CN108276441A - 环己胺二甲叉膦酸的制备方法 - Google Patents
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Abstract
本发明公开了环己胺二甲叉膦酸的制备方法,其制备方法包括以下步骤:首先,再反应釜中加入亚磷酸、盐酸,搅拌,滴加环己胺;升温滴加甲醛,降温加入晶种,保温1小时;最后升温补加剩余部分甲醛,先保温后降温结晶,离心出料得到环己胺二甲叉膦酸。本发明所述的发明方法化学稳定性好、制备方法简单,且使用方便,可用于缓蚀和阻垢等,适合推广应用。
Description
技术领域
本发明属于有机化合物合成技术领域,具体涉及到有机磷化合物环己胺二甲叉膦酸的制备方法。
背景技术
有机磷化合物是指含碳-磷键的化合物或含有机基团的磷酸衍生物。有机磷化合物在核酸、辅酶、有机磷神经毒气、有机磷杀虫剂、有机磷杀菌剂、有机磷除草剂、化学治疗剂、增塑剂、抗氧化剂、表面活性剂、络合剂、有机磷萃取剂、浮选剂和阻燃剂等方面应用广泛。
二甲叉磷酸衍生物类还是一类良好的阻垢剂,同时又具有良好的缓蚀作用。这类阻垢剂都含有两个磷酸基团直接与碳原子相连接,比C-O-P键更稳定。潘志权等以乙醇胺和3-氨甲基吡啶为原料分别与甲醛和亚磷酸通过Manich反应合成了乙醇胺二甲叉磷酸和3-氨甲基吡啶二甲叉磷酸,操作方法简单,实用性强,但收率较低。
矫成奇等以环己胺二甲叉膦酸为原料通过水热法设计合成了结构新颖、性能优良的金属磷酸盐配位聚合物晶体材料。该发明对有机磷化合物在化工行业的发展具有很大的促进作用。
发明内容
为克服现有技术的缺陷,本发明提供了一种环己胺二甲叉膦酸的制备方法,方法化学稳定性好、制备方法简单,且使用方便;该方法制备的环己胺二甲叉膦酸可用于阻垢和缓蚀等,适合推广应用。
一种环己胺二甲叉膦酸的制备方法,采用以下步骤:
(1)取亚磷酸溶液、盐酸溶液加入反应釜,开启搅拌;
(2)反应釜中滴加环己胺溶液,温度控制在65℃~70℃。
(3)反应釜中滴加甲醛溶液A,55min~60min内匀速滴加完毕;
(4)降温至100℃~110℃加入晶种,降温至75℃~80℃后保温1小时;
(5)将温度升高至95℃~98℃,补加甲醛溶液B,保温2小时;
(6)将温度降至95℃~98℃保温1小时,然后再提温至100℃~105℃回流保温2小时,最后降温结晶,梯度为5℃/h;
(7)离心,出料,得到环己胺二甲叉膦酸;
其中步骤(3)所述的甲醛A和步骤(5)所述的甲醛B之和为总甲醛量。
优选地,所述环己胺、亚磷酸、盐酸和总甲醛的物质的量之比=1 : 1.93~2.12:1.15~1.23 :2.20~2.37。
优选地,步骤(1)所述的亚磷酸溶液质量浓度为80%~82%。
优选地,步骤(2)所述环己胺溶液的质量浓度为99%-100%。
优选地,步骤(1)所述盐酸溶液的质量浓度为30%~31%。
优选地,步骤(3)所述甲醛溶液的质量浓度为40%~41%。
一种上述方法制备的环己胺二甲叉膦酸,所述环己胺二甲叉膦酸为白色晶体状,
结构式如下所示:
一种上述环己胺二甲叉膦酸做阻垢缓释剂应用。
有益效果
本发明所述的发明方法化学稳定性好、制备方法简单,且使用方便,可用于阻垢和缓蚀等,适合推广应用。
附图说明
图1 为实施例2制备的环己胺二甲叉膦酸的核磁共振碳谱图;
图2 为实施例2制备的环己胺二甲叉膦酸的核磁共振氢谱图。
具体实施方式
为了更好的理解本发明,下面结合具体实施例进一步阐述本发明的内容,但本发明的内容绝不仅仅局限于下面的实施例。
实施例1
取162.3g 质量浓度为81%的亚磷酸溶液、114g质量浓度为31%的盐酸溶液加入反应釜,开启搅拌;在反应釜中滴加79.2g环己胺,温度控制在65摄氏度;反应釜中滴加90.3g质量浓度为40%的甲醛溶液,一个小时滴加完毕;甲醛溶液滴加完毕后,降温至110摄氏度,加入晶种,降温至80摄氏度后保温1小时;将温度升高至95摄氏度,补加剩余38.7g甲醛溶液,保温两小时;将温度降至97摄氏度保温1小时,然后再提温至102摄氏度回流保温两个小时,最后降温结晶,梯度为5℃/h;结晶完成后离心,出料,得到白色晶体状的环己胺二甲叉膦酸。
由测试结果可知,烘干后晶体出料量为201g,活性为99.11%,亚磷酸含量为0.65%,环己胺二甲叉膦酸的收率为87.54%。
实施例2
