TW464640B - Process for making a coated fertilizer - Google Patents

Process for making a coated fertilizer Download PDF

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Publication number
TW464640B
TW464640B TW086100585A TW86100585A TW464640B TW 464640 B TW464640 B TW 464640B TW 086100585 A TW086100585 A TW 086100585A TW 86100585 A TW86100585 A TW 86100585A TW 464640 B TW464640 B TW 464640B
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TW
Taiwan
Prior art keywords
fertilizer
urethane resin
granular
resin
processing temperature
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TW086100585A
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Chinese (zh)
Inventor
Hiroshi Nakamura
Fumio Nanbu
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Sumitomo Chemical Co
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    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05GMIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
    • C05G5/00Fertilisers characterised by their form
    • C05G5/30Layered or coated, e.g. dust-preventing coatings
    • C05G5/37Layered or coated, e.g. dust-preventing coatings layered or coated with a polymer

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  • Life Sciences & Earth Sciences (AREA)
  • Pest Control & Pesticides (AREA)
  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Fertilizers (AREA)

Abstract

This invention provides a method for producing a granular coated fertilizer coated with a thermosetting resin, which is characterized by the following steps carried out in the order. (1) Granular fertilizer is kept in rolling state. (2) An uncured liquid thermosetting resin is added in an amount to provide 1-10 μm layer thickness coated onto the granular fertilizer kept in the rolling state. (3) The surface of each fertilizer granule is coated with the uncured thermosetting resin while keeping the rolling state. (4) The uncured thermosetting resin is cured while keeping the rolling state of the granular fertilizer. (5) Steps from the step (1) to the step (4) are further repeated for one or more times. This invention provides the method for industrial advantageous production of a sustained release coated fertilizer that is free from defect of coating film by applying a thermosetting resin to fertilizer.

Description

經濟部中央橾準局員工消費合作祍印製 6 4 64 0 A7 B7五、發明説明(1 ) 窈明所醒的坊妬頜城 本發明係有闞緩效性(亦稱作遲效性)粒狀肥枓之製造 方法*尤指藉由氨基甲酸S樹脂或瑁氧樹胞予Μ樹脂被覆 的锾效性肥料之製造方法。 用樹脂戎蠼、或蹢黃等被覆粒狀粒子使成膠囊化以控 制肥料之溶出速度之所謂媛效性肥料•其歷史久遠*例如 日本特公昭40-28927號公報、特公昭44-28457號公報、特 公昭3 7 - 1 5 3 8 2轚公報或特公昭4 2 - 1 3 6 8 1號公報等·即揭示 有各種被S材抖或被覆方法。至於由被覆材為多元異氰酸 酯化合物及多元酵化合物之反應物而成的氨基甲酸酯樹脂 之被覆肥科,揭示於美園專利第3,26 4,089號公報,而同 樣的•環氧樹脂被覆材則揭示於美國專利第3,264,088虢 公報。至於以氨基甲酸酯樹脂為被覆材之被覆肥料之製造 方法方面,於日本特表平1-50066 1 «公報則揭示有Μ使異 氰酸酯化合物過董反應於尿素肥料表面上Κ形成基層之被 覆層(base coat),並於其上使多元酵化合物反應於上述 過董的異氰酸_基為持徵之技術。於日本特表平7-500560 號公報,則揭示有將多元異氰酸酯化合物及多元酵化合物 之混合樹脂進行各曆為10〜30w·之塗布,以胺霧(amine 處理並使各磨硬化為特擞之技術。 然而|利用該等技術,並未能充分滿足塗_被控制成 較少缺陷的肥料溶出之目的,或製造方法上亦需經由複雜 的裝置•步除,工業規横的製造上有多種不利的方面。 Ί I 'IT (請先鬩讀背面之注意事項再填寫本f ) 本紙張尺度適用t國國家標隼(CNS ) A4規格(210X297公釐) 3 38636 464640 A7 B7 經濟部中央標準局員工消費合作社印製 五、發明説明( 2 ) 發 明 欲 解 決 的 課 m 本 發 明 之 的 t 係 提 供 Η 热 固 性 樹 脂 被 覆 的 無 塗 m 缺 陷 之 級 效 性 被 覆 肥 料 之 製 造 方 法 較 有 利 於 工 業 規 模 的 製 造 〇 解 決 課 顆 的 手 1 本 發 明 人 等 為 解 決 上 述 課 題 > 經 精 心 研 究 结 果 完 成 本 發 明 0 本 發 明 係 如 下 所 述 亦 即 1 . 於 以 熱 固 性 樹 脂 被 覆 的 粒 狀 被 覆 肥 枓 之 製 造 方 法 其 特 徵 在 於 Μ 下 列 步 驟 顚 序 而 成 (1 ) 將 粒 狀 m 科 製 成 轉 動 狀 態 的 步 驟 > (2) 於 處 於 該 轉 動 狀 態 的 粒 狀 肥 料 上 添 加 層 厚 成 1 至 10 U «1之量的液狀未硬化热固性樹脂之步W (3) 保 持 著 該 粒 狀 把 料 之 轉 動 狀 態 而 kk 該 未 硬 化 热 固 性 樹 脂 被 覆 各 m 料 粒 子 表 面 之 步 驟 (4) 保 持 著 該 粒 狀 肥 料 於 轉 動 狀 態 、 使 該 未 硬 化 熱 固 性 樹 脂 硬 化 的 步 驟 (5) 進 一 步 重 複 上 迷 (1 )至U) 之 步 味 1次或1 次 Μ 上 的 步 驟 而 成 者 0 2 . 如 上 述 1 之 被 覆 m 料 之 製 造 方 法 其 特 擞 在 於 熱 固 性 樹 脂 為 瑁 氧 樹 脂 或 胺 鹿 樹 脂 0 3 . 如 上 述 2 之 被 覆 IB 料 之 製 造 方 法 • 其 特 激 在 於 胺 磨 樹 脂 係 由 以 多 元 異 氰 酸 化 合 物 多 元 酵 及 胺 催 化 劑 為 必 須 成 分 而 成 者 0 4 . 如 上 述 1、 2或 3 之 被 覆 m 枓 之 製 造 方 法 » 其 特 激 在 於 熱 本紙張尺度適用中國國家標準(CNS ) A4規格(210X297公釐) 經濟部中央標苹局員工消費合作社印繁 4 64 0 A7 B7五、發明説明(3 ) 固性樹脂之被覆加工溫度之凝膠時間為5分鐘以下。 琎明夕窖确噍楼 Μ下*詳细說明本發明。 將粒吠肥料製成可轉動態的步驟之方法,其裝置上並 未予特別限制,惟可採用公知、慣用者•惟可例示有盤型 、轉鼓型等之轉動造粒機或糖衣機、轉動流動層型或流動 層型之被覆機等。而且•以該裝置附設有加溫設備者•較 適用於被覆加工之高精度化或加工時間之調整。 所使用的粒狀肥料·不論為習知的耙料之粒狀物之任 一種均可。其具傾例,可例舉:尿素、疏酸技、氯化銨、 磷酸銨、硝酸銨、石灰氬、硝酸納、乙醛縮合尿素等之氮 質肥料、熗成磷肥、重加《酸石灰、混合《酸®料等磷酸 質肥料、氯化鉀、碕酸鉀苦土、碳酸氫鉀、矽酸押肥枓等 之鉀質脃枓、磷酸鉀肥枓、硝酸鉀®料等之化成肥枓、或 有機質肥料等:,進而將該等肥料之混合物藉由本身公知的 方法造粒的粒狀肥枓。粒狀肥料之粒徑並未予特別限定。 惟以1〜5m·為製造上較佳的範圍。’ 以下說明所使用的熱固性樹脂。熱固性樹脂|可使用 公知者•具艚而言•則可列舉計有:環氧樹脂、不飽和聚 酷樹脂、酚榭脂酵酸樹脂、二甲笨樹脂、三聚氰胺樹脂、 呋哺樹脂、矽氧樹脂等之熱固性樹脂*視必要時自該等之 中選擇二種以上並予混合使用亦可。該等之中•由作業性 *性能方面覯之Μ環氧樹脂或胺酯澍脂為較佳,Μ於多元 異氰酸酯樹脂及多元酵化合物中配合有胺催化劑之氨基甲 (請先閱讀背面之注意事項再填寫本頁) 本紙乐尺度適用中國國家標準(CNS ) Λ4規格(2Ι〇Χ 297公釐) 5 38 6 36 4 經濟部中央標準局員工消費合作社印製 6 4 640 A7 B7五'發明説明(4 ) 酸酯(urethane)樹賭為尤佳。 