CN111718303A - 噻苯隆的制备方法 - Google Patents
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Abstract
本发明公开了噻苯隆的制备方法,包括以下步骤:步骤一,将5‑氨基‑1,2,3‑噻二唑加入反应釜中,在持续搅拌的情况下加入乙二醇二甲醚中,并继续搅拌至完全溶解;步骤二,将溶解混合物中滴加8滴三乙胺,并升温至40℃左右;步骤三,滴加苯基异腈酸酯,每36g苯基异腈酸酯在15min左右滴加完毕,并在40℃下保温6h;步骤四,反应结束后将混合物过滤即得噻苯隆成品;所述步骤一中的反应釜包括反应釜体、转轴、支撑板、支撑柱、转动组件、搅拌组件、滴加组件、水浴夹层、进水管和出水管,该发明,5‑氨基‑1,2,3‑噻二唑在乙二醇二甲醚内溶解快速;便于调节速度和时间;通过转动组件带动反应釜体翻转,利于反应物倾倒后过滤,即得噻苯隆成品。
Description
技术领域
本发明涉及噻苯隆技术领域,具体为噻苯隆的制备方法。
背景技术
噻苯隆,是一种新型高效的细胞分裂素用于组培能更好的促进植物的芽分化。对人畜低毒,适用于棉花作脱叶剂使用。但是现有的噻苯隆在制备过程中原料溶解速度不都快,时间成本高,且滴加速度时间不好控制,由此导致噻苯隆的制备时间长,不利于生产。
发明内容
本发明的目的在于提供噻苯隆的制备方法,以解决上述背景技术中提出的问题。
为了解决上述技术问题,本发明提供如下技术方案:噻苯隆的制备方法,包括以下步骤:
步骤一,将5-氨基-1,2,3-噻二唑加入反应釜中,在持续搅拌的情况下加入乙二醇二甲醚中,并继续搅拌至完全溶解;
步骤二,将溶解混合物中滴加8滴三乙胺,并升温至40℃左右;
步骤三,滴加苯基异腈酸酯,每36g苯基异腈酸酯在15min左右滴加完毕,并在40℃下保温6h;
步骤四,反应结束后将混合物过滤即得噻苯隆成品。
作为本发明进一步的方案:所述步骤一中,5-氨基-1,2,3-噻二唑的质量分数为99.2%,摩尔质量为0.3mol。
作为本发明进一步的方案:所述步骤三中,苯基异腈酸酯的摩尔质量为0.3mol。
作为本发明进一步的方案:所述步骤一、二和三中,5-氨基-1,2,3-噻二唑、乙二醇二甲醚和苯基异腈酸酯的质量比为1-1.1∶10∶1.1-1.3。
作为本发明进一步的方案:所述步骤一中的反应釜包括反应釜体、转轴、支撑板、支撑柱、转动组件、搅拌组件、滴加组件、水浴夹层、进水管和出水管,所述反应釜体的两侧分别通过转轴与支撑板转动连接,且支撑板的底部两侧通过两根支撑柱竖直设置在地面上,所述反应釜体一侧的转轴贯穿支撑板与转动组件连接,且反应釜体的顶部铰接的顶盖顶部中央嵌设有搅拌组件,所述搅拌组件两侧的顶盖上还嵌入安装有滴加组件,所述反应釜体的内壁内设置有水浴夹层,且水浴夹层位于反应釜体两侧的顶部均连接有进水管,所述水浴夹层位于反应釜体最底部连接有出水管。
作为本发明进一步的方案:所述转动组件由转动壳体、气缸、齿条和齿轮组成,所述转动壳体固接在支撑板一侧,且转动壳体的底部内壁安装有气缸,所述气缸的输出端与齿条一端固接,且齿条与齿轮相啮合,所述齿轮与转轴位于转动壳体内部的一端固接。
作为本发明进一步的方案:所述搅拌组件由搅拌电机、搅拌轴、搅拌支杆和搅拌叶片组成,所述搅拌电机嵌设在反应釜体的顶部铰接的顶盖顶部中央,且搅拌电机的输出端与反应釜体内部的搅拌轴顶端固接,所述搅拌轴的底部等距离分散固接有搅拌支杆一端,且搅拌支杆具有三根,每根所述搅拌支杆的另一端均固接有搅拌叶片,且搅拌叶片底部与反应釜体底部内壁弧形相适配。
