TW564253B - Hard polyurethane open-pore foamed body composition and manufacturing method thereof - Google Patents
Hard polyurethane open-pore foamed body composition and manufacturing method thereof Download PDFInfo
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564253564253
^Jl_89i〇5188 五、發明說明(1) 發明背景 發泡體是採 熱傳導及對 ’並且以閉 媒會破壞大 題未解決。 冷固化硬質 其發泡體具 申請人申請 内含此冷固 被製備用作 方式被併入 從曰本武田 TS-470 之 遍尋文獻並 加上該公司 明人遂決定 ,完成了一 及製備方 真空隔熱材 傳統作為隔熱材料的硬·質聚胺基甲酸乙酯 用發泡劑(冷媒)來形成泡體結構,為減少氣體 流熱傳導’必需尋找熱傳導率要小的適當冷媒 孔結構減少氣體對流熱傳導。然近來發現舊冷 氣中的臭氧層,而新冷媒又尚有很多複雜性問 因此目前已漸採用完全不含冷媒而以水發泡的 聚胺基甲酸乙酯發泡體應用在真空保温材上, 有細小泡孔及很好開孔性,絕熱效果良好。於 獲准之我國新型第1〇8173號新型專利中,一種 化硬質聚胺基曱酸乙酯發泡體的高阻氣性袋體 為一真空隔熱片,該專利内容在此以引用參考 本案。該冷固化硬質聚胺基甲酸乙酯發泡體係 公司購得’代號ACTOOL VW-75及代號ΤΑΚΕΝΑΤΕ 發泡液’經乳化後發泡成型而製得。然發明人 無該公司之上述商品的製造工藝被公開揭示, 刻意保護上述商品的製造工藝的秘密,本案發 自行開發此項技術,經潛心研究及多次實驗後 冷固化硬質聚胺基曱酸乙酯開孔發泡體的配方 法,其具有細小泡孔及良好開孔性,適合作為 料0 發明要旨 一依照本發明内容所完成的硬質聚胺基曱酸乙酯開孔 發泡體的組成物包含Α液及Β液,其中Α液包含··^ Jl_89i〇5188 V. Description of the invention (1) Background of the invention The foam is heat conduction and heat treatment, and the problem that the closed medium will destroy is unsolved. The cold-curing rigid foam body has the applicant's application. This cold-set is prepared and used as a way to be incorporated into the literature from Takeda TS-470 of Japan and added to the company's decision. Square vacuum insulation material Traditionally used as a heat insulation material, rigid polyurethane uses a foaming agent (refrigerant) to form a foam structure. In order to reduce the heat flow of gas flow, it is necessary to find an appropriate refrigerant pore structure with a small thermal conductivity. Reduce gas convection heat transfer. However, recently, the ozone layer in the old cold air was found, and the new refrigerant has many complications. Therefore, polyurethane foams that are completely free of refrigerant and water-foamed have been gradually applied to vacuum insulation materials. It has fine cells and good openness, and has good thermal insulation effect. In the approved new-type patent No. 108173, a high-barrier bag made of rigid polyurethane foam is a vacuum insulation sheet, the contents of which are incorporated herein by reference. . The cold-curing rigid polyurethane foaming system was purchased by the company with the code “ACTOOL VW-75” and the code “TAKENATEE foaming solution” after being emulsified and foamed. However, the inventor did not disclose the manufacturing process of the above-mentioned products of the company, and deliberately protected the secrets of the manufacturing process of the above-mentioned products. A method for formulating an open-cell foam of ethyl acetate, which has fine cells and good open-cell properties, and is suitable as material 0. Summary of the invention-a rigid polyurethane open-cell foam prepared in accordance with the present invention The composition contains liquid A and liquid B, where liquid A contains ...