就氨基甲酸海樹脂進一步說明之,則氨基甲酸樹脂為 藉由多元異氰酸_化合物及多元酵化合物經反應並予三次 元交瞄的樹脂之瘅稱|惟本發明所指的未固化氨基甲酸酷 樹脂•係指該多元異氰酸酯化合物及該多元酵化合物之混 合物,完全未經反應或將未予三次元化的程度事先使部分 反應者。為促進反應,而可先添加催化劑一事亦為有用的 技術。至於該未固化樹胞之形態,亦可為無溶劑型、溶液 型、水系乳液型等之任一者•惟尤K無溶«型且在加工溫 度時為液狀者較瘸合。 多元異氰酸g化合物並未予特別限定·惟若予具體的 例示時•則可例舉計有:甲笨二異氰酸醱(亦稱作TDD · 二笨基甲烷二異氣酸酯(亦稱作MD[)、蔡二異氰酸_、瞄 甲苯胺異氰酸酯、六亞甲二異氰酸酯、異佛爾酮二異氰酸 _、二甲笨二異氣酸酷等。視必要時可採用該等之混合物 r 。其中,以HDI或TDI或由該等衍生的寡聚艚較適合使用。 至於多元酵化合物方面*並未予待別限定,惟可列舉 計有採用例如多元酵、胺基酵、胺作為引發劑,對環氧乙 烷或環氧丙烷經予聚加成而得的聚醚聚醇、對四氫呋喃經 予聚合而得的聚四亞甲K二酵等之聚醚型多元酵、多元酵 及聚醚多元酵與羧酸化合物經予反睡等方法而得的聚酯型 多元酵等。此外,考慮生物分解性時亦可採用含有0H基之 天然物或其改質物。 至於反應催化_·可採用公知慣用者·惟具體的例示 本紙張尺度適用中國國家標準(CNS) A4規格(210XW7公釐) 6 3 8 6 3 6 氣------訂 (請先閱讀背面之注意事項再填寫本頁) 經濟部中央樣準局貝工消费合作社印製 6 4 6 4 0 A7 B7五、發明説明(5 ) 之,則以三伸乙二胺、N -甲基嗎福林、Η,Η -二甲基嗎福林 、二吖雙十一碳烯、2,4,6 -蓥(二甲基胺甲基)酚等胺催化 劑較遴合使用。 再者*視必要•亦可使用顔料或染料,或滑石粉、雲 母、矽石、碳黑、樹脂粉末等無機,有機粉粒體填充劑。 本發明之製造方法包括將在轉動狀態之粒狀肥料設定 於指定的加工溫度之步睇。至於加工溫度*上述未固化樹 脂之凝瞬時間在5分鐘以内*更宜在3分鐘Μ内。對添加上 述未固化樹脂並予被覆於在該轉動狀態之粒子上的步驟* 偽藉由將事先S合、绲合有硬化劑或催化劑之樹脂組成物 予Μ滴下、嗅霧等方法而投人者。戎亦可為分別添加主劑 、硬化劑、催化劑等並Μ樹脂被覆肥料粒子之際使各成分 混合的方法。 且*對經予被覆的樹脂之粘度*為於短時間内均勻的 被覆粒狀耙料s Μ於被覆步驟之溫度時之該未硬化樹脂之 被覆初期之黏度為由5CP至500CP之範圍内為佳;Μ自10CP 至100CP之範圍為最佳。 一次投人的樹脂量你予調整成纆予被覆的膜厚在1〜 10/i ·。Μ在2" _以上6w ·Κ下之範圍為最佳。在1ί/ β以 下時*被覆次數通多則不利於工業規棋的製造。另一方面 ,若嫫厚在l〇w·以上時,則會產生Μ下的問圉。 將液狀的未硬化樹腊投人於轉動狀態之肥料·首先由 於粒子之轉動會於粒子表面上形成均勻的未硬化樹脂層| 同時進行樹脂之硬化反應。此時1樹脂會睹著反(8之進行 (請先聞讀背面之注意事項再填寫本頁) 本紙張尺度適用中國國家標準(CNS ) Α4規格(210X29?公釐) 7 3 8 6 36 經濟部中央標隼局員工消費合作社印製 6 4 64 0 A7 B7五、發明説明(6 ) 而慢慢增加黏度、形成帶有電躲性。此時,樹脂之黏著性 增加而_由樹腊使肥料粒子相互黏著、並由多數的粒子形 成塊狀物;不致崩解成原來的粒子、即使崩解亦有對樹脂 表面造成損傷的顔慮。樹脂模在Μ上時|舍引起上 述般的問題*而未眭以硬化樹脂均匀的被覆涸別的粒子。 本發明人等認為若樹脂_較厚時,則由於粒子轉動使相互 粘著的粒子間拉離的力t不足所致。不論如何*欲一次Κ 較厚的樹脂膜被覆的情形* Μ —般的轉動型被覆法會產生 上述的不妥情形,要製造所期待的樹脂被覆的粒吠肥料則 有困_。 本發明之製造方法*係多次重複上逑步嫌而製得以所 期待的_厚被覆樹脂之粒狀肥枓。製品之被覆樹脂膜厚雖 依所期待的溶出樣式而異•惟通常係M20w*至200μ·為 較缠當的範圍。 經予被覆至最後一 1的被覆肥料1視必要•由於樹脂 會完全硬化•故亦可包括可予完全保持於指定的硬化溫度 之步驟。此外•為防止肥料之固结或狍肥之際之浮起,於 該被覆钯料表面上添加黏土等無機微粉亦為有用的技街。 實…豳I Μ下Μ實拖洌更具體的說明本發明,惟本發明並非受 此等實施例所限定者。 置..施軋丄 將2kg粒吠尿素(平均粒徑3.4·*)倒人附設有熱風發生 器之可控溫的傾斜盤型轉動造粒機(盤徑520»·),令其Μ (請先聞讀背面之注意事項再填寫本頁} 本紙張尺度適用中國國家標準(CNS ) Α4規格(210X297公釐) 8 3 8 6 3 6 464640 A7 經濟部中央標準局員工消費合作杜印繁 B7五、發明説明(7 ) 20〜30γρ·旋轉使粒狀肥料成為轉動狀態。加熱該裝置並 保持倒人的粒狀尿素之溫度於70〜75 t1 »並保持轉動狀態 。授拌混合被覆樹脂Polymeric MPI (住友Bayer urethane 公司製造,商 名:Sunidure 44V10M.7s ,支 _聚醚型多元醇(住友Bayer Urethane公司製造*商品名 :Sueiphene TM>5.3g及胺催化劑2,4,6-S(三甲基胺基甲 基)酚0.U*並予立即加人已被加溫且於轉動狀態之該粒 狀尿素内。該未硬化氨基甲酸酷樹脂組成物於室溢係液狀 。且,本實豳例所用的未硬化氨基甲__樹腊之凝孩時間 於65 υ為2分30秒。此外,已投入的樹脂量|對移入的肥 料為0.5重量% •被覆該粒徑之肥料之情形被覆樹脂之_ 厚成約3. lw·。以目視親察方式,已投入的樹脂被確認於 約30秒約略均勻的被覆於粒狀肥枓表面上》樹脂投人後3 分鐘後,取出一部分的試枓*認出樹脂廃於幾乎失去黏著 性之狀態。每隔3分》重複上述步驟16次,對肥科進行8重 * 量《被覆。最後將已被覆該樹脂之肥料在70〜75它保持10 分鏡,製出樹脂完全硬化的已被覆氨基甲酸酷樹脂之粒吠 肥料。全部步软之所需時間為約1小時,為有利於工菜規 模製造的方法。藉由該步嫌之樹脂被覆量由該被覆吧料截 面之SEM觀察可知樹脂膜之厚度約·。 對由上述步驟製得的樹睢被覆粒狀肥料評估25亡之IS 枓溶出行為。结果•該被覆尿素於約85日間溶出80½之肥 枓成分*確認出具有足夠的鑀效性。且肥料溶出之評估· 則依日本農林水產省環境技術研究所提案的方法(例如「 (請先閱讀背面之注意事項再填寫本頁) ,....... ia - -- 本紙張尺度適用中國國家標隼(CNS ) Λ4規格(210X 297公釐) 386 36 464640 經浒郎中央標隼局員工消費合作枉印製 A7 B7 五、發明説明(8 ) 詳解肥料分析法」越野正義編著,1988年)實Sfc。 當瓶W 2 將2kg粒狀尿素(平均粒徑3.4·β)與實施例1完全同法 使其成轉動狀態*保持於6 5〜7 0 X1 。而被覆樹脂則採用與 茛拖例1完全相同的成分、組成比。首先將胺催化劑0.U 加入多元酵成分5.3g内並予充分混合後•添加於該處於轉 動且加溫吠態之粒吠脃料。含胺之多元酵,可用目視方式 觀察出約30秒鎗均勻被覆於肥料表面的情形。其後|在保 持繼孃該肥料之轉動、加溫狀態下添加多元異氣酸®成分 4.7g。添加多元異氰酸酯成分後•於3分鐘後取出部分的 試料時•樹脂處於幾乎喪失钻著性的狀態。每隔4分鐘望 複上述步驟16次*對肥料進行8重量%被覆。 對由上述步嫌製得的澍脂被覆粒吠肥料與茛拖例1同 法評估25 C之肥料溶出行為。结果該被覆尿素於妁85日間 溶出80¾之肥声分,確認出具有足夠的嫒效性。 又,依本實拖例確認出分別添加多元異氰酸酷成分及 多元酵成分之方法亦屬可行。 當施例3 將2kg粒狀尿素(平均粒徑3.4f*in>與實拖例1完全同法 使其成為可轉動状態,保持於6 5〜7 0 t1 。而被覆樹脂則採 用與實腌例1完全相同的成分、姐成比。將已充分混合的 未硬化之該被覆用樹脂15g添加於處於加溫且轉動狀態之 該粒狀肥料*經由氨基甲酸酯樹脂被覆。已投人的樹脂最 對脃料為0 . 7 5重量% ,已被覆的該粒徑肥料之悄形,被覆 本纸張尺度適用中國國家標準(CNS ) Λ4規格(210X297公釐) 1〇 38636 (請先閱讀背而之注意事項再填寫本頁)Printed by the Central Economic and Technical Bureau of the Ministry of Economic Affairs on consumer cooperation 6 6 64 0 0 A7 B7 V. Description of the invention (1) Fang Jiecheng who was awakened by Ming Ming This invention has a slow-acting (also known as delayed effect) granular Manufacturing method of fertilizer * In particular, it is a manufacturing method of high-efficiency fertilizer coated with urethane S resin or oxygen dendrite. So-called potent fertilizers that are encapsulated with resin-coated granules or ochre yellow to form capsules to control the dissolution rate of the fertilizer. Its long history * For example, Japanese Patent Publication No. 40-28927 and Japanese Patent Publication No. 44-28457 Gazette, Japanese Patent Publication No. 3 7-1 5 3 8 2 or Japanese Patent Publication No. 4 2-1 3 6 81, etc., that is, various methods for shaking or covering S material are disclosed. As for the coating fertilizer family of the urethane resin, which is a reaction product of a polyisocyanate compound and a polyenzyme compound, the coating material