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TW205543B - A novel preparation method of the aliphatic acid metal salts - Google Patents

A novel preparation method of the aliphatic acid metal salts Download PDF

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Publication number
TW205543B
TW205543B TW81101957A TW81101957A TW205543B TW 205543 B TW205543 B TW 205543B TW 81101957 A TW81101957 A TW 81101957A TW 81101957 A TW81101957 A TW 81101957A TW 205543 B TW205543 B TW 205543B
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Taiwan
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reaction
fatty acid
metal salts
aqueous solution
salts
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TW81101957A
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Chinese (zh)
Inventor
Herng-Dar Hwu
Horng-Iuan Hsu
Jiann-Horng Chen
Shwu-Fang Jiang
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Industial Technology Res Inst
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Publication of TW205543B publication Critical patent/TW205543B/en

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Abstract

A preparation method of the aliphatic acid metal salts which is characterized in that the composite reaction takes place at the reaction temperature of between 60讈 to 100讈 and saponifies the alkaline aqueous solution of C7-C22 aliphatic acid with the water soluble metal salt acid aqueous solution; during the reaction process by alternate additions of the alkaline and acid aqueous solutions, the method repeatedly adjusts the reaction pH value to synthesize aliphatic acid metal salts of low aliphatic acid content, in which the aqueous metal salts are per se possessing usable acidity such as the compounds or their mixtures of chlorine salts, sulfate salts, nitrate salts, acetate salts of iron, aluminum, Cerium, Cobalt, Copper, Manganese, Magnesium, Calcium, Nickel.

Description

205543 Λ 6 Π 6 經濟部屮央標準Λ;β工消fr合作社印¾ 五、發明説明(1 ) 本發明是一種脂肪酸金颶鹽的新穎製備方法,藉由此 製備方法可有效降低脂肪酸之殘存含量,而所産製之脂肪 酸金颶鹽可成功的應用在光分解性塑膠上,做為該材料的 光敏感劑。 脂肪酸金屬鹽類做為光分解性塑膠中的光敏感劑,在 多項專利中皆曾掲示,如美國專利3840512,3865767, 3882058,便以 Ti, V,Cr, Mn, Fe, Co, Ni, Cu,等金屬 製成之脂肪酸金屬鹽類做為光敏感劑。其中在美國專利 3865767中所使用之光敏感劑為雙蹇類(Di-Soap),硬 Y 脂酸鐵(H0-F< ),其中Y為磺數6〜25的脂肪酸;該專 Y 利證實部份金屬配位基被脂肪酸取代後,與塑膠間便具有 良好之相容性,且為一極佳之光敏感劑。利用本專利製程 合成之脂肪酸金羼鹽便屬於此類化合物,應用在光分解性 塑膠上,具有良好加速塑膠分解之效果。除上述光敏感劑 用途外,脂肪酸金屬鹽類亦被廣泛應用,可作為塗料、油 墨等材料的乾燥硬化劑、塑膠、橡膠用之滑劑、不飽和聚 醋之硬化促進劑、或塑膠用之安定劑等。 脂肪酸金屬鹽類現有之合成方法大致可區分為下列三 類:第一類為熔融法,此方法是將脂肪酸加熱熔融後直接 與金羼氧化物或氩氧化物反應生成脂肪酸金屬鹽類,此方 法雖然生産設備較為簡單,但是有下列缺點:(a)高溫反 應,約在150C〜200T:,易使産品顔色變深;(b)反應不 (請先閲部背而之注意事項#堝寫木頁) 裝< 訂- 線< 本紙張尺度逍用中國國家楳準(CNS) T4規怙(210X297公;¢) 205543 A6 B6 五、發明說明(2 ) 經濟部中央標準局印製 {請先閲讀背面之注意事項再填寫本頁) .線· 易完全,反應物容易殘留在最終的脂肪酸金屬鹽中;(C) 生成的産物必需再加以粉碎磨細,增加生産程序;(d)金 屬氧化物,容易混入其他金屬離子,一般而言,純度都較 低,無法得到較高純度的産物。第二類為複式分解法,此 法是將脂肪酸與氫氧化鈉行皂化反應生成脂肪酸納後,再 加入金展鹽水溶液,生成脂肪酸金屬鹽,此反應溫度較低, 約在60¾〜901C之間,此法所製得的硬脂酸鹽可改善上述 熔融法大部份的缺陷,得到色相佳、金屬純度高、粉末細 的産物,是最常被使用的商業化生産方法。但是上述複式 分解法仍殘存多量未反應的脂肪酸或脂肪酸納於脂肪酸金 屬鹽中,造成産物純度不高之缺陷,如U.S.S.R專利SU 379565中以複式分解法生成硬脂酸鐵,便無法完全將硬脂 酸轉換成硬脂酸鐵,因而産物中會殘餘7〜10%未反應之 硬脂酸鈉。由於硬脂酸納會增加産物過濾上之困擾,故通 常商業化製程中須將其還原成硬脂酸。而美國專利 3840512中雖然證實脂肪酸與脂肪酸金屬鹽類在光分解反 應中具有加乘效應(Synergistic effect),會加速光分解; 然而由於脂肪酸分子量較低,當添加於塑驂中時容易游離 (migration)至塑膠表面,除了會影響塑膠本身的二次加 工性,(如印刷性、封口性等),亦會造成塑膠内硬脂酸濃 度之分佈不一,導致産品的分解速率隨著儲存的環境,時 間或産品部位而改變。為了減少硬脂酸殘存的含量,製程 上通常均藉助大量溶劑的清洗,但此方法卻會增加生産成 本,且易造成環境之汚染。