第5頁 564253 案號 89105188 五、發明說明(2) 100重量份羥官能基數為3至5和羥值為300至700 mgKOH/g的聚醚多元醇; 1至3 · 6重量份的非水解性聚矽氧界面活性劑; 0.2至3重量份的三級胺觸媒; 0.2至2.6重量份的水;及 〇· 2至2· 4重量份的碳原子數c2-C8多元醇增鏈劑;及 B液包含多異氰酸酯,其中B液與A液重量比介於0.7〜1.2。 選擇性的,本發明的A液可進一步含有〇.4至1重量%的 交聯劑,例如二乙醇胺、甘油、及三乙醇胺 (Triethanolamine) ° 合適的多異氰酸酯包括官能基為2 - 3的多異氰酸 酯,例如二伸苯基代甲烷二異氰酸酯(MD丨),伸甲苯基二 甲氰酸酯(TDI),六亞甲基二異氰酸酯,異佛爾酮二異氰 酸酯,二曱苯二異氰酸酯,三苯基代甲烷三異氰酸酯及它 們的混合物。較佳的,為以MD I為主之異氰酸酯官能基約 為2. 7的異氰酸酯混合物。 合適的C2-C8多元醇增鏈劑例如為伸丙基二醇或乙二 醇。 適用於本發明的三級胺觸媒可為聚胺基甲酸乙酯技藝 中已知之任何三級胺觸媒,較佳地為2,2 ’ -二嗎福咁二乙 基醚[2, 2’ -Dimorpholinodiethylether,(在此簡稱 DMDEE)],三伸乙基二胺[Triethylenediamine,(在此簡 稱 TEDA)],溶於二丙二醇中(dipropylene glycol)的 33% TEDA (在此簡稱TD - 33)及五曱二伸乙基三胺 [Pentamethyldiethylenetriamine,(在此簡稱 ,Page 5 564253 Case No. 89105188 V. Description of the invention (2) 100 parts by weight of a polyether polyol having 3 to 5 hydroxyl functional groups and a hydroxyl value of 300 to 700 mgKOH / g; 1 to 3.6 parts by weight of non-hydrolyzed Polysiloxane surfactant; 0.2 to 3 parts by weight of tertiary amine catalyst; 0.2 to 2.6 parts by weight of water; and 0.2 to 2.4 parts by weight of carbon atoms c2-C8 polyol chain extender And liquid B contains polyisocyanate, wherein the weight ratio of liquid B to liquid A is between 0.7 and 1.2. Optionally, the liquid A of the present invention may further contain 0.4 to 1% by weight of a cross-linking agent, such as diethanolamine, glycerol, and triethanolamine. Suitable polyisocyanates include polyfunctional groups having 2 to 3 Isocyanates such as diphenylmethane diisocyanate (MD 丨), tolyl dimethyl dicyanate (TDI), hexamethylene diisocyanate, isophorone diisocyanate, dibenzobenzenediisocyanate, triphenylbenzene Methyl triisocyanates and their mixtures. Preferably, it is an isocyanate mixture having an MD-based isocyanate functional group of about 2.7. Suitable C2-C8 polyol chain extenders are, for example, propylene glycol or ethylene glycol. The tertiary amine catalyst suitable for use in the present invention may be any tertiary amine catalyst known in the art of polyurethane, and is preferably 2,2'-dimorphofluordiethyl ether [2, 2 '-Dimorpholinodiethylether, (herein referred to as DMDEE)], Triethylenediamine (herein referred to as TEDA)], 33% TEDA dissolved in dipropylene glycol (herein referred to as TD-33) And pentamethyldiethylenetriamine, (herein referred to as,
564253 _素號89105188 年7月/〇曰 狄:t:_ 五、發明說明(3) PMDETA) ] ° 適用於本發明的聚醚多元醇係由甘油、蔗糖、己六醇 等多官能基與環氧烷(例如環氧丙烷、環氧乙烷)的聚合 物,例如購自Dow Chemical公司,代號V〇RAN〇L36〇、 VORANOL49 0之聚醚多元醇。 一適於製造本發明的硬質聚胺基曱酸乙酯開孔發泡體 的方法,包含下列步驟: a )混合1 0 0重量份羥官能基數為3至5和羥值為3 〇 〇至 7 0 0 mgKOH/g的聚醚多元醇,1至3· 6重量份的非水解性聚 矽氧界面活性劑,0 · 2至3重量份的三級胺觸媒,〇 · 2至2. 6 4 重量份的水’及0·2至2·4重量份的碳原子數C2-C8多元醇 增鏈劑而製得一 Α液; b) 預熱步驟a)的A液令其保持在25-45 °C的溫度; c) 另預熱多異氰酸醋的B液令其保持在25- 45 °C的溫 度; d) 將預熱後之a液及B液以B液與A液重量比介於0.7〜 1 · 2之比例迅速加予混合,並隨即將所獲得的混合物注入 於一溫度為35-5 5 t且溫度高於該A液及B液的混合物之模 具内同時進行固化及發泡;及 、 e) 從該模具内移出一聚胺基甲酸乙酯開孔發泡體。