WO2016090575A1 - 一种微胶囊化的铂金催化剂及其制备方法 - Google Patents
一种微胶囊化的铂金催化剂及其制备方法 Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
- C08G77/08—Preparatory processes characterised by the catalysts used
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- the invention relates to a kind of chemical reaction catalyst, in particular to a microencapsulated platinum catalyst and a preparation method thereof.
- Silicone rubber has a wide range of applications in various fields of the national economy because of its excellent resistance to high and low temperature, insulation, weather resistance, non-toxic, tasteless and environmentally friendly.
- two-component addition molding liquid silicone rubber is mostly, but the two-component addition liquid silicone rubber causes bubbles during the mixing process, and after mixing the two components, it is required to have a suitable operation time at room temperature. If the time is too long, the vulcanization is too slow, which will inevitably reduce the production efficiency; while the time is too short and the construction is tight, it may also cause the rubber gel. Therefore, it is imperative to develop a platinum catalyst suitable for the structuring of single-component addition-forming liquid silicone rubber microcapsules.
- the microencapsulated platinum catalyst can not catalyze at room temperature or at a lower temperature because platinum is isolated. When the temperature rises above the softening point of the resin, the platinum catalyst is released, thereby catalyzing the addition reaction. Joint into an elastomer. But when it rises to a certain temperature, it can be vulcanized faster or faster.
- the wall material of the encapsulated platinum catalyst has a low softening point temperature, and when the temperature rises to 100 degrees, the platinum can quickly flow out to play a catalytic role.
- the patent introduces the use of polystyrene, polymethyl methacrylate, phenyl silicone resin as the wall material, but it also has its drawbacks, the softening point of polystyrene is too high, when it rises to a certain temperature, the platinum catalyst can not flow smoothly and quickly; Polymethyl methacrylate and phenyl silicone resin are extremely brittle, and it is easy to break the shell during the stirring process, causing the platinum catalyst to flow out prematurely and not to isolate. .
- the present invention provides a microencapsulated platinum catalyst having a low softening point and a high toughness, and is suitable for low temperature.
- the preparation of the formed one-component addition molding liquid silicone rubber aims to solve the problem that the platinum softening point of the existing microcapsule platinum catalyst is too high or the toughness is insufficient, so that the platinum catalyst cannot flow out in a timely manner.
- a microencapsulated platinum catalyst wherein the raw material composition, according to the mass fraction, comprises the following components:
- the low softening point thermoplastic resin has a softening point of 60 to 80 degrees and is soluble in petroleum ether.
- microencapsulated platinum catalyst wherein the liquid platinum catalyst has a platinum content of 1000 to 8000 ppm.
- microencapsulated platinum catalyst wherein the petroleum ether has a boiling range of 30 to 60 degrees.
- microencapsulated platinum catalyst wherein the low softening point thermoplastic resin is polycaprolactone.
- microencapsulated platinum catalyst wherein the raw material composition, according to the mass fraction, further comprises the following components:
- the aqueous solution is stirred while uniformly adding a petroleum ether solution in an aqueous solution; after the dropwise addition is completed, nitrogen gas is introduced for 40 to 48 hours, and the mixture is centrifuged for solid-liquid phase separation, washed with methanol, and the solid phase is filtered, to obtain a microencapsulated solid phase;
- the platinum catalyst on the surface of the microcapsules was washed by washing with octamethylcyclotetrasiloxane.
- the liquid platinum catalyst has a platinum content of 1000 to 8000 ppm; the petroleum ether has a boiling range of 30 to 60 degrees; and the low softening point thermoplastic resin is polycaprolactone.
- the method for producing a microencapsulated platinum catalyst wherein the amount of the methanol is 100 parts by mass, and the amount of the octamethylcyclotetrasiloxane is 2000 parts.
- the microencapsulated platinum catalyst provided by the present invention and a preparation method thereof, the microencapsulated platinum catalyst, the microcapsule wall material has low softening point and high toughness, and has no catalytic activity at room temperature, when the temperature is It has a catalytic activity of up to 80 degrees and can be used for the preparation of low-temperature molding single-component addition liquid silicone rubber.