第三類方法為交換法,此方法 甲 4 (210X297 公嬗) 205543 A6 B6 經濟部中央標準局印製 五、’發明説明(3 ) 主要是在用生産三價或四價之高純度脂肪酸金屬鹽類,其 反應是將過量脂肪酸與烷基金屬鹽或醇基金羼鹽在大量溶 劑中進行交換反應,生成脂肪酸金羼鹽及醇,殘餘之脂肪 酸再以溶劑清洗。日本公開特許公報昭62-120339即是以 交換法生成硬脂酸鐵之專利,其反應是將過量之脂肪酸與 Fe(0CH)3溶解於THF中進行反應,生成硬脂酸鐵,由於 此方法是以大量THF為反應溶劑,使得生産成本提高,且 易造成污染問題,由於此反應是以過量脂肪酸進行反應, 因而會有約90%的脂肪酸無法進行反應而隨著溶劑排出, 增加産品的成本,削弱其競爭能力。 為消除上述三種製程之缺陷本發明將複式分解法加以 改進,主要係藉由反應物本身之酸鹼特性,以溶液交替添 加之方式,迫使未反應之脂肪酸繼缠反應,無需再經由有 機溶劑的清洗,即可得到色澤佳、粉末細、純度高的脂肪 酸金羼鹽,除了可有效的降低生産成本外,並已成功的應 用在光分解性塑膠上,做為有效之光敏感劑。 本發明是將硝數6至25的脂肪酸與氫氣化納於60t:〜 901C下在水中進行皂化反應,生成_狀的脂肪酸納後,再 將金屬鹽水溶液加入反應槽中,控制溫度在60¾〜90*0間, 進行複式分解反應,可生成脂肪酸金羼鹽。在反應完成後 濾除水份,再加入氫氣化鈉水溶液,使殘餘未反應之脂肪 酸進行皂化,生成脂肪酸納,控制反應之PH值在7以上, (一般多控制在7〜10之間),俟反窿槽溫度升高至反應溫 度後,將酸性之金屬鹽類水溶液加入,使部份皂化之脂肪 (請先閲讀背面之注意事項再填寫本百) •裝. •訂. •線. 甲 4 (210X297 公簷) 經濟部中央標準局印裝205543 Λ 6 Π 6 Standard of the Ministry of Economic Affairs Λ; Printed by β Gongxiao fr Cooperative Society ¾ V. Description of the invention (1) The present invention is a novel preparation method of fatty acid gold salt, by which the preparation method can effectively reduce the residual fatty acid Content, and the fatty acid gold salt produced can be successfully applied to photodegradable plastics as a photosensitizer for the material. Fatty acid metal salts are used as photosensitizers in photodegradable plastics, which have been shown in many patents, such as US Patent 3840512, 3865767, 3882058, Ti, V, Cr, Mn, Fe, Co, Ni, Cu , Fatty acid metal salts made of other metals are used as photosensitizers. Among them, the photosensitizer used in US Patent 3865767 is Di-Soap, hard Y ferric stearate (H0-F <), where Y is a fatty acid with a sulfonic acid number of 6 ~ 25; After some metal ligands are replaced by fatty acids, they have good compatibility with plastics and are an excellent photosensitizer. The fatty acid gold salt synthesized by this patent process belongs to this type of compound. It is applied to photodegradable plastics and has a good effect of accelerating the decomposition of plastics. In addition to the above photosensitizer applications, fatty acid metal salts are also widely used. They can be used as drying hardeners for paints, inks and other materials, as slip agents for plastics and rubber, as hardening accelerators for unsaturated polyester, or as plastics. Stabilizers, etc. The existing synthesis methods of fatty acid metal salts can be roughly divided into the following three categories: the first type is the melting method, this method is to directly react with gold oxide or argon oxide to produce fatty acid metal salts after heating and melting the fatty acid, this method Although the production equipment is relatively simple, it has the following disadvantages: (a) high temperature reaction, about 150C ~ 200T :, it is easy to make the product darker; (b) the reaction is not (please read the back of the department and the precautions first # 锅 写 木Page) Binding < Order-Line < This paper size is used in China National Standard (CNS) T4 regulations (210X297; ¢) 205543 A6 B6 5. Description of invention (2) Printed by the Central Standards Bureau of the Ministry of Economic Affairs {please Read the precautions on the back before filling in this page). Thread · Easy to complete, the reactants are likely to remain in the final fatty acid metal salt; (C) The resulting product must be crushed and ground to increase the production process; (d) Metal Oxides are easy to