is disclosed in Meiyuan Patent No. 3,26 4,089, and the same epoxy resin coating material It is disclosed in US Patent No. 3,264,088. As for the manufacturing method of the coating fertilizer using urethane resin as the coating material, Japanese Patent Application No. 1-50066 1 «Gazette discloses a coating layer that makes the isocyanate compound react on the urea fertilizer surface to form a base layer of K. (Base coat), and the method on which the polyisocyanate compound reacts with the isocyanate group of the above-mentioned manager is a characteristic technique. In Japanese Patent Publication No. 7-500560, it was revealed that a mixed resin of a polyisocyanate compound and a polyenzyme compound was applied for 10 to 30w · each, and treated with an amine mist (amine treatment and hardening each of the abrasives to special properties). However, the use of these technologies does not fully meet the purpose of dissolving the fertilizer that is controlled to have fewer defects, or the manufacturing method also requires complex equipment. A variety of disadvantages. Ί I 'IT (Please read the notes on the back before filling in this f) This paper size applies to the national standard of China (CNS) A4 specifications (210X297 mm) 3 38636 464640 A7 B7 Central Ministry of Economic Affairs Printed by the Consumer Bureau of the Standards Bureau 5. Description of the invention (2) Lessons to be solved by the invention m The t of the present invention provides 固 thermosetting resin-coated non-coated m-defective grade-coated fertilizer manufacturing method is more conducive to industrial scale Manufacture of 1 hand to solve lessons In order to solve the above-mentioned problems, the inventors completed the present invention through careful research. 0 The present invention is described below, that is, 1. The method for manufacturing a granular coating fertilizer covered with a thermosetting resin is characterized by the following steps: (1) Steps for turning granular m into a rotating state> (2) Adding liquid uncured thermosetting resin with a layer thickness of 1 to 10 U «1 to the granular fertilizer in the rotating state Step W (3) The step (4) of keeping the granular fertilizer in a rotating state and covering the surface of each m particle with the unhardened thermosetting resin, and curing the unhardened thermosetting resin Step (5) of step (1) to U) is repeated 1 or 1 times of step M, resulting in 0 2. As the above 1 m The manufacturing method is characterized in that the thermosetting resin is an epoxy resin or an amine deer resin. The manufacturing method of the coated IB material as described in the above 2 is special. The amine grinding resin is made of polyisocyanate, polyenzyme, and amine catalyst. The composition is 0 4. The manufacturing method of the coating m 枓 as above 1, 2 or 3 »Its special feature is that the paper size applies the Chinese National Standard (CNS) A4 specification (210X297 mm). Pingban employee consumer cooperatives Yinfan 4 64 0 A7 B7 V. Description of the invention (3) The gelation time of the coating temperature of the solid resin is less than 5 minutes.琎 明 夕 窖 定 噍 楼 M * Detailed description of the present invention. The method for making the granulated bark fertilizer into a dynamic step is not particularly limited in the device, but a known and customary person can be used. However, a rotary granulator or a sugar coating machine such as a disc type and a drum type can be exemplified. Rotating coating machine of flowing layer type or flowing layer type. In addition, those who have a heating device attached to this device are more suitable for high precision coating processing or adjustment of processing time. The granular fertilizer to be used may be any of the conventional granular materials of a rake. It has examples, such as urea, ammonium chloride, ammonium chloride, ammonium phosphate, ammonium nitrate, lime argon, sodium nitrate, acetaldehyde-condensed urea and other nitrogenous fertilizers, phosphorus fertilizers, and "acid lime" 、 Phosphate fertilizers such as acid fertilizers, potassium chloride, potassium arsenite, potassium bicarbonate, silicic acid fertilizer fertilizers, potassium phosphate fertilizers, potassium phosphate fertilizers, potassium nitrate fertilizers, etc. Or organic fertilizer, etc .: A granular fertilizer which is further granulated by a method known per se. The particle size of the granular fertilizer is not particularly limited. However, a range of 1 to 5 m · is preferred for manufacturing. ′ The thermosetting resin used is described below. Thermosetting resins | Known persons