作为本发明进一步的方案:所述滴加组件由滴加壳体、支架、滴加管、调节杆、通液孔、拉手、支座、活动槽、弹簧和卡块组成,所述滴加壳体通过支架安装在反应釜体的顶部铰接的顶盖顶部,所述滴加壳体的底部与滴加管的顶端连接,且连接处插接有调节杆,所述调节杆上开设有两个通液孔,且一端固接有拉手,所述滴加管靠近拉手的一侧固接有支座,且支座顶部等距离开设有若干活动槽,所述活动槽内设置有弹簧,且弹簧顶部固接卡块,所述卡块与调节杆侧面底部的卡孔为配合构件。
与现有技术相比,本发明所达到的有益效果是:该噻苯隆的制备方法,将5-氨基-1,2,3-噻二唑加入反应釜体内,再加入乙二醇二甲醚,利用搅拌组件使5-氨基-1,2,3-噻二唑在乙二醇二甲醚内快速溶解,减少时间成本;并利用滴加组件滴加三乙胺和苯基异腈酸酯,便于调节速度和时间;通过水浴夹层和进水管将反应釜体内壁升温至40℃左右,反应结束后,通过转动组件带动反应釜体翻转,利于反应物倾倒后过滤,即得噻苯隆成品。
附图说明
附图用来提供对本发明的进一步理解,并且构成说明书的一部分,与本发明的实施例一起用于解释本发明,并不构成对本发明的限制。在附图中:
图1是本发明的工艺流程图;
图2是本发明的反应釜结构示意图;
图3是本发明的反应釜内部结构示意图;
图4是图3中A区域结构放大示意图;
图5是本发明的反应釜的转动组件结构示意图。
图中:1、反应釜体;2、转轴;3、支撑板;4、支撑柱;5、转动组件;6、搅拌组件;7、滴加组件;8、水浴夹层;9、进水管;10、出水管;51、转动壳体;52、气缸;53、齿条;54、齿轮;61、搅拌电机;62、搅拌轴;63、搅拌支杆;64、搅拌叶片;71、滴加壳体;72、支架;73、滴加管;74、调节杆;75、通液孔;76、拉手;77、支座;78、活动槽;79、弹簧;710、卡块。
具体实施方式
下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
请参阅图1-5,本发明提供一种技术方案:噻苯隆的制备方法,包括以下步骤:
步骤一,将5-氨基-1,2,3-噻二唑加入反应釜中,5-氨基-1,2,3-噻二唑的质量分数为99.2%,摩尔质量为0.3mol,在持续搅拌的情况下加入乙二醇二甲醚中,并继续搅拌至完全溶解;
步骤二,将溶解混合物中滴加8滴三乙胺,并升温至40℃左右;
步骤三,滴加苯基异腈酸酯,每36g苯基异腈酸酯在15min左右滴加完毕,并在40℃下保温6h,苯基异腈酸酯的摩尔质量为0.3mol;
步骤四,反应结束后将混合物过滤即得噻苯隆成品;
步骤一、二和三中,5-氨基-1,2,3-噻二唑、乙二醇二甲醚和苯基异腈酸酯的质量比为1-1.1∶10∶1.1-1.3;
步骤一中的反应釜包括反应釜体1、转轴2、支撑板3、支撑柱4、转动组件5、搅拌组件6、滴加组件7、水浴夹层8、进水管9和出水管10,反应釜体1的两侧分别通过转轴2与支撑板3转动连接,且支撑板3的底部两侧通过两根支撑柱4竖直设置在地面上,反应釜体1一侧的转轴2贯穿支撑板3与转动组件5连接,且反应釜体1的顶部铰接的顶盖顶部中央嵌设有搅拌组件6,搅拌组件6两侧的顶盖上还嵌入安装有滴加组件7,反应釜体1的内壁内设置有水浴夹层8,且水浴夹层8位于反应釜体1两侧的顶部均连接有进水管9,水浴夹层8位于反应釜体1最底部连接有出水管10;