mix with other metal ions. Generally speaking, the purity is lower, and higher purity products cannot be obtained. The second type is the double decomposition method. This method involves saponification of fatty acid and sodium hydroxide to produce fatty acid sodium, and then adding Jinzhan salt aqueous solution to produce fatty acid metal salt. The reaction temperature is low, about 60¾ ~ 901C The stearate produced by this method can improve most of the defects of the above melting method, and obtain products with good hue, high metal purity and fine powder. It is the most commonly used commercial production method. However, the above double decomposition method still has a large amount of unreacted fatty acid or fatty acid contained in the fatty acid metal salt, resulting in the defect of low product purity. For example, in the USSR patent SU 379565, the double decomposition method is used to generate iron stearate. Fatty acid is converted into ferric stearate, so 7-10% unreacted sodium stearate will remain in the product. Since sodium stearate increases the difficulty in filtering the product, it is usually necessary to reduce it to stearic acid in commercial processes. In US Patent 3840512, although it is confirmed that fatty acids and fatty acid metal salts have a synergistic effect in the photolysis reaction, which will accelerate the photolysis; however, due to the low molecular weight of the fatty acid, it is easy to migrate when added in the plastic metamorphosis. ) To the surface of the plastic, in addition to affecting the secondary processing of the plastic itself (such as printability, sealing, etc.), it will also cause uneven distribution of the concentration of stearic acid in the plastic, resulting in the decomposition rate of the product with the storage environment , Time or product location. In order to reduce the residual content of stearic acid, the process usually uses a large amount of solvent to clean, but this method will increase the production cost and easily cause environmental pollution. The third method is the exchange method, this method A 4 (210X297 public transmutation) 205543 A6 B6 Printed by the Central Standards Bureau of the Ministry of Economy V. 'Invention Description (3) is mainly used to produce trivalent or tetravalent high-purity fatty acid metals For salts, the reaction is to exchange excess fatty acid with alkyl metal salt or alcohol base salt in a large amount of solvent to generate fatty acid salt and alcohol, and the residual fatty acid is then washed with solvent. Japanese Patent Laid-Open No. Sho 62-120339 is a patent for producing iron stearate by the exchange method. The reaction is to dissolve excess fatty acid and Fe (0CH) 3 in THF to produce iron stearate. Due to this method A large amount of THF is used as the reaction solvent, which increases the production cost and easily causes pollution problems. Since this reaction is carried out with excess fatty acids, about 90% of the fatty acids cannot be reacted and are discharged as the solvent increases the cost of the product. To weaken its competitiveness. In order to eliminate the defects of the above three processes, the present invention improves the compound decomposition method, mainly by the acid-base characteristics of the reactant itself, by the way of alternating solution