JP3915330B2 - Tablet molding method and tablet molding apparatus - Google Patents

Description

【００９１】
〔式中、Ｒｆは少なくとも１つのフッ素原子を含有する飽和又は不飽和のアルキル基を表し、Ｘはスルホンアミド、
【００９２】
【化２】

【００９３】
を表し、Ｙはアルキレンオキサイド基、アルキレン基を表し、Ｒｆ′は少なくとも１つのフッ素原子を含有する飽和又は不飽和の炭化水素基を表す。さらにＡは−ＳＯ₃Ｍ、−ＯＳＯ₃Ｍ、−ＣＯＯＭ、−ＯＰＯ₃（Ｍ₁）（Ｍ₂）、−ＰＯ₃（Ｍ₁）（Ｍ₂）等の親水基を表し、Ｍ、Ｍ₁、Ｍ₂はＨ、Ｌｉ、Ｋ、Ｎａ又はＮＨ₄を表し、ｍは０又は１、ｎは０又は１〜１０の整数を表す。〕
上記一般式〔Ｉ〕において、Ｒｆは少なくとも１つのフッ素原子を含有する飽和又は不飽和のアルキル基（例えばアルキル基、アルケニル基、アルキニル基）を表し好ましくは炭素数４〜１２、さらに好ましくは炭素数６〜９のアルキル基である。Ａは好ましくは−ＳＯ₃Ｍが挙げられ、Ｍ、Ｍ₁、Ｍ₂は好ましくはＬｉ，Ｋ，Ｎａ最も好ましくはＬｉである。ｍは０又は１、ｎは０又は１〜１０の整数を表すが、好ましくはｍ＝０、ｎ＝０である。
【００９４】
以下に一般式〔Ｉ〕で表される代表的な例示化合物を示すが、これに限られるものではない。
【００９５】
【化３】

【００９６】
【化４】

【００９７】
上記化合物のうち、特に好ましいものは、（Ｉ−１）、（Ｉ−２）、（Ｉ−４）である。
【００９８】
これら化合物は通常の方法で合成でき、市販品としても入手できる。
【００９９】
次に、一般式〔II〕で表される滑沢剤（界面活性剤）について説明する。
【０１００】
【化５】

【０１０１】
上記一般式〔II〕において、Ｒ₁はアルキル基又はアルケニル基を表し、Ｒ₂は水素原子、アルキル基又はヒドロキシアルキル基を表し、Ｒ₃及びＲ₄は独立に水素原子、水酸基、アルキル基又は−ＣＯＯＭ₂（Ｍ₂は水素原子又はアルカリ金属原子を表す）を表し、Ｘは−ＣＯ−又は−ＳＯ₂−を表し、Ｙは−Ｏ−、−Ｓ−又は−ＣＯＮＲ₅−（Ｒ₅は水素原子、アルキル基又はヒドロキシアルキル基を表す）を表し、Ｍ₁は水素原子又はアルカリ金属原子を表し、ｌは０又は１、ｍは０〜２の整数、ｎは１〜３の整数を表す。
【０１０２】
Ｒ₁は好ましくは炭素数５〜２０の直鎖又は分岐のアルキル基又はアルケニル基であり、Ｒ₂は好ましくは水素原子、炭素数１〜５の直鎖もしくは分岐アルキル基又はヒドロキシアルキル基である。
【０１０３】
次に一般式〔II〕で示される化合物の具体的な化合物例を以下に示す。
【０１０４】
【化６】

【０１０５】
【化７】

【０１０６】
【化８】

【０１０７】
【化９】

【０１０８】
上記化合物の他に特開昭６２−５６９６１号第４〜６頁記載の例示化合物〔ＩＩ〕−１〜５５等も使用することが出来る。
【０１０９】
上記例示化合物は、公知化合物、又は、市販されており通常ルートで入手が可能である。
【０１１０】
次に、一般式〔III〕または〔IV〕で表される滑沢剤（界面活性剤）について説明する。
【０１１１】
【化１０】

【０１１２】
式中、Ｒ₁、Ｒ₂、Ｒ₃、Ｒ₄及びＲ₅は各々アルキル基、アラルキル基、アルケニル基、スチリル基、シンナミル基を表し、ｌ１、ｌ２、ｌ３、ｌ４、ｌ５は各々０または１の整数を表し、ｎは２〜１００の整数を表す。但し、Ｒ₃がアルキル基でかつｌ３が１の場合は、ｌ１、ｌ２、ｌ４、ｌ５の少なくとも１つが１である。ｌ１、ｌ２、ｌ３、ｌ４、ｌ５が０のときは対応するＲ₁、Ｒ₂、Ｒ₃、Ｒ₄及びＲ₅は水素原子である。
【０１１３】
上記式において、Ｒ₁、Ｒ₂、Ｒ₃、Ｒ₄及びＲ₅で表されるアルキル基は炭素数が１〜２０のものであり、鎖状、環状のいずれのものであってもよく、鎖状の基としては直鎖、分岐のものを含み、具体的には例えばメチル、エチル、ｎ−プロピル、ｉ−プロピル、ブチル、ｔ−ブチル、ｓｅｃ−ブチル、アミル、ヘキシル、ヘプチル、オクチル、ノニル、デシル、オクタデシル等の各基が挙げられる。Ｒ₁、Ｒ₂、Ｒ₃、Ｒ₄及びＲ₅で表されるアラルキル基は、炭素数７〜２０のものであり、具体的には例えばベンジル、フェネチル、ジベンジル、２−ナフチルメチル等の各基が挙げられる。
【０１１４】
Ｒ₁、Ｒ₂、Ｒ₃、Ｒ₄及びＲ₅で表されるアルケニル基は、炭素数３〜２０のものであり、具体的には例えばアリル、４−ヘキセニル、４−デセニル、９−オクタデセニル等の各基が挙げられる。
【０１１５】
アラルキル基及びスチリル基の芳香環上には、置換基を有することができ、置換基としては例えばアルキル基（例えばメチル、エチル、プロピル、ｔ−アミル、ノニル等の各基）、アルコキシ基（例えばメトキシ、エトキシ、プロポキシ、２−エトキシエトキシ等の各基）、アリールオキシ基（例えばフェノキシ、ｐ−トリルオキシ、ｏ−クロロフェノキシ等の各基）等が挙げられる。具体的には例えばｐ−メトキシベンジル、２，４−ジメチルベンジル、ｐ−フェノキシフェネチル、ｐ−ブチルスチレン等の各基が挙げられる。
【０１１６】
【化１１】

【０１１７】
式中、Ｒは炭素数４〜２５の直鎖又は分岐状の置換基を有してもよいアルキル基又は
【０１１８】
【化１２】

【０１１９】
を表す（但し、Ｒ₁₁及びＲ₁₂はそれぞれ水素原子又は置換基を有してもよい炭素数１〜２０のアルキル基を表し、ｌは０〜４の整数を表す）。ｎ及びｍはそれぞれ、０又は１〜２５の整数を表すが、同時に０にはならない。Ａ及びＢはそれぞれ
【０１２０】
【化１３】

【０１２１】
を表し、同一でもまた異ったものでもよい（但し、ｎ１、ｍ１及びｌ１はそれぞれ０、１、２又は３を表すが、Ａ及びＢにおけるｍ１が同時に０にはならず、ｎ又はｍが０のときはｍ１は０にはならない）。Ｄは水素原子を表す。
【０１２２】
以下に、一般式〔III〕または〔IV〕で表される化合物の例示化合物を挙げる。
【０１２３】
【化１４】

【０１２４】
【化１５】

【０１２５】
【化１６】

【０１２６】
【化１７】

【０１２７】
【化１８】

【０１２８】
【化１９】

【０１２９】
次に、一般式〔Ｖ〕で表される滑沢剤（界面活性剤）について説明する。
【０１３０】
【化２０】

【０１３１】
〔式中、Ｒ₁は１価の有機基を表わし、Ｒ₂はエチレン基またはプロピレン基を表わし、ｍは４〜５０の整数を表わす。Ｘ₁は水素原子、−ＳＯ₃Ｍまたは−ＰＯ₃Ｍを表わす。ここでＭは水素原子、アルカリ金属原子または−ＮＨ₄を表わす。〕
次に前記一般式〔Ｖ〕で表される化合物について、さらに説明すると、前記一般式〔Ｖ〕中のＲ₁は一価の有機基、例えば炭素原子数が６〜２０、好ましくは６〜１２のアルキル基であり、ヘキシル、ヘプチル、オクチル、ノニル、デシル、ウンデシル又はドデシル等を表わす。又は炭素原子数が３〜２０のアルキル基で置換されたアリール基であり、置換基として好ましくは炭素原子数３〜１２のアルキル基であり、プロピル、ブチル、ペンチル、ヘキシル、ヘプチル、オクチル、ノニル、デシル、ウンデシル又はドデシル等を表わす。アリール基としてはフェニル、トリル、キシニル、ブフェニル又はナフチル等であり、好ましくはフェニル又はトリルである。アリール基にアルキル基が結合する位置としては、オルト、メタ、パラ位いずれでもよい。Ｒ₂はエチレン基またはプロピレン基を表わし、ｍは４〜５０の整数を表わす。Ｘ₁は水素原子、−ＳＯ₃Ｍ又は−ＰＯ₃Ｍ₂を示し、Ｍは水素原子、アルカリ金属原子（Ｎａ，Ｋ又はＬｉ等）又は−ＮＨ₄を表わす。
【０１３２】
以下に、一般式〔Ｖ〕で示される具体的例示化合物を示す。
【０１３３】
【化２１】

