CN116376343A - 一种高光谱涂料用包水微胶囊 - Google Patents
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Abstract
本发明公开了一种高光谱涂料用包水微胶囊,主要由壁材和芯材组成,壁材为脲醛树脂,芯材包括水、油溶性物质和乳化剂,制备方法包括以下步骤:将脲醛预聚体加入到水中,得O/W乳化液;将油溶性物质、消泡剂、乳化剂A以及水混合,得W/O乳化液;将W/O乳化液以及乳化剂B加入到O/W乳化液中,搅拌,形成W/O/W乳化液,搅拌,得微胶囊悬浮液;将冷却至室温的悬浮液,离心,干燥,即得。本发明采用原位聚合法制备包水微胶囊的技术,工艺简单、参数易控、微胶囊粒径可调,可以解决传统高光谱涂料不含水分或保水能力差,对植被背景中水份特征光谱吸收峰的模拟效果差、有效期短等技术难题,提高高光谱涂料的伪装能力。
Description
技术领域
本发明属于微胶囊技术领域,尤其涉及一种高光谱涂料用包水微胶囊。
背景技术
光学伪装高光谱涂料是军事侦察领域对抗敌方,提高己方战场生存能力的重要手段之一。高光谱成像探测技术在军事领域的迅速发展和应用,使军事伪装技术面临巨大挑战,对光学伪装高光谱涂料也提出了更高的要求。植被是伪装目标所处的常见背景之一,伪装高光谱涂料必须具有与植被近似的颜色,并且水分含量高,保水能力强,才能实现与绿色植被背景“同色同谱”,从而有效对抗新型高光谱成像探测技术。因此,如何提高伪装高光谱涂料的含水量及保水能力,是提高其对抗高光谱成像探测技术能力的关键技术之一。
发明内容
基于此,本发明提供了一种高光谱涂料用包水微胶囊,可将所制备的微胶囊以填料的方式对已实现工程应用的涂料进行改性,提升高光谱涂层中水份的特征吸收峰(970nm,1190nm,1430nm,1930nm)匹配性,实现与绿色植被背景的“同色同谱”,提高伪装高光谱涂料的反侦察能力。
为解决此技术问题,本发明的技术方案是:采用原位聚合法制备包水脲醛微胶囊,先在碱性条件下制备水溶性壁材预聚体,之后将芯材乳化液分散于预聚体水溶液中,在酸性条件下预聚体进一步聚合并在芯材表面沉积,最终将芯材包覆形成微胶囊。
具体地,本发明的技术方法如下:
一种高光谱涂料用包水微胶囊,主要由壁材和芯材组成,壁材为脲醛树脂,芯材包括水、油溶性物质和乳化剂,制备方法包括以下步骤:a)将脲醛预聚体加入到水中,得O/W乳化液;b)将油溶性物质、消泡剂、乳化剂A以及水混合,得W/O乳化液;c)将W/O乳化液以及乳化剂B加入到O/W乳化液中,搅拌,形成W/O/W乳化液,加入调酸剂调节体系pH值为1.5-3,升温至60-70℃,搅拌至完成胶囊化,加入调碱剂A至体系pH至6-7,得微胶囊悬浮液;d)将冷却至室温的悬浮液,离心,干燥,即得高光谱涂料用包水微胶囊。
优选地,制备方法包括以下步骤:
a)将尿素、甲醛按摩尔比1:1~1:4混合,采用调碱剂B调节体系pH值为8~9.5,升温至60~90℃,搅拌反应1.5h,得脲醛预聚体,再加入脲醛预聚体1~3倍体积的水搅拌冷却至室温,形成O/W乳化液;