addition, to force the unreacted fatty acid to follow the entanglement reaction, without the need for organic solvents After cleaning, you can obtain fatty acid gold salt with good color, fine powder and high purity. In addition to effectively reducing production costs, it has been successfully applied to photodegradable plastics as an effective light sensitizer. In the present invention, a fatty acid with a nitrate number of 6 to 25 and hydrogen gas are contained at 60t: ~ 901C to perform saponification reaction in water to produce fatty acid sodium, and then a metal salt aqueous solution is added to the reaction tank to control the temperature at 60¾ ~ Between 90 * 0, complex decomposition reaction can be carried out to produce fatty acid gold salt. After the reaction is completed, the water is filtered off, and then an aqueous solution of sodium hydroxide is added to saponify the remaining unreacted fatty acids to form fatty acid sodium, and the pH of the reaction is controlled to be above 7 (generally controlled between 7 and 10), After the temperature of the anti-tank tank is increased to the reaction temperature, add an acidic metal salt aqueous solution to partially saponify the fat (please read the precautions on the back before filling in this hundred) • Pack. • Order. • Line. A 4 (210X297 eaves) Printed by the Central Bureau of Standards of the Ministry of Economic Affairs

20554*5 A6 B6 五、發明説明(4 ) 酸納再與金屬鹽水溶液行複分解反應,控制反應之pH值在 7以下,(一般多控制在7〜2之間),使得殘餘之脂肪酸得 以進行反應,生成脂肪酸金屬鹽。此時仍剩餘少量的脂肪 酸,再如同上述方式加入氫氣化納和金屬鹽水溶液,再進 行皂化反應及複分解反應。藉由反應物NaOH及金屬鹽類本 身的酸齡特性,反覆添加調整反應之pH值,而有效的降低 未反應脂肪酸的含量。pH值調整次數的多寡除了可控制脂 肪酸之殘存量外,亦可控制金屬配位基上所接脂肪酸的含 董。實驗中調整次數一般多控制在3次左右,即可達到令 人滿意的結果。 玆以下列實施例更詳細説明本發明,但本發明不限於 這些實施例。 [實施例一]硬脂酸鐵之合成 將氫氧化納l〇g溶於500g水中,稱取75g硬脂酸(NV = 204)加入,加熱攪拌至90*C,使硬脂酸完全皂化,形成 透明膠狀之硬脂酸納,再缓慢加入氣化鐵溶液(0.4M)222ml 進行複式分解反應,待生成懸浮塊狀的紅色産物後,將反 應槽的水份濾除,完成了初步的合成反應。随後將156ml 的0.4M氫氧化納溶液及344ml的純水加入反應槽中,加熱 攪拌至9〇υ,使生成物中殘餘的硬脂酸進行皂化反應,再 將0.4Μ氛化鐵溶液55ml加入反應槽,使生成懸浮的硬脂酸 鐵鹽,接箸再加入93.6ml的氫氣化納溶液進行皂化反應後, 加入33ml氛化鐵溶液進行複分解反應,再加入50ml 0.4M (請先閲讀背面之注意事項再填寫本頁) •裴· •訂· •線· 甲 4 (210X297 公爱) 205543 五、發明説明(5) 氣氧化鈉溶液,俟皂化反應後,加入18ml 0.4Μ氛化鐵溶 液則生成最終産物硬脂酸鐵。合成後之産物及未經酸齡調 整之産物,經萃取滴定分析其硬脂酸含量,分別為1.4% 及14.8%,如表(一)所示證實經酸_調整後殘餘硬脂酸顯 著降低。再經FTIR及DSC測試,圖譜示如圖(一)〜圖(四), 由圖(一)及圖(二)FTIR分析可知在調整後,1707cm·1附近 的硬脂酸吸收峰已經不存在。而由圖(三)及圖(四)DSC分 析圖形亦可證實在酸驗調整後,低熔點的硬脂酸明顯消失。 [實施例二]硬脂酸铈之合成 經濟部屮央橾準而员工消奸合作杜印5i (請先閲讀背而之注意事項#蜞寫木頁) 於反應槽中,將氫氣化鈉10g溶於500g水中,稱取75g 硬脂酸(NV= 204)加入,加熱攪拌至90t:使硬脂酸完全皂 化形成透明膠狀之硬脂酸鈉,再緩慢加入氣化錨溶液 (0.3M)293ml進行複分解反應;於反應終了生成乳白色懸 浮物後,將反應的水份濾除。隨後量取0.4M氫氧化納溶液 125ml及純水375ml加入反應槽中、加熱攪拌至90它,使 生成物中殘餘的硬脂酸進行皂化反應,再將0.3M氣化姉溶 液58.8ml加入反應槽生成懸浮的硬脂酸铈鹽,接著加入 85ml的0.4M氫氣化納溶液進行皂化反應,隨後加入21ml氯 化鈽溶液進行複分解反應,再加入31ml氫氧化鈉溶液,俟 皂化反應後加入14.6nl 0.3M氣化鈽溶液,生成最終産物 硬脂酸铈。將合成後産物與未經酸驗調整之産物經分析其 硬脂含量分別1%及6.5%,如表(一)所示,證實經酸_調 整後殘餘硬脂酸顯著降低。再經FTIR及DSC測試,圖譜示 本紙张尺度边用中困B家標準(CNS) T4規格(210X297公釐) 3 Λ If κ 20 66 ΛΠ 經濟部中央標準局员工消仲合作社印5i 五、發明説明(6) 如圖(五)〜圖(八),由圖(五)及圖(六)FTIR分析可知在 1707(^4的硬脂酸吸收峰經由反覆酸鹸調整後已經不存在。 而由圖(七)及圖(八)DSC圖形亦可證實在酸鹼調整後,低 熔點的硬脂酸明顯消失。 [實施例三] 稱取實施例一、二中之硬脂酸鹽250g與4750g低密度 PE(台聚NA207-66,以下同)在140°C下以雙滾輪混練5〜 10分鐘,再以碎粒機粉碎成硬脂酸鹽含量5PHR的濃縮料。 以上述之濃縮料與PE混合後,再以吹袋機,吹製成0.03〜 0.04mm的PE薄膜,藉由改變濃縮料和PE的摻混比例,可得 到不同濃度之光分解性PE。 將吹製好之光分解性PE膜,置於氙弧光燈加速試驗機, 其中氙弧光光源以適當光罩處理後使其光源強度分佈與曰 光相近,將樣品置於離燈源508mm處,繞著燈源旋轉曝曬, 以得到均一之曝薩效果。控制試驗機中溫度為35±5%, 溫度為401C。每日觀察樣品記錄其破壞碎裂時間,碎裂時 間愈短顯示其光分解速度愈快。 表(一)數據顯示含不同濃度硬脂酸鹽類光敏感劑的光 解性塑膠,於氙弧光燈下曝曬之碎劣時間。