【０１３４】
【化２２】

【０１３５】
次に、一般式〔VI〕で表される滑沢剤（界面活性剤）について説明する。
【０１３６】
一般式〔VI〕
Ｒ−（Ｏ）_xＳ_yＯ_zＭ
〔式中、Ｒは置換又は無置換の脂肪族基、芳香族基又はヘテロ環基を表し、ｘは０又は１、ｙは１又は２、ｚは２〜８の整数を表し、Ｍはカチオンを表す。〕
一般式〔VI〕において、Ｒで表される脂肪族基としては、アルキル基、アルケニル基、アルキニル基などがあり、アルキル基としては、例えばメチル、エチル、ｉ−プロピル、ブチル、ｔ−ブチル、ペンチル、シクロペンチル、ヘキシル、シクロヘキシル、オクチル、ドデシル等の各基が挙げられる。これらのアルキル基は、更にハロゲン原子（例えば塩素、臭素、フッ素等のハロゲン原子）、アルコキシ基（例えばメトキシ、エトキシ、１，１−ジメチルエトキシ、ヘキシルオキシ、ドデシルオキシ等の各基）、アリールオキシ基（例えばフェノキシ、ナフチルオキシ等の各基）、アリール基（例えばフェニル、ナフチル等の各基）、アルコキシカルボニル基（例えばメトキシカルボニル、エトキシカルボニル、ブトキシカルボニル、２−エチルヘキシルカルボニル等の各基）、アリールオキシカルボニル基（例えばフェノキシカルボニル、ナフチルオキシカルボニル等の各基）、アルケニル基（例えばビニル、アリル等の各基）、複素環基（例えば２−ピリジル、３−ピリジル、４−ピリジル、モルホリル、ピペリジン、ピペラジル、ピリミジン、ピラゾリン、フリル等の各基）、アルキニル基（例えばプロパルギル基等）、アミノ基（例えばアミノ、Ｎ，Ｎ−ジメチルアミノ、アニリノ等の各基）、シアノ基、スルホアミド基（例えばメチルスルホニルアミノ、エチルスルホニルアミノ、ブチルスルホニルアミノ、オクチルスルホニルアミノ、フェニルスルホニルアミノ等の各基）によって置換されてもよい。
【０１３７】
アルケニル基としては、例えばビニル基、アリル基等が挙げられ、アルキニル基としては例えばプロパルギル基が挙げられる。
【０１３８】
Ｒで表される芳香族基としては、例えばフェニル基、ナフチル基等が挙げられる。
【０１３９】
Ｒで表されるヘテロ環基としては、例えばピリジル基（２−ピリジル、３−ピリジル、４−ピリジル等の各基）、チアゾリル基、オキサゾリル基、イミダゾリル基、フリル基、チェニル基、ピロリル基、ピラジニル基、ピリミジニル基、ピリダジニル基、セレナゾリル基、スルホラニル基、ピペジリニル基、ピラゾリル基、テトラゾリル基等が挙げられる。
【０１４０】
上記、アルケニル基、アルキニル基、芳香族基、複素環基は、いずれもＲで表されるアルキル基及びアルキル基の置換基、置換原子として示した基、原子と同様な基、原子によって置換することができる。
【０１４１】
Ｍで表されるカチオンとしては、好ましくは金属イオン又は有機カチオンである。金属イオンとしては、例えばリチウムイオン、ナトリウムイオン、カリウムイオン等が挙げられ、有機カチオンとしては、例えばアンモニウムイオン（アンモニウム、テトラメチルアンモニウム、テトラブチルアンモニウム等の各イオン）、ホスホニウムイオン（例えばテトラフェニルホスホニウムイオン等）、グアニジルイオン等が挙げられる。
【０１４２】
以下に一般式〔VI〕で表される化合物の具体例を挙げるが、本発明はこれらに限定されるものではない。
【０１４３】
VI−１ Ｃ₂Ｈ₅ＳＯ₃Ｎａ
VI−２ ＣＨ₃（ＣＨ₂）₆ＳＯ₃Ｎａ
VI−３ ＣＨ₃（ＣＨ₂）₇ＳＯ₃Ｎａ
VI−４ ＣＨ₃（ＣＨ₂）₅ＯＳＯ₃Ｎａ
VI−５ ＣＨ₃（ＣＨ₂）₆ＯＳＯ₃Ｎａ
VI−６ ＣＨ₃（ＣＨ₂）₇ＯＳＯ₃Ｎａ
VI−７ ＣＨ₃Ｏ（ＣＨ₂）₂ＳＯ₃Ｎａ
【０１４４】
【化２３】

【０１４５】
また、前記錠剤化において、前記滑沢剤とともに予め材料中に混入するバインダとしては糖類が好ましく、下記のものが使用できる。
【０１４６】
ここでいう糖類とは、単糖類とこれが複数個互いにグリコシド結合した多糖類及びこれらの分解物とをいう。
【０１４７】
単糖類とは、単一のポリヒドロキシアルデヒド、ポリヒドロキシケトン及びこれらの還元誘導体、酸化誘導体、デオキシ誘導体、アミノ誘導体、チオ誘導体など広い範囲の誘導体の総称である。
【０１４８】
多くの糖は、一般式ＣｎＨ₂ｎＯｎで表されるが、この一般式で表される糖骨格から誘導される化合物も含めて、本発明では単糖類と定義する。
【０１４９】
これらの単糖類のうちで好ましいものは、糖のアルデヒド基及びケトン基を還元して各々第一、第二アルコール基とした糖アルコールである。
【０１５０】
多糖類には、セルロース類、デンプン類、グリコーゲン類などが含まれ、セルロース類には、水酸基の一部又は全部がエーテル化されたセルロースエーテル等の誘導体を含み、デンプン類には加水分解して麦芽糖に至るまでの種々の分解生成物であるデキストリン類等を含む。セルロース類は溶解性の観点からアルカリ金属塩の形でもかまわない。
【０１５１】
これら多糖類で好ましく用いられるものは、セルロース類、デキストリン類及びシクロデキストリン類であり、より好ましくはシクロデキストリン類である。
【０１５２】
本発明に係る単糖類の具体的例示化合物を次に示す。
【０１５３】
〔例示化合物〕
Ｂ−（１） グリセルアルデヒド
Ｂ−（２） ジヒドロキシアセトン（二量体を含む）
Ｂ−（３） Ｄ−エリトロース
Ｂ−（４） Ｌ−エリトロース
Ｂ−（５） Ｄ−トレオース
Ｂ−（６） Ｌ−トレオース
Ｂ−（７） Ｄ−リボース
Ｂ−（８） Ｌ−リボース
Ｂ−（９） Ｄ−アラビノース
Ｂ−（１０） Ｌ−アラビノース
Ｂ−（１１） Ｄ−キシロース
Ｂ−（１２） Ｌ−キシロース
Ｂ−（１３） Ｄ−リキソース
Ｂ−（１４） Ｌ−リキソース
Ｂ−（１５） Ｄ−キシルロース
Ｂ−（１６） Ｌ−キシルロース
Ｂ−（１７） Ｄ−リブロース
Ｂ−（１８） Ｌ−リブロース
Ｂ−（１９） ２−デオキシ−Ｄ−リボース
Ｂ−（２０） Ｄ−アロース
Ｂ−（２１） Ｌ−アロース
Ｂ−（２２） Ｄ−アルトロース
Ｂ−（２３） Ｌ−アルトロース
Ｂ−（２４） Ｄ−グルコース
Ｂ−（２５） Ｌ−グルコース
Ｂ−（２６） Ｄ−マンノース
Ｂ−（２７） Ｌ−マンノース
Ｂ−（２８） Ｄ−グロース
Ｂ−（２９） Ｌ−グロース
Ｂ−（３０） Ｄ−イドース
Ｂ−（３１） Ｌ−イドース
Ｂ−（３２） Ｄ−ガラクトース
Ｂ−（３３） Ｌ−ガラクトース
Ｂ−（３４） Ｄ−タロース
Ｂ−（３５） Ｌ−タロース
Ｂ−（３６） Ｄ−キノボース
Ｂ−（３７） ジギタロース
Ｂ−（３８） ジギトキソース
Ｂ−（３９） シマロース
Ｂ−（４０） Ｄ−ソルボース
Ｂ−（４１） Ｌ−ソルボース
Ｂ−（４２） Ｄ−タガトース
Ｂ−（４３） Ｄ−フコース
Ｂ−（４４） Ｌ−フコース
Ｂ−（４５） ２−デオキシ−Ｄ−グルコース
Ｂ−（４６） Ｄ−プシコース
Ｂ−（４７） Ｄ−フルクトース
Ｂ−（４８） Ｌ−フルクトース
Ｂ−（４９） Ｌ−ラムノース
Ｂ−（５０） Ｄ−グルコサミン
Ｂ−（５１） Ｄ−ガラクトサミン
Ｂ−（５２） Ｄ−マンノサミン
Ｂ−（５３） Ｄ−グリセロ−Ｄ−ガラクトヘプトース
Ｂ−（５４） Ｄ−グリセロ−Ｄ−マンノヘプトース
Ｂ−（５５） Ｄ−グリセロ−Ｌ−マンノヘプトース
Ｂ−（５６） Ｄ−グリセロ−Ｄ−グロヘプトース
Ｂ−（５７） Ｄ−グリセロ−Ｄ−イドヘプトース
Ｂ−（５８） Ｄ−グリセロ−Ｌ−グルコヘプトース
Ｂ−（５９） Ｄ−グリセロ−Ｌ−タロヘプトース
Ｂ−（６０） Ｄ−アルトロヘプツロース
Ｂ−（６１） Ｄ−マンノヘプツロース
Ｂ−（６２） Ｄ−アルトロ−３−ヘプツロース
Ｂ−（６３） Ｄ−グルクロン酸
Ｂ−（６４） Ｌ−グルクロン酸
Ｂ−（６５） Ｎ−アセチル−Ｄ−グルコサミン
Ｂ−（６６） グリセリン
Ｂ−（６７） Ｄ−トレイット
Ｂ−（６８） Ｌ−トレイット
Ｂ−（６９） エリトリット（商品名、三菱化成食品エリスリトール）
Ｂ−（７０） Ｄ−アラビット
Ｂ−（７１） Ｌ−アラビット
Ｂ−（７２） アドニット
Ｂ−（７３） キシリット
Ｂ−（７４） Ｄ−ソルビット
Ｂ−（７５） Ｌ−ソルビット
Ｂ−（７６） Ｄ−マンニット
Ｂ−（７７） Ｌ−マンニット
Ｂ−（７８） Ｄ−イジット
Ｂ−（７９） Ｌ−イジット
Ｂ−（８０） Ｄ−タリット
Ｂ−（８１） Ｌ−タリット
Ｂ−（８２） ズルシット
Ｂ−（８３） アロズルシット
これら例示化合物のうち好ましく用いられる糖アルコール類としては、Ｂ−（６６）〜（８３）であり、より好ましくは、Ｂ−（６９）、（７４）〜（８３）である。
【０１５４】
本発明に係る多糖類及び糖分解物の具体的例示化合物を次に示す。
【０１５５】
Ｃ−（１） 麦芽糖
Ｃ−（２） セロビオース
Ｃ−（３） トレハロース
Ｃ−（４） ゲンチオビオース
Ｃ−（５） イソマルトース
Ｃ−（６） 乳糖
Ｃ−（７） ラフィノース
Ｃ−（８） ゲンチアノース
Ｃ−（９） スタキオース
Ｃ−（１０） キシラン
Ｃ−（１１） アラバン
Ｃ−（１２） グリコーゲン
Ｃ−（１３） デキストラン
Ｃ−（１４） イヌリン
Ｃ−（１５） レバン
Ｃ−（１６） ガラクタン
Ｃ−（１７） アガロース
Ｃ−（１８） アミロース
Ｃ−（１９） スクロース
Ｃ−（２０） アガロビオース
Ｃ−（２１） メチルセルロース
Ｃ−（２２） ジメチルセルロース
Ｃ−（２３） トリメチルセルロース
Ｃ−（２４） エチルセルロース
Ｃ−（２５） ジエチルセルロース
Ｃ−（２６） トリエチルセルロース
Ｃ−（２７） カルボキシメチルセルロース
Ｃ−（２８） カルボキシエチルセルロース
Ｃ−（２９） アミノエチルセルロース
Ｃ−（３０） ヒドロキシメチルセルロース
Ｃ−（３１） ヒドロキシエチルメチルセルロース
Ｃ−（３２） ヒドロキシプロピルセルロース
Ｃ−（３３） ヒドロキシプロピルメチルセルロース
Ｃ−（３４） ヒドロキシプロピルメチルセルロースアセテートサクシネート
Ｃ−（３５） カルボキシメチルヒドロキシエチルセルロース
Ｃ−（３６） α−デキストリン
Ｃ−（３７） β−デキストリン
Ｃ−（３８） γ−デキストリン
Ｃ−（３９） σ−デキストリン
Ｃ−（４０） ε−デキストリン
Ｃ−（４１） α−限界デキストリン
Ｃ−（４２） β−限界デキストリン
Ｃ−（４３） ホスホリラーゼ限界デキストリン
Ｃ−（４４） 可溶性デンプン
Ｃ−（４５） 薄手ノリデンプン
Ｃ−（４６） 白色デキストリン
Ｃ−（４７） 黄色デキストリン
Ｃ−（４８） ブリティッシュガム
Ｃ−（４９） α−シクロデキストリン
Ｃ−（５０） β−シクロデキストリン
Ｃ−（５１） γ−シクロデキストリン
Ｃ−（５２） メチル−α−シクロデキストリン
Ｃ−（５３） メチル−β−シクロデキストリン
Ｃ−（５４） メチル−γ−シクロデキストリン
Ｃ−（５５） ヒドロキシプロピル−α−シクロデキストリン
Ｃ−（５６） ヒドロキシプロピル−β−シクロデキストリン
Ｃ−（５７） ヒドロキシプロピル−γ−シクロデキストリン
Ｃ−（５８） マルトシクロデキストリン
糖類は、広く天然に存在しており、市販品を簡単に入手できる。又、種々の誘導体についても還元、酸化あるいは脱水反応などを行うことによって容易に合成できる。
【０１５６】
市販品として、シクロデキストリン類としては塩水港精糖（株）社製α−１００Ｈ、β−１００、γ−１００、Ｋ−１００、イソエリートＰ、イソエリートＰＨ、メチル−β−ＣＤ、ヒドロキシプロピル−β−ＣＤ、デンプンの分解物としては松谷化学工業（株）社製のパインフロー、パインデックスシリーズ、フードテックス、マックス１００、グリスターＰ、ＴＫ−１６、ＭＰＤ、Ｈ−ＰＤＸ、スタコデックス、日本油脂（株）社製オイルＱシリーズが挙げられる。
【０１５７】
その他のバインダとして好ましい化合物は下記一般式で表されるものである。
【０１５８】
ＨＯ−（Ａ₁−Ｏ）_l1−（Ａ₂−Ｏ）_l2−（Ａ₃−Ｏ）_l3−Ｈ
式中、Ａ₁、Ａ₂、Ａ₃はそれぞれ置換、無置換の直鎖または分岐のアルキレン基を表し、これらは同一であっても異なっていてもよい。
【０１５９】
また、置換基としては、ヒドロキシ基、カルボキシ基、スルホニル基、アルコキシ基、カルバモイル基、スルファモイル基があげられる。
【０１６０】
好ましく用いられるものは、Ａ₁、Ａ₂、Ａ₃がそれぞれ無置換であるものである。また最も好ましいものとしては、Ａ₁、Ａ₂、Ａ₃が−ＣＨ₂ＣＨ₂−、−ＣＨ（ＣＨ₃）−ＣＨ₂−である。
【０１６１】
ｌ１、ｌ２、ｌ３は、それぞれ０または０〜５００の整数を表す。ただし、ｌ１＋ｌ２＋ｌ３≧５である。
【０１６２】
これらのうちで、好ましく用いられるのはｌ１、ｌ２、ｌ３のうち少なくとも１つが１５以上のものであり、さらに好ましく用いられるのは２０以上のものである。
【０１６３】
この一般式で表される化合物の中でもっとも好ましいものはポリエチレングリコール（ＰＥＧと称することもある）である。
【０１６４】
また、ポリエチレングリコールの場合は、平均分子量が２０００〜２００００の範囲にあるものが好ましく、特に好ましくは３０００〜１５０００の範囲のものである。
【０１６５】
本発明において、写真感光材料用処理剤の錠剤成形の場合には、発色現像剤、黒白現像剤、漂白剤、定着剤、漂白定着剤、安定剤の錠剤成形に好ましく適用出来る。
【０１６６】
発色現像剤であるパラフェニレン系発色現像主薬のうち本発明の効果を良好に奏する化合物として、特開平５−２３２６５６号公報の段落番号００８３〜００８６に記載されている化合物が挙げられ、中でも特に下記化合物が好ましい。
【０１６７】
【化２４】