φ 較佳地’於步驟d)中該a液及B液的混合物於該模具内 的固化及發泡間為2分鐘至1 0分鐘。 發明之詳細說明 本發明揭示一種完全不採用冷媒而完全以水發泡的冷 固化硬質聚胺基甲酸乙酯(PU)發泡體,其泡體具有細小泡564253 _ Prime No. 89105188 / 〇 Di: t: _ 5. Description of the invention (3) PMDETA)] ° Polyether polyols suitable for the present invention are composed of polyfunctional groups such as glycerol, sucrose, hexadecanol and the like Polymers of alkylene oxides (such as propylene oxide and ethylene oxide) are, for example, polyether polyols purchased from Dow Chemical Company under the code VRANOLL360 and VORANOL490. A method suitable for manufacturing the rigid polyurethane open-cell foam of the present invention comprises the following steps: a) mixing 100 parts by weight of 3 to 5 hydroxyl functional groups and a hydroxyl value of 3 to 70 mgKOH / g polyether polyol, 1 to 3.6 parts by weight of a non-hydrolyzable polysiloxane surfactant, 0.2 to 3 parts by weight of a tertiary amine catalyst, 0.2 to 2. 6 4 parts by weight of water 'and 0.2 to 2.4 parts by weight of carbon atoms C2-C8 polyol chain extender to prepare a liquid A; b) preheating the liquid A in step a) to keep it at The temperature of 25-45 ° C; c) Preheating the B liquid of polyisocyanate to keep it at a temperature of 25-45 ° C; d) Preheating the liquids A and B with B and A The weight ratio of the liquid is 0.7 ~ 1 · 2, and the mixture is quickly added and mixed, and then the obtained mixture is injected into a mold at a temperature of 35-5 5 t and the temperature is higher than the mixture of the A liquid and the B liquid. Curing and foaming; and, e) removing a polyurethane open-cell foam from the mold. φ Preferably, in the step d), the mixture of the a liquid and the B liquid in the mold is cured and foamed for 2 minutes to 10 minutes. DETAILED DESCRIPTION OF THE INVENTION The present invention discloses a cold-curing rigid polyurethane (PU) foam that is completely foamed with water without using a refrigerant at all.
第7頁 564253 _____案號 891Q5188_^年夕月广^日__修正___ 五、發明說明(4) 孔及良好的開孔性,孔徑為0· 08mm或更小,開孔率為90% 或更高。當本發明的發泡體應用在冷束冷藏真空保溫材 時,絕熱效果良好,在經抽真空後其熱傳導係數於丨3 t可 降至〇· 01 W/mk。本發明的發泡體因不含冷媒,所以不會 破壞臭氧層。本發明的PU發泡體所使用的主要原料聚醚多 元醇及多異氰酸酯為一般傳統硬質PU發泡體所使用的原 料,該聚醚多元醇其合成起始物主要為蔗糖及甘油,具有 3-5個官能基和經值300〜700 mgKOH/g ;該多異氰酸g旨主要 為MDI與高官能基的異氰酸酯的混合物,其官能基約2.7。 形成細小的孔徑及聚合物支架有利於降低熱傳導,在4 使用冷媒的P U發泡上,只有較單純的膠化反應,而其發泡 現象的產生主要屬於冷媒蒸發膨脹的物理現象。由於我們 只採用水當發泡劑’因此必須完全藉由水與異氰酸酯的化 學反應來釋出^_氧化奴氣體造成膨服,亦即發泡反應及膠 化反應同時進行,這兩種反應需有適當的平衡性,而催化 劑的使用在平衡性上具有關鍵性影響。本發明配方所使用 的催化劑主要屬於三級胺化合物,例如D M D E E,τ E D A,T D -33 及PMDETA 等 〇 於本發明中以A液與B液混合後至瞬間要開始發泡膨脹 的時間為起發時間,當作發泡的速率參考值,另以反應物 混合後直到泡體表皮不黏的時間為"不黏時間”當作膠化速 率參考值。