從實結果可知, 由本專利所合成得到的硬脂酸鐵或硬脂酸铈具有良好之光 分解性,可以有效的將PE分解碎劣時間由1000小時以上縮 短成200〜600小時,達到光分解的目的。藉由添加硬脂酸 鹽種類之不同或添加量之多寡可控制光分解的速度。 (請先W1?背而之注意事項孙艰寫木页) 裝- 訂- 線· 本紙张尺度逍用中a國家楳準(CNS) T 4規格(2I0X297公;《:) 3 4 ¾ If: β η: 6 6 ΛΠ 五、發明説明(7 )表(一) 未調整酸鹼前 調整酸鹼後 硬脂酸鐵 14.8% 1.4% 硬脂酸鈽 6.5% 196 經濟部中央榣準妁β工消许合作杜印製 表(二) 脂肪酸金屬鹽種類及含量 碎製時間 空白 > lOOOhr 硬脂酸鐵0.03 phr 343hr 硬脂酸鐵0.1 phr 300hr 硬脂酸鐵0.25 phr 217hr 硬脂酸鐵0.5 phr 217hr 硬脂酸鈽0.03 phr 845hr 硬脂酸铈0.1 Phr 670hr 硬脂酸鈽0.25 phr 644hr 硬脂酸鈽0.5 phr 550hr (請先閲讀背而·乂注意事項#場寫本頁) 本紙张尺度遑用中8困家標準(CNS) Τ4規格(2]0父297公®)20554 * 5 A6 B6 V. Description of the invention (4) The metathesis reaction between sodium acid and metal salt aqueous solution to control the pH value of the reaction below 7, (usually between 7 ~ 2), so that the residual fatty acids can proceed The reaction produces fatty acid metal salts. At this time, a small amount of fatty acid remained, and then sodium hydroxide and metal salt aqueous solution were added as described above, and then the saponification reaction and the metathesis reaction were carried out. Through the acid age characteristics of the reactants NaOH and the metal salts themselves, it is added repeatedly to adjust the pH value of the reaction and effectively reduce the content of unreacted fatty acids. In addition to controlling the amount of fatty acids, the number of pH adjustments can also control the content of fatty acids attached to metal ligands. The number of adjustments in the experiment is generally controlled at about 3 times to achieve satisfactory results. The following examples illustrate the invention in more detail, but the invention is not limited to these examples. [Example 1] Synthesis of ferric stearate Dissolve 10g of sodium hydroxide in 500g of water, weigh in 75g of stearic acid (NV = 204), heat and stir to 90 * C to completely saponify stearic acid, After forming transparent colloidal sodium stearate, 222ml of vaporized iron solution (0.4M) was slowly added to carry out double decomposition reaction. After the formation of suspended red product, the water in the reaction tank was filtered to complete the preliminary Synthesis reaction. Subsequently, 156ml of 0.4M sodium hydroxide solution and 344ml of pure water were added to the reaction tank, which was heated and stirred to 9〇υ, so that the residual stearic acid in the product was subjected to saponification reaction, and then the 0.4M ferrized iron solution was 55ml Add to the reaction tank to produce suspended iron stearate, then add 93.6ml of hydrogenated sodium solution for saponification, then add 33ml of ferrized iron solution for double decomposition reaction, then add 50ml of 0.4M (please read the back (Notes to fill out this page) • Pei • • order • • line • A 4 (210X297 public love) 205543 5. Description of the invention (5) Sodium hydroxide gas solution, after the saponification reaction, add 18ml 0.4M ferrous iron solution Then the final product iron stearate is formed. The product after synthesis and the product without acid age adjustment were analyzed by extraction titration for stearic acid content, which were 1.4% and 14.8% respectively, as shown in Table (1), it was confirmed that the residual stearic acid after acid adjustment was significantly reduced . After FTIR and DSC tests, the graphs are shown in Figure (1) ~ Figure (4). From the analysis of Figures (1) and (2), the FTIR analysis