取162.3g质量浓度为81%的亚磷酸溶液、114g质量浓度为31%的盐酸溶液加入反应釜,开启搅拌;在反应釜中滴加79.2g环己胺,温度控制在70摄氏度;反应釜中滴加98.56g质量浓度为40%的甲醛溶液,一个小时滴加完毕;甲醛溶液滴加完毕后,降温至110摄氏度,加入晶种,降温至80摄氏度后保温1小时;将温度升高至97摄氏度,补加剩余42.24g甲醛溶液,保温两小时;将温度降至97摄氏度保温1小时,然后再提温至102摄氏度回流保温两个小时,最后降温结晶,梯度为5℃/h;结晶完成后离心,出料,得到白色晶体状的环己胺二甲叉膦酸。
由测试结果可知,烘干后晶体出料量为229.6g,活性为98.87%,亚磷酸含量为0.58%,环己胺二甲叉膦酸的收率为84.32%。
实施例3
取162.3g质量浓度为81%的亚磷酸溶液、114g质量浓度为31%的盐酸溶液加入反应釜,开启搅拌;在反应釜中滴加83.2g环己胺,温度控制在72摄氏度以内;反应釜中滴加98.56g质量浓度为40%的甲醛溶液,一个小时滴加完毕;甲醛溶液滴加完毕后,降温至105摄氏度,加入晶种,降温至78摄氏度后保温1小时;将温度升高至95摄氏度,补加剩余42.24g甲醛溶液,保温两小时;将温度降至97摄氏度保温1小时,然后再提温至102摄氏度回流保温两个小时,最后降温结晶,梯度为5℃/h;结晶完成后离心,出料,得到白色晶体状的环己胺二甲叉膦酸。
由测试结果可知,烘干后晶体出料量为196.2g,活性为96.78%,亚磷酸含量为1.04%,环己胺二甲叉膦酸的收率为82.7%。
实施例4
取170.4g质量浓度为81%的亚磷酸溶液、114g质量浓度为31%的盐酸溶液加入反应釜,开启搅拌;在反应釜中滴加79.2g环己胺,温度控制在70摄氏度以内;反应釜中滴加98.56g质量浓度为40%的甲醛溶液,一个小时滴加完毕;甲醛溶液滴加完毕后,降温至107摄氏度,加入晶种,降温至78摄氏度后保温1小时;将温度升高至95摄氏度,补加剩余42.24g甲醛溶液,保温两小时;将温度降至96摄氏度保温1小时,然后再提温至102摄氏度回流保温两个小时,最后降温结晶,梯度为5℃/h;结晶完成后离心,出料,得到白色晶体状的环己胺二甲叉膦酸。
由测试结果可知,烘干后晶体出料量为197g,活性为92.43%,亚磷酸含量为0.66%,环己胺二甲叉膦酸的收率为79.31%。
效果实验
性能测定
阻垢性能测定:硫酸钙阻垢性能测定方法
采用行业标准SY/T 5673-93《油田用防垢剂性能评定方法》进行测定。
在SO4 2-浓度为7100mg/L和Ca2+浓度为6800mg/L的水质条件下,分别加入不同投加量的阻垢剂,测定阻垢率。
表1 阻垢实验
以上所述仅为本发明的部分实施方式,应当指出,对于本领域的普通技术人员来说,在不脱离本发明创造构思的前提下,作出若干改进和变换,这些都属于本发明的保护范围。
Claims (9)
1.一种环己胺二甲叉膦酸的制备方法,其特征在于,采用以下步骤:
(1)取亚磷酸溶液、盐酸溶液加入反应釜,开启搅拌;
(2)反应釜中滴加环己胺溶液,温度控制在65℃~70℃;
(3)反应釜中滴加甲醛溶液A,55min~60min内滴加完毕;
(4)降温至100℃~110℃加入晶种,降温至75℃~80℃后保温1小时;
(5)将温度升高至95℃~98℃,补加甲醛溶液B,保温2小时;
(6)将温度降至95℃~98℃保温1小时,然后再提温至100℃~105℃回流保温2小时,最后降温结晶,降温的梯度为5℃/h;
(7)离心,出料,得到环己胺二甲叉膦酸;
其中步骤(3)所述的甲醛A和步骤(5)所述的甲醛B之和为总甲醛量。
2.根据权利要求1所述的制备方法,其特征在于,所述环己胺、亚磷酸、盐酸和总甲醛的物质的量之比=1 : 1.93~2.12 :1.15~1.23 :2.20~2.37。
3.根据权利要求1所述的制备方法,其特征在于,步骤(3)所述的滴加甲醛溶液为匀速滴加。
4.根据权利要求1所述的制备方法,其特征在于,步骤(1)所述的亚磷酸溶液质量浓度为80%~82%。
5.根据权利要求1所述的制备方法,其特征在于,步骤(2)所述环己胺溶液的质量浓度为99%~100%。
6.根据权利要求1所述的制备方法,其特征在于,步骤(1)所述盐酸溶液的质量浓度为30%~31%。
7.根据权利要求1所述的制备方法,其特征在于,步骤(3)所述甲醛溶液的质量浓度为40%~41%。
8.一种权利要求1-7所述的方法制备的环己胺二甲叉膦酸,其特征在于,所述环己胺二甲叉膦酸为白色晶体状。
9.一种权利要求8所述环己胺二甲叉膦酸做阻垢缓释剂应用。
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