- Figure 1 is an electron micrograph of a microencapsulated platinum catalyst in Example 1 of the present invention.
- Fig. 2 is a graph showing the results of viscosity change test of the silicone composition in Example 1 of the present invention.
- Fig. 3 is a graph showing the results of a viscosity change test of the silicone composition in Example 1 of the present invention.
- Figure 4 is a scanning electron micrograph of a microencapsulated platinum catalyst in Example 2 of the present invention.
- Fig. 5 is a graph showing the results of viscosity change test of the silicone composition in Example 2 of the present invention.
- Figure 6 is a graph showing the data of vulcanization curves of silicone compositions at different temperatures in Example 2 of the present invention.
- Fig. 7 is a graph showing the results of viscosity change test of the silicone composition in Example 3 of the present invention.
- Figure 8 is a graph showing the data of vulcanization curves of silicone compositions at different temperatures in Example 3 of the present invention.
- the present invention provides a microencapsulated platinum catalyst and a preparation method thereof.
- the present invention will be further described in detail below. It is understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
- microencapsulated platinum catalyst provided by the invention and the preparation method thereof, the microencapsulated platinum catalyst, the microcapsule wall material has low softening point and high toughness, and can be used for low temperature forming single component addition molding Catalytic reaction of silicone rubber.
- the raw material composition of the microencapsulated platinum catalyst includes, according to the mass fraction, the following components:
- the liquid platinum catalyst may have a platinum content of 1000 to 8000 ppm.
- the low softening point thermoplastic resin has a softening point of 60 to 80 degrees and is soluble in petroleum ether. For example, if the polycaprolactone has a softening point of 60 degrees, the softening point of the prepared microcapsule wall material will be relatively low.
- the degree of alcoholysis of the polyvinyl alcohol is 87-89%.
- the petroleum ether has a boiling range of 30 to 60 degrees.
- the raw material composition of the microencapsulated platinum catalyst may further include the following components in terms of mass fraction:
- the invention also provides a preparation method of the microencapsulated platinum catalyst, which comprises the following steps:
- microencapsulated platinum catalyst prepared by the method of the invention has an average particle diameter of about 2 micrometers, has no catalytic activity at room temperature, and has a rapid catalytic activity when the temperature rises above 80 degrees, and can be used for low temperature molding. Preparation of one-component addition molding liquid silicone rubber.
- Fig. 1 is an electron micrograph of the microencapsulated platinum catalyst of the first embodiment. As shown in Fig. 1, the microencapsulated platinum catalyst has an average particle diameter of about 2 ⁇ m.
- the viscosity change test results and the viscosity change test results of FIG. 5 and FIG. 6 that the viscosity of the composition does not change much at room temperature during the mixing of the mixture, which means that the microcapsules are not broken, indicating that the embodiment
- the prepared platinum catalyst has high toughness. When the temperature rises above 80 degrees, it has a rapid catalytic activity, indicating that the wall material of the platinum catalyst prepared in this example has a low softening point.
- the platinum content of the microencapsulated platinum catalyst was determined to be 1100 ppm. As shown in Fig. 2, the microencapsulated platinum catalyst has an average particle diameter of about 2 ⁇ m.
- the viscosity change test results and the viscosity change test results of FIG. 5 and FIG. 6 that the viscosity of the composition does not change much at room temperature during the mixing of the mixture, which means that the microcapsules are not broken, indicating that the embodiment
- the prepared platinum catalyst has high toughness. When the temperature of the composition rises above 80 degrees, it has a rapid catalytic activity, indicating that the wall material of the platinum catalyst prepared in this example has a low softening point.
- the viscosity change test results and the viscosity change test results of FIG. 7 and FIG. 8 that the viscosity of the composition does not change much at room temperature during the mixing of the mixture, which means that the microcapsules are not broken, indicating that the embodiment
- the prepared platinum catalyst has high toughness. When the temperature of the composition rises above 80 degrees, it has a rapid catalytic activity, indicating that the wall material of the platinum catalyst prepared in this example has a low softening point.