【０１６８】
ヒドロキシルアミンおよびその誘導体のうち、本発明の効果を良好に奏する化合物として、特開平５−２３２６５６号公報の段落番号０１００〜０１３０に記載されている化合物が挙げられ、中でもビス（スルホエチル）ヒドロキシルアミン２ナトリウム塩およびヒドロキシルアミンが好ましい。
【０１６９】
炭酸アルカリ金属塩のうち、本発明の効果を良好に奏する化合物は、特開平５−２３２６５６号公報の段落番号０１０５に記載された化合物が挙げられる。とりわけ好ましい化合物は炭酸カリウムである。
【０１７０】
アミノポリカルボン酸の第２鉄錯塩のうち、本発明の効果を良好に奏する化合物は、特願平５−１０６２７８号公報の段落番号００４０〜０１１０に記載された化合物が挙げられる。とりわけ好ましい化合物はエチレンジアミン四酢酸、１，３−プロピレンジアミン四酢酸およびジエチレントリアミン五酢酸のそれぞれ第２鉄錯塩である。
【０１７１】
黒白用現像剤に用いることが出来る現像主薬としては、特願平１１−９１３４３号公報記載のレダクトン類を含有することが好ましい。そのうち、特にＤ−１で示されるアスコルビン酸またはエリソルビン酸（立体異性）またはそれらの塩が好ましい。
【０１７２】
黒白用定着剤としては、同様に特願平１１−９１３４３号公報に記載のものが用いられるが、特に定着主薬としては、チオ硫酸塩を含有することが好ましい。チオ硫酸塩は具体的には、リチウム、カリウム、ナトリウム、アンモニウムの塩として用いられるが、本発明の効果よりナトリウム、カリウム塩が良い。
【０１７３】
【発明の効果】
上杵と下杵を有する錠剤成形装置を用い、圧縮成型材料を圧縮して錠剤を成形する際に、滑沢剤を効率的に且つ簡易に前記杵に供給することが出来る錠剤成形方法、錠剤成形装置、粉体供給方法および粉体供給装置を提供することが出来た。
【図面の簡単な説明】
【図１】本発明の錠剤成形装置の一形態を示す概略図である。
【図２】本発明の錠剤成形装置の一形態を示す概略斜視図である。
【図３】本発明の錠剤成形装置の下杵滑沢剤供給手段による滑沢剤供給工程を説明するための模式図である。
【図４】本発明において、本発明の錠剤成形装置の材料供給手段による材料供給工程を示す模式図である。
【図５】本発明の錠剤形成装置の材料表面滑沢剤供給手段による材料表面滑沢剤供給工程を説明するための模式図である。
【図６】本発明の錠剤形成装置における圧縮成型工程を説明するための模式図である。
【図７】本発明の錠剤形成装置に適用しうるクリーニング手段を示す模式図である。
【図８】本発明の粉体供給装置の一形態を示す模式図である。
【図９】本発明の粉体供給装置に用いることの出来る除電装置の一形態を示す模式図である。
【図１０】本発明の粉体供給装置の一形態を示す模式図である。
【図１１】本発明の粉体供給装置の一形態を示す模式図である。
【図１２】本発明の粉体供給装置の一形態を示す模式図である。
【符号の説明】
１ 下杵滑沢剤供給部
２ 材料供給部
３ 材料表面滑沢剤供給部
４ 第１圧縮成型部（予圧）
５ 第２圧縮成型部（本圧）
６ 排出ガイド
７ クリーニング部
８ａ，８ｂ 除湿エア吹付部
１０ ターンテーブル
１１ 貫通孔
１２ 上杵
１３ 下杵
１４，１５ 偏心ローラ
２０ 下杵滑沢剤供給手段
２５ 材料表面滑沢剤供給手段
３０ 材料供給手段
４０ ホッパ（粉体貯留手段）
４１ エア供給管
４２ 粉体噴射管
５０ 回転軸
５１ エア噴射孔
５３ａ，５３ｂ 攪拌子
６０ コイルバネ
７０ 除電装置（除電手段）[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a tablet molding method, a tablet molding device, a powder supply method, and a powder supply device, and more specifically, a tablet molding method, a tablet molding device, a powder supply device, and a powder characterized by the supply of a lubricant. The present invention relates to a body supply device.
[0002]
[Prior art]
Conventionally, a pair of upper and lower ridges that have a plurality of through holes on the circumference of a thick disk and that can reciprocate in the direction of the through holes by sliding with the inner wall of the through holes, 2. Description of the Related Art A tablet forming apparatus (tablet press) is known that supplies powder or granules as a compression molding material between a punch and a lower punch and compresses to form a tablet. The compression molding material has a high surface activity and contains a binder to obtain the hardness of the tablet. Therefore, the compression molding material is an obstacle called sticking that adheres to the surface that comes into contact with the compression molding material of the through-hole or bag. Is prone to occur. When a tableting machine continuously molds tablets, it is necessary that the through holes and the punches are always clean, and sticking of the compression molding material must be avoided.
[0003]
In order to deal with such problems, Japanese Patent Publication No. 41-11273 proposes a technique for injecting a lubricant onto the upper and lower eyelids before supplying the compression molding material. However, this method did not allow the lubricant to adhere to the upper arm sufficiently uniformly.
[0004]
For this reason, in order to adhere the lubricant to the soot more sufficiently uniformly, a technique for providing a spray chamber surrounding the through hole and the soot and injecting the lubricant in the spray chamber is disclosed in JP-A-56-14098. And JP-A-7-124231. Although this method can surely attach the lubricant to the upper eyelid as compared with the technique of Japanese Patent Publication No. 41-11273, it requires a large apparatus for providing a spray chamber. It could not be said that it was preferable in terms of cost.
[0005]
On the other hand, as a device for supplying the lubricant to the tableting machine, a spray-type device in which the lubricant is sprayed from the nozzle together with air is generally used, but the lubricant becomes lumpy and easily clogged. There was a problem that it was difficult to inject at a constant concentration.
[0006]
[Problems to be solved by the invention]
An object of the present invention is to efficiently and easily supply a lubricant to the wrinkle when a tablet is formed by compressing a compression molding material using a tablet forming apparatus having an upper wrinkle and a lower wrinkle. A tablet forming method, a tablet forming apparatus, a powder supply method, and a powder supply apparatus are provided.
[0007]
[Means for Solving the Problems]
The above object of the present invention can be achieved by the following constitution.
[0008]
1. A compression molding material is compressed between the upper and lower ridges using a tablet molding device having a through-hole and an upper and lower ridge that can reciprocate in the direction of the through-hole by sliding with the inner wall of the through-hole. In a tablet molding method for molding a tablet,
  A material supplying step of supplying a compression molding material of powder or granules to a concave portion formed by the upper surface of the lower rod and the inner wall of the through hole, the lower rod being at a position below the upper end of the through hole; ,
  A material surface lubricant supply step for supplying a lubricant, which is a powder surfactant, to the surface of the compression molding material supplied in the material supply step.And
  Further, the material surface lubricant supplying step for supplying the powder lubricant includes a stirring step for stirring the powder stored in the storage means in the storage means for storing the lubricant, and the storage means A discharge step of taking out and releasing a part of the powder in the inside, and performing static elimination of the powder in the stirring stepA tablet forming method characterized by the above.
[0009]
2. 2. The tablet molding method according to 1 above, further comprising a lower glaze lubricant supply step for supplying a lubricant to the upper surface of the lower glaze before the material supply step.
[0010]
3. 3. The lower glaze lubricant supply step, wherein the lubricant is supplied to the upper surface of the lower collar at a position where the upper surface of the lower collar is below the upper end of the through hole. Tablet molding method.
[0011]
4). In the lower glaze lubricant supplying step, the upper surface of the lower collar is flush with the upper end of the through hole, or the upper surface of the lower collar is on the upper side of the upper end of the through hole. 3. The tablet forming method as described in 2 above, wherein an agent is supplied.
[0012]
5. Any one of the above 1 to 4 characterized in that the material supply step performs quantitative determination by pouring the compression molding material into the recess formed by the lower wall and the inner wall of the through hole, and then slicing at the upper end of the through hole. The tablet forming method according to any one of the above.
[0013]
6). The tablet molding method according to any one of 1 to 5 above, wherein the compression molding material is a solid photographic developer.
[0014]
7). A through-hole, and an upper and lower heel that can reciprocate in the direction of the through-hole by sliding with the inner wall of the through-hole, compressing a compression molding material between the upper and lower heels, In the tablet molding apparatus for molding, a material supply means for supplying a powder or granule compression molding material to a recess formed by the lower heel and the inner wall of the through hole, and a compression molding material supplied by the material supply means Material surface lubricant supply means for supplying lubricant, which is a powder surfactant, to the surfaceAnd
  Further, the material surface lubricant supply means for supplying the powder lubricant includes a stirring means for stirring the powder stored in the storage means, and a storage means for storing the lubricant in the storage means. A discharging means for taking out and discharging a part of the powder, and further a discharging means for discharging the powder.A tablet forming apparatus characterized by:
[0015]
8). The material supply means includes material input means for inputting a compression molding material into the concave portion, and material quantification means for slicing and quantifying the compression molding material charged by the material injection means at the upper end of the through hole. 8. The tablet forming apparatus as described in 7 above.
[0016]
9. 9. The tablet molding apparatus as described in 7 or 8 above, further comprising a lower glaze lubricant supply means for supplying a lubricant to the upper surface of the lower glaze.
[0017]
10. The lower arm lubricant supply means supplies the lubricant at a position where the upper surface of the lower arm is below the upper end of the through hole. Tablet molding device.
[0018]
11. The lower arm lubricant supply means supplies the lubricant at a position where the upper surface of the lower arm and the upper end of the through hole are flush with each other or the upper surface of the lower arm is above the upper end of the through hole. The tablet molding apparatus according to any one of 7 to 10 above.
[0020]
12. The stirring step and the discharging step are performed simultaneously.1The tablet forming method according to 1.
[0021]
13. In the discharging step, the powder is discharged by air pressure.1Or 12The tablet forming method according to 1.
[0022]
14. The temperature of the air for generating the air pressure is 10 to 30 ° C. and the humidity is 40% Rh or less.3The tablet forming method according to 1.
[0023]
15. The average particle size of the powder is 125 μm or less,1, 13 or 14The tablet formation method as described in any one of these.
[0026]
16. The stirrer is a conductive stirrer and also serves as a static eliminator7The tablet forming apparatus according to 1.
[0027]
17. The above-mentioned 1 characterized in that the discharging means has a mechanism for discharging powder by air pressure.6The tablet forming apparatus according to 1.
[0028]
DETAILED DESCRIPTION OF THE INVENTION
Hereinafter, embodiments of the present invention will be described with reference to the drawings, but the present invention is not limited thereto.
[0029]
FIG. 1 is a schematic view showing an embodiment of the tablet forming apparatus of the present invention, and FIG. 2 is a schematic perspective view showing an embodiment of the tablet forming apparatus of the present invention.
[0030]
In FIG. 1, a plurality of through-holes 11 are provided at equal intervals along the circumferential direction on the peripheral edge of a disc-shaped turntable 10 placed horizontally.
[0031]
1 and 2, a lower arm lubricant supply section that supplies lubricant to at least the upper surface (compression molding surface) of the lower arm 13 in the rotation direction of the turn table 10 around the turn table 10. 1. A material supply unit 2 (including a material input unit and a material quantification unit) for supplying a compression molding material (hereinafter simply referred to as a material) to a recess formed by the upper surface of the lower rod 13 and the inner wall of the through hole 11; The material surface lubricant supply unit 3 for supplying the lubricant on the material supplied to the first compression molding unit for applying a preload to the material supplied to the recess (the lubricant is supplied to the surface) 4. Second compression molding unit 5 for applying a main pressure to the material after preloading, a taking-out means (not shown) for taking out the molded tablet from the molding unit, and taking out the taken tablet from the turntable Ejection guide to remove (tablet removal hand 6) A cleaning unit 7 for cleaning the compression molding surface (part) after taking out the tablet, and between the second compression molding unit 5 and the material supply unit 2 and between the material supply unit 2 and the first compression molding unit 4. One or a plurality of dehumidified air blowing portions 8a and 8b are arranged between each.
[0032]
