH01293128A (en) | 1988-05-18 | 1988-05-18 | Granulating method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP12290588A JPH01293128A (en) | 1988-05-18 | 1988-05-18 | Granulating method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01293128A true JPH01293128A (en) | 1989-11-27 |
Family
ID=14847514
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP12290588A Pending JPH01293128A (en) | 1988-05-18 | 1988-05-18 | Granulating method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01293128A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5387415A (en) * | 1992-01-17 | 1995-02-07 | Alfatec Pharma Gmbh | Aloe vera juice containing pellets process for production thereof and the use thereof as pharmaceutical, cosmetic and peroral agents |
| US5405616A (en) * | 1992-01-17 | 1995-04-11 | Alfatec Pharma Gmbh | Means for containing active substances, having a shell of hydrophilic macromolecules, active substances and process for preparation thereof |
-
1988
- 1988-05-18 JP JP12290588A patent/JPH01293128A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5387415A (en) * | 1992-01-17 | 1995-02-07 | Alfatec Pharma Gmbh | Aloe vera juice containing pellets process for production thereof and the use thereof as pharmaceutical, cosmetic and peroral agents |
| US5405616A (en) * | 1992-01-17 | 1995-04-11 | Alfatec Pharma Gmbh | Means for containing active substances, having a shell of hydrophilic macromolecules, active substances and process for preparation thereof |
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