CN102492397B - Preparation method of microencapsulated phase change material with high phase change latent heat value - Google Patents

Preparation method of microencapsulated phase change material with high phase change latent heat value Download PDF

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CN102492397B
CN102492397B CN 201110380869 CN201110380869A CN102492397B CN 102492397 B CN102492397 B CN 102492397B CN 201110380869 CN201110380869 CN 201110380869 CN 201110380869 A CN201110380869 A CN 201110380869A CN 102492397 B CN102492397 B CN 102492397B
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phase change
erythritol
latent heat
parts
prepared
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CN102492397A (en
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潘炳力
赵菁
杜三明
逄显娟
赵飞
张玉清
张永振
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河南科技大学
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Abstract

一种高相变潜热值微胶囊化相变材料的制备方法,通过赤藓糖醇、去离子水、二亚乙基三胺、聚山梨酯-80和斯盘-80制备赤藓糖醇溶液,通过异氰酸酯溶解在液体石蜡油中制得异氰酸酯溶液,将赤藓糖醇溶液滴加到液体石蜡油中制得油包水乳液,再将异氰酸酯溶液滴加到油包水型乳液中,反应后过滤、烘干固体物得到产品。 One kind of high phase transition microencapsulated latent heat of a phase change material prepared by erythritol, deionized water, diethylene triamine, polysorbate-80 and Si-80 was prepared erythritol after dissolving an isocyanate prepared isocyanate solution in a liquid paraffin oil, erythritol alcohol was added dropwise to the liquid paraffin oil prepared in water in oil emulsion, and then the isocyanate was added dropwise to water in oil type emulsion, the reaction filtering and drying the solid product was obtained. 本发明通过选择常见相变物质中相变潜热值最大的赤藓糖醇做胶囊芯材,使用本发明方法制备的微胶囊化相变材料,其相变潜热值在230J/g左右,与现有技术制备的微胶囊化相变材料的相变潜热值相比有很大程度的提高。 The present invention, by selecting a common phase change material in the latent heat value of the maximum erythritol do capsule core material prepared using the process of the invention microencapsulated phase change material, which latent heat value of about 230J / g, and now there are prepared with art microencapsulated phase change material has a latent heat value greatly improved compared.

Description

一种高相变潜热值微胶囊化相变材料的制备方法技术领域[0001] 本发明涉及一种功能性复合材料的制备方法,具体的说是一种高相变潜热值微胶囊化相变材料的制备方法。 TECHNICAL FIELD one kind of high phase transition microencapsulated latent heat of phase change materials [0001] The present invention relates to a functional composite material preparation, specifically a high phase transition microencapsulated latent heat phase transition the method of preparing the material. 背景技术[0002] 微胶囊化相变材料是采用微胶囊技术将固液相变材料用合成高分子材料或无机化合物以物理或化学方法包覆起来的常态下稳定的固体微粒,这种固体微粒可在很窄的温度范围内吸收或释放可观的相变潜热,具有较显著的蓄热调温功能,通过选择适当的囊材可有效改善相变储能材料在发生固液相变时的泄漏、相分离、体积膨胀、有腐蚀性、热稳定性差等问题。 [0002] microencapsulated phase change materials is the use of microencapsulation technology with solid-liquid phase change material in a stable synthetic polymer material or an inorganic compound is physically or chemically coated up normally solid particles, such solid particles can be absorbed in a very narrow temperature range or release of significant latent heat, the heat accumulator having a more significant temperature control function, by selecting a suitable capsule material can effectively improve the phase change energy storage material in the event of leakage of the solid-liquid phase change , phase separation, volume expansion, corrosive, and poor thermal stability. [0003] 微胶囊化相变材料的相变潜热值是评价其性能的重要指标。 [0003] microencapsulated latent heat value of the phase change material is an important index of the performance. 微胶囊化相变材料的相变潜热值主要由芯材的相变潜热值决定,另外与相变材料的微胶囊化率(包封率)即壳层的含量多少有关系。 Microencapsulated latent heat value of the phase change material is mainly determined by the latent heat of the phase change of the core material, and further the content of microencapsulated phase change material (encapsulation efficiency), that is how much the shell relationship. 理论上来说,微胶囊化率的极限值为100%,微胶囊化相变材料的相变潜热值可以接近相变材料的相变潜热。 Theoretically, microencapsulated limit rate is 100%, the value of latent heat microencapsulated phase change material of phase change material may be closer to the latent heat. 但实际上,微胶囊化率通常不会超过80%,微胶囊化相变材料由于壳层材料的引入通常会造成相变潜热值大幅度下降,目前报道或公开的微胶囊化相变材料其相变潜热值大多低于100J/g。 But in fact, microencapsulated rate typically will not exceed 80% microencapsulated phase change material due to the introduction of the sheathing material is usually latent heat will cause a significant decline in value, the current disclosure reports or microencapsulated phase change materials which most latent heat value of less than 100J / g. 发明内容[0004] 为解决微胶囊化相变材料的相变潜热值较低的问题,本发明提供了一种高相变潜热值微胶囊化相变材料的制备方法。 [0004] In order to solve with microencapsulated phase change material becomes lower latent heat problem, the present invention provides a high phase transition latent heat change material prepared microencapsulated phase. [0005] 本发明为解决上述技术问题采用的技术方案为:一种高相变潜热值微胶囊化相变材料的制备方法,包含以下步骤:[0006] I)制备赤藓糖醇溶液:按重量比取8-15份的赤藓糖醇溶解在16-30份的去离子水中,再依次加入1-5份的二亚乙基三胺、0.01-1份的聚山梨酯-80和0.05-2份的斯盘_80, 搅拌均匀后制得赤藓糖醇溶液,备用;[0007] 2)将1-8份的异氰酸酯溶解在12-17份的液体石蜡油中,制得异氰酸酯溶液,备用;[0008] 3)将步骤I中制得的赤藓糖醇溶液在500-5000rpm的搅拌速度下,以10g/min的滴加速度均匀滴加到40-60份的液体石蜡油中,滴加完毕后再持续搅拌0.5-1.5h制成油包水型乳液,备用;[0009] 4)将步骤2中的异氰酸酯溶液在50-60°C、1000rpm的搅拌速度下,以0.5g/min的滴加速度均匀滴加到步骤3中的油包水型乳液中,备用;[0010] 5)使步骤4中的混合物在60°C的条件下持续反应lh,然 [0005] aspect of the invention to solve the above problems is used: one kind of high phase transition latent heat method of preparing microencapsulated phase change materials, comprising the steps of: [0006] I) Preparation of solution of erythritol: Press taking the ratio of 8-15 parts by weight of erythritol dissolved in 16-30 parts of deionized water, and then were added 5 parts of diethylene triamine, 0.01 parts of polysorbate-80 and 0.05 -2 parts Span _80, after stirring uniformly to prepare erythritol solution, standby; [0007] 2) 1-8 parts isocyanate was dissolved in 12-17 parts of liquid paraffin oil, the isocyanate solution prepared standby; [0008] 3) prepared in step I erythritol solution under stirring rate 500-5000rpm to 10g / min acceleration drops uniformly dropwise added 40-60 parts of a liquid paraffin oil, after complete addition stirring was continued 0.5-1.5h made of water-in-oil emulsion, the standby; [0009] 4) the isocyanate solution from step 2 at 50-60 ° C, the stirring speed 1000rpm, to 0.5g / the uniformly dropping min step 3 was added dropwise to water-in-oil emulsion, the backup; [0010] 5) reacting 4 step lh the reaction mixture was continued under conditions of 60 ° C, then 过滤,过滤后的固体物用蒸馏水洗涤,再放入真空烘箱中干燥,获得产品。 