200416248 玫、發明說明： 【發明所屬之技術領域】 本發明〈標的係—種組合物’其包含化合物㈤，其係選 自鹼土金屬氫氧化物’以及化合物[b]，其係由以二羧 基化合物及諸等副產物為基礎之混合物所構成，該混合物 係藉著製備在驗性試劑之存在下由酉旨及酉同之縮合反應所取 得之yS-二羧基化合物而產生。 本發明之標的亦係、該組合物之取得，以及其作為包含齒 代聚合物之調配物之安定劑之用途。 【先前技術】 咸已熟知商代聚合物’特別如以氯乙缔為基礎者，必須 使用諸多安定劑。該等安定劑係用以在形成該等聚合物時 使其進行熱安定而使用，但其亦係在使用該等聚合物時使 其安定而使用，例如，在面對紫外線時。同時，咸亦已知 鹼土金屬（！弓）及/或過度金屬（辞）致基化合物、有機-錫類 型化合物、或錯基礎性化合物之使用。 合其他化合物使用，諸如，舉例而言…嶋： 酿、亞磷酸鹽等類型之有機化合物，或是諸如水滑石等之 無機化合物。 、在部刀應用4頁域中，#別諸如窗型材之應用領域，高純 度有機安定劑化合物之使用（其目此係一重要之成本）係可 接雙者。 相对的’在其他之應用領域中，如此昂貴之安定劑之使 用卻係不可考慮者’諸如’在其中該聚合物組合物並不— 87201 200416248200416248 Rose, description of the invention: [Technical field to which the invention belongs] The subject of the present invention is a composition 'comprising compound ㈤, which is selected from the group consisting of alkaline earth metal hydroxides' and compound [b], which is composed of a dicarboxyl group. The compound and various by-products are based on a mixture, which is produced by preparing a yS-dicarboxy compound obtained by a condensation reaction and a common condensation reaction in the presence of an analytical reagent. The subject matter of the present invention is also the acquisition of the composition and its use as a stabilizer for formulations containing dental polymers. [Prior art] It is well known that commercial polymers', especially those based on chloroethyl chloride, must use many stabilizers. These stabilizers are used to thermally stabilize the polymers when they are formed, but they are also used to stabilize the polymers when they are used, for example, in the face of ultraviolet light. At the same time, salt is also known for the use of alkaline earth metals (! Bow) and / or transition metals (words) based compounds, organic-tin type compounds, or wrong basic compounds. Used in combination with other compounds, such as, for example, 嶋: organic compounds such as fermented, phosphite, or inorganic compounds such as hydrotalcite. 4. In the field of 4 pages of Ministry of Knife Application, #Does not apply to such fields as window profiles. The use of high-purity organic stabilizer compounds (which is an important cost for this purpose) can be used for both. In contrast, 'in other fields of application, the use of such an expensive stabilizer is not considered', such as' in which the polymer composition is not-87201 200416248
义頊為曰色之應用領域中。目前，其係使用無機安定劑， 並為級校正之溶液對抗熱安定之問題。相對的，其亦每厂、 必須改良此等安定特性，特別係藉由該安定劑組合物 合物基礎性調配物中之較佳相容性Q 本發明之目標係提供一種組合物，其可作為包含至少— 種氯代聚合物之調配物 < 安定劑，其係有效者，且其在昂 貴安定劑之使用並不合理之領域中係經濟可行者，但其I 不限於此等。本發明之目標亦係提供一種組合物，其;= 其作為包含至少一種氯代聚合物之調配物之安定劑之用途 而以實用形式存在。 ” 【發明内容】 此等及其他目標係由本發明而達成，其標的因此係—種 組合物，其包含： *顆粒形式之化合物[a]，其係無機化合物或乙醯丙酮鋅； *化合物[b]，其係由以重量計⑴抓之万·二叛基化合物 及以重量計5-99%之副產物為基礎之混合物所構成，該混 合物係藉著製備在驗性試劑之存在下由醋及酮之縮合反應 所取得之万-二羧基化合物而產生。 本發明之另一標的係製備該組合物之方法，其中係在足 以使化合物_融狀態之溫度下，於攪拌下，使化合物 [b]接觸化合物[a]。 u 二發明？另—標的係由該組合物作為嶋合靖別 系氷虱乙烯)基礎性調配物之安定劑之用途而構成。 8720! 本發明組合物之使用可以低成本取得良好之安定特性。 200416248 本發明之其他特徵及搭处 、士 更形明確。 …由_下文之敘述及實例而 【實施方式】 1咸明確指明，本發明之組合物係—種組合物，亦即一種 產物，其係用以引入齒代聚合物基礎性調配物中者。在本 專利申請案中，就本發明之組合物而言，咖合物因此 並不-括以鹵代聚合物為基礎或包含其之組合物。 化口物[a]《顆粒至少係部份由化合物阳包裹或由其彼此 連、、、口。因此’孩組合物可以由一層化合物[b]塗覆之化合物 [a]個相粒形式存在，該化合物剛係塗覆化合物㈤之全 部表面或僅堡覆其—部份。該組合物亦可以其中散布化合 物W顆粒之化合物[b]連續基質形式存在。此—形式並不^ P于、I且口物本身係為顆粒形式者。該組合物亦可以化合物 [a]顆粒〈附聚物形式存在，該等顆粒係以或多或少隨機分 布之化合物[b]彼此連結(非連續基質)。此一形式並不排除 該組合物本身係為顆粒形式者。 如上文所指出者，本發明之標的係一種組合物，其包含 化^物[a]以及由以重量計贴㈣之^二幾基化合物及以 重量計5-9G%之副產物為基礎之混合物所構成之化合物 []咸/m。物係藉著製備在鹼性試劑之存在下由酯及酮之 縮合反應所取得之二羧基化合物而產生。 畎典機化合物㈤而S，可舉例者包括驗土金屬氫氧化 物、水滑石、碳酸鈣、二氧化鈦。 化口物[b]/化合物间之重量比係大於或等於"丨⑻，更特 87201 200416248 、、系大灰或等於1/50 ’較佳係大於或等於丨/2〇。同時， 該重量比較佳係小於或等賴，更特定言之係小於或等於 1/3，較佳係小於或等於。 化合物[a]較佳係氫氧化鈣。 此：’根據本發明之一較佳實施方式，化合物[幻代表平 均直徑小於或等於·酔之顆粒’較佳係介於2辦及脾 間者。 、化合物[b]係以方_二羧基化合物及諸等副產物為基礎之 混合物。 。口物係藉著製備在鹼性試劑之存在下由酯及酮之縮 合反應所取得之点-二羧基化合物而產生。 、，、。之用於别述縮合反應中之酯係符合下列化學 式R C〇〇R…其中叫戈表烴基，其具有玉至纖碳原子， 或可經-或多個_〇、-C〇_〇…c〇_基團中斷；R2代表烴基， 其包含1至4個碳原子。 ,更特疋& 基團R1代表烷基、醯基，其係直鏈或支 、：為Cl C30 ’較佳係CrC24 ; c6_C30芳基，其係經至少一個 CrClQ烷基、MiQ燒氧基、#原子、及/或矽原子取代或 未、&取代，CrCl4環脂族基團。該基團或可具有碳-碳雙 鍵且其或可經一或多個_〇_、-ca〇_…c(>基團中斷。 在可旎<諸等基團中，可舉例者包括月桂基、肉豆蔻 基硬知基、異硬脂基、椋櫚基、二十二烷基、二十四烷 2、油醯基、棕櫊油醯基、亞麻油醯基、次亞麻油醯基、 F基，其或可帶有一或多個烷基、烷氧基取代基。 87201 200416248 就基團R2而言，其較佳係代表CrC4烷基。須注意者，根 據？Μ驗性試劑之性質’選擇其對應之醇於該縮合反應之條 件下為揮發性者之基團R2可能係有利者。 特別較佳者，該基團係甲基。 須注意者，該酯可以其單純形式存在，或是以部分或完 全鈿合^形式存在。根據本發明之—實施方式，如該酯於 酉曰基< α位置具有氫原子，其即可部分或全部以石-酮酯 之形式使用。在此情形下，在前述之酯化學式中，可在上 述之醋化學式中以RCOR4取代基_。在此情形下，該式 變成R1C〇R，1C〇〇R2，R1具有和上文相同之意義，RU亦相同， 惟其係代表雙價基團。 、更特疋3炙，用於該縮合反應中之酮係符合下列化學 式R C〇CH2R4，其中化代表烴基，其具有工至％個後原子， 或可、工或夕個_〇_、-Ca〇_、（〇_基團中斷；％代表氯原子 或包含至多4個碳原子之烴基。 軚佳者’基團R3代表烷基、醯基，其係直鏈或支鏈，為 A ^3〇c c" ί 'ί ^°24 ； C6'C3°" ^ ^ # M ^ ^ ~ 代.crcio’r 商原子、及/或珍原子取代或未經取 ㈠3·】4,衣脂族基團。該基團或可具有碳-竣雙鍵，且复 或可經一或多個-0…C0_0_、_C0_基團中斷。 、 在^之諸等基圏中’可舉例者包括月桂基、肉豆爷 土 '硬月日基、異硬脂基、棕搁基、二十其、 l 基、油B喪其 p j日 70 土 一十四坡 油I基、棕櫚油醯基、亞麻油 苄基，其或 ㈣-基、次亞麻油醯基、 87201 Ά有-或多個燒基、垸氧基取代基。 -10- 200416248 就基團R4而言，其較佳係代表CrC：4烷基。特別較佳者， 该基團係甲基。 一般而言，該酮對該酯之莫耳比係介於2/3至m之間。較 佳者，該酯係以相對該酮至多30%之莫耳過量存在，且更 佳者，其係5至20%莫耳過量。 該縮合反應可製備式RiC〇CH2COR3之石-二羧基化合物， 其中Ri及R3具有前文祥述之意義。須注意者，其並不排除 其中Ri及R3係以使該/3 -二羧基化合物以環形式存在之方式 彼此連結。 根據本發明之一實施方式，該反應係在溶劑之存在下進 行。該溶劑係選自在該等反應條件下呈鈍性之化合物。 在傳統上，其係選自芳族、脂族、或環狀之烴丨烴級 份、it 〇 較佳者，該溶劑係選自烷基苯（諸如，甲苯）、二烷基 苯、及三烷基苯，但其亦可選自異丙醚；甲苯、二甲苯係 較佳者。 ’ 此外，該縮合反應係在鹼性試劑之存在下進行。更特定 吕之，該試劑係選自胺基化物、氰化物、含丨至4個碳原子 之醇。 一般而言，在該反應過程中存在之鹼性試劑莫耳數係使 該驗性試劑/酯及酮總莫耳數之莫耳比為約1。 根據第一實施方式，該縮合反應係在氰化鈞之存在下進 行’或較佳係在胺基化鈉之存在下進行。 在胺基化鈉存在之情形下，較佳係在鈍性大氣下進行該 87201 -11 - 200416248 反應’較佳係在氮氣之氣洗下進行。 此外，該反應較佳係在介於30及60t間之溫度下進行。 根據本發明之第二實施方式，該鹼性試劑係醇化鈉，其 中该對應之醇在該縮合反應之條件下為揮發性者。較佳 者’遠醇化物係曱醇納。 此外，在此情形下，該溶劑係選自具有較該反應溫度高 出至少20°C之沸點溫度者。 較佳者’反應係在該溶劑之回流溫度下進行。 不論所定之變數為何，該反應較佳係將該酮引入含有該 鹼性試劑（以及該溶劑，如必要時）之酯中進行。 根據該鹼性試劑之性質，可合理預見回收之方式，其或 為氣產物，或為醇產物。 在孩試劑係醇化物之特定情形下，在其於反應混合物中 出現之過程中同時除去該醇產物之方式代表一種極佳之流 程特性，且其可造成例如所欲万_二羧基化合物產率之增 加0 在茲反應終了之時，同樣，不論所定之變數為何，該反 應介質較佳係經酸化。 就此目的而言，其係將該反應混合物引入一酸之水溶液 中其I佳係醋酸、鹽酸、及硫酸。茲將該水層之阳定為 較佳係介於1及3間之值。 在以水m洗至少一次後，以任何習知之方法除去該溶 劑，例如，藉由蒸發，並取得粗製產物。 3粗製產物包含所欲之万-二羧基化合物 87201 200416248 (RiCOCI^COR^) ’以及其對稱同系物（Rlc〇CH2C〇Ri、 R^COCH^COR^)，亦包含諸等副產物。 須 >王意者，該等副產物之確切組成因過於複雜而無法評 估。其特別可來自該等万_二羧基化合物彼此間之丁烯醛 化作用、包含醯胺官能基之化合物種之出現（如該鹼性試 劑包含氮時）。 根據本發明之第一變化，化合物[b]包含對應於該縮合反 應所產生粗產物之混合物。 在孩變化之情形下，万_二羧基化合物之含量係介於以 重量計之做95%之間，較佳係介於以重量計之微之 間，且副產物〈含量係以重量計之5至嶋，較佳係以重量 計之20至60%。 根據此變化之化合物[b]係以分割固體之形式存在，根據 所用之實施方式’其可為时或片狀物之形式。 在該化合物之諸等實施方式中，可舉例者包括，但不限 於，剝離、於溶劑中之沈殿、低溫研磨、於氣流中之霧化 /乾燥。 剥離法可耩著使該溶液通過— 、、 ^ 待，冷郃爻旋轉滾筒而除 去$亥反應混合物之溶劑。於兮、、会μ 於及表同表面固化之產物再由刮 刀以片狀物形式回收。 ’將熔融形式之該粗製 孩化合物在此溫度下並 舉例而言，乙醇或甲 在溶劑中沈澱之技術係由，例如 產物傾倒至室溫下之一化合物中， 非該粗製產物之良好溶劑，諸如； 醇，再分離所形成之沈澱物而構成 87201 -13 - 200416248 就低溫研磨而言，其一 他鈍性液態氣體（諸如，（ 得之數釐米至數公分大/ 行0 一般係在研磨器中引入液態氮或其 C〇2)以及藉由粗研磨或剝離技術取 小塊狀形式之反應粗製產物而進 最後， 務化/乾燦法係藉由通過順流或逆流Righteousness is the application of color. At present, it uses an inorganic stabilizer and is a grade-corrected solution to counter the problem of thermal stability. In contrast, it is also necessary to improve these stability characteristics per plant, especially by virtue of better compatibility in the basic formulation of the stabilizer composition. The object of the present invention is to provide a composition which can As a stabilizer containing at least one chlorinated polymer < stabilizer, it is effective and it is economically feasible in areas where the use of expensive stabilizers is not reasonable, but its I is not limited to these. It is also an object of the present invention to provide a composition which is present in a practical form as a stabilizer for a formulation comprising at least one chlorinated polymer. [Summary of the Invention] These and other objectives are achieved by the present invention, and the subject matter thereof is a composition comprising: * Compound [a] in the form of particles, which is an inorganic compound or zinc acetoacetone; * Compound [ b], which is composed of a 10,000 dibenzyl compound grabbed by weight and a by-product based on 5-99% by weight of a mixture, which is prepared by preparing in the presence of a test reagent It is produced by the 10,000-dicarboxy compound obtained by the condensation reaction of vinegar and ketone. Another object of the present invention is a method for preparing the composition, wherein the compound is stirred at a temperature sufficient to make the compound in a molten state under stirring. [b] The contact compound [a]. u Second invention? Another-the target system is composed of the use of the composition as a stabilizer for the basic formulation of Jingbei line ice vinyl) 8720! Composition of the present invention It can be used at low cost to obtain good stability characteristics. 200416248 The other features of the present invention, its usefulness, and the shape of it are clear.… The following description and examples and [Embodiments] 1 clearly indicate that the composition of the present invention -A composition, that is, a product, which is used to introduce a base polymer into a formulation. In this patent application, as far as the composition of the present invention is concerned, the coffee composition is not Compositions based on or containing halogenated polymers. Mouthpieces [a] "Particles are at least partially enclosed by compounds or connected to each other, so that the composition can be composed of a layer of compound [ b] The coated compound [a] exists in the form of phase particles, the compound has just been coated on the entire surface of the compound 或 or only covers it-part. The composition can also be a compound [b] in which the particles of the compound W are dispersed Continuing matrix form exists. This-the form is not P, I and the mouthpiece itself is in the form of particles. The composition can also exist in the form of compound [a] particles <agglomerates, these particles are in more or more The less randomly distributed compounds [b] are connected to each other (discontinuous matrix). This form does not exclude that the composition itself is in the form of particles. As noted above, the subject of the present invention is a composition comprising ^ 物 [a] and by weight The compound consisting of a mixture of quinone compounds and a by-product of 5-9G% by weight [] salt / m. The compound is prepared by the condensation reaction of an ester and a ketone in the presence of a basic reagent It is produced by the obtained dicarboxyl compound. The typical organic compounds and S can be exemplified by soil test metal hydroxide, hydrotalcite, calcium carbonate, and titanium dioxide. The weight ratio between the compound [b] / compound is greater than Or equal to " 丨 ⑻, more specifically 87201 200416248, is a large gray or equal to 1/50 'preferably greater than or equal to / 2/2. At the same time, the weight is better than less than or equal, more specifically Less than or equal to 1/3, preferably less than or equal to. Compound [a] is preferably calcium hydroxide. This: 'According to a preferred embodiment of the present invention, the compound [magic represents an average diameter of less than or equal to 酔Granules' are preferably between the two offices and the spleen. Compound [b] is a mixture based on a square dicarboxylic compound and various by-products. . Mouth products are produced by preparing a point-dicarboxy compound obtained by the condensation reaction of an ester and a ketone in the presence of a basic reagent. ,,,. The ester used in other condensation reactions conforms to the following chemical formula RC〇〇R ... Among them is called epitope hydrocarbyl, which has jade to fiber carbon atoms, or can pass-or more _〇, -C〇_〇 ... c The O group is interrupted; R2 represents a hydrocarbyl group containing 1 to 4 carbon atoms. More specifically, the 疋 & group R1 represents an alkyl group, a fluorenyl group, which is a linear or branched group: Cl C30 'preferably CrC24; c6_C30 aryl group, which is at least one CrClQ alkyl group, MiQ alkoxy group , # Atom, and / or silicon atom are substituted or unsubstituted, & substituted, CrCl4 cycloaliphatic group. The group may have a carbon-carbon double bond and it may be interrupted by one or more _〇_, -ca〇 _... c (> groups. Among the various groups, examples are These include lauryl, myristyl stearyl, isostearyl, palmityl, behenyl, tetracosane 2, oleyl, palmitoyl, linoleyl, sub- Hesperidinyl and F groups may or may not have one or more alkyl or alkoxy substituents. 87201 200416248 As far as the group R2 is concerned, it preferably represents a CrC4 alkyl group. It should be noted that according to the test It is probably advantageous to select a group R2 whose corresponding alcohol is volatile under the conditions of the condensation reaction. Particularly preferred, the group is methyl. It should be noted that the ester may be Exist in a simple form, or in a partially or fully coupled form. According to an embodiment of the present invention, if the ester has a hydrogen atom at the 酉 < α position, it may be partially or wholly in the form of a stone-ketoester. In this case, in the aforementioned chemical formula of the ester, the RCOR4 substituent can be substituted in the aforementioned chemical formula of the vinegar. In this case This formula becomes R1COR, 1COR2, R1 has the same meaning as above, and RU is also the same, but it represents a bivalent group. 2,3, more specifically, ketones used in the condensation reaction It conforms to the following chemical formula RC〇CH2R4, wherein Hua represents a hydrocarbyl group, which has a work-up to% of the rear atom, or can be, work-up or a _〇_, -Ca〇_, (〇_ group interruption;% represents a chlorine atom or contains A hydrocarbon group of up to 4 carbon atoms. The group R3 represents an alkyl group, a fluorenyl group, which is a straight or branched chain, and is A ^ 3〇c c " ί 'ί ^ ° 24; C6'C3 ° & quot ^ ^ # M ^ ^ ~ Generation. Crcio'r Quotient atom and / or Jane atom substituted or unselected · 3] 4, aliphatic group. This group may have a carbon-complete double bond, and It may be interrupted by one or more groups of -0 ... C0_0_, _C0_. Among the basic groups, examples include lauryl, myrtle, hard moonyl, isostearyl , Brown base, twenty bases, l base, oil B, pj day 70 soil fourteen slope oil I base, palm oil base, linseed oil benzyl, or its base, linseed oil base, 87201 Ά Yes-or more Alkoxy substituent. -10- 200416248 As far as the group R4 is concerned, it preferably represents CrC: 4 alkyl group. Particularly preferred, the group is methyl. Generally speaking, the ketone is The molar ratio is between 2/3 and