CN109077288A - 一种焦香香精的制备方法 - Google Patents
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Abstract
本发明涉及一种焦香香精的制备方法,该制备方法将热反应与渗透汽化过程进行结合,并通过工艺创新实现了制备无色透明、强度高、稳定性好的焦香香精,解决了传统焦香香精产品颜色深、储藏稳定性差等问题,本发明得到的焦香香精适用性广,可用于日化、烟草和食品行业。
Description
技术领域
本发明涉及精细化工领域,特别涉及一种焦香香精的制备方法。
背景技术
焦香是一种生活中常见的香气,无论是烟草还是食品饮料,甚至是化妆品中都存有焦香的香气香味。焦香香精可通过单体原料调配,如甲基环戊烯醇酮、麦芽酚、乙基麦芽酚、呋喃酮等香原料均带有焦甜的属性,可用于调配焦香香精,但人工调配的香精缺少自然属性,化学气重,协调性差。焦香香精也可通过热反应技术进行制备,但传统热反应技术制备的焦香香精均呈黑褐色,而且由于反应不完全,产品稳定性差,在储藏过程中会继续反应,生成大分子的类黑素等,影响产品品质,而且传统热反应制备得到的焦香香精香气强度低,常需要进行进一步的人工修饰才能使用,如CN103704659A公开的一种焦香香精,是在焦糖反应香精的基础上,添加人工合成的香料进一步调配才得到。
发明内容
为克服现有技术的不足,本发明的目的在于提供一种焦香香精的制备方法,该制备方法包括以下步骤:
(1)将甘蔗浓缩汁、复合氨基酸、还原糖和水加入反应釜中,升温至85-95℃进行密闭反应2-8h;所述的甘蔗浓缩汁、复合氨基酸、还原糖和水按1:0.1-0.5:0.2-0.8:2-5的质量比添加;所述的复合氨基酸为L-脯氨酸、L-丙氨酸、L-甘氨酸、L-谷氨酸复配而成,优选L-脯氨酸、L-丙氨酸、L-甘氨酸、L-谷氨酸按1:2:1:1的质量比复配;所述的还原糖为异麦芽酮糖、果葡糖浆或半乳糖,优选异麦芽酮糖;
(2)开启真空泵,调节三通控制阀,使反应釜、冷凝器、缓存罐、渗透汽化设备、U型管和回流导管之间形成循环回路,提高反应温度至反应釜中反应料液沸腾,使蒸汽从反应釜出,经过冷凝器冷凝后进入缓存罐,恒流泵将冷凝液泵入渗透汽化设备进行渗透汽化,再依次流经U型管、回流导管最后返回反应釜中,同步进行热反应和渗透汽化过程,从料液沸腾开始计时,维持2-4h;
(3)降低反应温度至60-80℃,调节三通控制阀,关闭步骤(2)的循环回路,使反应釜、渗透体化设备、冷凝器、U型管和回流导管相通,形成新的循环回路,然后泵入食用酒精至反应釜中,蒸汽从反应釜出,经过渗透汽化设备进行渗透汽化,再经过冷凝器冷凝,依次流经U型管、回流导管最后返回反应釜中,至料液不再沸腾,关闭真空泵,停止反应和渗透汽化,取冷阱中的收集的渗透液即为焦香香精;所述的食用酒精的添加量为反应料液质量的5-10%。
所述的硅橡胶复合膜按照以下方法制备:
a、制备铸膜液:取聚二甲基硅氧烷溶于正己烷中,搅拌均匀后加入碳分子筛,超声分散,然后加入二乙烯基苯,二月桂酸二丁基锡,继续搅拌,混合均匀后,离心脱泡制成铸膜液;所述聚二甲基硅氧烷在铸膜液中的浓度为20-40wt%,聚二甲基硅氧烷与二乙烯基苯的质量比为1:0.25-0.5,聚二甲基硅氧烷与二月桂酸二丁基锡的质量比为1:0.005-0.05,聚二甲基硅氧烷与碳分子筛的质量比为1:0.05-0.2,碳分子筛比表面积≥150m2g-1、粒径≤8μm;
b、制备渗透汽化膜:将步骤a的铸膜液倒在聚偏氟乙烯底膜上刮膜,常温晾干,然后放入烘箱内进行交联和老化,制得渗透汽化膜;控制渗透汽化膜的分离层厚度为100-110μm。
本发明的焦香香精的制备方法具有以下优势。