can be used. • In particular, you can include: epoxy resin, unsaturated resin, phenol resin, dimethyl resin, melamine resin, furan resin, silicone Thermosetting resins such as resins * If necessary, two or more kinds may be selected and mixed for use. Among these, • M epoxy resin or amine ester grease is preferred in terms of workability and performance. M is a carbamate with an amine catalyst in a polyisocyanate resin and a polyenzyme compound (please read the note on the back first) Please fill in this page for more details.) This paper scale is applicable to the Chinese National Standard (CNS) Λ4 specification (2Ι〇 × 297 mm) 5 38 6 36 4 Printed by the Consumers Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs 6 4 640 A7 B7 Five 'Invention Description (4) Ester (urethane) tree gambling is particularly preferred. To further explain the urethane sea resin, the urethane resin is a name for a resin that is reacted by a polyisocyanate compound and a polyenzyme compound and subjected to three-dimensional cross-linking. However, the uncured urethane according to the present invention Cool resin means a mixture of the polyisocyanate compound and the polyenzyme compound that has not been reacted at all or has not been three-dimensionally reacted in advance. It is also useful to add a catalyst first to promote the reaction. As for the shape of the uncured dendritic cell, it can be any of solvent-free type, solution type, and water-based emulsion type. However, it is more suitable if it is K insoluble type and is liquid at the processing temperature. The polyisocyanate g compound is not particularly limited, but if it is specifically exemplified, it can be exemplified by: methylbenzyl diisocyanate (also known as TDD · dibenzylmethane diisonate ( Also known as MD [), Cai Diisocyanate, Toluidine isocyanate, hexamethylene diisocyanate, isophorone diisocyanate, dimethylbenzyl diisocyanate, etc. can be used if necessary. These mixtures r. Among them, HDI or TDI or oligomeric fluorene derived from these are more suitable for use. As for the polyzyme compound *, it is not limited, but it can be exemplified by the use of polyzyme, amine group, etc. Polyether polyols, such as polyether polyols obtained by pre-addition of ethylene oxide or propylene oxide, and polytetramethylene K dienzymes obtained by pre-polymerization of tetrahydrofuran, are used as initiators. Polyester polyenzyme obtained by methods such as fermentation, polyenzyme, polyether polyenzyme, and carboxylic acid compounds by anti-sleeping. In addition, when considering biodegradability, natural substances containing 0H groups or their modified products can also be used. As for the reaction catalysis, you can use the well-known customary. National Standard (CNS) A4 Specification (210XW7mm) 6 3 8 6 3 6 Gas --- Order (Please read the precautions on the back before filling this page) Central Samples Bureau, Ministry of Economic Affairs, Shellfish Consumer Cooperative Printed 6 4 6 4 0 A7 B7 5. In the description of the invention (5), triethylene ethylene diamine, N-methylmorpholine, fluorene, hydrazone-dimethylmorpholine, diazine 11 Amine catalysts such as carbene, 2,4,6-pyrene (dimethylaminomethyl) phenol are more suitable for use. Furthermore * if necessary • pigments or dyes, or talc, mica, silica, carbon Black, resin powder and other inorganic and organic powder and granular fillers. The manufacturing method of the present invention includes the step of setting the granular fertilizer in a rotating state at a specified processing temperature. As for the processing temperature * the instant setting time of the above uncured resin Within 5 minutes * more preferably within 3 minutes M. For the step of adding the above uncured resin and coating it on the particles in the rotating state *, a resin obtained by combining and hardening a hardener or a catalyst in advance The composition is injected into the method of dropping, smelling, etc. Rong can also add a main agent, a hardener, and a catalyst separately. A method of mixing the components while the fertilizer particles are coated with the resin, and * the viscosity of the resin to be coated * is the uniform coating of the granular rake material in a short time at the temperature of the coating step. The initial viscosity of the hardened resin is preferably in the range of 5CP to 500CP; the range of M from 10CP to 100CP is the best. You can adjust the amount of resin in one shot so that the film thickness of the coating is 1 ~ 10 / i ·· Μ is in the range of 2 " _above 6w · K is the best. When it is less than 1ί / β, * the number of times