m. Preferably, the ester is present in a molar excess of up to 30% relative to the ketone, and more preferably, it is a molar excess of 5 to 20%. The condensation reaction can prepare a stone-dicarboxyl compound of the formula RiC0CH2COR3, wherein Ri and R3 have the meanings described above. It should be noted that it does not exclude that Ri and R3 are used to make the / 3-dicarboxyl compound ring The ways in which forms exist are linked to each other. According to one embodiment of the present invention, the reaction is performed in the presence of a solvent. The solvent is selected from compounds which are passive under these reaction conditions. Traditionally, it is selected from the group consisting of aromatic, aliphatic, or cyclic hydrocarbons. The hydrocarbon fraction, it is preferred. The solvent is selected from the group consisting of alkylbenzenes (such as toluene), dialkylbenzenes, and Trialkylbenzene, but it can also be selected from isopropyl ether; toluene and xylene are preferred. In addition, the condensation reaction is performed in the presence of a basic reagent. More specifically, the reagent is selected from the group consisting of amines, cyanides, and alcohols having from 4 to 4 carbon atoms. In general, the molar number of alkaline reagents present during the reaction is such that the molar ratio of the total molar number of the test reagent / ester and ketone is about one. According to the first embodiment, the condensation reaction is performed in the presence of cyanide, or preferably in the presence of sodium amide. In the presence of sodium amide, it is preferred to perform the 87201-11-200416248 reaction 'in an inert atmosphere, preferably under a nitrogen gas wash. In addition, the reaction is preferably carried out at a temperature between 30 and 60 t. According to a second embodiment of the present invention, the alkaline reagent is sodium alcoholate, wherein the corresponding alcohol is volatile under the conditions of the condensation reaction. The more preferred 'far alcoholate' is sodium methoxide. Further, in this case, the solvent is selected from those having a boiling point temperature higher than the reaction temperature by at least 20 ° C. Preferably, the reaction is carried out at the reflux temperature of the solvent. Regardless of the variables set, the reaction is preferably carried out by introducing the ketone into an ester containing the basic reagent (and the solvent, if necessary). Based on the nature of the alkaline reagent, it is reasonably foreseeable that the recovery method is either a gas product or an alcohol product. In the particular case of alcohol reagents, the manner in which the alcohol product is removed simultaneously during its appearance in the reaction mixture represents an excellent process characteristic, and it can cause, for example, the desired yield of the dicarboxylic compound The increase of 0 is at the end of the reaction. Similarly, the reaction medium is preferably acidified regardless of the set variables. For this purpose, the reaction mixture is introduced into an aqueous solution of an acid. Preferred are acetic acid, hydrochloric acid, and sulfuric acid. The yang of this water layer is preferably set to a value between 1 and 3. After washing with water m at least once, the solvent is removed by any conventional method, for example, by evaporation, and a crude product is obtained. 3 The crude product contains the desired 10,000-dicarboxy compound 87201 200416248 (RiCOCI ^ COR ^) 'and its symmetrical homologues (Rlc0CH2C0Ri, R ^ COCH ^ COR ^), and also contains various by-products. For > Wang Yi, the exact composition of these by-products is too complex to evaluate. It can particularly come from the butenalization of these 10,000-dicarboxylic compounds with each other, the appearance of compounds containing amidine functional groups (such as when the basic reagent contains nitrogen). According to a first variation of the invention, the compound [b] comprises a mixture corresponding to the crude product produced by the condensation reaction. In the case of changes, the content of 10,000-dicarboxylic compounds is between 95% by weight, preferably between slightly by weight, and the content of by-products <by weight 5 to 嶋, preferably 20 to 60% by weight. The compound [b] according to this change exists in the form of a divided solid, and it may be in the form of an hour or a sheet according to the embodiment used '. Among the various embodiments of the compound, examples include, but are not limited to, peeling, immersion in a solvent, low-temperature grinding, and atomization / drying in an air stream. The stripping method may be carried out by passing the solution through, and waiting for, coldly rotating the drum to remove the solvent of the reaction mixture. The products cured on the surface of Yu Xi, Yu and Yu are recovered by the scraper as a sheet. 'The technique for precipitating the crude compound in molten form at this temperature and, for example, ethanol or formazan in a solvent is, for example, pouring the product into a compound at room temperature, which is not a good solvent for the crude product, For example, alcohol, and then separate the formed precipitate to form 87201 -13-200416248. In terms of low temperature grinding, other inert liquid gases (such as, (a few centimeters to several centimeters large / line 0 are generally used in grinding) Introduce liquid nitrogen or Co2) into the device and take the reaction crude product in the form of small blocks by rough grinding or stripping technology. Finally, the commercialization / dry-can method is adopted by co-current or counter-current
引入之鈍性 第—、交化，化合物[b]包含對應於在純化步 一羧基化合物分離後所回收產物之混合 根據居又化其係使該粗製產物在適當之溶劑中進行再 醇’諸如’乙醇。自含有該溶劑以及副產物 及万-二羧基化合物之溶液中，分離經純化之点_二羧基化 合物’特別係藉由過濾。接著以除去該結晶溶劑之方法處 里3 /容液例如’藉由蒸發。如此而根據此第二變化回收 化合物[b]。 根據本發明之此實施方式，万-二羧基化合物之含量係 介於以重量計之1及低於40%之間，較佳係介於以重量計之 3及低於40%之間，且副產物之含量係以重量計之高於6〇〇/〇 至99% ’較佳係以重量計之高於60至95%。 根據此第二變化之化合物[b]可以固體及/或糊狀形式存 在。 明確可知，化合物[b]可為如前文所述由縮合反應產生之 混合物’或者其可包含由不同縮合反應而產生之混合物之 結合。 87201 -14 - 200416248 本發明之組合物或可包含至少—種酸之無機傳感物 (capte^y其係選自如銘及/或鎂之沙銘酸鹽、硫酸鹽、及 /或碳酸鹽、水滑石、e義es。該酸之無機傳感物可係化 合物[a]’ ^ ’如化合物[a]係水滑石或碳酸鈣。該酸之無 機傳感物或者可係包含於該组合物中之不同於化合物[a]之 化合物，亦即，一種添加劑。 、須提及者，水滑石類型之化合物係對應於下列之化學 式：Mgl_為_，-*_〇，其中χ係介於〇 (不含〇)及〇 5 間，An-代表一陰離子，特別諸如碳酸根，η係自，且 m係正數。 可使用諸等實質上非晶形之化合物，其具有式剛〆 ΑΙΑ、（c〇2)x、（H2〇)z，其中x、y、及z符合下列之不等式： 〇 < Μ 0.7 ’ 〇 < y m，且z 2 3。此等化合物特別述於專利申 請案EP 209 864中。 此外，邊等％ *cat〇ltes 之式 Ca3Al2(〇H)ac^A12(Si〇)4(〇H)u 化合物適合作為無機類型之鹽酸傳感化合物。 在石夕銘酸鹽中，可舉例者包括，例如，驗金屬切銘酸 鹽’其係晶體、合成性、具有介相重量計13及25%間之 水3里、具有組成0.7_1M2〇.Al2〇3_1.3-2.4Si〇2，其中Μ係代表鹼 金屬，特別諸如，鈉。特別適用者係類型NaA之济石，諸 如專利US 4,590,233中所述者。 在化3物[a]係驗土金屬氫氧化物（如，氫氧化齊）之情形 下或者，在忒組合物包含作為添加劑之酸傳感物之情形 下’其總含量係以重量計2.5至50%，較佳者係相較於驗土 87201 -15 - 200416248 金屬氫氧化物之重量以重量計之5至25%。 本發明之組合物或可包含至少·一種添加劑化合物，其係 選自包含選自元素週期表第IIA、IIB、IVB欄之金屬之化合 物（見於 Bulletin de ia Soci0t6 Chimique de France，no· 1，Jan· 1966之增 刊），或是包含一種添加劑，其係選自尿嘧啶類型之化合 物。該添加劑化合物可係化合物[a]。該添加劑化合物或可 且較佳係包含於該組合物中之不同於化合物[a]之化合物。 就該等包含金屬之化合物而言，該金屬更特定言之係選 自鈣、鋇、鎂、鐵、鋅、錫、或鉛。 須 >王意者，可預期多種此等安定劑化合物之結合，諸 如’舉例而Ί： ’鈣及鋅基礎性安定劑化合物之混合物。 