转动组件5由转动壳体51、气缸52、齿条53和齿轮54组成,转动壳体51固接在支撑板3一侧,且转动壳体51的底部内壁安装有气缸52,气缸52的输出端与齿条53一端固接,且齿条53与齿轮54相啮合,齿轮54与转轴2位于转动壳体51内部的一端固接;
搅拌组件6由搅拌电机61、搅拌轴62、搅拌支杆63和搅拌叶片64组成,搅拌电机61嵌设在反应釜体1的顶部铰接的顶盖顶部中央,且搅拌电机61的输出端与反应釜体1内部的搅拌轴62顶端固接,搅拌轴62的底部等距离分散固接有搅拌支杆63一端,且搅拌支杆63具有三根,每根搅拌支杆63的另一端均固接有搅拌叶片64,且搅拌叶片64底部与反应釜体1底部内壁弧形相适配;
滴加组件7由滴加壳体71、支架72、滴加管73、调节杆74、通液孔75、拉手76、支座77、活动槽78、弹簧79和卡块710组成,滴加壳体71通过支架72安装在反应釜体1的顶部铰接的顶盖顶部,滴加壳体71的底部与滴加管73的顶端连接,且连接处插接有调节杆74,调节杆74上开设有两个通液孔75,且一端固接有拉手76,滴加管73靠近拉手76的一侧固接有支座77,且支座77顶部等距离开设有若干活动槽78,活动槽78内设置有弹簧79,且弹簧79顶部固接卡块710,卡块710与调节杆74侧面底部的卡孔为配合构件。
基于上述,本发明的优点在于:将5-氨基-1,2,3-噻二唑加入反应釜体1内,再加入乙二醇二甲醚,利用搅拌电机61带动搅拌轴62旋转,使得搅拌支杆63和搅拌叶片64将5-氨基-1,2,3-噻二唑在乙二醇二甲醚内完全溶解;并将滴加三乙胺和苯基异腈酸酯加入两个滴加壳体71中,此时调节杆74通过拉手76使得通液孔75并不位于滴加管73内,此时通过拉手76再次拉动或推动调节杆74,使得通液孔75移至滴加管73内,并通过弹簧79和卡块710将调节杆74位置固定,利用通液孔75的数目或露出面积调整滴加速度,进行三乙胺的滴加;通过水浴夹层8和进水管9将反应釜体1内壁升温至40℃左右,再次利用滴加组件7滴加苯基异腈酸酯,每36g苯基异腈酸酯在15min左右滴加完毕,并在40℃下保温6h,反应结束后,通过气缸52带动齿条53移动,使得齿轮54和转轴2带动反应釜体1翻转,利于反应物倾倒后过滤,即得噻苯隆成品。
需要说明的是,在本文中,诸如第一和第二等之类的关系术语仅仅用来将一个实体或者操作与另一个实体或操作区分开来,而不一定要求或者暗示这些实体或操作之间存在任何这种实际的关系或者顺序。而且,术语“包括”、“包含”或者其任何其他变体意在涵盖非排他性的包含,从而使得包括一系列要素的过程、方法、物品或者设备不仅包括那些要素,而且还包括没有明确列出的其他要素,或者是还包括为这种过程、方法、物品或者设备所固有的要素。
最后应说明的是:以上所述仅为本发明的优选实施例而已,并不用于限制本发明,尽管参照前述实施例对本发明进行了详细的说明,对于本领域的技术人员来说,其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换。凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (8)
1.噻苯隆的制备方法,其特征在于:包括以下步骤:
步骤一,将5-氨基-1,2,3-噻二唑加入反应釜中,在持续搅拌的情况下加入乙二醇二甲醚中,并继续搅拌至完全溶解;
步骤二,将溶解混合物中滴加8滴三乙胺,并升温至40℃左右;
步骤三,滴加苯基异腈酸酯,每36g苯基异腈酸酯在15min左右滴加完毕,并在40℃下保温6h;