of coverage is not conducive to the manufacture of industrial chess. On the other hand, if the thickness is l0w · The above will cause a problem under M. Put the liquid unhardened wax into a rotating fertilizer. · First, due to the rotation of the particles, a uniform unhardened resin layer will be formed on the surface of the particles | Simultaneous resin The hardening reaction. At this time, 1 resin will see the countermeasures (the progress of 8 (please read the precautions on the back before filling in this page) The paper size applies the Chinese National Standard (CNS) Α4 specification (210X29? Mm) 7 3 8 6 36 Economy Printed by the Consumer Standards Cooperative of the Ministry of Standards and Technology Bureau 6 4 64 0 A7 B7 V. Invention Description (6) Slowly increase the viscosity and form a layer with electrical hiding. At this time, the adhesiveness of the resin increases and the fertilizer is made of tree wax The particles adhere to each other and form a mass from a large number of particles; they do not disintegrate into the original particles, and even if they disintegrate, there is a concern that the surface of the resin will be damaged. When the resin mold is on the M, it will cause the above-mentioned problems * The other particles are not uniformly coated with the hardened resin. The present inventors believe that if the resin is thicker, the force t to pull apart the particles that are adhering to each other due to the rotation of the particles is insufficient. No matter how One time when κ is thicker than the resin film coating * M-The general rotating type coating method will produce the above-mentioned problems, and it is difficult to produce the desired resin-coated granular bark fertilizer. Repeatedly repeating the previous steps The expected _thickness of the coated resin is thick. Although the thickness of the coated resin film varies depending on the expected dissolution pattern, it is usually a range of M20w * to 200μ. It is covered to the end. -1 Covered Fertilizer 1 as necessary • Since the resin will completely harden, it can also include a step that can be completely maintained at the specified hardening temperature. In addition, in order to prevent the fertilizer from consolidating or rising during manure, It is also a useful technique to add inorganic fine powder such as clay on the surface of the coated palladium material. Actually, the present invention will be described more specifically, but the present invention is not limited by these examples. Shi Huan 丄 pours 2kg granulated urea (average particle size 3.4 · *) into a temperature-controllable tilting disc-type rotary granulator (disk diameter 520 »·) with a hot air generator. Read the notes on the reverse side and fill out this page again} This paper size applies to Chinese National Standard (CNS) Α4 specification (210X297 mm) 8 3 8 6 3 6 464640 A7 Employees ’cooperation with Central Standards Bureau of the Ministry of Economic Affairs Du Yinfan B7 V. Invention Explanation (7) 20 ~ 30γρ · rotation makes granular fertilizer into Rotating state. Heat the device and keep the inverted granular urea at 70 ~ 75 t1 »and keep it in a rotating state. Mix and mix the coating resin Polymeric MPI (manufactured by Sumitomo Bayer urethane, trade name: Sunidure 44V10M.7s, branch _Polyether polyol (manufactured by Sumitomo Bayer Urethane Co., Ltd. * Trade name: Sueiphene TM> 5.3g and amine catalyst 2,4,6-S (trimethylaminomethyl) phenol 0.U * and added immediately The granular urea that has been warmed and in a rotating state. The unhardened urethane resin composition is in the form of a room overflow liquid. In addition, the curing time of the uncured carbamate __ tree wax used in this example is 2 minutes and 30 seconds at 65 υ. Lw ·。 In addition, the amount of resin input | 0.5% by weight of the transferred fertilizer • In the case of coating the fertilizer of this particle size, the thickness of the coating resin is about 3. lw ·. By visual inspection, the injected resin was confirmed to be coated on the surface of the granular fertilizer in an approximately uniform manner in about 30 seconds. 