忒包含至少一種第IIB及ΠΑ欄元素之添加劑而言，特別可 舉例者包括有機酸之金屬鹽（皂），諸如，脂族、芳族羧 酸、或脂肪酸、或酚鹽或芳族醇化物。 最系使用者係，例如，馬來酸、醋酸、雙醋酸、丙酸、 ^酸、乙基-2-己酸、癸酸、十一烷酸、月桂酸、肉豆蔻 酸棕摘酸、硬月曰酸、油酸、萬麻醇酸、蘿酸（二十二碳 ^酸）、踁基硬脂酸、羥基十一烷酸、苯甲酸、苯基乙 酸對第二丁基苯甲酸、及水楊酸之IIA或ΠΒ元素鹽、酚 1奈知或經一或多個烷基取代之酚（如，壬基苯酚）之醇 衍生物。 Υ者邊添加劑係選自鹼土金屬之丙酸鹽、油酸鹽、 更^酸座月桂酸鹽、萬麻醇酸鹽、二十二碳貌酸鹽、苯 力瓜對第二丁基笨甲酸鹽、水楊酸鹽、馬來酸鹽、 87201 -16- 200416248 單-乙基-2-己酸鹽、壬基酚鹽、環烷酸鹽。 就含錄之化合物而言，特別可舉例者係述於 ENCYCLOPEDIA of PVC，Leonard I. NASS (1976) p. 299-303者。 此等化合物係極廣泛不同之化合物，其中最常使用者係 二代碳酸鉛、三代硫酸鉛、四代硫酸鉛、二代亞磷酸鉛、 原矽酸鉛、鹼式矽酸鉛、矽酸鉛及硫酸鉛之共沈澱物、鹼 式氣矽酸鉛、矽膠及原矽酸鉛之共沈澱物、二代鄰苯二酸 鉛、中性硬脂酸鉛、二代硬脂酸鉛、四代富馬酸鉛、二代 馬來酸鉛、乙基-2-己酸鉛、月桂酸鉛。 就以錫為基礎之化合物而言，特別可參照著作”Plastics Additives Handbook’’，Gachter/Muller (1985) p. 204-210或"Encyclopedia of PVCf,5 Leonard I. Nass (1976) p. 313-325 ^ 此等化合物特別係單或雙燒基錫之致酸鹽以及單或雙燒 基锡之硫鮮鹽。 在此等化合物中，最常使用者係二-正-甲基錫、二-正-丁基錫、或二-正-辛基錫之衍生物，諸如，舉例而言，二 月桂酸二丁基錫、馬來酸二丁基錫、月桂酸-馬來酸二丁 基錫、雙（單-CVCV烷基馬來酸）二丁基錫、二丁基錫之雙 (月桂基-硫醇鹽）、S-Sf(異辛基巯基乙酸）二丁基錫、沒-疏 基丙酸二丁基錫、馬來酸二-正-辛基錫聚合物、雙-s-s彳異 辛基巯基乙酸）二-正-辛基錫、iS -巯基丙酸二-正-辛基 錫.。上述化合物之單燒基衍生物亦係可用者。 選自尿嘧淀之添加劑更特定言之係6-胺基-尿•淀或6-胺 基-硫代尿嘧啶類型之衍生物，其在位置1及3具有取代 87201 -17- 200416248 基。該等位於位置1及3之取代基更特定言之係crCi2烷基、Introduced bluntness, cross-linking, compound [b] contains a mixture corresponding to the product recovered after the carboxyl compound is separated in the purification step. According to the reactivation, the crude product is re-alcoholized in an appropriate solvent such as 'Ethanol. From the solution containing the solvent, the by-products and the ten-dicarboxylic compound, the purified point-dicarboxy compound 'is specifically separated by filtration. Then, the crystallization solvent is removed by a method such as 3 'by evaporating. Thus, the compound [b] was recovered based on this second change. According to this embodiment of the present invention, the content of the 10,000-dicarboxy compound is between 1 and less than 40% by weight, preferably between 3 and less than 40% by weight, and The content of by-products is higher than 600/99 to 99% by weight 'preferably higher than 60 to 95% by weight. The compound [b] according to this second variation may exist in a solid and / or pasty form. It is clear that the compound [b] may be a mixture produced by a condensation reaction as described above 'or it may include a combination of mixtures produced by different condensation reactions. 87201 -14-200416248 The composition of the present invention may include an inorganic sensory substance (capte ^ y which is selected from the group consisting of ammonium salt and / or magnesium salt salt, sulfate, and / or carbonate, Hydrotalcite, e.es. The inorganic sensory substance of the acid may be compound [a] '^' such as compound [a] is a hydrotalcite or calcium carbonate. The inorganic sensory substance of the acid may be included in the composition The compound is different from the compound [a], that is, an additive. It should be mentioned that the compound of the hydrotalcite type corresponds to the following chemical formula: Mgl_ is _,-* _ 〇, where χ is between Between 〇 (excluding 〇) and 〇5, An- represents an anion, especially such as carbonate, η is from, and m is a positive number. Various substantially amorphous compounds can be used, which have the formulas 〆ΑΙΑ, ( c2) x, (H2〇) z, where x, y, and z meet the following inequality: 〇 < M 0.7 '〇 < ym, and z 2 3. These compounds are described in particular in the patent application EP 209 864. In addition, the compounds of the formula of Ca3Al2 (〇H) ac ^ A12 (Si〇) 4 (〇H) u with equal percentage * cat〇ltes are suitable as inorganic compounds. Hydrochloric acid sensing compounds. For example, in Shi Ximing acid salt, for example, the metal chelate acid salt is a crystal, synthetic, and has a mesophase between 13 and 25% of water within 3 miles, It has a composition of 0.7_1M2.Al2O3_1.3-2.4Si02, where M represents an alkali metal, especially such as sodium. Particularly suitable is a spar of type NaA, such as described in patent US 4,590,233. 3 [a] In the case of soil metal hydroxides (eg, hydrazine hydroxide) or in the case where the tritium composition contains an acid sensor as an additive, its total content is 2.5 to 50 by weight %, Preferably the amount is 5 to 25% by weight compared to the test soil 87201 -15-200416248. The composition of the present invention may include at least one additive compound, which is selected from the group consisting of Compounds of metals selected from columns IIA, IIB, IVB of the Periodic Table of the Elements (see Bulletin de ia Soci0t6 Chimique de France, no. 1, Jan. 1966 supplement), or contain an additive selected from the uracil type Compound. The additive compound can be a compound [A]. The additive compound may and may be a compound different from compound [a] included in the composition. For these metal-containing compounds, the metal is more specifically selected from calcium Barium, Magnesium, Iron, Zinc, Tin, or Lead. As required by the king, a combination of many of these stabilizer compounds can be expected, such as, for example, 'a mixture of calcium and zinc-based stabilizer compounds.添加剂 For additives containing at least one of the elements of columns IIB and IIA, particularly examples include metal salts (soaps) of organic acids, such as aliphatic, aromatic carboxylic acids, or fatty acids, or phenates or aromatic alcoholates . Most users are, for example, maleic acid, acetic acid, diacetic acid, propionic acid, acetic acid, ethyl-2-hexanoic acid, capric acid, undecanoic acid, lauric acid, myristic palmitic acid, hard Yue Yue acid, oleic acid, manganic acid, rosic acid (docosa carbonic acid), fluorenyl stearic acid, hydroxyundecanoic acid, benzoic acid, phenylacetic acid p-second butyl benzoic acid, and Salts of element IIA or IIB of salicylic acid, alcohol derivatives of phenol-1 or phenols substituted with one or more alkyl groups (eg, nonylphenol). The additives are selected from the group consisting of propionates, oleates, laurates, ketomalates, docosamates, and butyl parabens of alkaline earth metals. Acid salt, salicylate, maleate, 87201 -16- 200416248 mono-ethyl-2-hexanoate, nonylphenolate, naphthenate. As for the contained compounds, particular examples are those described in ENCYCLOPEDIA of PVC, Leonard I. NASS (1976) p. 299-303. These compounds are very different compounds. The most common users are the second generation lead carbonate, the third generation lead sulfate, the fourth generation lead sulfate, the second generation lead phosphite, lead orthosilicate, basic lead silicate, lead silicate. And co-precipitate of lead sulfate, basic gas lead silicate, co-precipitate of silicon rubber and lead orthosilicate, second generation lead phthalate, neutral lead stearate, second generation lead stearate, fourth generation Lead fumarate, lead maleate II, lead ethyl-2-hexanoate, lead laurate. For tin-based compounds, reference may be made in particular to the work "Plastics Additives Handbook", Gachter / Muller (1985) p. 204-210 or " Encyclopedia of PVCf, 5 Leonard I. Nass (1976) p. 313 -325 ^ These compounds are in particular the acid salts of mono- or di-carbamic tin and the sulphur salts of mono- or di-carbamic tin. Among these compounds, the most common users are di-n-methyltin, di -Derivatives of n-butyltin, or di-n-octyltin, such as, for example, dibutyltin dilaurate, dibutyltin maleate, dibutyltin maleate, di (mono-CVCV alkane) Maleic acid) dibutyltin, dibutyltin bis (lauryl-thiolate), S-Sf (isooctylmercaptoacetic acid) dibutyltin, mesyl-butylpropionate dibutyltin, maleate di-n- Octyltin polymer, bis-ss iso-octylmercaptoacetate) di-n-octyltin, iS-mercaptopropionate di-n-octyltin. Mono-derivatives of the above compounds are also available The additive selected from uracil is more specifically 6-amino-urine or 6-amino-thiouracil type derivative, which is in position 1 and 3 have substituents 87201 -17- 200416248. These substituents at positions 1 and 3 are more specifically crCi2 alkyl,