The dehumidified air also has the effect of blowing off the adhering powder in addition to drying the side and lower surfaces of the upper collar 12, the upper surface of the lower collar 13, the surface of the supplied compression molding material, and the surrounding atmosphere. Further, in the dehumidified air blowing unit 8b, the blown dehumidified air hits the upper rod 12 and the lower rod 13 and diffuses to the surrounding atmosphere while gradually losing momentum, and dries the surface of the material supplied by the material supply unit 2 There is also an effect. Furthermore, since the tablet forming apparatus is normally used in a box, the dehumidifying air blown out from the dehumidifying air spraying portions 8a and 8b is diffused into the atmosphere in the box, so that the dew point in the box is also lowered. Note that the dehumidified air mentioned here for photographic processing agents refers to air conditioned to a dew point of 15 ° C. or lower. If the dew point exceeds 15 ° C, the material may absorb moisture and have an adverse effect. In the embodiment, the air flow rate of the dehumidified air is 0.3 m in the dehumidified air spraying portion 8a.^Three/H-0.7m^Three/ H, in the dehumidified air blowing unit 8b, it is sufficient that the compression molding material supplied by the material supply unit 2 is not scattered. In the dehumidified air spraying portion 8a, if it is less than the numerical range, there is no spraying effect, and if it exceeds the numerical range, the powder may be scattered and the working environment is likely to deteriorate. The number of the dehumidifying air spraying steps can be reduced or omitted depending on the compression molding material and the working environment.
[0033]
By repeating the steps from the above-mentioned lubricant supply, material supply, compression molding to dehumidified air, the compression molding material is tableted continuously and efficiently.
[0034]
In FIG. 2, reference numerals 12 and 13 denote cylindrical upper and lower eyelids, and these both eyelets are provided in a number corresponding to each through hole 11.
[0035]
At least the lower surface of the upper collar 12 and the upper surface (substantially compression-molded surface) of the lower collar 13 are mirror-finished made of hard chrome plating, and each has a corresponding through-hole 11 from above and below. On the other hand, it can be fitted.
[0036]
Here, the fitting means a state in which the outer periphery of the flange can reciprocate in the direction of the through hole (vertical direction) by sliding against the corresponding inner wall of the through hole 11.
[0037]
When the turntable 10 is rotated, the pair of upper rods 12 and lower rods 13 corresponding to the through-holes 11 are revolved so that the relative positional relationship with the corresponding through-holes is always maintained. .
[0038]
At the position of the first compression molding portion (preload) 4, an eccentric roller 14 that applies a downward pressing force to the upper rod 12 is disposed above the turntable 10, and the lower rod 13 is moved upward. An eccentric roller 15 for applying the pressing force is arranged below the turntable 10. Hereinafter, the pressing force is simply referred to as pressure.
[0039]
Further, an eccentric roller 14-1 that applies a downward pressure to the upper collar 12, which is larger than that by the first compression molding means 4, is provided at the position of the second compression molding portion (main pressure) 5 of the turntable 10. Similarly, an eccentric roller 15-1 that applies an upward pressure to the lower rod 13 is arranged below the turntable 10.
[0040]
In this embodiment, the preload is set to about 1 ton and the main pressure is set to about 10 ton.
[0041]
The diameter of the compression molding surface of the ridge was 30 mm.
[0042]
FIG. 3 is a schematic diagram for explaining a lubricant supply process by a lower lubricant supply means of the tablet forming apparatus (lower adhesive lubricant supply unit) of the present invention.
[0043]
FIG. 3 (a) shows a step of supplying a lubricant to a recess (compression molded portion) formed by the lower collar upper surface and the inner wall of the through hole, where the upper surface of the lower collar is below the upper end of the through hole. 3 (b) shows a step of supplying a lubricant when the upper surface of the lower collar is flush with the upper end of the through hole. FIG. 3 (c) shows a process of supplying the lubricant with the upper surface of the lower collar above the upper end of the through hole. The process of supplying a lubricant at a position is shown. In the figure, 12a is the upper and lower surface, 13a is the lower and upper surface, 20 is the powder supply device, K is the lubricant to be sprayed, and the other member numbers are the same as those described above.
[0044]
In FIG. 3 (a), the lubricant can be simultaneously supplied to the lower iron upper surface 13a and the inner wall of the through hole 11, and in FIGS. 3 (b) and (c), the lower iron upper surface 13a is surely and sufficiently provided. It has the merit of supplying lubricant.
[0045]
The lubricant agent may be supplied in any state of FIGS. 3A to 3C by the lower arm lubricant supply means, and continuously while the lower arm 13 is raised or lowered. It doesn't matter.
[0046]
FIG. 4 is a schematic diagram showing a material supply process by the material supply means of the tablet molding apparatus (material supply unit) of the present invention in the present invention. In the figure, Z is a compression molding material (material), 30 is a material supply means, 31 is a material supply means, an upstream wall surface end portion (material input means) located at the most upstream of the turntable 10, and 32 is located at the most downstream. It is the downstream wall surface end (material quantification means).
[0047]
The material Z is dropped from the upper hopper (not shown) to the material supply means 30 and fills the material supply means 30 as shown in the figure. The turntable 10 is moved in the direction of the arrow in the drawing by the rotation, and the lubricant is sprayed by the lower glaze lubricant supply means 20 described in FIG. When the recessed portion 16 passes through the upstream wall surface end 31 of the material supply means 30, the material Z filled in the material supply means 30 is charged into the recess 16 by its own weight. Further, when the turntable 10 moves in the direction of the arrow and the downstream wall end 31 passes over the recess 16, the material Z is scraped to be flush with the upper end of the turntable 10 and quantified. .
[0048]
FIG. 5 is a schematic diagram for explaining a material surface lubricant supply step by a material surface lubricant supply means of the tablet forming apparatus (material surface lubricant supply unit) of the present invention. In the figure, reference numeral 25 denotes a material surface lubricant supply means. Other member numbers are the same as those described above.
[0049]
The lubricant K is sprayed and supplied to the surface of the material Z by the material surface lubricant supply means 25 onto the surface of the material Z supplied to the recess 16 by the material supply means described in FIG. The material surface lubricant supply means 25 may be the same as or different from the above-mentioned lower iron lubricant supply means 20.
[0050]
FIG. 6 is a schematic diagram for explaining a compression molding process in the tablet molding apparatus of the present invention.
[0051]
When the through hole 11 reaches the position of the material supply means 2 shown in FIG. 1 due to the rotation of the turntable 10, the upper rod 12 retreats upward as shown in FIG. 6A, and the upper surface of the lower rod 13 and the through hole The material is supplied through the material supply means 2 to the concave portion (compression molding portion) 16 formed by the inner wall surface of 11. Further, when the position of the surface lubricant supply means 3 is reached, the lubricant is supplied to the surface of the supplied material Z. This is the same as described with reference to FIGS.
[0052]
As the tablet material, a powder of a photographic processing agent or a powder obtained by processing this powder into granules with a binder is used.
[0053]
Next, the compression molding portion 16 supplied with the material reaches the position of the first compression molding means 4 shown in FIG. 1, and the eccentric rollers 14 and 15 are moved to the upper punch 12 and the lower punch as shown in FIG. 6 (b). Apply pressure to 13.
[0054]
In other words, the material in the compression molding part (recessed part) 16 is preliminarily compression molded with the pressure resulting from the movement of both the scissors 12 and 13 in the direction of the arrow, and at the same time, the air contained in the material is removed.
[0055]
Next, as the turntable 10 is further rotated, the upper rod 12 retreats upward from the turntable 10 as shown in FIG.
[0056]
Then, the compression molding portion 16 having the pre-loaded material reaches the position of the second compression molding means 5 shown in FIG. 1, and the eccentric rollers 14-1 and 15-1 act as shown in FIG. 6 (b). Then, a pressure larger than the above-described pressure is applied to the upper eyelid 12 and the lower eyelid 13, and as a result, the compression molding of the material in the compression molding portion 16 is finished, and a photographic processing agent as a tablet is completed here.
[0057]
Next, while the turntable 10 is rotating, the lower punch 13 is raised through a drive mechanism (not shown) so that the tablet protrudes from the compression molding portion 16, that is, the through hole 11 onto the upper surface of the turntable 10. (See FIG. 6 (c)), the tablet is taken out.
[0058]
The tablet taking-out means is an appropriate mechanism, such as a cam, for giving the movement amount as described above to the lower eyelid 13.
[0059]
The tablet is discharged from the turntable through the discharge guide 6 fixedly disposed near the upper surface of the turntable 10 by the subsequent rotation of the turntable 10.
[0060]
When the turntable 10 further rotates and the through-hole 11 reaches the section where the cleaning means 7 is located, the brush is operated to clean the compression molding surfaces of the two flanges 12 and 13.
[0061]
FIG. 7 is a schematic view showing a cleaning means applicable to the tablet forming apparatus of the present invention.
[0062]
While the turntable 10 rotates and the through-hole 11 and both the rods 12 and 13 reach the cleaning place, the upper surface of the lower rod 13 slightly protrudes from the surface of the turntable 10 (the upper end portion of the through-hole 11). In addition, the related means (members) are configured so that a predetermined gap can be formed between the upper rod 12 and the lower rod 13 in this state.
[0063]
Then, a brush 17 (see FIG. 7) constituting the cleaning means 7 is moved from a predetermined position into the gap formed as described above, and the tip of the brush is moved through the movement of the brush. The lower surface, the side surface tip, and the upper surface (compression molding surface) or side surface tip of the lower collar 13 are brought into contact with each other to clean the portion.
[0064]
FIG. 7 shows the cleaning state, FIG. 7A shows a reciprocating cleaning method for the brush 17, and FIG. 7B shows a rotational cleaning method for the brush.
[0065]
FIG. 8 is a schematic view showing an embodiment of the powder supply apparatus of the present invention. Of course, it can be preferably used as the above-mentioned lower arm lubricant supply means or material surface lubricant supply means. In the figure, 40 is a hopper (storage means) for storing powder such as a lubricant, 41 is an air supply pipe, 50 is a rotating shaft, 60 is a coil spring, 70 is a static eliminating device, and 42 is a powder injection pipe. The static eliminator 70 may be replaced with ground, or may be a combination of the static eliminator and ground. Use of the static eliminator alone has the advantage of excellent portability, and when used in combination with ground, there is an effect of extending the life of the static eliminator. The neutralizing device is not particularly limited as long as it has an effect of removing static electricity from the powder, including a commercially available one. A preferred static eliminating device will be described later with reference to FIG.