實驗結果發現催化劑用量加大而導致其膠化速 率增快時,所形成的聚合物支架有較小的趨向(分別以下 列貝知例1中的第1、2、3試驗,第4、5、6試驗,及第7、 8試驗為一組加予比較)°合適的催化劑用量為0· 2〜3%(以Page 7 564253 _____ Case No. 891Q5188_ ^ Yan Xi Yue Guang ^ __ Amendment ___ V. Description of the invention (4) Holes and good opening properties, the hole diameter is 0.08mm or less, and the opening ratio is 90 % Or higher. When the foam of the present invention is applied to a cold beam refrigerated vacuum insulation material, the thermal insulation effect is good, and its thermal conductivity can be reduced to 0.01 W / mk after being evacuated. Since the foam of the present invention does not contain a refrigerant, it does not damage the ozone layer. The main raw materials used in the PU foam of the present invention are polyether polyols and polyisocyanates, which are the raw materials used in general conventional rigid PU foams. The starting materials for the synthesis of the polyether polyols are mainly sucrose and glycerol. -5 functional groups and a value of 300 ~ 700 mgKOH / g; the polyisocyanate g is mainly a mixture of MDI and a highly functional isocyanate, and its functional group is about 2.7. The formation of small pores and polymer scaffolds is conducive to reducing heat conduction. On PU foam using refrigerant, there is only a simpler gelation reaction, and the foaming phenomenon is mainly a physical phenomenon of refrigerant evaporation and expansion. Since we only use water as the foaming agent, we must completely release the ^ _ oxide gas to cause swelling through the chemical reaction between water and isocyanate, that is, the foaming reaction and the gelation reaction are performed simultaneously. These two reactions require There is proper balance, and the use of catalysts has a critical impact on balance. The catalyst used in the formulation of the present invention mainly belongs to tertiary amine compounds, such as DMDEE, τ EDA, TD-33, and PMDETA, etc. In the present invention, the time from when the A liquid and the B liquid are mixed to the instant when foaming and expansion begin is The development time is taken as the reference value of the foaming rate, and the time after the reactants are mixed until the foam skin is not sticky is the "non-sticky time" as the reference value for the gelation rate. The experimental results show that the increase in the amount of catalyst caused When the gelation rate is increased, the formed polymer scaffolds have a smaller tendency (the first, second, and third tests, the fourth, fifth, and sixth tests, and the seventh and eighth tests respectively in Example 1 below). The test is a group of comparisons. ° The appropriate catalyst dosage is 0.2 to 3% (in terms of
564253564253