Filtration, the solid was filtered and washed with distilled water, and then dried in a vacuum oven to give the product. [0011] 上述的异氰酸酯可以为单异氰酸酯、二异氰酸酯和多异氰酸酯。 [0011] The isocyanates may be monoisocyanates, diisocyanates and polyisocyanates. [0012] 本发明中,当参`与反应的各物质量较大时,为保证效率和质量,可设计多个滴加点和搅拌点,每个滴加点的滴加速度、搅拌速度均与上述的滴加速度、搅拌速度相吻合。 [0012] In the present invention, when the mass of each parameter 'when reacting is large, in order to ensure the quality and efficiency, can be designed and a plurality of points added dropwise with stirring drops of the acceleration of each point of the dropwise addition, the stirring rate were the above-described dropping, stirring rate coincide. [0013] 有益效果:本发明通过选择常见相变物质中相变潜热值最大的赤藓糖醇做胶囊芯材,使用本发明方法制备的微胶囊化相变材料,其相变潜热值在230J/g左右,而现有国产的微胶囊化相变材料的相变潜热值一般为110J/g,进口的产品相变潜热值为151.6J/g,因此使用本方法制得的微胶囊化相变材料与现有技术制备的微胶囊化相变材料的相变潜热值相比有很大程度的提高。 [0013] Advantageous Effects: The present invention, by selecting a common phase change material in the latent heat value of the maximum erythritol do capsule core material prepared using the process of the invention microencapsulated phase change material, which latent heat value of 230J / g, while the domestic conventional microencapsulated phase change material of phase change latent heat is typically 110J / g, imported products latent heat is 151.6J / g, thus resulting microencapsulation using the present methods with latent heat value change material prepared microencapsulated prior art phase change material has a largely improved compared. 具体实施方式[0014] 实施例1[0015] 一种高相变潜热值微胶囊化相变材料的制备方法,包含以下步骤:[0016] I)制备赤藓糖醇溶液:取Sg的赤藓糖醇溶解在22g的去离子水中,再依次加入2g 的二亚乙基三胺、0.05g的聚山梨酯-80和0.1g的斯盘-80,搅拌均匀后制得赤藓糖醇溶液,备用;[0017] 2)将Ig的甲苯二异氰酸酯溶解在17g的液体石蜡油中,制得甲苯二异氰酸酯溶液,备用;[0018] 3)将步骤I中制得的赤藓糖醇溶液在500rpm的搅拌速度下,以10g/min的滴加速度均匀滴加到50g的液体石蜡油中,滴加完毕后再持续搅拌0.5-1.5h制成油包水型乳液, 备用;[0019] 4)将步骤2中的甲苯二异氰酸酯溶液在50°C、1000rpm的搅拌速度下,以0.5g/min 的滴加速度均匀滴加到步骤3中的油包水型乳液中,备用;[0020] 5)将步骤4中的混合物升温至60°C,持续反应lh,然后过滤,过滤后的溶质用蒸馏水洗涤,再放入 DESCRIPTION OF EMBODIMENTS [0014] Example 1 [0015] A method of preparing high phase transition material microencapsulated latent heat of phase change, comprising the steps of: [0016] I) Preparation of erythritol solution: Take Sg erythritol sugar alcohols is dissolved in 22g of deionized water, and then were added 2g of diethylene triamine, 0.05 g of the polysorbate-80 and 0.1g of Span -80, stir to obtain a solution of erythritol, alternate; [0017] 2) the Ig-tolylene diisocyanate was dissolved in 17g of liquid paraffin oil, prepared tolylene diisocyanate solution, standby; [0018] 3) step I prepared in erythritol solution 500rpm the stirring rate at 10g / min acceleration drops uniformly dropwise added 50g of liquid paraffin oil, the addition was complete stirring was continued 0.5-1.5h then made water-in-oil emulsion, the standby; [0019] 4) toluene diisocyanate solution in step 2 at 50 ° C, under 1000rpm stirring speed to 0.5g / dropping rate min uniformly dropwise added in step 3 water in oil type emulsion, the standby; [0020] 5) step 4 the mixture is warmed to 60 ° C, the reaction was continued LH, then filtered, washed with distilled water filtered solute, and then into 空烘箱中,在80°C的温度下烘干,获得粒径在30-50微米的产品。 Air oven at drying temperature to 80 ° C, the product is obtained in the particle size of 30-50 microns. [0021] 将得到的产品使用美国PE公司的差示扫描量热仪,在升温速率10°C /min的条件下测得本产品的相变潜热值为231.2J/g,远高于现有进口产品的151.6J/g和国产产品的110.0J/g。 [0021] The products obtained using the US company PE differential scanning calorimeter, as measured under the conditions of heating rate 10 ° C / min according to the latent heat of the product is 231.2J / g, much higher than conventional imported products 151.6J / g and domestic products 110.0J / g. [0022] 实施例2[0023] 一种高相变潜热值微胶囊化相变材料的制备方法,包含以下步骤:[0024] I)制备赤藓糖醇溶液:取Ilg的赤藓糖醇溶解在19g的去离子水中,再依次加入2g的二亚乙基三胺、0.05g的聚山梨酯-80和0.1g的斯盘-80,搅拌均匀后制得赤藓糖醇溶液,备用;[0025] 2)将5g的二苯甲烷二异氰酸酯溶解在13g的液体石蜡油中,制得二苯甲烷二异氰Ife酷溶液,备用;[0026] 3)将步骤I中制得的赤藓糖醇溶液在1500rpm的搅拌速度下,以10g/min的滴加速度均匀滴加到50g的液体石蜡油中,滴加完毕后再持续搅拌0.5-1.5h制成油包水型乳液,备用;[0027] 4)将步骤2中的二苯甲烷二异氰酸酯溶液在50°C、1000rpm的搅拌速度下,以0.5g/min的滴加速度均匀滴加`到步骤3中的油包水型乳液中,备用;[0028] 5)将步骤4中的混合物升温至60°C,持续反应lh,然后过滤,过滤后的溶质用蒸馏水洗涤,再放入 [0022] Example 2 [0023] A method of preparing high phase transition material microencapsulated latent heat of phase change, comprising the steps of: [0024] I) Preparation of erythritol solution: Take Ilg dissolution of erythritol in 19g deionized water, and then were added 2g of diethylene triamine, 0.05 g of the polysorbate-80 and 0.1g of Span -80, stir to obtain a solution of erythritol, standby; [ 0025] 2) the diphenylmethane 5g of diisocyanate was dissolved in 13g of liquid paraffin oil, prepared diphenylmethane diisocyanate Ife cool solution, standby; [0026] 3) step I prepared in erythritol alcohol solution at a stirring rate of 1500rpm to 10g / min acceleration drops uniformly dropwise added 50g of liquid paraffin oil, the addition was complete stirring was continued 0.5-1.5h then made water-in-oil emulsion, the standby; [0027 ] 4) in step 2 of diphenylmethane diisocyanate solution was 50 ° C, the stirring speed 1000rpm, to 0.5g / min in dropping rate `uniformly dropwise to step 3 water-in-oil emulsion, the standby ; [0028] 5) step 4 the mixture was warmed to 60 ° C, the reaction was continued LH, then filtered, the solute after filtration washing with distilled water and then placed 真空烘箱中,在80°C的温度下烘干,获得粒径在5-20微米的产品。 A vacuum oven at the drying temperature to 80 ° C, the product obtained in the 5-20 micron particle size. [0029] 将得到的产品使用美国PE公司的差示扫描量热仪,在升温速率10°C /min的条件下测得本产品的相变潜热值为237.lj/g,远高于现有进口产品的151.6J/g和国产产品的110.0J/g。 [0029] The products obtained using the US company PE differential scanning calorimeter, as measured under the conditions of heating rate 10 ° C / min according to the product value of latent heat 237.lj / g, much higher than the current imported products 151.6J / g and domestic products 110.0J / g. [0030] 实施例3[0031] 一种高相变潜热值微胶囊化相变材料的制备方法,包含以下步骤:[0032] I)制备赤藓糖醇溶液:取15g的赤藓糖醇溶解在13g的去离子水中,再依次加入2g的二亚乙基三胺、0.05g的聚山梨酯-80和0.1g的斯盘-80,搅拌均匀后制得赤藓糖醇溶液,备用;[0033] 2)将8g的三苯甲烷三异氰酸酯溶解在12g的液体石蜡油中,制得三苯甲烷三异氰Ife酷溶液,备用;[0034] 3)将步骤I中制得的赤藓糖醇溶液在3000rpm的搅拌速度下,以10g/min的滴加速度均匀滴加到50g的液体石蜡油中,滴加完毕后再持续搅拌0.5-1.5h制成油包水型乳液,备用;[0035] 4)将步骤2中的三苯甲烷三异氰酸酯溶液在50°C、1000rpm的搅拌速度下,以0.5g/min的滴加速度均匀滴加到步骤3中的油包水型乳液中,备用;[0036] 5)将步骤4中的混合物升温至60°C,持续反应lh,然后过滤,过滤后的溶质用蒸馏水洗涤,再放入 [0030] Example 3 [0031] A method for preparing high phase transition microencapsulated latent heat of the phase change material, comprising the steps of: [0032] I) Preparation of erythritol solution: Take 15g of erythritol dissolved in 13g deionized water, and then were added 2g of diethylene triamine, 0.05 g of the polysorbate-80 and 0.1g of Span -80, stir to