[0066]
In a state where powder (not shown) such as a lubricant is stored in the hopper 40, the rotating shaft 50 is rotated in the direction of arrow Ra by a drive source (not shown). The rotating shaft 50 is threaded 52a and 52b so that the powder in the hopper 40 can be conveyed in the direction of the powder injection tube 42 as the rotating shaft 50 rotates. Since the powder injection tube 42 is disposed above the lowermost end of the hopper 40, the threading 52b of the rotary shaft 50 located from the position where the powder injection tube 42 of the hopper 40 is disposed to the lowermost end of the hopper 40 is The direction of rotation is opposite to the threading 52a of the rotary shaft 50 located above the powder injection tube. When the rotating shaft 50 rotates in the direction of the arrow Ra by this threading method, the powder in the hopper 40 can be efficiently conveyed.
[0067]
Two sets of stirrers 53 a and 53 b (stirring means) are connected to the rotating shaft 50, and the stirrers 53 a and 53 b also rotate with the rotation of the rotating shaft 50, and the powder stored in the hopper 40. The body is stirred (stirring step). There is no restriction | limiting in the number and shape of a stirrer, What is necessary is just to be able to stir powder. The material of the stirrers 53a and 53b is not particularly limited, but is preferably made of a conductive material such as metal (conductive stirrer). Further, in the case of a conductive stirrer, it is connected to the static eliminator 70 through a cam 54, a cam follower 61, and a coil spring 60 described later (in this case, all are conductive members). It is effective in suppressing the generation of static electricity and preventing clogging due to the powder becoming lumpy. In this case, the stirrer 53b, the cam 54, the cam follower 61, the coil spring 60, and the static eliminator 70 are all static elimination means. Of course, only the coil spring 60, only the coil spring 60 and the cam follower 61, or only the coil spring 60, the cam follower 61 and the cam 54 from the side close to the static eliminator 70 are conductive members, and may have a static elimination effect. In addition, it is more preferable in terms of preventing static electricity that the static elimination device 70 is connected to the surface of the hopper 40 and the outside of the powder injection tube 42 to eliminate static electricity.
[0068]
The connecting portion of the stirrer 53b with the rotating shaft 50 is a cam 54. When the cam 54 rotates together with the rotating shaft 50, the cam follower 61 in the shape of a crown having a plurality of protrusions escapes from the rotation of the cam 54. The upper and lower vibrations are lowered by the coil spring 60 (arrow S). Although the cam follower 61 has a crown shape as an example in FIG. 8, the cam 54 and the cam follower 61 may be an opposite cam in which the cam 54 and the cam follower 61 are positioned upside down as long as the cam follower 61 can move up and down in association with the coil spring 60. There are no particular restrictions on the type of cam such as a double cam or a cylindrical cam, and a cam shape such as a waveform. The coil spring 60 is provided so as to surround the rotating shaft 50 and has one end connected to the cam follower 61 and vibrates up and down in the direction of arrow S together with the cam 61. The other end of the coil spring 60 is connected to a static eliminator 70 outside the hopper 40, and the vertical vibration of the coil spring 60 is restricted here, so that the coil spring 60 itself expands and contracts. The expansion and contraction movement of the coil spring 60 eliminates clogging and lumps of the powder in the hopper, and it is possible to stably transfer a certain amount of powder to the entrance of the powder injection tube 42.
[0069]
The rotating shaft 50 is hollow and has a plurality of air injection holes 51.
[0070]
The rotary shaft 50 is connected to the air supply pipe 41 via the rotary joint 55, and when the air supply valve 43 is opened, air is supplied in the direction of the white arrow so that air is injected from the plurality of air injection holes 51. It has become. Then, in the spiral groove of the thread cutting 52a to the entrance of the powder injection tube 42 by the above-mentioned mechanism, the transferred powder and the air injected from the air injection hole 51 are mixed, and the powder injection tube 42 is blown into the air (release process by air pressure). Here, the air supply pipe 41 and the air injection hole 51 correspond to the discharge means.
[0071]
Then, the powder is supplied in the form of a spray in the direction of the black arrow, and the powder is supplied from the tip of a nozzle (not shown). As the nozzle, a conventionally known spray nozzle can be used. Further, by providing a suction nozzle or the like in the vicinity of the injection nozzle and collecting the scattered powder and returning it to the hopper 40, the powder can be recycled. Furthermore, by providing an air supply unit for supplying air into the powder injection pipe 42 or vibration applying means for vibrating the powder injection pipe 42 at one to a plurality of locations in the middle of the powder injection pipe 42, It is possible to stably supply the powder without clogging.
[0072]
In the powder supply apparatus of FIG. 8, it is possible to simultaneously perform the discharging step while performing the stirring step. Further, by performing the stirring step and the discharging step at the same time, it is possible to achieve a stable powder supply without clogging. Further, it is effective to prevent clogging of the powder not to be bent as a straight tube between the connecting portion of the powder injection tube 42 and the hopper 40 and a fixed length L. The fixed length L varies as appropriate depending on the physical properties of the powder, air pressure, and the like, but is preferably 50 mm or more to the entire length of the powder injection tube 42.
[0073]
When the powder used in this powder supply apparatus is a lubricant, it can be used as a lower lubricant supply means or a material surface lubricant supply means of the tablet forming apparatus of the present invention. Is preferable in manufacturing.
[0074]
FIG. 9 shows a static eliminator that can be preferably used in the powder supply apparatus of the present invention.
[0075]
The member number 71 is a light bulb, preferably a fluorescent lamp, and the static electricity generated by the powder supply device or the like is transmitted to the terminal of the fluorescent lamp 71 through the electric discharge line 77a or 77b, and is emitted and consumed as electric power. is there. By connecting the coil 72 to both terminals or one terminal of the fluorescent lamp 71, static electricity can be converted into light emission more efficiently.
[0076]
The fluorescent lamp 71 is wrapped with a cushion 73 for protection, and further covered with a metal outer cylinder 75 via a filler 74. Both ends of the outer cylinder 75 are wire meshes 76 that can take out the electric discharge wires 77 a and 77 b out of the electric discharge device 70. The static elimination wire 77a may be connected to the powder supply device, and the static elimination wire 77b may be connected to or wound around the outer cylinder 75 to neutralize the static elimination device 70 itself.
[0077]
FIG. 10 is a schematic view showing another embodiment of the powder supply apparatus of the present invention. In the figure, members having the same numbers as those in FIG. 8 are the same as those in FIG.
[0078]
The powder supply apparatus in FIG. 10 extends the rotating shaft 50 upward and protrudes upward from the hopper 40, and rotates the rotating shaft 50 (Ra) by a driving source (not shown) on the upper side. Air is also blown by the upper rotary joint 55, the air supply pipe 41 and the air supply valve 43.
[0079]
In addition to supplying air to the rotating shaft 50, air is separately blown into the hopper 40 (air supply pipe 41a and air supply valve 43a) or air is blown into the powder injection pipe 42 (air supply pipe 41b and air supply). By performing the valve 43b), it is possible to adjust the supply amount of powder (concentration adjustment).
[0080]
FIG. 11 is a schematic view showing another embodiment of the powder supply apparatus of the present invention. In the figure, members having the same numbers as those in FIG. 8 or 10 are the same as those in FIG. 8 or FIG.
[0081]
Similarly to FIG. 10, the powder supply apparatus of FIG. 11 extends the rotating shaft 50 upward, and rotates the rotating shaft 50 and supplies air on the upper side of the hopper 40. In the powder supply apparatus of FIG. 11, the powder injection tube 42 has a rotating shaft 50b and is rotated in the direction of Rb by a drive source (not shown) via a rotary joint 55b. Similar to the rotary shaft 50, the rotary shaft 50b has a thread 52c that scrapes and transfers the powder efficiently. It is hollow and has a plurality of air injection holes 51b. Air is blown into the rotary shaft 50b by an air injection pipe 41b and an air supply valve 43b to assist the supply of powder. With this configuration, the powder can be supplied smoothly and without clogging. Also, the concentration of the powder can be adjusted.
[0082]
FIG. 12 is a schematic view showing another embodiment of the powder supply apparatus of the present invention. In the figure, members having the same numbers as those in FIG. 8, 10 or 11 are the same. Similarly to FIG. 10 or FIG. 11, the powder supply device of FIG. 11 extends the rotary shaft 50 upward, and rotates the rotary shaft 50 and supplies air on the upper side of the hopper 40.
[0083]
In the powder supply apparatus of FIG. 12, the lower end portion of the rotary shaft 50 is open, and a connecting portion 50c made of a flexible material and an air tube 50d connected to the connecting portion 50c are placed in the powder injection tube 42. It is settled. The air tube 50d is provided with a plurality of pores 41c from which air can be ejected to extrude powder. The air tube 50d may be connected to an injection nozzle for injecting powder, or may be interrupted in the middle of the powder injection tube 42. When it is necessary to bend the powder injection tube 42 depending on the installation position and the injection direction of the powder supply device, some connecting portions 50c made of a flexible material are provided in the middle of the air tube 50d. You may make it connect with. Even with this configuration, it is possible to provide a powder supply device that is less likely to be clogged or have powder stagnation.
[0084]
By using the characteristic parts of the respective powder supply apparatuses shown in FIGS. 8, 10, 11 and 12 in appropriate combinations, a powder supply apparatus adapted to the use conditions can be configured.
[0085]
When the average particle size of the powder (preferably lubricant) used in the powder supply apparatus of the present invention is 125 μm or less, there is no clogging and a uniform amount can be injected, and the powder supply The effect of the apparatus can be fully exhibited. A more effective effect can be expected when the particle size of the powder is 125 μm or less and 90% by weight or more.
[0086]
In addition, when powder is injected and supplied by pneumatic pressure using the powder supply device, the powder supply device is clogged so that the temperature of the air is 10 to 30 ° C. and the humidity is 40% Rh or less. And a uniform amount of stable injection can be achieved.
[0087]
The tablet forming method using the tablet forming apparatus and the powder supplying method using the powder supplying apparatus of the present invention can be applied to any tablet, but can be preferably applied particularly to tablet formation of processing agents for photographic materials. .
[0088]
The compounds represented by the general formulas [I] to [VI] are listed below as examples of preferable lubricants for tableting a photographic light-sensitive material processing agent.
[0089]
The compound represented by the general formula [I] (surfactant, fluoroanionic surfactant) will be described.
[0090]
[Chemical 1]