CrQ晞基' crCs環燒基、CrC9垸笨基；該等基團或可經— 至二個CrC4燒基或燒氧基、CrCs環燒基、經基、或氯原子 取代。此類型添加劑之使用特別已述於Ep 1 〇46 668、us 4 656 209 中。 如其存在於本發明之組合物中，添加劑化合物之總含量 係介於相較化合物[a]之重量以重量計之01及100%間，較佳 者係介於相較相同參數以重量計之1及50%間。 根據本發明之另一變化，該组合包含至少 :，其係選自壤；-元醇；多元醇；包含-或多個環Γ官 月匕基〈化合物；飽和或不飽和脂膀酸以及其酿；異氛尿酸 酿；聚矽氧烷油或樹脂或石夕烷；單獨或混合物形式。 在可用〈|中，特別可提及者包括褐煤酸g旨壤、聚乙辦 蠟或其氧化衍生物、以及石蠟。 m 尤7C醇^，其稷佳係脂族醇、飽和或 12至30個碳原子。舉例而言，可提及者包含，h限;:口 二桂肉…、硬脂醇、異硬脂醇、_醇、二十二 / 油知、油醇、瓢兒菜醇 物形式。 t 早獨或混合 …多元醇較佳可包含2至32個碳原子、具有 .. 等羥基官能基可由諸等 ^ 固羚基；該 ^寺原子攜帶，較隹去# 連位或非連位。 “邊寺碳原子， 在此等化合物中，可摇 _ Μ 及者包括諸等二醇， %、1，2-丁二酵、丁二 4如’丙二 _ 知' 己二醇、十二烷二 -18 > 200416248 醇、新戊二醇，諸等多元 四醇、二季戊四醇、4如’三μ基丙燒、季戊 梨糖醇、甘油、具有二二、木糖醇、甘露糖醇、山 土 1〇之聚合度 寡口人 物、錢硬脂醇、惹麻醇。 义甘由暴木物此口 其他亦為適用之多亓 分乙龜基化）構成。 &係由聚乙料（其或可經部 物ΐ有:Γ多個環氧官能基之化合物較佳係選自環氧化植 物油，諸如，環氧士 a、丄 ^ ?、 大…由、每氧萬麻油、環氧亞麻子油、 衣乳…油、以及裱氧脂肪酸酯。 在脂肪酸中（其重縣令+、 、 3又係包含12至30個碳原子、飽和 或不飽和、直鏈或支鏈、 ^ 漣且或可包含一或多個羥基之羧 酸），可提及者，例如，颍π 硬月曰、異硬脂酸、月桂酸、肉 豆蔻酸、棕櫚酸、油醢、盐妒, ， 由I 維鉍（二十二碳烷酸）、亞麻油 酸、次亞麻油酸、蓖麻醇酸、#i基硬脂酸、或任何其他來 自甘油酯或三甘油酯、天然或非天然性、適用於本發明之 酸。該等酸可以單獨或混合物形式使用。 就前述諸等酸之酯而言，特別適用者包括取自含工至· 碳原子之醇之酯，或是取自多元醇之一元或多元酯，諸 如，舉例而言，甘油、伸烷二醇（如，丙二醇）之衍生物。 亦可使用異氰尿酸酯，特別係具有一或多個羥基者，諸 如’舉例而言，三（2-羥乙基）異氰尿酸酯。 在聚矽氧烷油或樹脂中，可提及者包括，例如，聚二燒 基矽氧烷油或聚氫烷基矽氧烷油，其中該烷基包含丨至3個 碳原子，且較佳係對應甲基。 87201 -19- 200416248 此等油係對應於下列之通式·· Υα[(κ)^κ>〇]Χ_γ，其中民 係相同或不同，代表包含個碳原子之烷基（且較佳係甲 基）或氫原子(惟該兩基團中僅有其一係氫原子），Y代表气 原子或（R，)3Si，其中R，係相同或不同，代表包含1至3個碳2 亍之烷基（較佳係甲基）。係數x係廣泛不同者，但更特定士 之’其係介於5及300之間。 耶通用者包括聚甲矽氧烷官能化油，諸如，舉例而言， T -¾基丙稀油。 斤取後，就聚矽氧烷樹脂而言，特別係使用由聚氳烷基矽 氧浼油在鉑基礎性催化劑之存在下對帶有乙烯基之聚矽氧 燒油作用所取得之樹脂。 亦可使用由至少一種式（R〇)3SiF或（RO)2(Me)SiF之矽烷之水 解或自動縮合作用所取得之聚矽氧烷樹脂，其中R係相同 或不同’代表包含！至4個碳原子之烷基，F更特定言之代 表下列之基團，· _CH=CH2、<CH2)3〇H、-((：秘_腿2 …(CH2)r nhch2ch2nh2 > kch2)3o-c〇.ch-ch2 > -(CH2)3OCH2CHCH2 ^ \ / o -(CH2)3〇-CO-(CH3)CH=CH2。 亦可使用前述之矽烷。 田本發明之組合物包含一或多種選自前述者之添加劑 時’其總含量係介於相較化合物[a]之重量以重量計之01及 100/〇間’較佳者係介於相較相同參數以重量計之1及50% 間。 戈/、存在於本發明之組合物中，共添加劑之總含量係介 87201 -20- 200416248 於相較化合物|；a]之重量以重.量計之0.1及100%間，較佳者係 介於相較相同參數以重量計之1及50%間。 本發明之組合物較佳係含有一添加劑化合物及一共添加 劑。 本發明之組合物係以分割固體之形式存在，其平均大小 係大於或等於2 μπι，更特定言之係大於或等於1〇 μιη，較佳 係大於或等於100 μιη。此外，該平均大小係小於或等於2〇 mm，更特足5之係小於或等於，較佳係小於或等於1CrQ fluorenyl 'crCs cycloalkyl, CrC9 fluorenyl; these groups may be substituted by two to CrC4 alkyl or alkoxy, CrCs cycloalkyl, via radical, or chlorine atom. The use of this type of additives has been described in particular in Ep 1046 668, us 4 656 209. If it is present in the composition of the present invention, the total content of the additive compound is between 01 and 100% by weight compared to the weight of the compound [a], and the better is between the same parameters by weight. Between 1 and 50%. According to another variation of the invention, the combination comprises at least: selected from the group consisting of:-alcohols; polyhydric alcohols;-containing one or more cyclic guanyl group compounds; saturated or unsaturated fatty acids and their Brewing; isouric acid brewing; polysiloxane oil or resin or petrolatum; alone or as a mixture. Among the available <|, particular mention may be made of montanic acid, polyethylene wax or its oxidized derivative, and paraffin. m especially 7C alcohol ^, which is preferably an aliphatic alcohol, saturated or 12 to 30 carbon atoms. By way of example, mention may be made of, h-limit ;: mouthfuls of cinnamon ..., stearyl alcohol, isostearyl alcohol, alcohol, twenty-two / oil know, oleyl alcohol, scabella alcohol form. t Early alone or mixed ... Polyols may preferably contain 2 to 32 carbon atoms, have ... functional groups such as hydroxyl groups can be ^ solid group; the ^ temple atom is carried, compared with #linked or non-linked . "Bian Si carbon atom. Among these compounds, Kom _ M and diols include various diols,%, 1,2-butanediol, butane 4 such as 'propylene di-k', hexanediol, twelve Alkandi-18 > 200416248 Alcohol, neopentyl glycol, various polytetraols, dipentaerythritol, 4 such as' triμpropylpropane, pentaerythritol, glycerol, dioxane, xylitol, mannose The degree of polymerization of alcohol, mountain soil 10, oligomeric characters, money stearyl alcohol, and ramesterol. Yigan is composed of violaceous wood and other suitable multi-component acetylated turtles.) &Amp; B material (which may include: Γ multiple epoxy functional compounds are preferably selected from epoxidized vegetable oils, such as epoxy a, 丄 ^?, Large ... by, per sesame oil, Epoxy linseed oil, dressing oil ... oil, and mounting oxygen fatty acid esters. Among the fatty acids (the heavy county order +,, 3, which contains 12 to 30 carbon atoms, saturated or unsaturated, straight or branched chain) , ^ And carboxylic acids that may or may contain one or more hydroxyl groups) can be mentioned, for example, 颍 π stearic acid, isostearic acid, lauric acid, myristic acid, palmitic acid, Oil tincture, salt jealousy, made of 1-dimensional bismuth (docosacoic acid), linoleic acid, hypolinolenic acid, ricinoleic acid, # i-based stearic acid, or any other derived from glycerides or triglycerides Ester, natural or non-natural, acids suitable for use in the present invention. These acids can be used alone or in mixtures. As for the esters of the aforementioned acids, particularly suitable include those derived from alcohols containing carbon atoms to carbon atoms. Esters, or mono- or polyhydric esters derived from polyols, such as, for example, derivatives of glycerol, butanediol (e.g., propylene glycol). Isocyanurates can also be used, especially having one or more Individual hydroxyl groups, such as, for example, tris (2-hydroxyethyl) isocyanurate. Among polysiloxane oils or resins, mention may be made of, for example, polydithiosiloxane oils. Or polyhydroalkylsiloxane oil, in which the alkyl group contains 3 to 3 carbon atoms, and preferably corresponds to a methyl group. 