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Abstract
一种微胶囊化的铂金催化剂及其制备方法，其原料组成，按照质量分数计，包括以下组分：液体铂金催化剂、低软化点热塑性树脂、聚乙烯醇、去离子水、石油醚；所述低软化点热塑性树脂的软化点为60～80度，并且能溶解于石油醚中。所述微胶囊化的铂金催化剂，其微胶囊壁材的软化点低、韧性大，在室温下没有催化活性，当温度升到80度以上，具有很快的催化活性，能用于低温成型单组份加成型液体硅橡胶的制备。
Description
本发明涉及一类化学反应催化剂，尤其涉及一种微胶囊化的铂金催化剂及其制备方法。
硅橡胶因其具有良好的耐高低温、绝缘性、耐候性及无毒无味环保等优异性能，在国民经济的各个领域有着广泛的应用。目前双组份加成型液体硅橡胶居多，但是双组份加成型液体硅橡胶在混合过程中，会引起气泡，并且两个组分混合后，要求室温下有一个适宜的操作时间。时间过长，硫化太慢，势必降低生产效率；而时间过短，施工紧张，还可能造成胶料凝胶。因此开发一种适用于单组分加成型液体硅橡胶微胶囊结构化的铂金催化剂势在必行。这种微胶囊化的铂金催化剂在室温下或较低温度下，由于铂被隔离，起不到催化作用，当温度升至高于树脂软化点后，释放出铂金催化剂，从而催化加成反应，交联成弹性体。但当升至一定温度后，则又能较快或很快硫化。
随着硅橡胶的发展，用于针织品、棉织品、莱卡弹性布料的装饰图案及标识的硅胶也越来越多，这些产品需要的成型温度又较低，通常在100度以下，因此就需要微胶囊化的铂金催化剂的壁材具备低的软化点温度，当温度升至100度，铂金能很快地流出，起到催化的作用。有专利介绍用聚苯乙烯、聚甲基丙烯酸甲酯、苯基硅树脂做壁材，但也有其弊端，聚苯乙烯软化点太高，当升到一定温度，铂金催化剂不能顺利快速地流出；而聚甲基丙烯酸甲酯、苯基硅树脂极脆，在搅拌过程中很容易破壳，导致铂金催化剂过早地流出，起不到隔离作用
。
因此，现有技术还有待于改进和发展。
鉴于上述现有技术的不足，本发明中提一种微胶囊化的铂金催化剂及其制备方法，所述微胶囊化的铂金催化剂，其微胶囊壁材的软化点低、韧性大，适用于低温成型单组份加成型液体硅橡胶的制备，旨在解决现有微胶囊的铂金催化剂的壁材软化点过高或韧性不足导致铂金催化剂不能适时地流出的问题。
本发明的技术方案如下：
一种微胶囊化的铂金催化剂，其中，其原料组成，按照质量分数计，包括以下组分：
液体铂金催化剂 2~10份；
低软化点热塑性树脂 15~25份；
聚乙烯醇 15~20份；
去离子水 300份；
石油醚 300~500份；
所述低软化点热塑性树脂的软化点为60~80度，并且能溶解于石油醚中。
所述的微胶囊化的铂金催化剂，其中，所述液体铂金催化剂的铂金含量在1000~8000ppm。
所述的微胶囊化的铂金催化剂，其中，所述石油醚的沸程为30~60度。
所述的微胶囊化的铂金催化剂，其中，所述低软化点热塑性树脂为聚己内酯。
所述的微胶囊化的铂金催化剂，其中，其原料组成，按照质量分数计，还包括以下组分：
甲醇 100份；
八甲基环四硅氧烷 2000份。
一种如上所述的微胶囊化的铂金催化剂的制备方法，其中，包括以下步骤：
将聚乙烯醇溶解于去离子水中，得到溶解有聚乙烯醇的水溶液；
把低软化点热塑性树脂、液体铂金催化剂溶解于石油醚中，得到溶解有液体铂金催化剂、软化点热塑性树脂的石油醚溶液；