[0091]
[Wherein Rf represents a saturated or unsaturated alkyl group containing at least one fluorine atom, X represents a sulfonamide,
[0092]
[Chemical 2]

[0093]
Y represents an alkylene oxide group or an alkylene group, and Rf ′ represents a saturated or unsaturated hydrocarbon group containing at least one fluorine atom. A is -SO_ThreeM, -OSO_ThreeM, -COOM, -OPO_Three(M₁) (M₂), -PO_Three(M₁) (M₂) And the like, M, M₁, M₂Is H, Li, K, Na or NH_FourM represents 0 or 1, and n represents 0 or an integer of 1 to 10. ]
In the general formula [I], Rf represents a saturated or unsaturated alkyl group containing at least one fluorine atom (for example, an alkyl group, an alkenyl group, an alkynyl group), preferably 4 to 12 carbon atoms, more preferably carbon. It is an alkyl group of several 6-9. A is preferably -SO_ThreeM, M, M₁, M₂Is preferably Li, K, Na, most preferably Li. m represents 0 or 1, and n represents 0 or an integer of 1 to 10, preferably m = 0 and n = 0.
[0094]
Although the typical exemplary compound represented with general formula [I] below is shown, it is not restricted to this.
[0095]
[Chemical Formula 3]

[0096]
[Formula 4]

[0097]
Of the above compounds, particularly preferred are (I-1), (I-2), and (I-4).
[0098]
These compounds can be synthesized by ordinary methods and can also be obtained as commercial products.
[0099]
Next, the lubricant (surfactant) represented by the general formula [II] will be described.
[0100]
[Chemical formula 5]

[0101]
In the above general formula [II], R₁Represents an alkyl group or an alkenyl group, R₂Represents a hydrogen atom, an alkyl group or a hydroxyalkyl group, R_ThreeAnd R_FourIs independently a hydrogen atom, a hydroxyl group, an alkyl group or —COOM₂(M₂Represents a hydrogen atom or an alkali metal atom), and X represents —CO— or —SO.₂-Y represents -O-, -S- or -CONR._Five-(R_FiveRepresents a hydrogen atom, an alkyl group or a hydroxyalkyl group), M₁Represents a hydrogen atom or an alkali metal atom, l represents 0 or 1, m represents an integer of 0 to 2, and n represents an integer of 1 to 3.
[0102]
R₁Is preferably a linear or branched alkyl or alkenyl group having 5 to 20 carbon atoms, and R₂Is preferably a hydrogen atom, a linear or branched alkyl group having 1 to 5 carbon atoms, or a hydroxyalkyl group.
[0103]
Next, specific compound examples of the compound represented by the general formula [II] are shown below.
[0104]
[Chemical 6]

[0105]
[Chemical 7]

[0106]
[Chemical 8]

[0107]
[Chemical 9]

[0108]
In addition to the above compounds, exemplified compounds [II] -1 to 55 described in JP-A No. 62-56961, pages 4 to 6 can be used.
[0109]
The above exemplified compounds are known compounds or are commercially available and can be obtained by ordinary routes.
[0110]
Next, the lubricant (surfactant) represented by the general formula [III] or [IV] will be described.
[0111]
[Chemical Formula 10]

[0112]
Where R₁, R₂, R_Three, R_FourAnd R_FiveEach represents an alkyl group, an aralkyl group, an alkenyl group, a styryl group, or a cinnamyl group, each of l1, l2, l3, l4, and l5 represents an integer of 0 or 1; However, R_ThreeIs an alkyl group and l3 is 1, at least one of l1, l2, l4, and l5 is 1. When l1, l2, l3, l4, and l5 are 0, the corresponding R₁, R₂, R_Three, R_FourAnd R_FiveIs a hydrogen atom.
[0113]
In the above formula, R₁, R₂, R_Three, R_FourAnd R_FiveThe alkyl group represented by formula (1) has 1 to 20 carbon atoms, and may be either a chain or a cyclic group. The chain group includes a straight chain and a branched one, specifically Examples include methyl, ethyl, n-propyl, i-propyl, butyl, t-butyl, sec-butyl, amyl, hexyl, heptyl, octyl, nonyl, decyl, octadecyl and the like. R₁, R₂, R_Three, R_FourAnd R_FiveIs a group having 7 to 20 carbon atoms, and specific examples thereof include benzyl, phenethyl, dibenzyl, 2-naphthylmethyl and the like.
[0114]
R₁, R₂, R_Three, R_FourAnd R_FiveAre those having 3 to 20 carbon atoms, and specific examples include allyl, 4-hexenyl, 4-decenyl, 9-octadecenyl and the like.
[0115]
The aromatic ring of the aralkyl group and the styryl group can have a substituent. Examples of the substituent include an alkyl group (for example, each group such as methyl, ethyl, propyl, t-amyl, nonyl), an alkoxy group (for example, Methoxy, ethoxy, propoxy, 2-ethoxyethoxy and the like), aryloxy groups (for example, phenoxy, p-tolyloxy, o-chlorophenoxy and the like) and the like. Specific examples include groups such as p-methoxybenzyl, 2,4-dimethylbenzyl, p-phenoxyphenethyl and p-butylstyrene.
[0116]
Embedded image

[0117]
In the formula, R is an alkyl group which may have a linear or branched substituent having 4 to 25 carbon atoms, or
[0118]
Embedded image

[0119]
(However, R₁₁And R₁₂Each represents a hydrogen atom or an alkyl group having 1 to 20 carbon atoms which may have a substituent, and l represents an integer of 0 to 4). n and m each represents 0 or an integer of 1 to 25, but are not 0 at the same time. A and B are each
[0120]
Embedded image

[0121]
May be the same or different (provided that n1, m1 and l1 represent 0, 1, 2 or 3, respectively, but m1 in A and B are not simultaneously 0 and n or m is When it is 0, m1 is not 0). D represents a hydrogen atom.
[0122]
Examples of the compound represented by the general formula [III] or [IV] are listed below.
[0123]
Embedded image

[0124]
Embedded image

[0125]
Embedded image

[0126]
Embedded image

[0127]
Embedded image

[0128]
Embedded image

[0129]
Next, the lubricant (surfactant) represented by the general formula [V] will be described.
[0130]
Embedded image