shows that after adjustment, the stearic acid absorption peak near 1707cm · 1 no longer exists. . The DSC analysis graphs in Figures (3) and (4) can also confirm that the low-melting stearic acid disappeared after the acid test adjustment. [Example 2] Synthesis of cerium stearate, the Ministry of Economic Affairs, the central government, and the employee's rape cooperation Du Yin 5i (please read the back and the precautions # 蜞 写 木 页) in the reaction tank, 10g sodium hydrogen Dissolve in 500g of water, weigh 75g of stearic acid (NV = 204) and add, heat and stir to 90t: make the stearic acid completely saponified to form transparent colloidal sodium stearate, then slowly add the gasification anchor solution (0.3M) 293ml was subjected to metathesis reaction; after the end of the reaction, a milky white suspension was formed, and the reaction water was filtered off. Then weigh 125ml of 0.4M sodium hydroxide solution and 375ml of pure water into the reaction tank, heat and stir to 90%, so that the residual stearic acid in the product can be saponified, and then add 58.8ml of 0.3M gasified sister solution to the reaction The tank produces suspended cerium stearate, then add 85ml of 0.4M hydrogenated sodium solution for saponification reaction, then add 21ml of plutonium chloride solution for metathesis reaction, then add 31ml of sodium hydroxide solution, add 14.6nl after saponification 0.3M vaporized plutonium solution to produce the final product cerium stearate. After analyzing the product and the product without acid test adjustment, the stearin content was analyzed by 1% and 6.5% respectively, as shown in Table (1), which confirmed that the residual stearic acid after acid adjustment was significantly reduced. After further testing by FTIR and DSC, the graph shows that the paper is used in the B-standard (CNS) T4 specification (210X297 mm) 3 Λ If κ 20 66 ΛΠ Printed by the Employee of the Central Standards Bureau of the Ministry of Economic Affairs, Cooperative Society 5i V. Invention Explanation (6) As shown in Figures (5) to (8), the FTIR analysis of Figures (5) and (6) shows that the stearic acid absorption peak at 1707 (^ 4) is no longer present after being adjusted by the repeated acid halide. The DSC graphs in Figures (7) and (8) can also confirm that the low-melting stearic acid disappears obviously after the acid-base adjustment. [Example 3] Weigh 250g of stearate in Examples 1 and 2. 4750g of low-density PE (Taiju NA207-66, the same below) is kneaded with a double roller at 140 ° C for 5 to 10 minutes, and then crushed into a concentrate with a stearate content of 5PHR using a granulator. After mixing with PE, it is blown into a PE film of 0.03 ~ 0.04mm with a bag blowing machine. By changing the blending ratio of the concentrate and PE, different concentrations of photodegradable PE can be obtained. Decomposable PE film, placed in Xenon arc lamp acceleration test machine, in which the xenon arc light source is treated with an appropriate mask to make it light The intensity distribution is similar to that of the light. Place the sample at 508mm away from the light source and rotate it around the light source to obtain a uniform exposure effect. Control the temperature in the testing machine to 35 ± 5% and the temperature to 401C. Observe daily The sample records the time of