一边在水溶液中匀速滴加石油醚溶液一边搅拌水溶液；滴加完毕后，通入氮气40~48h，离心进行固液相分离，用甲醇洗涤、抽滤固相，得到微胶囊化的固相；用八甲基环四硅氧烷洗涤，把微胶囊表面上的铂金催化剂洗干净。
所述液体铂金催化剂的铂金含量在1000~8000ppm；所述石油醚的沸程为30~60度；所述低软化点热塑性树脂为聚己内酯。
所述的微胶囊化的铂金催化剂的制备方法，其中，按照质量分数计，所述甲醇的用量为100份，所述八甲基环四硅氧烷的用量为2000份。
所述的微胶囊化的铂金催化剂的制备方法，其中，用八甲基环四硅氧烷洗涤的过程为：
先用八甲基环四硅氧烷洗涤1遍，抽滤，再用八甲基环四硅氧烷洗涤3遍。
有益效果：本发明所提供的微胶囊化的铂金催化剂及其制备方法，所述微胶囊化的铂金催化剂，其微胶囊壁材的软化点低、韧性大，在室温下没有催化活性，当温度升到80度以上，具有很快的催化活性，能用于低温成型单组份加成型液体硅橡胶的制备。
图1为本发明实施例1中微胶囊化的铂金催化剂的电镜扫描图。
图2为本发明实施例1中有机硅组合物的粘度变化测试结果图表。
图3为本发明实施例1中有机硅组合物在粘度变化测试结果图表。
图4为本发明实施例2中微胶囊化的铂金催化剂的电镜扫描图。
图5为本发明实施例2中有机硅组合物的粘度变化测试结果图表。
图6为本发明实施例2中有机硅组合物在不同温度下硫化曲线数据图表。
图7为本发明实施例3中有机硅组合物的粘度变化测试结果图表。
图8为本发明实施例3中有机硅组合物在不同温度下硫化曲线数据图表。
本发明提供一种微胶囊化的铂金催化剂及其制备方法，为使本发明的目的、技术方案及效果更加清楚、明确，以下对本发明进一步详细说明。应当理解，此处所描述的具体实施例仅仅用以解释本发明，并不用于限定本发明。
本发明所提供的一种微胶囊化的铂金催化剂及其制备方法，所述微胶囊化的铂金催化剂，其微胶囊壁材的软化点低、韧性大，能够用于低温成型单组份加成型硅橡胶的催化反应。
具体地，所述微胶囊化的铂金催化剂的原料组成，按照质量分数计，包括以下组分：
液体铂金催化剂 2~10份；
低软化点热塑性树脂 15~25份；
聚乙烯醇 15~20份；
去离子水 300份；
石油醚 300~500份；
其中，所述液体铂金催化剂的铂金含量可为1000~8000ppm。
所述低软化点热塑性树脂的软化点为60~80度，并且能溶解于石油醚中。如聚己内酯，其软化点60度，所制备得到的微胶囊壁材软化点就会比较低。
所述聚乙烯醇的醇解度为87-89%。
所述石油醚的沸程为30~60度。
所述微胶囊化的铂金催化剂的原料组成，按照质量分数计，还可以包括以下组分：
甲醇 100份；
八甲基环四硅氧烷 2000份。
所述甲醇与八甲基环四硅氧烷的作用均为洗涤成品。
本发明中还提供所述微胶囊化的铂金催化剂的制备方法，具体包括以下步骤：
按比例将聚乙烯醇加入到装有去离子水中烧杯中溶解，得到溶解有聚乙烯醇的水溶液；把低软化点热塑性树脂、液体铂金催化剂溶解到石油醚中，得到溶解有液体铂金催化剂、软化点热塑性树脂的石油醚溶液；把水溶液转移至装有搅拌桨的三口烧瓶中，把石油醚溶液转移至滴液漏斗中，缓缓滴加至三口烧瓶中，一边滴加一边搅拌滴加完毕，通入氮气，继续搅拌40~48h后，离心，用甲醇洗涤、抽滤；最后用八甲基环四硅氧烷洗涤4~5遍，把微胶囊表面上的铂金催化剂洗干净，即可得低温加成型液体硅橡胶微胶囊结构化的铂金催化剂。