obtain a solution of erythritol, standby; [ 0033] 2) triphenylmethane 8g triisocyanates ester was dissolved in 12g of liquid paraffin oil, prepared triphenylmethane isocyanurate Ife cool solution, standby; [0034] 3) a step of erythritol I prepared in alcohol solution at 3000rpm stirring speed to 10g / min acceleration drops uniformly dropwise added 50g of liquid paraffin oil, the addition was complete stirring was continued 0.5-1.5h then made water-in-oil emulsion, the standby; [0035 oil 3] 4) in the step 2 triphenylmethane triisocyanate solution at 50 ° C, the stirring speed 1000rpm, to 0.5g / min in dropping rate uniformly dropwise added water type emulsion of the step, the backup; [0036] 5) step 4 the mixture was warmed to 60 ° C, the reaction was continued LH, then filtered, the solute was filtered washed with distilled water, then add 空烘箱中,在80°C的温度下烘干,获得粒径在0.1-5微米的产品。 Air oven at drying temperature to 80 ° C, the product is obtained in the particle size of 0.1 to 5 microns. [0037] 将得到的产品使用美国PE公司的差示扫描量热仪,在升温速率10°C /min的条件下测得本产品的相变潜热值为238.0J/g,远高于现有进口产品的151.6J/g和国产产品的110.0J/g。 [0037] The products obtained using the US company PE differential scanning calorimeter, as measured under the conditions of heating rate 10 ° C / min according to the latent heat of the product is 238.0J / g, much higher than conventional imported products 151.6J / g and domestic products 110.0J / g.

Claims (1)

1.一种高相变潜热值微胶囊化相变材料的制备方法,其特征在于,包含以下步骤:1)制备赤藓糖醇溶液:按重量比取8-15份的赤藓糖醇溶解在16-30份的去离子水中, 再依次加入1-5份的二亚乙基三胺、0.01-1份的聚山梨酯-80和0.05-2份的斯盘-80,搅拌均匀后制得赤藓糖醇溶液,备用;2)将1-8份的异氰酸酯溶解在12-17份的液体石蜡油中,制得异氰酸酯溶液,备用;3)将步骤I中制得的赤藓糖醇溶液在500-5000rpm的搅拌速度下,以10g/min的滴加速度均匀滴加到40-60份的液体石蜡油中,滴加完毕后再持续搅拌0.5-1.5h制成油包水型乳液,备用;4)将步骤2中的异氰酸酯溶液在50-60°C、1000rpm的搅拌速度下,以0.5g/min的滴加速度均匀滴加到步骤3中的油包水型乳液中,备用;5)使步骤4中的混合物在60°C的条件下持续反应lh,然后过滤,过滤后的固体物用蒸馏水洗涤,再放入真空烘箱中干燥 A high phase transition latent heat microencapsulated phase change material preparation process, characterized in that it comprises the following steps: 1) preparing a solution of erythritol by weight: 8-15 parts by taking the ratio of erythritol dissolved in 16-30 parts of deionized water, and then were added 5 parts of diethylene triamine, 0.01 parts of polysorbate-80 and 0.05 parts Span 80, manufactured by stir obtained erythritol solution standby; 2) 1-8 parts isocyanate was dissolved in 12-17 parts of liquid paraffin oil, to obtain an isocyanate solution, standby; 3) step I prepared in erythritol 500-5000rpm solution at a stirring rate of at 10g / min acceleration drops uniformly dropwise added 40-60 parts of a liquid paraffin oil, after the addition was complete stirring was continued 0.5-1.5h made of water-in-oil emulsion, alternate; 4) an isocyanate solution in step 2 50-60 ° C, the stirring speed 1000rpm, to 0.5g / min in dropping rate in step 3 was added dropwise to a uniform water in oil type emulsion, the standby; 5 ) in step 4 lh the reaction mixture was continued under conditions of 60 ° C, then filtered, the filtered solids were washed with distilled water, and then dried in a vacuum oven ,获得产品。 To obtain the product.
CN 201110380869 2011-11-25 2011-11-25 Preparation method of microencapsulated phase change material with high phase change latent heat value CN102492397B (en)

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