destruction and fragmentation. The shorter the fragmentation time, the faster the photodecomposition rate. Table (1) The data shows that the photolytic plastics containing different concentrations of stearate photosensitizers are exposed to xenon arc lamps. It can be seen from the actual results that the iron stearate or cerium stearate synthesized by this patent has good photodegradability, and can effectively reduce the PE degradation and breakage time from more than 1000 hours to 200 ~ 600 hours. To achieve the purpose of photodecomposition. The speed of photodecomposition can be controlled by adding different types of stearate or the amount of addition. (Please W1? Contrary Notes Sun Jian writes a wooden page) Binding-Binding-Line · The standard of this paper is the Chinese National Standard (CNS) T 4 specification (2I0X297; ":") 3 4 ¾ If: β η: 6 6 ΛΠ V. Description of invention (7) Table (1) Unadjusted acid and alkali Before adjusting acid and alkali, iron stearate 14.8% 1.4% stearic acid 6.5% 196 Ministry of Economic Affairs, Central Ministry of Economic Affairs, β-consumer cooperation, du printing, tabulation (2) Types and contents of fatty acid metal salts Breaking time blank> lOOOOhr ferric stearate 0.03 phr 343hr ferric stearate 0.1 phr 300hr stearin Ferric acid 0.25 phr 217hr Ferric stearate 0.5 phr 217hr Plutonium stearate 0.03 phr 845hr Cerium stearate 0.1 Phr 670hr Plutonium stearate 0.25 phr 644hr Plutonium stearate 0.5 phr 550hr (please read beforehand # 场 write this page) This paper standard is not used in the 8-sleeper standard (CNS) Τ4 specification (2) 0 father 297 Gong ®)

Claims (1)

六、中請專利範圓 1. 一種脂肪酸金屬鹽之製備方法,其特徵傜利用反應溫度介 於60 °C至100 °C之複式反應中,皂化碩數在c 7〜C 22脂肪 酸之鹼性水溶液與水溶性金屬鹽類酸性水溶液,於反應過 程中利用此鹼性及酸性水溶液交替添加,反覆調整反應酸 鹼值的方法,合成低脂肪酸含量之脂肪酸金屬鹽類,其中 的水溶性金屬鹽類是指本身具有可被利用之酸性者,如鐵、 鋁、鈽、鈷、銅、錳、鎂、鈣、鎳之氯化鹽、硫酸鹽、硝 酸鹽、醋酸鹽類化合物或混合物。 2. 如申請專利範圍第1項的製備方法,其中脂肪酸碩數以C8 〜C 2。者為佳。 3. 如申請專利範圍第1項的製備方法,其中反應溫度以80°C 〜90°C最為適宜。 (访^-聞讀背面之-意事項再填商本頁 ,发_ .打· 經濟部十央標^^π工消«'合作社印览 .線·6. Zhongyuan Patent Fan Yuan 1. A preparation method of fatty acid metal salt, which is characterized by the use of a compound reaction with a reaction temperature ranging from 60 ° C to 100 ° C. Aqueous solution and water-soluble metal salt acidic aqueous solution, use this alkaline and acidic aqueous solution alternately during the reaction process, and repeatedly adjust the reaction pH value method to synthesize fatty acid metal salts with low fatty acid content, of which water-soluble metal salts Refers to those with inherently usable acidity, such as iron, aluminum, plutonium, cobalt, copper, manganese, magnesium, calcium, nickel chloride, sulfate, nitrate, acetate compounds or mixtures. 2. The preparation method as claimed in item 1 of the patent application, wherein the fatty acid master number is C8 ~ C2. The better. 3. The preparation method as described in item 1 of the patent application scope, in which the reaction temperature is most suitable from 80 ° C to 90 ° C. (Visit ^-Read the back of the page-Matters needing attention and then fill out this page, send _. Hit · the Ministry of Economic Affairs ten central standard ^^ π 工 消 «'Cooperative Society Print. Line ·
TW81101957A 1992-03-16 1992-03-16 A novel preparation method of the aliphatic acid metal salts TW205543B (en)

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