采用本发明所述方法制备得到的微胶囊化的铂金催化剂，平均粒径为2微米左右，室温下没有催化活性，当温度升到80度以上，具有很快的催化活性，能用于低温成型单组份加成型液体硅橡胶的制备。
以下通过具体实施例对本发明的具体实施方式作进一步详细的说明。
实施例1
首先将15份的聚乙烯醇溶解到装有300份去离子水的烧杯中，然后把18份聚己内酯、5份含有2800ppm液体铂金催化剂溶解到300份石油醚中，把溶解好的聚乙烯醇水溶液转移至装有搅拌桨、通入氮气口的2L三口烧瓶中，然后把溶解有液体铂金催化剂、软化点热塑性树脂的石油醚溶液转移至滴液漏斗中，缓缓滴加至三口烧瓶中，一边滴加一边搅拌，滴加完毕，通入空气48h后，离心，用100份甲醇洗涤、抽滤，最后用500份八甲基环四硅氧烷洗涤1遍，抽滤，然后再加入1500份八甲基环四硅氧烷洗涤3遍，把微胶囊表面上的铂金催化剂洗干净，抽滤即可得所述微胶囊化的铂金催化剂。
经过检测，所述微胶囊化的铂金催化剂中铂含量为700ppm。图1为本实施例1中所述微胶囊化的铂金催化剂的电镜扫描图，如图1所示，所述微胶囊化的铂金催化剂的平均粒径为2微米左右。
取该催化剂1.5份，1.5份氢含量质量分数为0.4硅氢交联剂，100份基胶，基胶是由30份硅微粉、70份乙烯基硅油，经过硅烷偶联剂150℃热处理4h后得到的，搅拌均匀制备成液体有机硅组合物。
从图5和图6的粘度变化测试结果和粘度变化测试结果可以看出，在混料搅拌过程中，室温下组合物的粘度没有多大变化，也就说明微胶囊没有破壳，表明本实施例所制备得到的铂金催化剂韧性大。当温度升到80度以上，具有很快的催化活性，表明本实施例所制备得到的铂金催化剂的壁材软化点低。
实施例2
首先将18份的聚乙烯醇溶解到装有300份去离子水的烧杯中，然后把15份聚己内酯、4.5份含有4000ppm液体铂金催化剂溶解到400份石油醚中，把溶解好的聚乙烯醇水溶液转移至装有搅拌桨、通入氮气口的2L三口烧瓶中，然后把溶解有液体铂金催化剂、软化点热塑性树脂的石油醚溶液转移至滴液漏斗中，缓缓滴加至三口烧瓶中，一边滴加一边搅拌，滴加完毕，通入空气48h后，离心，用100份甲醇洗涤、抽滤，最后用500份八甲基环四硅氧烷洗涤1遍，抽滤，然后再加入1500份八甲基环四硅氧烷洗涤3遍，把微胶囊表面上的铂金催化剂洗干净，抽滤即可得所述微胶囊化的铂金催化剂。
经过检测，所述微胶囊化的铂金催化剂中铂含量为1100ppm。如图2所示，所述微胶囊化的铂金催化剂的平均粒径为2微米左右。
取该催化剂1.5份，1.5份氢含量质量分数为0.4硅氢交联剂，100份基胶，基胶是由30份硅微粉、70份乙烯基硅油，经过硅烷偶联剂150℃热处理4h后得到的，搅拌均匀制备成液体有机硅组合物。
从图5和图6的粘度变化测试结果和粘度变化测试结果可以看出，在混料搅拌过程中，室温下组合物的粘度没有多大变化，也就说明微胶囊没有破壳，表明本实施例所制备得到的铂金催化剂韧性大。当组合物温度升到80度以上，具有很快的催化活性，表明本实施例所制备得到的铂金催化剂的壁材软化点低。
实施例3