b)将按重量份计的3~5份的油溶性物质和0.01~0.5份消泡剂混合均匀,再加入0.1~1.5份HLB值为3~6的乳化剂A搅拌均匀,加入水,搅拌速率为3000~12000rpm的条件下,搅拌10~15min形成W/O乳化液;
c)将W/O乳化液和按重量份计的0.01~0.5份HLB值为8~18的乳化剂B加入到O/W乳化液中,搅拌速率为3000~12000rpm的条件下,搅拌10~15min形成W/O/W乳化液;采用调酸剂溶液调节体系pH值为1.5~3,缓慢升温至60~70℃,搅拌反应2~4h完成胶囊化过程,加入调碱剂A将体系pH值调至6~7,得到微胶囊悬浮液;
d)将微胶囊悬浮液冷却至室温,离心,洗涤,干燥,即得高光谱涂料用包水微胶囊。
优选地,油溶性物质选自甲苯、庚烷、液体石蜡、二氯甲烷、三氯甲烷、四氯化碳、四氯乙烯、乙酸乙酯、环己烷和石油醚中的任意一种或多种。
优选地,乳化剂A选自脂肪酸失水山梨醇酯、脂肪酸二乙醇酰胺、烷基单甘油醚、烷基聚葡糖苷、烷基糖酐、聚乙二醇和聚氧乙烯二醇中的任意一种。
优选地,乳化剂B选自三乙醇胺油酸酯、失水山梨醇单月桂酸酯、吐温20、吐温21、吐温40、吐温60、吐温65、吐温80、吐温81和吐温85中的任意一种或多种。
优选地,调酸剂为HCl溶液或NH4Cl溶液。
优选地,消泡剂选自戊醇、二异丁基甲醇、辛醇、丙二醇、甲醇、乙醇、异丙醇、正丁醇或正辛醇中的任意一种或多种。
优选地,调碱剂A以及调碱剂B相互独立地选自NaOH溶液、碳酸钠溶液或三乙醇胺中的任意一种或多种。
通过采用上述技术方案,本发明的有益效果是:
本发明采用操作简单的原位聚合法制备包水微胶囊的技术,使其制备的微胶囊满足尺寸小、稳定性强、不易渗漏,与涂料加工工艺相适应的要求;此制备工艺简单,工艺参数易控制,微胶囊尺寸可控;此工艺制备的微胶囊具有较高的包覆率和芯材含量,包覆率可达82~92%,芯材含量可达50~70%;此工艺制备的微胶囊用于伪装高光谱涂料,可以解决传统高光谱涂料不含水分或保水能力差,对植被背景中水分特征光谱吸收峰(970nm,1190nm,1430nm,1930nm)的模拟效果差、有效期短等技术难题,提高高光谱涂料的伪装能力。
说明书附图
图1为实施例1-3提供的包水微胶囊与对照例的反射光谱曲线。
具体实施方式
为了进一步解释本发明的技术方案,下面结合具体实施例来对本发明进行详细阐述。
在下述实施例中,除另有说明外,各个原料均为市售产品。
实施例1
本实施例提供了一种高光谱涂料用包水微胶囊,其制备方法如下:
a)将尿素4.0g、甲醛溶液(37%)10.8g加入到容器中搅拌,采用三乙醇胺调节体系pH值为8.5,缓慢升温至70℃,水浴恒温搅拌反应1.5h,得透明粘稠的可溶性脲醛预聚体,再加入其2倍体积的水搅拌冷却至室温,形成O/W乳化液,其中,壁材原料为尿素和甲醛;
b)首先将四氯乙烯6.0g和正辛醇0.5g混合均匀,再加入1.5g乳化剂脂肪酸失水山梨醇酯Span 80搅拌均匀,加入芯材去离子水20.0g,均质机在搅拌速率为3000rpm的条件下,搅拌10min形成W/O乳化液;
c)将步骤b)得到的W/O乳化液和0.3g乳化剂吐温80加入到步骤a)制备的预聚体溶液中,搅拌速率为5000rpm的条件下,搅拌10min形成W/O/W乳化液;采用HCl溶液调节体系pH值为2.0,缓慢升温至70℃,搅拌反应2.5h完成微胶囊的胶囊化过程,最后通过加入NaOH溶液将体系pH值调至6~7,得到包水微胶囊的悬浮液;