聚醚多原醇重量為基準)。 若添加二醇類增鏈劑幾乎不影響反應速率,但對聚合 物支架及平均孔徑有降低作用(參見實施例2,以第g〜1 ^ 驗與第2試驗為一組加予比較),增鏈劑用量為〇. 2〜2. (以聚醚多疋醇重量為基準),最適當的增鏈劑為伸丙基二 醇[Propylene glyC〇i,(在此簡稱 pEG)]、乙二醇 — [Diethylene glycol,(在此簡稱DEG)]。而水在此具有發 泡劑及交聯劑的作用,對發泡體的孔徑、密度具有影響x (實施例3 )。水用量為〇 · 2 ~ 2 · 6 % (以聚醚多元醇重量基 準)。 _ 因為發泡體為開孔結構,沒有閉孔氣泡的支撐力,較 易於塌陷及收縮,加入一額外的交聯劑可硬化泡體,因其 活性很高,在用量上須小心斟酌,以避免形成過多斷裂交 支點’額外的交聯劑用量為〇 · 4〜丨% (以聚醚多元醇重量為 基準),最適當的交聯劑為二乙醇胺[Diethan〇Umine,-(在此簡稱DIE)]。 由於採用完全水發泡,因此界面活性劑使用非水解性 聚矽氧聚合物,其用量上對於開孔性及孔徑有很大影響, 適當的界面活性劑才能形成良好的孔徑及開孔率(實施例 4),界面活性劑用量為1〜3· 6%(以聚醚多元重量為基準),嫌 最適當的界面活性劑為美國〇以所生產之Niax silic〇ne L - 6 1 6 4。當發泡體开> 成較細小的孔徑及聚合物支架,並且 具有良好開孔率時,將其封裝成真空保溫片,則可達到降 低熱傳導目的(實施例5 )。Polyether polyortho-alcohol is based on weight). Adding a diol-based chain extender hardly affects the reaction rate, but has a reducing effect on the polymer scaffold and the average pore diameter (see Example 2, comparing g ~ 1 ^ test with the second test as a group), The amount of chain extender is 0.2 ~ 2. (Based on the weight of polyether polyol), the most suitable chain extender is propylene glycol [Propylene glyC0i, (herein referred to as pEG)], B Diol — [Diethylene glycol, (herein referred to as DEG)]. On the other hand, water acts as a foaming agent and a cross-linking agent, and has an effect on the pore diameter and density of the foam x (Example 3). The amount of water used is from 0.2 to 2.5% (based on the weight of polyether polyol). _ Because the foam has an open-cell structure and does not have the support of closed-cell bubbles, it is easier to collapse and shrink. Adding an additional cross-linking agent can harden the foam. Because of its high activity, the dosage must be carefully considered to Avoid the formation of excessive breaking and branching points' The amount of additional crosslinking agent is 0.4 ~ 丨% (based on the weight of the polyether polyol). The most suitable crosslinking agent is diethanolamine [Diethan〇Umine,-(herein referred to as DIE)]. Due to the use of complete water foaming, the surfactant uses a non-hydrolyzable polysiloxane polymer. The amount of the surfactant has a great influence on the porosity and pore size. A proper surfactant can form a good pore size and porosity ( Example 4), the amount of the surfactant is 1 to 3.6% (based on the weight of the polyether multiple weight). The most suitable surfactant is the United States. Niax silicone L-6 1 6 4 . When the foam is formed into a relatively small pore size and a polymer stent, and has a good porosity, it can be packaged into a vacuum insulation sheet to reduce the heat conduction (Example 5).