首先将18份的聚乙烯醇溶解到装有300份去离子水的烧杯中，然后把25份聚己内酯、9.5份含有8000ppm液体铂金催化剂溶解到400份石油醚中，把溶解好的聚乙烯醇水溶液转移至装有搅拌桨、通入氮气口的2L三口烧瓶中，然后把溶解有液体铂金催化剂、软化点热塑性树脂的石油醚溶液转移至滴液漏斗中，缓缓滴加至三口烧瓶中，一边滴加一边搅拌，滴加完毕，通入空气48h后，离心，用100份甲醇洗涤、抽滤，最后用500份八甲基环四硅氧烷洗涤1遍，抽滤，然后再加入1500份八甲基环四硅氧烷洗涤3遍，把微胶囊表面上的铂金催化剂洗干净，抽滤即可得所述微胶囊化的铂金催化剂。
取该催化剂1.5份，1.5份氢含量质量分数为0.4硅氢交联剂，100份基胶，基胶是由30份硅微粉、70份乙烯基硅油，经过硅烷偶联剂150℃热处理4h后得到的，搅拌均匀制备成液体有机硅组合物。
从图7和图8的粘度变化测试结果和粘度变化测试结果可以看出，在混料搅拌过程中，室温下组合物的粘度没有多大变化，也就说明微胶囊没有破壳，表明本实施例所制备得到的铂金催化剂韧性大。当组合物温度升到80度以上，具有很快的催化活性，表明本实施例所制备得到的铂金催化剂的壁材软化点低。
应当理解的是，本发明的应用不限于上述的举例，对本领域普通技术人员来说，可以根据上述说明加以改进或变换，所有这些改进和变换都应属于本发明所附权利要求的保护范围。
Claims (9)
- 一种微胶囊化的铂金催化剂，其特征在于，其原料组成，按照质量分数计，包括以下组分：液体铂金催化剂 2~10份；低软化点热塑性树脂 15~25份；聚乙烯醇 15~20份；去离子水 300份；石油醚 300~500份；所述低软化点热塑性树脂的软化点为60~80度，并且能溶解于石油醚中。
- 根据权利要求1所述的微胶囊化的铂金催化剂，其特征在于，所述液体铂金催化剂的铂金含量在1000~8000ppm。
- 根据权利要求1所述的微胶囊化的铂金催化剂，其特征在于，所述石油醚的沸程为30~60度。
- 根据权利要求1所述的微胶囊化的铂金催化剂，其特征在于，所述低软化点热塑性树脂为聚己内酯。
- 根据权利要求1所述的微胶囊化的铂金催化剂，其特征在于，其原料组成，按照质量分数计，还包括以下组分：甲醇 100份；八甲基环四硅氧烷 2000份。
- 一种如权利要求1所述的微胶囊化的铂金催化剂的制备方法，其特征在于，包括以下步骤：将聚乙烯醇溶解于去离子水中，得到溶解有聚乙烯醇的水溶液；把低软化点热塑性树脂、液体铂金催化剂溶解于石油醚中，得到溶解有液体铂金催化剂、软化点热塑性树脂的石油醚溶液；一边在水溶液中匀速滴加石油醚溶液一边搅拌水溶液；滴加完毕后，通入氮气继续搅拌40~48h，离心进行固液相分离，用甲醇洗涤、抽滤固相，得到微胶囊化的固相；用八甲基环四硅氧烷洗涤，把微胶囊表面上的铂金催化剂洗干净。
- 根据权利要求6所述的微胶囊化的铂金催化剂的制备方法，其特征在于，所述液体铂金催化剂的铂金含量在1000~8000ppm；所述石油醚的沸程为30~60度；所述低软化点热塑性树脂为聚己内酯。
- 根据权利要求6所述的微胶囊化的铂金催化剂的制备方法，其特征在于，按照质量分数计，所述甲醇的用量为100份，所述八甲基环四硅氧烷的用量为2000份。
- 根据权利要求6所述的微胶囊化的铂金催化剂的制备方法，其特征在于，用八甲基环四硅氧烷洗涤的过程为：先用八甲基环四硅氧烷洗涤1遍，抽滤，再用八甲基环四硅氧烷洗涤3遍。
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