87201 -19- 200416248 These oils correspond to the following general formula ... κ) ^ κ > 〇] χ_γ, in which the same or different civil groups represent alkyl groups containing carbon atoms (and preferably methyl groups) Or a hydrogen atom (only one of the two groups is a hydrogen atom), Y represents a gas atom or (R,) 3Si, where R, is the same or different, represents an alkyl group containing 1 to 3 carbon atoms (Preferably methyl). The coefficient x is widely different, but more specifically it's between 5 and 300. Ye general includes polysiloxane functional oils such as, for example, T-¾-based propylene oil. For polysiloxane resins, polysiloxane based on polysiloxanes is used in the presence of platinum-based catalysts for polysiloxane resins. Resin obtained by oil burning. It is also possible to use a polysiloxane resin obtained by hydrolysis or automatic condensation of at least one silane of formula (R0) 3SiF or (RO) 2 (Me) SiF, where R is the same Or different 'stands for include! An alkyl group of 4 carbon atoms, F more specifically represents the following groups, _CH = CH2, < CH2) 3〇H,-((:: _ leg 2 ...... (CH2) r nhch2ch2nh2 > kch2 ) 3o-co.ch-ch2 >-(CH2) 3OCH2CHCH2 ^ \ / o-(CH2) 3〇-CO- (CH3) CH = CH2. The aforementioned silane can also be used. The composition of the present invention contains One or more additives selected from the foregoing, whose total content is between 01 and 100/0 by weight compared to the weight of the compound [a] is more preferably between the same parameters by weight Between 1 and 50%. Ge /, Existing in the composition of the present invention, the total content of co-additives is between 87201 -20- 200416248 compared to the compound |; a] 0.1 and 100% by weight. Preferably, it is between 1 and 50% by weight compared to the same parameter. The composition of the present invention preferably contains an additive compound and a co-additive. The composition of the present invention exists in the form of divided solids , Its average size is greater than or equal to 2 μm, more specifically is greater than or equal to 10 μm, preferably greater than or equal to 100 μm. In addition, the average size is less than Or equal to 20 mm, more specific is less than or equal to 5, preferably less than or equal to 1
根據該顆粒之大，According to the size of the particles,
使化合物[b]接觸化合物[a]而進行製 溫 備。 化合物[b]係在進行接觸之前預先呈 根據第一實施方式， 熔融形式。 〜方式可為在攪拌下使其在化合物[a] 在此情形下，較佳士 之上進行霧化。 舉例而言，該操 進行。 該操作可在旋轉滾筒中 以流化床、輸送床 根據第二實施方式， 狀形式之化合物[b]進行 其可使化合物[a]與呈固體及/或糊 混合0 接著，在攪拌下， 或係藉由攪拌本身戶 升同溫度以造成化合物[b]之熔融，其 87201 斤^成之加熱’或是藉由外在之溫度升 -21 - 200416248 南而進行。 此徑徕作較佳可在快速攪袢器 當然，咸可以使化合物[b]/化合物[a]之重量比為大於二、 等於1/100之諸等比例添加化合物[a]及[b]，更特定今+ 3 係大 於或等於1/50，較佳係大於或等於1/2〇。此外，今舌曰， 吸里！比較 佳係小於或等於1/2，更特定言之係小於或等於1/3，較佳係 小於或等於1/4。 ， 進行該混合操作之溫度係取決於化合物[b]之性暂。、㈤ 八 孩溫 度係大於或等於化合物w之熔點溫度，且較佳係約為該溫 度。 A酿 在酸傳感物、添加劑化合物、及/或共添加劑存在時， 諸如前文所述，其可根據多種可能性而進行添加。 第一種可能性係使化合物[a]與無機性質之添加劑進行混 合，接著再使其整體與化合物[b]及有機性質之添加劑進行 接觸，根據前述之第一或第二變化進行。此種方法就其中 該等有機添加劑（如其存在）係液態且具有可與化合物问相 容之熔點溫度之情形而言可係較佳者。就相容而言，其更 特疋T s係指Μ等有機性質之添加劑具有近似於化合物[b] <熔點溫度，或者，其所具有之熔點溫度係化合物问並不 會分解或產生化學轉化之溫度，又或者，其在化合物[b]呈 熔融狀態之溫度下並不會分解或產生化學轉化。 另一種可能性則係在使化合物[a]及[b]進行接觸之前，或 是在進行該接觸之後，加入該等添加劑。 明確言之，不論茲等添加劑為何，其皆可同時或順序進 87201 200416248 行添加。 為以至少一種鹵 以至少一種氯代 氣乙烯*為基礎者） 本發明之另一標的係由該前述組合物作 代聚合物為基礎之調配物（更特定言之係 聚合物為基礎者，且較佳係以至少一種聚 之安定劑之用途而構成。 在1 匕目的中，就以重量計100份之自代聚合物而言，本發 明組a物《含量代表以重量計之〇 5 Λ ^ h，較佳者係相較 相Η參數以重量計之1至12份。 就聚氯乙晞而言，其係指其聚人 文k ^ 係虱乙缔均聚物之諸 寺組合物。該均聚物可經，例如 】如虱化作用進行化學修 飾0 在使用本發明之組合物時，諸多氯乙缔之共聚物亦可獲 得安足。此等共聚物特別係自氯乙烯與具有可聚合性雙键 :早體間之共聚合作用所取得之聚合物，諸如，舉例而 ^ :醋酸乙缔酿、亞乙烯基氯；馬來酸、富馬酸、或其 ^，/心，諸如，乙#、丙、缔、己缔；丙缔酸醋或甲基丙 ’布鉍酯；苯乙烯；乙烯醚，諸如，乙烯基十二烷醚。 一省又而β，琢等共聚物含有至少5〇%以重量計之氯乙烯 土凡且較佳係至少80%以重量計之此等基元。 曰水氯乙烯（單獨或混合其他聚合物形式）係最常用於本發 明安疋調配物中之氯代聚合物。 《:般而言，所有類型之聚氯乙烯皆係適用者，不論其製 、、弋為何。因此，舉例而言，以固體、懸浮液、乳液形 式進仃〈作用流程取得之聚合物皆可在使用本發明之組合 S72〇l -23 200416248 物時獲得安定，且不論該聚合物之固有黏度為何。 頊）王意者，如上述之酸傳感物、添加劑化合物、及/或 :添加劑並未包含於該組合物中，其各皆可有利含於使用 3組合物之調配物中。 I根據本發明之一實施方式，該齒代聚合物係用於包含至 少一種增塑劑之調配物中。 在可用之增塑劑中，適用者包括烷基鄰苯二酸酯，諸 (乙基2 -己基）鄰苯一酸酯，C6_CS直鏈二酸酯，諸 如，己二酸酯；檸檬酸酯；苯甲酸之一元酸或多元酸酯， 2如，苯曱酸酯、偏苯三酸酯；苯酚之磷酸酯、磺酸酯； 單獨或混合物形式。 在其存在時，增塑劑之總含量係介於相較於以重量計ι〇〇 份代聚合物而言以重量計之5及200份之間。 該氣代聚合物調配物可包含至少一種添加劑，其係選自 包含選自元素週期表第ΠΑ、IIB、勵欄之金屬之化合物。 如其存在時，就1〇〇克之鹵代聚合物而言，此等化合物之 含量一般係在0.1及4克間不等，較佳係〇3及2克間之函代聚 合物。 該氯代聚合物調配物亦可包含至少_種鹽酸傳感物，諸 如前文所述者。 如酸傳感物存在於該調配物中，且較佳者係如此，就1〇〇 克之鹵代聚合物而言，此等化合物之總含量係介於⑽认川 克間，更特足言之，其係介於相較相同參數之〇 〇5及5克 間。 87201 -24- 200416248 該聚合物調配物尚可包含添加物，選自二輕基吹咬、尿 嘧啶或硫代尿嘧啶類型之化合物（特別諸如前述者）、脫氫 醋酸。更特定言之，就二羥基吡啶而言，可使用2,6-二甲 基一 #艾版1，4 -一每基峨淀類型者，其中該等式;^〇(2：〇-之羧酸基團（可為相同或不同）係使R代表烷基、直鏈或支 鏈、C1-C36 ;環狀基團，具有小於14個碳原子，且或可帶 有雙鍵及/或至少一個C1-C22烷基取代基；芳基，具有小 於14個碳原子，且或可帶有至少一個C1-C22烷基取代基。 如此等化合物存在於該調配物中，就1〇〇克之鹵代聚合物 而言’其含量一般係介於0.005及5克間不等，較隹者，其就 100克之鹵代聚合物而言係介於0.2及1.5克間不等。 該鹵代聚合物調配物亦或可包含至少一種共添加劑，其 係選自一元醇及/或多元醇，特別諸如該等在有關本發明 組合物之敘述中所提及者。 如該調配物包含此種類型之共添加劑，就100克之li代聚 合物而言，其總含量較佳係介於0.05及5克間。更特定言 之，就100克之鹵代聚合物而言，其係小於2克。 該調配物亦可包含至少一種化合物，其包含一或多個環 氧官能基。 如此種類型之化合物存在於該鹵代聚合物調配物中’就 100克之鹵代聚合物而言，其總含量較佳係介於0.5及10克之 間。 其並不排除該鹵代聚合物調配物包含至少一種化合物’ 其選自蠟；飽和或不飽和脂肪酸以及其酯；聚碎氧燒油或 87201 200416248 樹脂或矽烷；單獨或混合物形式。 如其存在，就100克之_代聚合物而言，此種類型化合物 之總含量一般係介於〇.〇5及2克間不等。 須 >王意者，各化合物（酸傳感物、添加劑、及共添加劑） 存在於画代聚合物調配物中之總含量係以此等化合物在本 發明組合物中之分別含量計算（如其存在）。 該調配物亦可包含有機亞磷酸酯類型之化合物，諸如， 舉例而言，三烷基、芳基、三芳基、二烷基芳基 '或二芳 基烷基亞磷酸酯，其中辭彙烷基係指一元醇或多元醇 之te基，而辭彙芳基係指苯酚或經烷基取代苯酚之芳 狹基團。亦可使用亞磷酸鈣，諸如，類型之 化合物，以及亞磷酸-羥基-鋁_鈣複合物。 在其使用時，就100克之鹵代聚合物而言，此種類型添加 物之含量一般係介於0.1及7克間。 该鹵代聚合物基礎性調配物亦可包含一或多種填料。此 等化合物一般係選自滑石、碳酸鈣、高嶺土、石灰，單獨 或混合物形式。 如該碉配物具有一或多種填料，根據該聚合物之終應用 方式以及所用之塑形方法，就100克之鹵代聚合物而言，其 總含量一般係2至150克。更特定言之，在目標為取得型材 之調配物中，舉例來說，就1〇〇克之鹵代聚合物而言，該填 料之含量係介於2及8克間。在目標為纜線類型應用之調配 物之中，舉例來說，就100克之自代聚合物而言，該填料之 含量更特定言之係介於30及150克間。 87201 -26- 200416248 根據目標應用之不同’可在該調配物中補入 添加物。 九足 因此，該調配物可包含絲抗氧化劑、抗糊，諸如， 2-羥基二苯甲酮、2_羥基苯并三唑、或是經位阻化之胺， 其一般稱為Hals。 當其存在時’就⑽克之函代聚合物而言，此種類型添加 物之含量一般係介於0·05及3克間不等。 此外，該等調配物亦可包含有色或白色之色素，特別諸 如，硫化錦、二氧化获娃丨# 口 虱化鈦特別係王金紅石形式者，且輕 已經表面處理。 須压思者，引入該調配物中之色素量具有廣泛之差異缴 化’且其特別係取決 彩。同時，舉例而 者巴说力以及所欲之終色 +例而Τ，且如該聚合物組合物包含豆 100克之鹵代聚人札γ^ 就 、 气氷。物而j，色素之量可自0.1至20克不等，並 相較相同參數較佳係自G.5至15克。 ’、 Λ月、、且合物之鹵代聚合物調配物特 硬型材、管、4 义衣備 寸出接頭、硬膜、軟膜、纜線、塗層。 包含本發明如人仏、 曰 '' 〈自代聚合物碉配物可以任何熟習技 ，云者所知 <方法進行塑形。 因此，亦可分 或在預先製備多種此等組成份之混合物 之组成^自代來合物中納入本發明之組合物以及各種不同 傳統之納人女^ 物。 万法極適合用於取得i代聚合物基礎性調配 87201 -27- 200416248 因此，且僅就舉例而言，可在配備高速作用之槳葉及逆 槳葉系統之混合器中進行此種操作。 一般而言，該混合操作係在低於130°C之溫度下進行。 一但完成混合之後，即可根據該領域之習慣方法，進行 該組合物之塑形，諸如，射出、擠出吹塑、擠塑、軋光、 或旋轉模塑、塗布。 進行塑形之溫度一般係自150至22CTC不等。 現將提供可具體說明但不限制本發明之實例。 實例 1 /本發明組合物 a)粗產物.之製備 在配備冷凝器、攪拌裝置、可連結真空或氮氣源之2000 cm3反應器中，加入260毫升之曱苯，接著在氮氣下，加 入78克之NaNH2。 接著將該介質之溫度升高至40°C，並在整個反應及結束 之過程中維持在該溫度下。 將該裝置整體置於7 1〇4 Pa之壓力下。 傾倒加入310克之工業硬脂酸甲酯（含10%之棕櫚酸甲 酷）°接著，以3小時之時間，加入120克之乙感苯° 攪拌該反應介質45分鐘(溫度40°C，在7 104Pa之壓力下）。 接著將該熱反應混合物引入稀釋至10%之硫酸溶液中， 其添加使該水層在傾析後之pH值為1.5。 在清洗兩次後，使該溶液通過一持續冷卻之旋轉滾筒而 蒸發甲苯，以產生呈片狀物形式之粗產物。 87201 -28- 200416248 如此取得之粗產物，其在°C下呈固體，含78%之/3 -二酮 (CPG層析分析）。 b)本發明組合物之製備 自下述之方法取得該組合物： 在8(TC下加熱先前取得之粗產物，接著在一快速攪拌器 中，於攪拌下，將其加入氫氧化#5顆粒中。 其比例如下：粗產物/氫氧化鈣：1/17。 取得呈乾燥狀態之粉末。 2/ _代聚合物調配物 無安定劑系統之起始調配物包含： * 1⑻份之 PVC(K-Wert70，Solvm271PC，由 Solvay 出售）， * 90份之填料（碳酸鈣EXH1)， * 60份之增塑劑（含0.5%雙酚A之安定性二異癸基鄰苯二 酸酯）。 在一 Papenmeier類型之攪拌器中，於60°C下，以2400 t/min之 速度混合此等組成份。 安定劑系統： *硬脂酸鋅： 0.3份 *本發明組合物： 5.3份 將該安定劑系統納入該混合物中，其中該組合物係由上 所產生。 在一軋光機上，於180°C下，在5分鐘内，不研磨而轉化 該調配物之整體。 如此取得厚度約等於3 mm之薄片。 87201 -29- 200416248 含有該安定劑系統之調配物之長期安定性係80分鐘。其 對應於該試樣出現分解情形（變黑）之溫度，不確定ΔΤ = 1 分鐘。測量係根據EN60811標準進行，以pH試紙修正。 