564253 __案號 89105188 fz年7月/〇日_修正 _ 五、發明說明(6) 多元醇重量為基準。 實施例1 將100重量份的聚醚多元醇(官能基數4.3,羥值 49 0 ),2重量份水,3重量份界面活性劑[Osi所生產之Niax si 1 icone L-6164]及觸媒等混合均勻成A料後再以溫度 2 7 °C〜33 °C進行預熱,B料多異氰酸酯(主要為MDI與高官能 基的異氰酸酯的混合物,其官能基數2. 7)以溫度27 t〜 3 3 °C進行預熱’待溫度均勻後各置入兩步驟發泡機的料桶 中,經發泡機將A料與B料混合物後注入溫度為37 。(; Λ 的模具中發泡。觸媒的種類與用量,多異氰酸酯的肖ϋ 反應結果被列於下表。 均孔徑 (mm) 0. 088 0. 092 0. 085 0.097 0.082 0.076 0.115 0. 103 不黏 ^ 時間 3分3 5秒 2分1 4秒 56秒 3分1 〇秒 2分31秒 1分47秒 8分2 5秒 2分1 3秒 聚合物 °· 033 〇· 03 0 · 027 0· 026 0· 025 0· 021 °· 036 0· 026 試異氰 觸媒 起發 塗 酸酉旨 __ 時間 1 122% 0. 4°/〇(TEDA) 52 秒 2 120% 0. 6%(TEDA) 37 秒 3 122% 1% (TEDA) 23 秒 4 9 6°/〇 0· 8%(TD-33 ) 5 9 秒 5 9 2°/〇 1 · 20/〇(TD-33 ) 5 3 秒 6 92% 1· 6%(TD-33) 39 秒 788% 0· 2%(PMDETA)35 秒 8 88% 0·4%(PMDETA)21 秒564253 __Case No. 89105188 July / 〇 fz_ Amendment _ V. Description of the invention (6) Polyol weight is used as the basis. Example 1 100 parts by weight of a polyether polyol (number of functional groups: 4.3, hydroxyl value: 49 0), 2 parts by weight of water, 3 parts by weight of a surfactant [Niax si 1 icone L-6164 produced by Osi], and a catalyst After mixing evenly, material A is preheated at a temperature of 2 7 ° C ~ 33 ° C, and material B is a polyisocyanate (mainly a mixture of MDI and a highly functional isocyanate, and the number of functional groups is 2.7) to a temperature of 27 t. ~ 3 3 ° C for preheating '. After the temperature is uniform, put it into the bucket of the two-step foaming machine, mix the A and B materials through the foaming machine and inject the temperature to 37 ° C. (; Λ foamed in the mold of Λ. The type and amount of catalyst, and the Shaw reaction results of polyisocyanate are listed in the following table. Average pore diameter (mm) 0. 088 0. 092 0. 085 0.097 0.082 0.076 0.115 0. 103 Not sticky ^ Time 3 minutes 3 5 seconds 2 minutes 1 4 seconds 56 seconds 3 minutes 1 0 seconds 2 minutes 31 seconds 1 minute 47 seconds 8 minutes 2 5 seconds 2 minutes 1 3 seconds Polymer ° · 033 〇 03 0 · 027 0 · 026 0 · 025 0 · 021 ° · 036 0 · 026 Trial of isocyanate catalyst for acid coating purpose__ Time 1 122% 0.4 ° / 〇 (TEDA) 52 seconds 2 120% 0. 6% (TEDA) 37 seconds 3 122% 1% (TEDA) 23 seconds 4 9 6 ° / 〇0 · 8% (TD-33) 5 9 seconds 5 9 2 ° / 〇1 · 20 / 〇 (TD-33) 5 3 seconds 6 92% 1.6% (TD-33) 39 seconds 788% 0.2% (PMDETA) 35 seconds 8 88% 0.4% (PMDETA) 21 seconds
第10頁 564253 案號 89105188 泠年7月,ο曰 修正 五、發明說明(7) 架,及良好的開孔性(8 0 %以上)。此外,當催化劑用量加 大時,會導致其膠化速率增快,所形成的聚合物支架有減 小的趨向。 實施例2 除了觸媒限定為0.6重量份的TEDA及進一步加入增鏈 劑外,重覆實施例1的步驟。增鏈劑的種類與用量,多異 氰酸酯的用量及反應結果被列於下表。Page 10 564253 Case No. 89105188 In July, ο Amendment V. Description of the invention (7) Frame, and good openness (above 80%). In addition, when the amount of catalyst is increased, the gelation rate will be increased, and the polymer scaffolds formed will tend to decrease. Example 2 The procedure of Example 1 was repeated except that the catalyst was limited to 0.6 parts by weight of TEDA and a chain extender was further added. The type and amount of chain extender, the amount of polyisocyanate, and the reaction results are listed in the table below.