d)将步骤c)得到的悬浮液自然冷却至室温,经离心、去离子水洗涤,在50℃条件下干燥24h,即得包水微胶囊。
实施例2
本实施例提供了一种高光谱涂料用包水微胶囊,其制备方法如下:
a)将尿素4.0g、甲醛溶液(37%)5.4g加入到容器中搅拌,采用三乙醇胺调节体系pH值为9,缓慢升温至80℃,水浴恒温搅拌反应1.5h,得透明粘稠的可溶性脲醛预聚体,再加入其2倍体积的水搅拌冷却至室温,形成O/W乳化液;其中,壁材原料为尿素和甲醛;
b)首先将环己烷7.5g和正辛醇0.5g混合均匀,再加入1.8g乳化剂脂肪酸失水山梨醇酯Span 80搅拌均匀,加入芯材去离子水18.0g,均质机在搅拌速率为6000rpm的条件下,搅拌10min形成W/O乳化液;
c)将步骤b)得到的W/O乳化液和0.5g乳化剂吐温80加入到步骤a)制备的预聚体溶液中,搅拌速率为10000rpm的条件下,搅拌10min形成W/O/W乳化液;采用HCl溶液调节体系pH值为1.5,缓慢升温至70℃,搅拌反应2.5h完成微胶囊的胶囊化过程,最后通过加入NaOH溶液将体系pH值调至6~7,得到包水微胶囊的悬浮液;
d)将步骤c)得到的悬浮液自然冷却至室温,经离心、去离子水洗涤,在50℃条件下干燥24h,即得包水微胶囊产品。
实施例3
本实施例提供了一种高光谱涂料用包水微胶囊,其制备方法如下:
a)将尿素4.0g、甲醛溶液(37%)8.1g加入到容器中搅拌,采用三乙醇胺调节体系pH值为8.5,缓慢升温至70℃,水浴恒温搅拌反应1.5h,得透明粘稠的可溶性脲醛预聚体,再加入其2倍体积的水搅拌冷却至室温,形成O/W乳化液;其中,壁材原料为尿素和甲醛;
b)首先将石油醚9.0g和正辛醇0.5g混合均匀,再加入2.0g乳化剂脂肪酸失水山梨醇酯Span 80搅拌均匀,加入芯材去离子水30.0g,均质机在搅拌速率为10000rpm的条件下,搅拌10min形成W/O乳化液;
c)将步骤b)得到的W/O乳化液和1.0g乳化剂吐温80加入到步骤a)制备的预聚体溶液中,搅拌速率为12000rpm的条件下,搅拌10min形成W/O/W乳化液;采用HCl溶液调节体系pH值为2.5,缓慢升温至70℃,搅拌反应3h完成微胶囊的胶囊化过程,最后通过加入NaOH溶液将体系pH值调至6~7,得到包水微胶囊的悬浮液;
d)将步骤c)得到的悬浮液自然冷却至室温,经离心、去离子水洗涤,在50℃条件下干燥24h,即得包水微胶囊产品。
对照例
新鲜采摘的常绿灌木黄杨叶片。
测试例1
利用光学显微镜测量分析,实施例1-3所制得的包水微胶囊的平均粒径分别为30μm、15μm和25μm。
测试例2
紫外分光光度计
对实施例1-3提供的包水微胶囊材料与对照例中的叶片,通过紫外分光光度计测试反射光谱曲线,测试范围200nm-2500nm,测试速率120nm/min,测试结果如图1所示。
由图1可知,实施例1-3制备的包水微胶囊的反射光谱曲线在“水峰”位置(970nm,1190nm,1430nm,1930nm)具有明显吸收,具备明显的含水、保水能力,可以解决传统高光谱涂料不含水分或保水能力差,对绿色植被背景中水分特征光谱吸收峰模拟效果差、有效期短等技术难题,有效提高了高光谱涂料的伪装能力。