87201Compound [b] is prepared by contacting compound [a]. The compound [b] is in a molten form according to the first embodiment before being brought into contact. ~ The method may be that it is atomized on the compound [a] in this case, preferably by stirring. This operation is performed, for example. This operation can be carried out in a rotating drum in a fluidized bed, a conveying bed according to the second embodiment, in the form of the compound [b] which can mix the compound [a] with a solid and / or paste. Then, under stirring, Or it can be caused by melting the compound [b] by stirring at the same temperature and heating it at 87201 kg ', or by raising the external temperature to -21-200416248. This path is best used in a fast stirrer. Of course, salty can add compounds [a] and [b] in equal proportions of compound [b] / compound [a] to greater than two and equal to 1/100. More specifically, +3 is greater than or equal to 1/50, and preferably greater than or equal to 1/20. In addition, this tongue said, suck! More preferably, it is less than or equal to 1/2, more specifically, it is less than or equal to 1/3, and more preferably, it is less than or equal to 1/4. The temperature at which this mixing operation is performed depends on the nature of compound [b]. The temperature is equal to or greater than the melting point of compound w, and is preferably about that temperature. In the presence of an acid sensor, an additive compound, and / or a co-additive, such as described above, it can be added according to a variety of possibilities. The first possibility is to mix the compound [a] with an additive of an inorganic nature, and then contact the whole with the compound [b] and an additive of an organic nature, according to the aforementioned first or second variation. This method may be preferred where the organic additives, if present, are liquid and have a melting point temperature compatible with the compound. As far as compatibility is concerned, its more specific: T s means that organic additives such as M have an approximate temperature of the compound [b] < melting point, or that the melting point temperature of the additive does not decompose or produce chemistry. The temperature of the conversion, or the temperature at which the compound [b] is in a molten state does not decompose or cause chemical conversion. Another possibility is to add the additives before or after the compounds [a] and [b] are brought into contact. To be clear, regardless of the additives, they can be added simultaneously or sequentially in line 87201 200416248. Based on at least one halogen based on at least one chlorinated ethylene * Another object of the present invention is a formulation based on the aforementioned composition as a polymer substitution (more specifically, a polymer based formulation, And it is preferably constituted by the use of at least one poly-stabilizing agent. In 1 dagger, in the case of 100 parts by weight of the self-generation polymer, the content "a" of the group "a" in the present invention represents 0.55 by weight Λ ^ h, the better is 1 to 12 parts by weight compared to the relative parameters. For polyvinyl chloride, it refers to the various temple compositions whose poly-human k ^ is a homologous polymer of lice. The homopolymer can be chemically modified, for example, by liceification. When using the composition of the present invention, a number of vinyl chloride copolymers can also be sedated. These copolymers are particularly derived from vinyl chloride and Polymerizable double bond: polymer obtained by copolymerization between early bodies, such as, for example, ^: ethyl acetate, vinylidene chloride; maleic acid, fumaric acid, or its , Such as, B #, C, D, D, D; Acrylic acid or methyl propionate bismuth ester; Phenyl ethyl Vinyl ethers, such as vinyl dodecane ether. A provincial and beta copolymer contains at least 50% by weight of vinyl chloride, and preferably at least 80% by weight of these groups. Hydrochloride (individually or in combination with other polymer forms) is the chlorinated polymer most commonly used in the formulations of the present invention. ": In general, all types of polyvinyl chloride are suitable, regardless of What is its composition, and so on? Therefore, for example, polymers obtained in the form of solids, suspensions, and emulsions can be stabilized when using the composition of the present invention S72001-23200416248, and Regardless of the inherent viscosity of the polymer. 顼) Wang Yi, as described above, the acid sensor, the additive compound, and / or: the additives are not included in the composition, and each of them can be advantageously used in the 3 combination. In the formulation of things. I According to one embodiment of the present invention, the dental polymer is used in a formulation comprising at least one plasticizer. Among the usable plasticizers, those suitable include alkyl phthalates, (ethyl 2-hexyl) phthalates, C6_CS linear diesters, such as adipic acid esters, and citrates. ; Monocarboxylic acid or polybasic acid ester of benzoic acid, 2 For example, benzoic acid ester, trimellitic acid ester; Phosphate ester, sulfonic acid ester; Individual or mixture form. When present, the total plasticizer content is between 5 and 200 parts by weight compared to 500,000 parts by weight of the substituted polymer. The gas-substituted polymer formulation may include at least one additive selected from a compound comprising a metal selected from the group consisting of Periodic Table of Elements IIA, IIB, and Bar. When present, the content of these compounds in the case of 100 grams of halogenated polymer generally ranges between 0.1 and 4 grams, and is preferably a functional polymer between 0 and 2 grams. The chlorinated polymer formulation may also include at least one hydrochloric acid sensor, as described above. If an acid-sensing substance is present in the formulation, and is preferably the case, the total content of these compounds is between 100 grams of halogenated polymer, and more specifically, In other words, it is between 0.05 and 5 grams with the same parameters. 87201 -24- 200416248 The polymer formulation may further comprise additives selected from the group consisting of dilight-based bites, uracil or thiouracil types (especially such as the foregoing), dehydroacetic acid. More specifically, in the case of dihydroxypyridine, 2,6-dimethyl- # AI version 1,4-one-based Edian type can be used, where the equation; ^ 〇 (2: 0- 之The carboxylic acid group (which may be the same or different) is such that R represents an alkyl group, a straight or branched chain, C1-C36; a cyclic group having less than 14 carbon atoms, and may have a double bond and / or At least one C1-C22 alkyl substituent; an aryl group having less than 14 carbon atoms, and may or may carry at least one C1-C22 alkyl substituent. Such compounds are present in the formulation for 100 grams. As far as halogenated polymers are concerned, their content generally ranges between 0.005 and 5 grams, and in the case of 100 grams of halogenated polymers, it ranges between 0.2 and 1.5 grams. The formulation may also include at least one co-additive, which is selected from monohydric and / or polyhydric alcohols, in particular such as those mentioned in the description of the composition of the invention. If the formulation comprises this type As for the co-additive, the total content of 100 g of the li-generation polymer is preferably between 0.05 and 5 g. More specifically, 100 g of halogen For polymers, it is less than 2 grams. The formulation may also contain at least one compound, which contains one or more epoxy functional