試驗 異氰 增鏈劑 平均孔徑 聚合物支架 酸酯 _ (mm) (mm) 9 122% 0. 4% (PEG) 0. 08 0.023 10 122% 0. 8% (PEG) 0. 085 0. 027 11 110% 1. 2% (PEG) 0. 07 0. 029 12 98% 1. 8°/〇 (PEG) 0. 079 0. 021 13 96% 0. 4% (DEG) 0. 072 0.019 14 102% 1% (DEG) 0. 079 0. 024 15 100% 1. 8°/〇 (DEG) 0. 067 0.026 16 100% 2. 4% (DEG) 0. 075 0.021Test isocyanate chain extender average pore polymer scaffold _ (mm) (mm) 9 122% 0.4% (PEG) 0.08 0.023 10 122% 0.8% (PEG) 0.885 0.027 11 110% 1.2% (PEG) 0.07 0. 029 12 98% 1.8 ° / 〇 (PEG) 0.079 0.02 021 13 96% 0.4% (DEG) 0.072 0.019 14 102 % 1% (DEG) 0.079 0. 024 15 100% 1.8 ° / 〇 (DEG) 0.067 0.026 16 100% 2.4% (DEG) 0.075 0.021
比較實施例第2試驗與上表的資料可看出增鏈劑的使 用具有降低泡孔及聚合物支架的大小的效用。 實施例3 除了增鏈劑限定為1. 2重量份的DEG及變化水的用量It can be seen from the comparison between the second test of the example and the above table that the use of the chain extender has the effect of reducing the size of the cells and the polymer scaffold. Example 3 In addition to the chain extender defined as 1.2 parts by weight of DEG and the amount of changing water
第11頁 564253 修正 案號 89105188 五、發明說明(8) 外,重覆實施例2的步驟。水的用量,多異氰酸酯的用量 及反應結果被列於下表。 試驗 異氰 酸酯 水 平均孔徑 (mm) 聚合物支架 (mm) 密度 (kg/m3、 17 104% 0. 6% 0. 068 0.023 102 18 102% 1% 0. 081 0. 023 62 19 10% 2. 2% 0.067 0. 025 63 從上表的資料可看出水用量對發泡體的孔徑、密度具H 有影響,其用量在〇. 6 %(以聚醚多元醇重量基準)時即可形 成較細小孔徑的發泡體。 實施例4 除了將水限定為2重量份、進一步加入額外的0. 6重量 份交聯劑D I E及變化N i a X s i 1 i c ο n e L _ 6 1 6 4界面活性劑的 用量外,重覆實施例3的步驟。Niax silicone L - 6164界 面活性劑的用量及反應結果被列於下表。Page 11 564253 Amendment No. 89105188 V. Description of the invention (8) Repeat the steps of the second embodiment. The amount of water, the amount of polyisocyanate and the reaction results are listed in the table below. Test isocyanate average pore size (mm) Polymer stent (mm) Density (kg / m3, 17 104% 0. 6% 0. 068 0.023 102 18 102% 1% 0. 081 0. 023 62 19 10% 2.2 2 % 0.067 0. 025 63 From the data in the table above, it can be seen that the amount of water has an effect on the pore size and density of the foam. The amount of water can form a finer when 0.6% (based on the weight of polyether polyol). Example 4 In addition to limiting water to 2 parts by weight, additional 0.6 parts by weight of cross-linking agent DIE and varying N ia X si 1 ic ο ne L _ 6 1 6 4 surfactant In addition to the amount used, the steps of Example 3 were repeated. The amount of Niax silicone L-6164 surfactant and the reaction results are listed in the table below.
試 異氰 界面 平均孔徑 聚合物支架 猃 酸酯 活性劑 (mm) (ram) 開孔率 20 92°/〇 1°/〇 0.095 0.019 95.4% 21 93% 1. 6°/〇 0. 078 0.016 89. 8% 22 93% 2°/〇 0.087 0.018 94.5% 第12頁 564253Isocyanate interface average pore size polymer scaffold acetate active agent (mm) (ram) Porosity 20 92 ° / 〇1 ° / 〇0.095 0.019 95.4% 21 93% 1. 6 ° / 〇.0.0 0.016 89 8% 22 93% 2 ° / 〇0.087 0.018 94.5% Page 12 564253