3 minutes after the resin was injected, a part of the test was taken out. * The resin was found to have almost lost adhesion. The state of sex. Repeat the above steps 16 times every 3 minutes ", and perform 8 reams * on the fertility branch. Finally, hold the resin-coated fertilizer at 70 ~ 75 and hold it for 10 minutes to produce a granulated bark fertilizer of coated urethane resin completely cured by the resin. The time required for all the steps to soften is about 1 hour, which is a method that is conducive to the scale production of industrial vegetables. From the SEM observation of the cross section of the coating material, the thickness of the resin film was about ·· from the resin coating amount of the step. The dissolution behavior of IS plutonium at 25 deaths was evaluated for the bark-coated granular fertilizer prepared by the above procedure. Result • The coated urea dissolved 80½ fat components in about 85 days. It was confirmed that it had sufficient efficacy. And the evaluation of fertilizer dissolution is based on the method proposed by the Japanese Ministry of Agriculture, Forestry and Fisheries Research Institute of Environmental Technology (for example, "(Please read the precautions on the back before filling out this page), ... ia--this paper size Applicable to China National Standards (CNS) Λ4 specifications (210X 297 mm) 386 36 464640 Economic cooperation between the Central Bureau of Standards and Labor of the People's Republic of China printed A7 B7 V. Description of the invention (8) Detailed fertilizer analysis method " 1988) Real Sfc. When the bottle W 2 was used, 2 kg of granular urea (average particle size 3.4 · β) was exactly the same as in Example 1 to make it into a rotating state * and maintained at 6 5 to 7 0 X1. On the other hand, the coating resin uses the same ingredients and composition ratios as those in Example 1. First add the amine catalyst 0.U to 5.3g of the multi-enzyme ingredient and mix thoroughly. • Add to the granulated bark material in the rotating and warming bark state. Polyamines containing amines can be visually observed to cover the surface of the fertilizer uniformly in about 30 seconds. After that, 4.7g of polyisoacid® was added while maintaining the rotation and heating of the fertilizer. After adding the polyisocyanate component • When taking out a part of the sample 3 minutes later • The resin is almost in a state where drilling properties are lost. The above steps were repeated 16 times every 4 minutes * The fertilizer was covered with 8% by weight. The fat dissolution behavior of 25 C fertilizer was evaluated in the same manner as the butter-coated granular bark fertilizer prepared from the above steps and buttercup example 1. As a result, the coated urea dissolved 80¾ of fat content in 妁 85 days, and confirmed that it had sufficient effectiveness. In addition, according to the actual examples, it was confirmed that the method of separately adding a polyisocyanate component and a polyzyme component is also feasible. In Example 3, 2 kg of granular urea (average particle size 3.4f * in >) was made into a rotatable state in exactly the same manner as in Example 1. It was kept at 6 5 ~ 7 0 t1. The coating resin was cured and cured. Example 1 has exactly the same composition and ratio. 15 g of the coating resin that has been fully hardened and uncoated is added to the granular fertilizer that is in a heated and rotating state * and is coated with a urethane resin. The resin is 0.75% by weight. The size of the coated fertilizer has a quiet shape. The size of the paper is covered by the Chinese National Standard (CNS) Λ4 specification (210X297 mm). 1038636 (Please read first (Further considerations please fill out this page)

T 6 4 經濟部中央標準局員工消費合作社印製 4 64 0 A7 B7五、發明説明(9 ) 樹脂之膜厚成約4.3^·。可用目視觀察方式確認出已投人 的樹脂於約3 0秒鐘約略均匀的被覆於粒狀肥料表面之情形 。樹脂投入後約3分鐘後•取出一部分的試料•樹脂處於 幾乎失去黏著性之狀態|每隔3分鐘重搜上述步驟16次, 對肥料進行1 2重量%被覆。最後添加(c u t c i a y ) 1 0 s,於7 0 〜75C保持10分鎗•製得氨基甲酸酷被覆粒狀肥料。 對由上述步驟製得的樹脂被覆粒狀Μ枓與實陁例1同 法評估25Τ1之肥料溶出行為。结果該被S尿素於約85日間 溶出80¾之肥料分*確認出具有足狗的缓效性。 bh舲例1 除一次添加的樹脂量為40g% <餘與實胞例1完全同法 操作嘗試製造樹脂被覆肥料。且,該樹脂量對粒狀肥料而 言成 12.4wm。 以目視親察方式•可確認出投人的樹脂以妁30秒妁略 均勻的被覆粒狀肥料表面。約2分鐘後樹脂會增黏且帶有 » 曳躲性•粒子間相互黏著而生成多數粒子凝集的塊狀物· 其後乃形成不能崩解。 ‘ hh舲例2 除樹脂成分不添加胺催化劑外*餘與實胞例1完全同 法操作官試製造樹脂被覆靶料,不添加胺催化劑時*該樹 脂之凝膠時間為20分鐘*添加第1次之澍脂後經3分鐘後取 出試料時,樹脂並未硬化,仍保持液狀。又,經遇】〇分鐘 後同樣的取出試料*観察出樹脂係增黏的鈷稱吠液髖。於 處該狀態之該肥料内同樣的灌績加人樹脂•粒子間相互黏 本紙張尺度適用中國國家標準(CNS ) Λ4規格(210X297公嫠) 1 1 3 86 3 6 (請先閱讀背面之注意事項再填寫本頁) 464640 A7 B7 五、發明説明(1 0 ) 著而生成多數粒子凝集的塊狀物*其後乃形成不能崩解。 