[0131]
[In the formula, R₁Represents a monovalent organic group, R₂Represents an ethylene group or a propylene group, and m represents an integer of 4 to 50. X₁Is a hydrogen atom, -SO_ThreeM or -PO_ThreeRepresents M. Where M is a hydrogen atom, an alkali metal atom or -NH._FourRepresents. ]
Next, the compound represented by the general formula [V] will be described further. R in the general formula [V]₁Is a monovalent organic group such as an alkyl group having 6 to 20 carbon atoms, preferably 6 to 12 carbon atoms, and represents hexyl, heptyl, octyl, nonyl, decyl, undecyl, dodecyl or the like. Or an aryl group substituted with an alkyl group having 3 to 20 carbon atoms, preferably an alkyl group having 3 to 12 carbon atoms, and propyl, butyl, pentyl, hexyl, heptyl, octyl, nonyl , Decyl, undecyl or dodecyl. The aryl group is phenyl, tolyl, xinyl, buphenyl or naphthyl, and is preferably phenyl or tolyl. The position at which the alkyl group is bonded to the aryl group may be in the ortho, meta, or para position. R₂Represents an ethylene group or a propylene group, and m represents an integer of 4 to 50. X₁Is a hydrogen atom, -SO_ThreeM or -PO_ThreeM₂M represents a hydrogen atom, an alkali metal atom (Na, K, Li or the like) or —NH_FourRepresents.
[0132]
Specific examples of the compound represented by the general formula [V] are shown below.
[0133]
Embedded image

[0134]
Embedded image

[0135]
Next, the lubricant (surfactant) represented by the general formula [VI] will be described.
[0136]
Formula (VI)
R- (O)_xS_yO_zM
[In the formula, R represents a substituted or unsubstituted aliphatic group, aromatic group or heterocyclic group, x represents 0 or 1, y represents 1 or 2, z represents an integer of 2 to 8, and M represents a cation. Represents. ]
In the general formula [VI], examples of the aliphatic group represented by R include an alkyl group, an alkenyl group, and an alkynyl group. Examples of the alkyl group include methyl, ethyl, i-propyl, butyl, t-butyl, Examples include pentyl, cyclopentyl, hexyl, cyclohexyl, octyl, dodecyl and the like. These alkyl groups further include halogen atoms (for example, halogen atoms such as chlorine, bromine and fluorine), alkoxy groups (for example, methoxy, ethoxy, 1,1-dimethylethoxy, hexyloxy, dodecyloxy and the like), aryloxy Groups (for example, groups such as phenoxy and naphthyloxy), aryl groups (for example, groups of phenyl, naphthyl and the like), alkoxycarbonyl groups (for example, groups of methoxycarbonyl, ethoxycarbonyl, butoxycarbonyl, 2-ethylhexylcarbonyl and the like), Aryloxycarbonyl groups (eg, groups such as phenoxycarbonyl and naphthyloxycarbonyl), alkenyl groups (eg, groups such as vinyl and allyl), heterocyclic groups (eg, 2-pyridyl, 3-pyridyl, 4-pyridyl, morpholyl, Piperidine, piperazil, pipe Each group such as midine, pyrazoline and furyl), alkynyl group (eg propargyl group etc.), amino group (eg amino, N, N-dimethylamino, anilino etc.), cyano group, sulfoamide group (eg methylsulfonylamino) , Each group such as ethylsulfonylamino, butylsulfonylamino, octylsulfonylamino, phenylsulfonylamino, etc.).
[0137]
Examples of the alkenyl group include a vinyl group and an allyl group, and examples of the alkynyl group include a propargyl group.
[0138]
Examples of the aromatic group represented by R include a phenyl group and a naphthyl group.
[0139]
Examples of the heterocyclic group represented by R include a pyridyl group (each group such as 2-pyridyl, 3-pyridyl, 4-pyridyl), thiazolyl group, oxazolyl group, imidazolyl group, furyl group, chenyl group, pyrrolyl group, Examples include a pyrazinyl group, a pyrimidinyl group, a pyridazinyl group, a selenazolyl group, a sulfolanyl group, a piperidinyl group, a pyrazolyl group, and a tetrazolyl group.
[0140]
The above alkenyl group, alkynyl group, aromatic group, and heterocyclic group are all substituted with an alkyl group represented by R, a substituent of the alkyl group, a group shown as a substituent atom, a group similar to the atom, or an atom. be able to.
[0141]
The cation represented by M is preferably a metal ion or an organic cation. Examples of metal ions include lithium ions, sodium ions, and potassium ions. Examples of organic cations include ammonium ions (each ion such as ammonium, tetramethylammonium, and tetrabutylammonium) and phosphonium ions (for example, tetraphenylphosphonium). Ions), guanidyl ions, and the like.
[0142]
Specific examples of the compound represented by the general formula [VI] are shown below, but the present invention is not limited thereto.
[0143]
VI-1 C₂H_FiveSO_ThreeNa
VI-2 CH_Three(CH₂)₆SO_ThreeNa
VI-3 CH_Three(CH₂)₇SO_ThreeNa
VI-4 CH_Three(CH₂)_FiveOSO_ThreeNa
VI-5 CH_Three(CH₂)₆OSO_ThreeNa
VI-6 CH_Three(CH₂)₇OSO_ThreeNa
VI-7 CH_ThreeO (CH₂)₂SO_ThreeNa
[0144]
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[0145]
Moreover, in the said tableting, saccharides are preferable as a binder previously mixed in a material with the said lubricant, The following can be used.
[0146]
The term “saccharide” as used herein refers to a monosaccharide, a polysaccharide in which a plurality of these are glycosided to each other, and a degradation product thereof.
[0147]
The monosaccharide is a general term for a wide range of derivatives such as single polyhydroxyaldehyde, polyhydroxyketone and their reduced derivatives, oxidized derivatives, deoxy derivatives, amino derivatives and thio derivatives.
[0148]
Many sugars have the general formula CnH₂Although represented by nOn, a compound derived from a sugar skeleton represented by this general formula is also defined as a monosaccharide in the present invention.
[0149]
Among these monosaccharides, preferred are sugar alcohols obtained by reducing the aldehyde group and ketone group of the sugar to give primary and secondary alcohol groups, respectively.
[0150]
Polysaccharides include celluloses, starches, glycogens and the like. Celluloses include derivatives such as cellulose ethers in which some or all of the hydroxyl groups are etherified. It includes dextrins, which are various decomposition products leading to maltose. Cellulose may be in the form of an alkali metal salt from the viewpoint of solubility.
[0151]
Those polysaccharides preferably used are celluloses, dextrins and cyclodextrins, and more preferably cyclodextrins.
[0152]
Specific exemplary compounds of monosaccharides according to the present invention are shown below.
[0153]
[Exemplary compound]
B- (1) Glyceraldehyde
B- (2) Dihydroxyacetone (including dimer)
B- (3) D-erythrose
B- (4) L-erythrose
B- (5) D-Threose
B- (6) L-Treose
B- (7) D-ribose
B- (8) L-ribose
B- (9) D-arabinose
B- (10) L-arabinose
B- (11) D-xylose
B- (12) L-xylose
B- (13) D-lyxose
B- (14) L-lyxose
B- (15) D-xylulose
B- (16) L-xylulose
B- (17) D-ribulose
B- (18) L-ribulose
B- (19) 2-Deoxy-D-ribose
B- (20) D-Allose
B- (21) L-Allose
B- (22) D-altrose
B- (23) L-altrose
B- (24) D-glucose
B- (25) L-glucose
B- (26) D-Mannose
B- (27) L-Mannose
B- (28) D-Growth
B- (29) L-Growth
B- (30) D-Idose
B- (31) L-Idose
B- (32) D-galactose
B- (33) L-galactose
B- (34) D-talose
B- (35) L-talose
B- (36) D-Kinoboth
B- (37) Digitalose
B- (38) Digitoki sauce
B- (39) Simarose
B- (40) D-sorbose
B- (41) L-sorbose
B- (42) D-Tagatose
B- (43) D-Fucose
B- (44) L-Fucose
B- (45) 2-deoxy-D-glucose
B- (46) D-psicose
B- (47) D-fructose
B- (48) L-fructose
B- (49) L-Rhamnose
B- (50) D-Glucosamine
B- (51) D-Galactosamine
B- (52) D-Mannosamine
B- (53) D-glycero-D-galactoheptose
B- (54) D-glycero-D-mannoheptose
B- (55) D-glycero-L-mannoheptose
B- (56) D-glycero-D-gloheptose
B- (57) D-glycero-D-idheptose
B- (58) D-glycero-L-glucoheptose
B- (59) D-Glycero-L-taroheptose
B- (60) D-Altoroheptulose
B- (61) D-Mannoheptulose
B- (62) D-Altro-3-heptulose
B- (63) D-glucuronic acid
B- (64) L-glucuronic acid
B- (65) N-acetyl-D-glucosamine
B- (66) Glycerin
B- (67) D-Trait
B- (68) L-Trait
B- (69) Elite (trade name, Mitsubishi Chemical Food Erythritol)
B- (70) D-Arabit
B- (71) L-Arabit
B- (72) Adnit
B- (73) Xylit
B- (74) D-Sorbit
B- (75) L-Sorbit
B- (76) D-man knit
B- (77) L-Man knit
B- (78) D-exit
B- (79) L-Exit
B- (80) D-Talit
B- (81) L-Talit
B- (82) Zulsit
B- (83) Allozulcit
Among these exemplified compounds, sugar alcohols preferably used are B- (66) to (83), and more preferably B- (69) and (74) to (83).
[0154]
Specific exemplary compounds of polysaccharides and sugar decomposition products according to the present invention are shown below.
[0155]
C- (1) Maltose
C- (2) Cellobiose
C- (3) Trehalose
C- (4) Gentiobiose
C- (5) Isomaltose
C- (6) Lactose
C- (7) Raffinose
C- (8) Gentianose
C- (9) Stachyose
C- (10) Xylan
C- (11) Alabang
C- (12) Glycogen
C- (13) Dextran
C- (14) Inulin
C- (15) Leban
C- (16) Galactan
C- (17) Agarose
C- (18) Amylose
C- (19) Sucrose
C- (20) Agarobiose
C- (21) Methylcellulose
C- (22) Dimethylcellulose
C- (23) Trimethylcellulose
C- (24) Ethylcellulose
C- (25) Diethylcellulose
C- (26) Triethylcellulose
C- (27) Carboxymethylcellulose
C- (28) Carboxyethyl cellulose
C- (29) aminoethylcellulose
C- (30) Hydroxymethylcellulose
C- (31) Hydroxyethyl methylcellulose
C- (32) Hydroxypropylcellulose
C- (33) Hydroxypropyl methylcellulose
C- (34) Hydroxypropyl methylcellulose acetate succinate
C- (35) Carboxymethyl hydroxyethyl cellulose
C- (36) α-dextrin
C- (37) β-dextrin
C- (38) γ-dextrin
C- (39) σ-dextrin
C- (40) ε-dextrin
C- (41) α-limit dextrin
C- (42) β-limit dextrin
C- (43) phosphorylase limiting dextrin
C- (44) soluble starch
C- (45) Thin Nori starch
C- (46) White dextrin
C- (47) Yellow dextrin
C- (48) British gum
C- (49) α-cyclodextrin
C- (50) β-cyclodextrin
C- (51) γ-cyclodextrin
C- (52) Methyl-α-cyclodextrin
C- (53) Methyl-β-cyclodextrin
C- (54) Methyl-γ-cyclodextrin
C- (55) Hydroxypropyl-α-cyclodextrin
C- (56) Hydroxypropyl-β-cyclodextrin
C- (57) Hydroxypropyl-γ-cyclodextrin
C- (58) maltocyclodextrin
Saccharides exist widely in nature, and commercial products are easily available. Various derivatives can also be easily synthesized by performing reduction, oxidation or dehydration reaction.
[0156]
As commercial products, as cyclodextrins, α-100H, β-100, γ-100, K-100, Isoelite P, Isoelite PH, Methyl-β-CD, Hydroxypropyl-manufactured by Shimizu Minato Sugar Co., Ltd. Beta-CD and starch degradation products are Pine Flow, Paindex Series, Foodtex, Max 100, Glister P, TK-16, MPD, H-PDX, Stacodex, Nippon Oil & Fats manufactured by Matsutani Chemical Industry Co., Ltd. Examples include the Oil Q series manufactured by Co., Ltd.
[0157]
Preferred compounds as other binders are those represented by the following general formula.
[0158]
HO- (A₁-O)_l1-(A₂-O)_l2-(A_Three-O)_l3-H
Where A₁, A₂, A_ThreeEach represents a substituted or unsubstituted linear or branched alkylene group, which may be the same or different.
[0159]
Examples of the substituent include a hydroxy group, a carboxy group, a sulfonyl group, an alkoxy group, a carbamoyl group, and a sulfamoyl group.
[0160]
What is preferably used is A₁, A₂, A_ThreeAre each unsubstituted. Most preferred is A.₁, A₂, A_ThreeIs -CH₂CH₂-, -CH (CH_Three) -CH₂-.
[0161]
l1, l2, and l3 each represents 0 or an integer of 0 to 500. However, l1 + l2 + l3 ≧ 5.
[0162]
Among these, at least one of l1, l2, and l3 is preferably 15 or more, and more preferably 20 or more.
[0163]
Among the compounds represented by the general formula, polyethylene glycol (sometimes referred to as PEG) is most preferable.
[0164]
In the case of polyethylene glycol, those having an average molecular weight in the range of 2000 to 20000 are preferred, and those in the range of 3000 to 15000 are particularly preferred.
[0165]
In the present invention, in the case of tablet formation of a processing agent for photographic light-sensitive materials, it can be preferably applied to tablet formation of a color developer, a black and white developer, a bleaching agent, a fixing agent, a bleach-fixing agent, and a stabilizer.
[0166]
Among the paraphenylene color developing agents that are color developers, compounds that exhibit the effects of the present invention can be exemplified by compounds described in paragraph Nos. 0083 to 0086 of JP-A-5-232656. Compounds are preferred.
[0167]
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[0168]
Among the hydroxylamines and derivatives thereof, compounds that exhibit the effects of the present invention are exemplified by compounds described in paragraph Nos. 0100 to 0130 of JP-A-5-232656, and among them, bis (sulfoethyl) hydroxylamine 2 Sodium salt and hydroxylamine are preferred.
[0169]
Among the alkali metal carbonates, examples of the compound that exhibits the effects of the present invention well include the compounds described in paragraph No. 0105 of JP-A-5-232656. A particularly preferred compound is potassium carbonate.
[0170]
Among the ferric complex salts of aminopolycarboxylic acid, examples of the compound that exhibits the effect of the present invention well include the compounds described in paragraph Nos. 0040 to 0110 of Japanese Patent Application No. 5-106278. Particularly preferred compounds are ferric complex salts of ethylenediaminetetraacetic acid, 1,3-propylenediaminetetraacetic acid and diethylenetriaminepentaacetic acid, respectively.
[0171]
As a developing agent that can be used for the developer for black and white, it is preferable to contain reductones described in Japanese Patent Application No. 11-91343. Of these, ascorbic acid or erythorbic acid (stereoisomerism) represented by D-1 or a salt thereof is particularly preferable.
[0172]
As the black-and-white fixing agent, those described in Japanese Patent Application No. 11-91343 are used as well. In particular, the fixing agent preferably contains a thiosulfate. Specifically, thiosulfate is used as a lithium, potassium, sodium, or ammonium salt, but sodium or potassium salt is preferable from the effect of the present invention.
[0173]
【The invention's effect】
Tablet forming method and tablet capable of efficiently and easily supplying a lubricant to the ridge when a tablet is formed by compressing a compression molding material using a tablet forming apparatus having an upper ridge and a lower ridge A molding apparatus, a powder supply method, and a powder supply apparatus could be provided.
[Brief description of the drawings]
FIG. 1 is a schematic view showing an embodiment of a tablet forming apparatus of the present invention.
FIG. 2 is a schematic perspective view showing an embodiment of the tablet forming apparatus of the present invention.
FIG. 3 is a schematic view for explaining a lubricant supply process by a lower lubricant supply means of the tablet forming apparatus of the present invention.
FIG. 4 is a schematic view showing a material supply process by a material supply means of the tablet molding apparatus of the present invention in the present invention.
FIG. 5 is a schematic diagram for explaining a material surface lubricant supply step by a material surface lubricant supply means of the tablet forming apparatus of the present invention.
FIG. 6 is a schematic view for explaining a compression molding process in the tablet forming apparatus of the present invention.
FIG. 7 is a schematic view showing a cleaning means applicable to the tablet forming apparatus of the present invention.
FIG. 8 is a schematic view showing an embodiment of the powder supply apparatus of the present invention.
FIG. 9 is a schematic view showing an embodiment of a static eliminator that can be used in the powder supply apparatus of the present invention.
FIG. 10 is a schematic view showing an embodiment of the powder supply apparatus of the present invention.
FIG. 11 is a schematic view showing an embodiment of the powder supply apparatus of the present invention.
FIG. 12 is a schematic view showing an embodiment of the powder supply apparatus of the present invention.
[Explanation of symbols]
1 Shimojo Lubricant Supply Department
2 Material supply section
3 Material surface lubricant supply section
4 First compression molding part (preload)
5 Second compression molding part (main pressure)
6 Discharge guide
7 Cleaning section
8a, 8b Dehumidification air spraying part
10 Turntable
11 Through hole
12 upper arm
13 Shimojo
14, 15 Eccentric roller
20 Shimojo lubricant supply means
25 Material surface lubricant supply means
30 Material supply means
40 hopper (powder storage means)
41 Air supply pipe
42 Powder injection tube
50 axis of rotation
51 Air injection hole
53a, 53b Stir bar
60 Coil spring
70 Static elimination device (static elimination means)