(1)通过本发明制备得到的焦香香精呈无色透明状,水溶性好,避免了传统热反应香精的呈现黑褐色的问题,在应用时对应用产品状态无影响,故应用范围广,适用于日化、烟草和各类型食品。
(2)通过本发明制备得到的焦香香精,无残留的氨基酸和还原糖,储存过程中不会继续发生美拉德反应,产品在香气和体系两个方面均稳定。
(3)本发明的制备方法中,在同步热反应和渗透汽化过程中,通过添加食用酒精并切换循环回路,能够促进中后段口感物质透过渗透汽化膜,并在冷阱中得到富集,使香气强度得到显著增强,而且留香持久,无需进行额外的人工调香修饰,即可应用。
(4)本发明通过使用特殊的填充有特定规格的碳分子筛的特殊渗透汽化膜,能够选择性的分离焦香的香气香味成分,得到的焦香香精香气真实。
(5)本发明的还原糖优选使用异麦芽酮糖,能够使制备得到的焦香香精在中段突出,圆润,有效防止头香太冒的问题,香精品质高。
附图说明
下面结合附图对本发明的具体实施方式作进一步详细说明。
图1 是实施例1-4焦香香精制备装置示意图,图中标记的含义如下:
1反应釜;2酒精储罐;3冷凝器;4缓存罐;5渗透汽化设备;6冷阱;7真空泵;8冷凝器;9U型管;10回流导管。
具体实施方式
以下结合具体实例对本发明的技术方案做进一步的说明。
实施例1
按以下步骤制备渗透汽化膜:
a、制备铸膜液:取100g聚二甲基硅氧烷溶于正己烷中,搅拌均匀后加入20g碳分子筛(比表面积172.4m2g-1,粒径5.6μm),超声分散,然后加入30g二乙烯基苯,3g二月桂酸二丁基锡,继续搅拌,混合均匀后,离心脱泡制成铸膜液;控制聚二甲基硅氧烷在铸膜液中的浓度为25wt%;
b、制备渗透汽化膜:将步骤a的铸膜液倒在聚偏氟乙烯底膜上刮膜,常温晾干,然后放入烘箱内于90℃进行交联和老化,制得分离层厚度为103μm的渗透汽化膜。
实施例2
以实施例1的渗透汽化膜进行渗透汽化,焦香香精按以下方法制备:
(1)将10kg甘蔗浓缩汁、1kg复合氨基酸、2kg异麦芽酮糖和20kg水加入反应釜中,升温至85℃进行密闭反应8h;复合氨基酸为L-脯氨酸、L-丙氨酸、L-甘氨酸、L-谷氨酸按1:2:1:1的质量比复配得到;
(2)开启真空泵,调节三通控制阀,使反应釜、冷凝器、缓存罐、渗透汽化设备、U型管和回流导管之间形成循环回路,提高反应温度至反应釜中反应料液沸腾,使蒸汽从反应釜出,经过冷凝器冷凝后进入缓存罐,恒流泵将冷凝液泵入渗透汽化设备进行渗透汽化,再依次流经U型管、回流导管最后返回反应釜中,同步进行热反应和渗透汽化过程,从料液沸腾开始计时,维持4h;
(3)降低反应温度至80℃,调节三通控制阀,关闭步骤(2)的循环回路,使反应釜、渗透体化设备、冷凝器、U型管和回流导管相通,形成新的循环回路,然后泵入3.3kg浓度95wt%的食用酒精至反应釜中,蒸汽从反应釜出,经过渗透汽化设备进行渗透汽化,再经过冷凝器冷凝,依次流经U型管、回流导管最后返回反应釜中,至料液不再沸腾,关闭真空泵,停止反应和渗透汽化,取冷阱中的收集的渗透液即为焦香香精。
本实施例的焦香香精以0.06wt‰添加至烟丝中能够明显改进卷烟的吸味,赋予令人愉快的蜜甜香,木香和烤香。
实施例3
以实施例1的渗透汽化膜进行渗透汽化,焦香香精按以下方法制备:
(1)将10kg甘蔗浓缩汁、5kg复合氨基酸、8kg半乳糖和50kg水加入反应釜中,升温至95℃进行密闭反应2h;所述的复合氨基酸为L-脯氨酸、L-丙氨酸、L-甘氨酸、L-谷氨酸按1:1:2:1的质量比复配;
(2)开启真空泵,调节三通控制阀,使反应釜、冷凝器、缓存罐、渗透汽化设备、U型管和回流导管之间形成循环回路,提高反应温度至反应釜中反应料液沸腾,使蒸汽从反应釜出,经过冷凝器冷凝后进入缓存罐,恒流泵将冷凝液泵入渗透汽化设备进行渗透汽化,再依次流经U型管、回流导管最后返回反应釜中,同步进行热反应和渗透汽化过程,从料液沸腾开始计时,维持2h;