步骤四,反应结束后将混合物过滤即得噻苯隆成品。
2.根据权利要求1所述的噻苯隆的制备方法,其特征在于:所述步骤一中,5-氨基-1,2,3-噻二唑的质量分数为99.2%,摩尔质量为0.3mol。
3.根据权利要求1所述的噻苯隆的制备方法,其特征在于:所述步骤三中,苯基异腈酸酯的摩尔质量为0.3mol。
4.根据权利要求1所述的噻苯隆的制备方法,其特征在于:所述步骤一、二和三中,5-氨基-1,2,3-噻二唑、乙二醇二甲醚和苯基异腈酸酯的质量比为1-1.1∶10∶1.1-1.3。
5.根据权利要求1所述的噻苯隆的制备方法,其特征在于:所述步骤一中的反应釜包括反应釜体(1)、转轴(2)、支撑板(3)、支撑柱(4)、转动组件(5)、搅拌组件(6)、滴加组件(7)、水浴夹层(8)、进水管(9)和出水管(10),所述反应釜体(1)的两侧分别通过转轴(2)与支撑板(3)转动连接,且支撑板(3)的底部两侧通过两根支撑柱(4)竖直设置在地面上,所述反应釜体(1)一侧的转轴(2)贯穿支撑板(3)与转动组件(5)连接,且反应釜体(1)的顶部铰接的顶盖顶部中央嵌设有搅拌组件(6),所述搅拌组件(6)两侧的顶盖上还嵌入安装有滴加组件(7),所述反应釜体(1)的内壁内设置有水浴夹层(8),且水浴夹层(8)位于反应釜体(1)两侧的顶部均连接有进水管(9),所述水浴夹层(8)位于反应釜体(1)最底部连接有出水管(10)。
6.根据权利要求5所述的噻苯隆的制备方法,其特征在于:所述转动组件(5)由转动壳体(51)、气缸(52)、齿条(53)和齿轮(54)组成,所述转动壳体(51)固接在支撑板(3)一侧,且转动壳体(51)的底部内壁安装有气缸(52),所述气缸(52)的输出端与齿条(53)一端固接,且齿条(53)与齿轮(54)相啮合,所述齿轮(54)与转轴(2)位于转动壳体(51)内部的一端固接。
7.根据权利要求5所述的噻苯隆的制备方法,其特征在于:所述搅拌组件(6)由搅拌电机(61)、搅拌轴(62)、搅拌支杆(63)和搅拌叶片(64)组成,所述搅拌电机(61)嵌设在反应釜体(1)的顶部铰接的顶盖顶部中央,且搅拌电机(61)的输出端与反应釜体(1)内部的搅拌轴(62)顶端固接,所述搅拌轴(62)的底部等距离分散固接有搅拌支杆(63)一端,且搅拌支杆(63)具有三根,每根所述搅拌支杆(63)的另一端均固接有搅拌叶片(64),且搅拌叶片(64)底部与反应釜体(1)底部内壁弧形相适配。
8.根据权利要求5所述的噻苯隆的制备方法,其特征在于:所述滴加组件(7)由滴加壳体(71)、支架(72)、滴加管(73)、调节杆(74)、通液孔(75)、拉手(76)、支座(77)、活动槽(78)、弹簧(79)和卡块(710)组成,所述滴加壳体(71)通过支架(72)安装在反应釜体(1)的顶部铰接的顶盖顶部,所述滴加壳体(71)的底部与滴加管(73)的顶端连接,且连接处插接有调节杆(74),所述调节杆(74)上开设有两个通液孔(75),且一端固接有拉手(76),所述滴加管(73)靠近拉手(76)的一侧固接有支座(77),且支座(77)顶部等距离开设有若干活动槽(78),所述活动槽(78)内设置有弹簧(79),且弹簧(79)顶部固接卡块(710),所述卡块(710)与调节杆(74)侧面底部的卡孔为配合构件。
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