發 之 明 效 被 性 效 媛 之 陷 〇 缺造 瞋製 塗的 無模 的規 覆業 被 Η 脂於 樹利 性有 固較 ’ Μ法 明造 發製 ώ本之 依料 肥 覆 (請先閱讀背面之注意事項再填寫本頁) 經濟部中央標準局負工消費合作社印製 本紙張尺度適用中國國家橾準(CNS ) Α4規格(210X297公釐) 2 1Λ 3863 6T 6 4 Printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs 4 64 0 A7 B7 V. Description of the invention (9) The resin film thickness is about 4.3 ^ ·. It can be confirmed by visual observation that the resin that has been injected is approximately uniformly coated on the surface of the granular fertilizer in about 30 seconds. About 3 minutes after the resin was put in. • A part of the sample was taken out. • The resin was in a state of almost losing its adhesiveness. The above steps were repeated 16 times every 3 minutes, and the fertilizer was coated with 12% by weight. Finally, (c u t c i a y) 1 0 s is added, and a 10-minute gun is held at 70 to 75C. A carbamate-coated granular fertilizer is obtained. For the resin-coated granular MG prepared by the above procedure, the dissolution behavior of 25T1 fertilizer was evaluated in the same manner as in Example 1. As a result, 80% of the fertilizer which was dissolved by S urea in about 85 days * was confirmed to have the slowing effect of a foot dog. bh Example 1 Except that the amount of resin added at one time was 40 g%, and the rest was exactly the same as that of Cell Example 1. An attempt was made to manufacture a resin-coated fertilizer. The amount of the resin was 12.4 wm for the granular fertilizer. Visual inspection method • It can be confirmed that the injected resin covers the surface of the granular fertilizer in approximately 30 seconds. After about 2 minutes, the resin will thicken and have "shadow resistance". • Particles will stick to each other to form agglomerates of a large number of particles. After that, they will not disintegrate. 'hh 舲 Example 2 Except for the resin component without the addition of an amine catalyst * Except for the same method as in the case of the real cell example, the trial-manufactured resin-coated target was manufactured without the addition of an amine catalyst * The gel time of the resin was 20 minutes * When the sample was taken out 3 minutes after the first fat application, the resin did not harden and remained liquid. Also, the sample was taken out in the same manner after 0 minutes *. The resin thickened cobalt was called bark fluid hip. In this state, the same filling performance of the fertilizer is added with resin and particles are adhered to each other. The paper size applies the Chinese National Standard (CNS) Λ4 specification (210X297 cm) 1 1 3 86 3 6 (Please read the note on the back first Please fill in this page for more details) 464640 A7 B7 V. Description of the invention (1 0) Agglomerates with a large number of particles are formed by this method. The effect of the hair is trapped by the effect of the sex. The moldless covering industry is lacking in manufacturing and coating. It is more beneficial to the tree and is more profitable. (Please read first.) Note on the back, please fill out this page again.) The paper size printed by the Central Standards Bureau of the Ministry of Economic Affairs and the Consumer Cooperatives is printed on the paper. Applicable to China National Standards (CNS) Α4 size (210X297 mm) 2 1Λ 3863 6

Claims (1)

4 6 4 64 0 H3 經濟郞中央標準局員工福利委員會印製 第86100585號專利申請案 申請專利範圍修正本 (90年9月12日) 1. 一種以氨基甲酸樹脂被覆的粒狀被覆肥科之製造方法 ,其特激在於依下列步驟順序進行: (1) 使粒狀肥料於加工溫度下成為轉動狀態的步 驟, (2) 於處於該加工溫度下之轉動態的粒狀肥料上 添加層厚成1至l〇w id之量的液狀未硬化氨基甲酸酷樹 脂之步驟* (3) 保持著該粒狀肥料於加工溫度下之轉動狀態 Μ該未硬化氨基甲酸酯樹脂被覆各肥料粒子表面之 步驟, (4) 保持著該粒狀肥料於加工溫度下之轉動狀態 ,使該未硬化氨基甲酸酯樹脂硬化的步驟* (5) 進一步重複上述(1)至(4)之步驟*待該氨基 甲酸酯樹脂失去黏性後再進行1次或1次Μ上的重覆步 驟而成者。 2. 如申請專利範圍第1項之被覆肥料之製造方法,其特 激在於氨基甲酸酷樹脂係Μ聚異氰酸酯化合物、多元 醇化合物及胺催化劑為必須成分而成者。 3. 如申請專利範圍第1或2項之被覆肥料之製造方法 ,其特激在於氨基甲酸酯樹脂之被覆加工溫度之凝膠 時間為5分鐘以下。 本紙張尺度適用中圉國家標準(CNS )Α4規格(210X 297公ft) 1 38636 4 6 4 64 0 H3 經濟郞中央標準局員工福利委員會印製 第86100585號專利申請案 申請專利範圍修正本 (90年9月12日) 1. 一種以氨基甲酸樹脂被覆的粒狀被覆肥科之製造方法 ,其特激在於依下列步驟順序進行: (1) 使粒狀肥料於加工溫度下成為轉動狀態的步 驟, (2) 於處於該加工溫度下之轉動態的粒狀肥料上 添加層厚成1至l〇w id之量的液狀未硬化氨基甲酸酷樹 脂之步驟* (3) 保持著該粒狀肥料於加工溫度下之轉動狀態 Μ該未硬化氨基甲酸酯樹脂被覆各肥料粒子表面之 步驟, (4) 保持著該粒狀肥料於加工溫度下之轉動狀態 ,使該未硬化氨基甲酸酯樹脂硬化的步驟* (5) 進一步重複上述(1)至(4)之步驟*待該氨基 甲酸酯樹脂失去黏性後再進行1次或1次Μ上的重覆步 驟而成者。 2. 如申請專利範圍第1項之被覆肥料之製造方法,其特 激在於氨基甲酸酷樹脂係Μ聚異氰酸酯化合物、多元 醇化合物及胺催化劑為必須成分而成者。 3. 如申請專利範圍第1或2項之被覆肥料之製造方法 ,其特激在於氨基甲酸酯樹脂之被覆加工溫度之凝膠 時間為5分鐘以下。 本紙張尺度適用中圉國家標準(CNS )Α4規格(210X 297公ft) 1 386364 6 4 64 0 H3 Printed by the Employees Welfare Committee of the Central Bureau of Economic Standards (No. 86100585) for the amended scope of patent application (September 12, 1990) 1. A granular coating of urethane resin The manufacturing method is characterized by the following steps: (1) the step of turning the granular fertilizer into a rotating state at the processing temperature, and (2) adding a layer thickness to the granular fertilizer at the processing temperature under dynamic conditions Step of forming a liquid unhardened urethane resin in an amount of 1 to 10w id * (3) Maintaining the rotating state of the granular fertilizer at a processing temperature M The unhardened urethane resin covers each fertilizer particle Steps on the surface, (4) Steps of hardening the unhardened urethane resin while maintaining the rotating state of the granular fertilizer at the processing temperature * (5) Repeating the above steps (1) to (4) * After the urethane resin has lost its tackiness, it is a step of repeating the process once or once. 2. For the manufacturing method of coated fertilizer in item 1 of the scope of patent application, the urethane resin M polyisocyanate compound, polyol compound and amine catalyst are the essential components. 