(3)降低反应温度至60℃,调节三通控制阀,关闭步骤(2)的循环回路,使反应釜、渗透体化设备、冷凝器、U型管和回流导管相通,形成新的循环回路,然后泵入3.65kg浓度为95wt%的食用酒精至反应釜中,
蒸汽从反应釜出,经过渗透汽化设备进行渗透汽化,再经过冷凝器冷凝,依次流经U型管、回流导管最后返回反应釜中,至料液不再沸腾,关闭真空泵,停止反应和渗透汽化,取冷阱中的收集的渗透液即为焦香香精。
实施例4
作为对比,以实施例3的原料在同样的反应温度和反应时间条件下进行热反应,但不进行渗透汽化步骤,最终反应釜中的反应产物为焦香香精,状态为黑褐色。
实施例2-4得到的焦香香精对比如下表所示,通过传统热反应技术得到的焦香香精(实施例4)在风味和稳定性方面明显劣于本发明方法制备得到的焦香香精(实施例2-3)。
Claims (5)
1.一种焦香香精的制备方法,其特征在于包括以下步骤:
(1)将甘蔗浓缩汁、复合氨基酸、还原糖和水加入反应釜中,升温至85-95℃进行密闭反应2-8h;所述的复合氨基酸为L-脯氨酸、L-丙氨酸、L-甘氨酸、L-谷氨酸复配而成,优选L-脯氨酸、L-丙氨酸、L-甘氨酸、L-谷氨酸按1:2:1:1的质量比复配;
(2)开启真空泵,调节三通控制阀,使反应釜、冷凝器、缓存罐、渗透汽化设备、U型管和回流导管之间形成循环回路,提高反应温度至反应釜中反应料液沸腾,使蒸汽从反应釜出,经过冷凝器冷凝后进入缓存罐,恒流泵将冷凝液泵入渗透汽化设备进行渗透汽化,再依次流经U型管、回流导管最后返回反应釜中,同步进行热反应和渗透汽化过程,从料液沸腾开始计时,维持2-4h;
(3)降低反应温度至60-80℃,调节三通控制阀,关闭步骤(2)的循环回路,使反应釜、渗透体化设备、冷凝器、U型管和回流导管相通,形成新的循环回路,然后泵入食用酒精至反应釜中,蒸汽从反应釜出,经过渗透汽化设备进行渗透汽化,再经过冷凝器冷凝,依次流经U型管、回流导管最后返回反应釜中,至料液不再沸腾,关闭真空泵,停止反应和渗透汽化,取冷阱中的收集的渗透液即为焦香香精;
所述的渗透汽化设备中的渗透汽化膜为填充碳分子筛的硅橡胶复合膜。
2.根据权利要求1所述的焦香香精的制备方法,其特征在于所述的硅橡胶复合膜按照以下方法制备:
a、制备铸膜液:取聚二甲基硅氧烷溶于正己烷中,搅拌均匀后加入碳分子筛,超声分散,然后加入二乙烯基苯,二月桂酸二丁基锡,继续搅拌,混合均匀后,离心脱泡制成铸膜液;所述聚二甲基硅氧烷在铸膜液中的浓度为20-40wt%,聚二甲基硅氧烷与二乙烯基苯的质量比为1:0.25-0.5,聚二甲基硅氧烷与二月桂酸二丁基锡的质量比为1:0.005-0.05,聚二甲基硅氧烷与碳分子筛的质量比为1:0.05-0.2,碳分子筛比表面积≥150m2g-1、粒径≤8μm;
b、制备渗透汽化膜:将步骤a的铸膜液倒在聚偏氟乙烯底膜上刮膜,常温晾干,然后放入烘箱内进行交联和老化,制得渗透汽化膜;控制渗透汽化膜的分离层厚度为100-110μm。
3.根据权利要求1所述的焦香香精的制备方法,其特征在于所述的甘蔗浓缩汁、复合氨基酸、还原糖和水按1:0.1-0.5:0.2-0.8:2-5的质量比添加。
4.根据权利要求1所述的焦香香精的制备方法,其特征在于所述的还原糖为异麦芽酮糖、果葡糖浆或半乳糖,优选异麦芽酮糖。
5.根据权利要求1所述的焦香香精的制备方法,其特征在于所述的食用酒精的添加量为反应料液质量的5-10%。
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