groups. Such compounds are present in the halogenated polymer formulation 'as 100 For halogenated polymers, the total content is preferably between 0.5 and 10 grams. It does not exclude that the halogenated polymer formulation contains at least one compound 'selected from waxes; saturated or unsaturated fatty acids and its Ester; polyoxygenated oil or 87201 200416248 resin or silane; alone or in mixture. If it exists, the total content of this type of compound is generally between 0.05 and 2 grams for 100 grams of polymer. Requirement > Wang Yizhi, the total content of each compound (acid sensor, additive, and co-additive) in the graphic polymer formulation is the difference between these compounds in the composition of the present invention Content calculation (if present) The formulation may also include compounds of the organic phosphite type, such as, for example, trialkyl, aryl, triaryl, dialkylaryl 'or diarylalkylene Acid esters, where the term alkyl refers to the te group of a monohydric or polyhydric alcohol, and the term aryl refers to phenol or an aromatic narrow group of phenol substituted with an alkyl group. Calcium phosphite can also be used, such as, Compounds, and phosphorous acid-hydroxy-aluminum-calcium complexes. When used, the content of this type of additive is generally between 0.1 and 7 grams for 100 grams of halogenated polymer. The halogenated polymerization The basic formulation may also contain one or more fillers. These compounds are generally selected from talc, calcium carbonate, kaolin, lime, alone or in a mixture. If the compound has one or more fillers, according to the polymer For the final application method and the shaping method used, the total content of 100 grams of halogenated polymer is generally 2 to 150 grams. More specifically, in a formulation whose goal is to obtain profiles, for example, for 100 grams of halogenated polymer, the filler content is between 2 and 8 grams. Among formulations targeted for cable-type applications, for example, for 100 grams of self-generating polymers, the filler content is more specifically between 30 and 150 grams. 87201 -26- 200416248 Depending on the target application, it can be supplemented with additives. Ninefoot The formulation may therefore include silk antioxidants, anti-pastes, such as 2-hydroxybenzophenone, 2-hydroxybenzotriazole, or a sterically hindered amine, which is commonly referred to as Hals. When it exists', in the case of gram grams of functional polymers, the content of this type of additive generally ranges between 0.05 and 3 grams. In addition, these formulations can also contain colored or white pigments, such as sulfide bromide and dioxide to obtain baby 丨 # mouth lice titanium is particularly in the form of king rutile, and has been lightly surface treated. For those who need to think about it, the amount of pigments introduced into the formulation has a wide range of variations' and it depends in particular on the prize. At the same time, for example, let's say the power and the desired final color + example and T, and if the polymer composition contains 100 grams of beans, halogenated poly azalea ^^, air ice. The amount of pigment and j can range from 0.1 to 20 grams, and is preferably from G. 5 to 15 grams compared to the same parameters. ′, Λ month, and the halogenated polymer formulation of the compound is a special hard profile, tube, 4 ready-made connector, hard film, soft film, cable, coating. Compounds containing the present invention, such as human, can be shaped by any method known to those skilled in the art. Therefore, the composition of the present invention, as well as a variety of different traditions, can also be incorporated into the composition of a mixture of a plurality of these components, or prepared in advance. Wanfa is very suitable for obtaining the basic blend of the i-generation polymer 87201 -27- 200416248 Therefore, and by way of example only, this operation can be performed in mixers equipped with high-speed blades and reverse blade systems. Generally, the mixing operation is performed at a temperature below 130 ° C. Once the mixing is completed, the composition can be shaped according to customary methods in the field, such as injection, extrusion blow molding, extrusion, calendering, or rotary molding, coating. The shaping temperature generally ranges from 150 to 22CTC. Examples will now be provided that can specifically illustrate but not limit the invention. Example 1 / Composition of the present invention a) Crude product. Preparation In a 2000 cm3 reactor equipped with a condenser, a stirring device, which can be connected to a vacuum or nitrogen source, 260 ml of toluene was added, followed by 78 g of nitrogen under nitrogen. NaNH2. The temperature of the medium was then raised to 40 ° C and maintained at that temperature throughout the reaction and termination. The entire device was placed under a pressure of 7104 Pa. Pour and add 310 grams of industrial methyl stearate (containing 10% methyl palmitate) ° Then, over a period of 3 hours, add 120 grams of ethyl benzene ° Stir the reaction medium for 45 minutes (temperature 40 ° C, at 7 Under the pressure of 104Pa). The hot reaction mixture was then introduced into a 10% sulfuric acid solution, which was added so that the pH of the aqueous layer after decantation was 1.5. After washing twice, the solution was passed through a continuously cooled rotating drum to evaporate the toluene to produce a crude product in the form of flakes. 87201 -28- 200416248 The crude product thus obtained was solid at ° C and contained 78% of 3-dione (CPG chromatography analysis). b) Preparation of the composition of the present invention. The composition was obtained from the following method: The previously obtained crude product was heated at 8 ° C., and then added to a rapid stirrer under stirring to add # 5 particles of hydroxide. The ratio is as follows: crude product / calcium hydroxide: 1/17. The powder is obtained in a dry state. 2 / _ generation polymer formulations The initial formulation of the stabilizer-free system contains: * 1 part of PVC (K -Wert70, Solvm271PC, sold by Solvay), * 90 parts of filler (calcium carbonate EXH1), * 60 parts of plasticizer (stable diisodecyl phthalate containing 0.5% bisphenol A). In a Papenmeier type mixer, these components are mixed at a speed of 2400 t / min at 60 ° C. Stabilizer system: * zinc stearate: 0.3 parts * composition of the present invention: 5.3 parts of the stabilizer The agent system is incorporated into the mixture, wherein the composition is produced from above. On a calender, at 180 ° C, within 5 minutes, the whole of the formulation is transformed without grinding. The thickness obtained in this way is approximately equal to 3 mm thin sheet. 87201 -29- 200416248 formulation containing the stabilizer system Long-term stability train 80 min., Which corresponds to the case of the sample appears decomposition (dark) of temperature uncertainty ΔΤ = 1 min. Measurement system according to EN60811 standard correction to pH paper. 87201