案號 89105j@ 五、發明說明(9) 從上表的資料可看出非k & 1.1 ffl ^ ^1%( ^ ^ ^ ^权解性聚矽氧聚合物界面活性 劑用里在1 Μ以承越多元醇重景A唯、 的發泡體。 里基準)時即可形成細小孔徑 實施例5 使用100重量份的聚醚多元 ,ΠΛ, 9舌旦於> 0 _ 夕兀官能基數4· 3,羥值 490) ’2重里伤水’ 2重量份及品V-. •r τ 界面活性劑[〇Si所生產之Niax silicone L 一 6164] ,1·2 重量价梯 μ 士 η η β壬- 里伤增鍵劑DEG,〇· 6重量份觸 媒TEDA及0· 6重1份交聯劑die,w 。 a 1 β 以及8 9重量份多異氰酸酯 (主要為MDI與高官能基的異氰酸萨& , 2.”依實施m的步驟製備出一硬 PU開孔發泡體:性質被列於下表。從下列表中的數據可看 出本施例的硬質PU開孔發泡體具有細小的孔徑及聚合物支 架,並且具有良好開孔率,且將其封裝保溫片時, 可達到降低熱傳導的目的。 封裝成真空片 熱傳導係數, W/mk 0. 01Case No. 89105j @ V. Description of the invention (9) It can be seen from the information in the table above that non-k & 1.1 ffl ^ ^ 1% (^ ^ ^ ^ right-dissolving polysiloxane polymer surfactant is used in 1 Μ The finer the polyol is, the better the foam is A. The fine pore diameter can be formed when Example 5 uses 100 parts by weight of a polyether polyhydric, ΠΛ, 9 and more. 0 _ Xiwu functional group number 4 · 3, Hydroxyl value 490) 2 parts by weight of wound water V-. • r τ Surfactant [Niax silicone L-6164 produced by Si], 1.2 Weight price ladder μ ± η η β Non-trauma bond increasing agent DEG, 0.6 parts by weight of catalyst TEDA and 0.6 parts by weight of 1 crosslinking agent die, w. a 1 β and 8 9 parts by weight of polyisocyanate (mainly MDI and highly functional isocyanate & 2. "A hard PU open-cell foam was prepared according to the procedure of m: properties are listed below Table. From the data in the following table, it can be seen that the rigid PU open-cell foam of this example has a small pore size and a polymer stent, and has a good open cell ratio. When it is packaged with a thermal insulation sheet, it can reduce heat conduction. Purpose: Thermal conductivity of packaged vacuum sheet, W / mk 0. 01
平均聚合物 未封裝成 試孔徑支架 真空片熱傳 ^ LmL· LrnL· 開孔車 w/mk 230.068 0.019 95.7% 0· 〇38 對照例: 將100重量份的聚醚多元醇(官能基數4· 5,羥值36〇),多 異氰酸酷(主要為MDI與高官能基的異氰酸酯的混合物,其 官能基數2 · 7)與下表所列的成份依實施例一的步驟製備硬The average polymer is not encapsulated into a test hole holder vacuum sheet heat transfer ^ LmL · LrnL · Opening car w / mk 230.068 0.019 95.7% 0 · 〇38 Comparative Example: 100 parts by weight of a polyether polyol (number of functional groups 4.5 , Hydroxyl value 36〇), polyisocyanate (mainly a mixture of MDI and a highly functional isocyanate, the number of functional groups 2 · 7) and the ingredients listed in the table below to prepare hard
第13頁 564253 案號 89105188Page 13 564253 Case number 89105188
泠年?月/Q 修正 五、發明說明(10) 質PU發泡體 試異氰水 猃酸酯— 24 1 2 4 % 3 % 觸媒 # 醋酸鉀 - 1.5% 硬酯酸鈣 - 1.5% DMDEE 3 % - 27 116% 1·4% 醋酸鉀0.2% Y- 1 0 76 2* + DMDEE0. 2 % 8 % 28 116% 1.4% 醋酸鉀0.2%L-6164 + DMDEE0. 2 % 1 % 未添加 未發泡成形 OSi生產之界面活性劑silicon Y- 1 0 7 6 2 2 5 1 2 4 % 3 % 2 6 1 2 4 % 3 % 界面活性劑平均孔 徑mm ) # # 0. 155 0.160Ling Nian? Month / Q Amendment V. Description of the invention (10) Quality PU foam test of isocyanate—24 1 2 4% 3% Catalyst # potassium acetate-1.5% calcium stearate-1.5% DMDEE 3%- 27 116% 1.4% potassium acetate 0.2% Y- 1 0 76 2 * + DMDEE 0.2% 8% 28 116% 1.4% potassium acetate 0.2% L-6164 + DMDEE 0.2% 1% OSi Silicon Y- 1 0 7 6 2 2 5 1 2 4% 3% 2 6 1 2 4% 3% Mean pore diameter of surfactant mm) # # 0. 155 0.160
氺 由上表的資料可看出觸媒成份不適當或不使用界面活 性劑無法有效形成發泡的結果,或則將產生粗大的泡體孔 徑及支架。氺 From the information in the table above, it can be seen that the results of improper catalyst composition or the ineffective formation of foam without the use of surfactants, or the formation of coarse foam pores and scaffolds.
第14頁Page 14
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