Claims (8)
1.一种高光谱涂料用包水微胶囊,主要由壁材和芯材组成,其特征在于,所述壁材为脲醛树脂,所述芯材包括水、油溶性物质和乳化剂,
制备方法包括以下步骤:
a)将脲醛预聚体加入到水中,得O/W乳化液;
b)将油溶性物质、消泡剂、乳化剂A以及水混合,得W/O乳化液;
c)将所述W/O乳化液以及乳化剂B加入到所述O/W乳化液中,搅拌,形成W/O/W乳化液,加入调酸剂调节体系pH值为1.5-3,升温至60-70℃,搅拌至完成胶囊化,加入调碱剂A至体系pH至6-7,得微胶囊悬浮液;
d)将冷却至室温的悬浮液,离心,干燥,即得高光谱涂料用包水微胶囊。
2.根据权利要求1所述的高光谱涂料用包水微胶囊,其特征在于,制备方法包括以下步骤:
a)将尿素、甲醛按摩尔比1:1~1:4混合,采用调碱剂B调节体系pH值为8~9.5,升温至60~90℃,搅拌反应1.5h,得脲醛预聚体,再加入所述脲醛预聚体1~3倍体积的水搅拌冷却至室温,形成O/W乳化液;
b)将按重量份计的3~5份的油溶性物质和0.01~0.5份消泡剂混合均匀,再加入0.1~1.5份HLB值为3~6的乳化剂A搅拌均匀,加入水,搅拌速率为3000~12000rpm的条件下,搅拌10~15min形成W/O乳化液;
c)将所述W/O乳化液和0.01~0.5份HLB值为8~18的乳化剂B加入到所述O/W乳化液中,搅拌速率为3000~12000rpm的条件下,搅拌10~15min形成W/O/W乳化液;采用调酸剂溶液调节体系pH值为1.5~3,缓慢升温至60~70℃,搅拌反应2~4h完成胶囊化过程,加入调碱剂A将体系pH值调至6~7,得到微胶囊悬浮液;
d)将所述微胶囊悬浮液冷却至室温,离心,洗涤,干燥,即得高光谱涂料用包水微胶囊。
3.根据权利要求1或2所述的高光谱涂料用包水微胶囊,其特征在于,所述油溶性物质选自甲苯、庚烷、液体石蜡、二氯甲烷、三氯甲烷、四氯化碳、四氯乙烯、乙酸乙酯、环己烷和石油醚中的任意一种或多种。
4.根据权利要求1或2所述的高光谱涂料用包水微胶囊,其特征在于,所述乳化剂A选自脂肪酸失水山梨醇酯、脂肪酸二乙醇酰胺、烷基单甘油醚、烷基聚葡糖苷、烷基糖酐、聚乙二醇和聚氧乙烯二醇中的任意一种。
5.根据权利要求1或2所述的高光谱涂料用包水微胶囊,其特征在于,所述乳化剂B选自三乙醇胺油酸酯、失水山梨醇单月桂酸酯、吐温20、吐温21、吐温40、吐温60、吐温65、吐温80、吐温81和吐温85中的任意一种或多种。
6.根据权利要求1或2所述的高光谱涂料用包水微胶囊,其特征在于,所述调酸剂为HCl溶液或NH4Cl溶液。
7.根据权利要求1或2所述的高光谱涂料用包水微胶囊,其特征在于,所述消泡剂选自戊醇、二异丁基甲醇、辛醇、丙二醇、甲醇、乙醇、异丙醇、正丁醇或正辛醇中的任意一种或多种。
8.根据权利要求2所述的高光谱涂料用包水微胶囊,其特征在于,所述调碱剂A以及所述调碱剂B相互独立地选自NaOH溶液、碳酸钠溶液或三乙醇胺中的任意一种或多种。
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