Claims (17)

A compression molding material is compressed between the upper and lower ridges using a tablet molding device having a through-hole and an upper and lower ridge that can reciprocate in the direction of the through-hole by sliding with the inner wall of the through-hole. In a tablet molding method for molding a tablet,
A material supplying step of supplying a compression molding material of powder or granules to a concave portion formed by the upper surface of the lower rod and the inner wall of the through hole, the lower rod being at a position below the upper end of the through hole; ,
On the surface of the compression molding material fed by the material supplying step, it possesses a material surface lubricant supplying step of supplying a lubricant which is a powder of a surfactant,
Further, the material surface lubricant supplying step for supplying the powder lubricant includes a stirring step for stirring the powder stored in the storage means in the storage means for storing the lubricant, and the storage means And a discharging step of taking out and discharging a part of the powder in the inside, wherein the charge is removed from the powder in the stirring step .   2. The tablet molding method according to claim 1, further comprising a lower glaze lubricant supplying step for supplying a lubricant to the upper surface of the lower glaze before the material supplying step.   The said lower arm lubricant supply process supplies lubricant to the upper surface of the lower arm at the position where the upper surface of the lower arm is below the upper end of the through hole. Tableting method.   In the lower glaze lubricant supplying step, the upper surface of the lower collar is flush with the upper end of the through hole, or the upper surface of the lower collar is on the upper side of the upper end of the through hole. The tablet forming method according to claim 2, wherein an agent is supplied.   5. The material supply step according to claim 1, wherein after the compression molding material is put into a concave portion formed by a lower heel and an inner wall of the through hole, the material is rubbed at the upper end of the through hole and quantified. The tablet molding method according to any one of the above.   6. The tablet molding method according to any one of claims 1 to 5, wherein the compression molding material is a solid photographic processing agent. A through-hole, and an upper and lower heel that can reciprocate in the direction of the through-hole by sliding with the inner wall of the through-hole, compressing a compression molding material between the upper and lower heels, In the tablet molding apparatus for molding, a material supply means for supplying a powder or granule compression molding material to a recess formed by the lower heel and the inner wall of the through hole, and a compression molding material supplied by the material supply means the lubricant is a powder of a surfactant possess the material surface lubricant supply means for supplying to the surface,
Further, the material surface lubricant supply means for supplying the powder lubricant includes a stirring means for stirring the powder stored in the storage means, and a storage means for storing the lubricant in the storage means. and a release means for releasing removed a portion of the powder, further tableting apparatus which is characterized in that have a charge removing means for neutralizing the powder.   The material supply means includes material input means for inputting a compression molding material into the concave portion, and material quantification means for slicing and quantifying the compression molding material charged by the material injection means at the upper end of the through hole. The tablet molding apparatus according to claim 7, wherein   The tablet molding apparatus according to claim 7 or 8, further comprising a lower glaze lubricant supplying means for supplying a lubricant to the upper surface of the lower glaze.   The lower arm lubricant supply means supplies the lubricant at a position where the upper surface of the lower arm is below the upper end of the through hole. Tableting equipment.   The lower arm lubricant supply means supplies the lubricant at a position where the upper surface of the lower arm and the upper end of the through hole are flush with each other or the upper surface of the lower arm is above the upper end of the through hole. The tablet molding apparatus according to any one of claims 7 to 10, wherein: The tablet forming method according to claim 1, wherein the stirring step and the releasing step are performed simultaneously. The tablet forming method according to claim 1 or 12, wherein in the releasing step, the powder is released by air pressure. The tablet molding method according to claim 13, wherein the temperature of the air for generating the air pressure is 10 to 30 ° C and the humidity is 40% Rh or less. The tablet molding method according to any one of claims 1, 13, and 14, wherein an average particle size of the powder is 125 µm or less. 8. The tablet molding apparatus according to claim 7, wherein the stirring means is a conductive stirrer and also serves as a static elimination means. The tablet forming apparatus according to claim 16, wherein the discharging means has a mechanism for discharging powder by air pressure.

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