3. For the manufacturing method of coated fertilizers in the scope of patent application No. 1 or 2, it is particularly exciting that the gelation time of the coating processing temperature of the urethane resin is 5 minutes or less. This paper size applies the China National Standard (CNS) A4 specification (210X 297 ft) 1 38636 4 6 4 64 0 H3 Economic and Central Standards Bureau Staff Welfare Committee Printed No. 86100585 Patent Application Amended Patent Scope (90 (September 12, 2010) 1. A method for manufacturing a granular coating fertilizer family covered with urethane resin, which is particularly exciting in the following steps: (1) a step of turning the granular fertilizer at a processing temperature (2) The step of adding a liquid unhardened urethane resin with a layer thickness of 1 to 10w id to the granular fertilizer under dynamic conditions at the processing temperature * (3) maintaining the granular form The rotating state of the fertilizer at the processing temperature. The step of coating the surface of each fertilizer particle by the unhardened urethane resin. (4) maintaining the rotating state of the granular fertilizer at the processing temperature, so that the unhardened urethane Resin hardening step * (5) The steps (1) to (4) above are further repeated * After the urethane resin loses its tackiness, it is performed by repeating the step once or once. 2. For the manufacturing method of coated fertilizer in item 1 of the scope of patent application, the urethane resin M polyisocyanate compound, polyol compound and amine catalyst are the essential components. 3. For the manufacturing method of coated fertilizers in the scope of patent application No. 1 or 2, it is particularly exciting that the gelation time of the coating processing temperature of the urethane resin is 5 minutes or less. This paper size is applicable to China National Standard (CNS) A4 (210X 297 ft) 1 38636
TW086100585A 1996-01-23 1997-01-21 Process for making a coated fertilizer TW464640B (en)

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MY120571A (en) 1998-05-22 2005-11-30 Sumitomo Chemical Co Granular coated fertilizer and method for producing the same
JP2002068880A (en) * 2000-06-14 2002-03-08 Chisso Corp Coated bioactive granular material and method of manufacturing for the same
DE10158693A1 (en) 2001-11-29 2003-06-26 Ashland Suedchemie Kernfest Coated granular fabrics
JP5604819B2 (en) * 2009-07-09 2014-10-15 住友化学株式会社 Method for producing resin-coated granular fertilizer
JP5760357B2 (en) * 2009-10-06 2015-08-12 セントラル硝子株式会社 Method for producing coated water-soluble granular material
JP5810544B2 (en) 2010-03-31 2015-11-11 セントラル硝子株式会社 Coated granule and method for producing the coated granule
JP2012046382A (en) * 2010-08-27 2012-03-08 Sumitomo Chemical Co Ltd Method for producing resin-coated granular fertilizer
KR20230115299A (en) 2020-12-14 2023-08-02 스미또모 가가꾸 가부시끼가이샤 Manufacturing method of coated granular fertilizer and coated granular fertilizer

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JPS5238361A (en) * 1975-09-22 1977-03-24 Ube Industries Slowly available coated granular fertilizer
DE3544451C1 (en) * 1985-12-16 1987-01-15 Ashland Suedchemie Kernfest Process for producing a water-permeable coating on granular, water-soluble substances and its application
US4804403A (en) * 1986-08-18 1989-02-14 Melamine Chemicals, Inc. Attrition-resistant, controlled release fertilizers
JPH04305085A (en) * 1991-03-29 1992-10-28 Yuukishitsu Hiryo Seibutsu Kassei Riyou Gijutsu Kenkyu Kumiai Coated granulated fertilizer and production thereof
JPH0772114B2 (en) * 1991-06-26 1995-08-02 セントラル硝子株式会社 Fertilizer coating composition, coated granular fertilizer and method for producing the same
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JPH082988A (en) * 1994-06-17 1996-01-09 Reitetsuku Kk Production of slow-acting coated granular fertilizer
US5599374A (en) * 1994-09-23 1997-02-04 Rlc Technologies, L.L.C. Process for producing improved sulfur-coated urea slow release fertilizers
US5698002A (en) * 1994-11-21 1997-12-16 Lesco Inc. Controlled release fertilizers utilizing an epoxy polymer primer coat and methods of production

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