CN117586135A - 一种生物质基表面活性剂型增稠剂及其制备方法 - Google Patents
一种生物质基表面活性剂型增稠剂及其制备方法 Download PDFInfo
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- C07C215/02—Compounds containing amino and hydroxy groups bound to the same carbon skeleton having hydroxy groups and amino groups bound to acyclic carbon atoms of the same carbon skeleton
- C07C215/40—Compounds containing amino and hydroxy groups bound to the same carbon skeleton having hydroxy groups and amino groups bound to acyclic carbon atoms of the same carbon skeleton with quaternised nitrogen atoms bound to carbon atoms of the carbon skeleton
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C213/00—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton
- C07C213/04—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton by reaction of ammonia or amines with olefin oxides or halohydrins
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K23/00—Use of substances as emulsifying, wetting, dispersing, or foam-producing agents
- C09K23/18—Quaternary ammonium compounds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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Abstract
本发明公开了一种生物质基表面活性剂型增稠剂及其制备方法。其结构式如式(A)所示。本发明还提供一种增稠(增粘)体系,包括式(A)所示化合物、无机盐及水。本发明制备得到了一种新型的生物质基表面活性剂型增稠剂,通过调节所述生物质基表面活性剂型增稠剂与无机盐的质量比及体系中无机盐的浓度,体系的粘稠度显著增加,所述生物质基表面活性剂型增稠剂来源于生物质且易降解,是一种环境友好的增稠剂。
Description
技术领域
本发明属于表面活性剂科学与应用技术领域,具体涉及一种生物质基表面活性剂型增稠剂及其制备方法。
背景技术
增稠剂是近年来迅速发展起来的一类新型功能材料,主要用于提高产品的黏度或稠度。具有用量小、增稠明显、使用方便等特点,被广泛地应用到制药、印染、涂料、化妆品、食品添加剂、采油、造纸加工等工业。
天然增稠剂多数从含多糖类的粘质物的植物和海藻类制取,如淀粉,阿拉伯树胶,瓜尔豆胶,角叉菜胶,果胶,琼脂和海藻酸等。亦有从含蛋白质的动植物制取,如明胶,酪蛋白和酷蛋白酸钠等。亦有从微生物中制取的,如汉生胶(黄原胶)等。合成增稠剂,如羧甲基纤维素钠CMC,丙二醇酸藻蛋白酸酯,纤维素乙醇酸和聚丙烯酸钠,淀粉乙醇酸钠,淀粉磷酸钠,甲基纤维素和聚丙烯酸钠等。
生物质基表面活性剂利用来源于生物质中广泛存在的原料,价格低廉,绿色环保。利用来源于生物质中的山梨醇为原料,通过简易的方法合成、制备出表面活性剂。将生物质基表面活性剂用作增稠剂鲜有报道。
发明内容
本发明的目的之一是提供式(A)所示化合物:
上述式(A)所示化合物通过包括如下步骤的方法制备得到:使得式2所示溴代山梨醇与N,N-二甲基十六胺反应,即得,
上述方法中,式2所示溴代山梨醇与N,N-二甲基十六胺的摩尔比可为1:2.0-2.5,具体可为1:2.1;
所述反应的温度可为40-80℃,最优为45℃;
所述反应的时间可为6-48h,最优为12h;
所述反应的溶剂可为无水甲醇、无水乙醇、乙腈等;具体可为无水甲醇;
式2所示溴代山梨醇的制备方法记载于中国专利201710041387.9中。
上述式(A)所示化合物在制备增稠(增粘)剂中的应用也属于本发明的保护范围。
本发明还提供一种增稠(增粘)体系。
本发明所提供的增稠(增粘)体系,包括式(A)所示化合物、无机盐及水,
所述增稠(增粘)体系中,式(A)所示化合物的质量浓度可为0.65wt%-3.28wt%;无机盐的质量浓度可为0-3%wt,端点值0不可取;
具体地,式(A)所示化合物的质量浓度为2.59wt%,无机盐的质量浓度为0.3-2.0wt%,具体可为0.6-1.6wt%;
或,无机盐的质量浓度为1.2wt%,式(A)所示化合物的质量浓度为0.65wt%-3.28wt%;
所述无机盐可选自:氯化钠、氯化镁、氯化铵、溴化钠、溴化钾、氯化钾、氯化镁、氯化铜、氯化锌、硫酸钠、醋酸钠和三氯化铁中至少一种。
具体地,式(A)所示化合物的质量浓度大于等于2.59wt%(2.59wt%-3.28wt%),无机盐的质量浓度为1.2wt%,所得体系为凝胶体系。
上述增稠(增粘)体系通过包括如下步骤的方法制备得到:
将式(A)所示化合物溶于水,加热溶解,向所得溶液中加入无机盐,搅拌均匀,冷却至室温,得到增稠(增粘)体系。
本发明制备得到了一种新型的生物质基表面活性剂型增稠剂,通过调节所述生物质基表面活性剂型增稠剂与无机盐的质量比及体系中无机盐的浓度,体系的粘稠度显著增加,且制得的增稠体系具有一定的抗剪切能力和粘弹性。所述生物质基表面活性剂型增稠剂来源于生物质,用量少,易降解,是一种环境友好的增稠剂。此类表面活性剂的在较低浓度能和多种廉价无机盐形成水性增稠体系,用量少,是绿色高效环保型增稠体系。该表面活性剂作为增稠剂有望在水性涂料、化妆品、日化用品、润湿等领域实现应用。
附图说明
图1为本发明对比例中所得溶液的照片。
图2为本发明实施例3中所得凝胶的照片。
图3为本发明实施例5中NaCl的添加量对溶液粘度的影响。
图4为本发明实施例6中式(A)所示化合物的添加量对溶液粘度的影响。
图5为本发明实施例7中不同无机盐种类制得的增粘溶液抗剪切能力的比较。
图6为本发明实施例8中所得凝胶体系的模量随剪切速率的变化。
具体实施方式
下面结合具体实施方式对本发明进行进一步的详细描述,给出的实施例仅为了阐明本发明,而不是为了限制本发明的范围。以下提供的实施例可作为本技术领域普通技术人员进行进一步改进的指南,并不以任何方式构成对本发明的限制。
下述实施例中的实验方法,如无特殊说明,均为常规方法,按照本领域内的文献所描述的技术或条件或者按照产品说明书进行。下述实施例中所用的材料、试剂等,如无特殊说明,均可从商业途径得到。
实施例1、式(A)所示化合物的制备
将12.0g(3.89mmol)式2所示溴代山梨醇,22.05g(8.18mmol)N,N-二甲基十六胺,60mL无水甲醇加入反应容器,升温至45℃搅拌24h,反应结束后将反应液减压浓缩,用丙酮/乙醇(v/v=2:1)重结晶得到白色固体式(A)所示化合物,收率86%。结构验证数据如下:1H-NMR(400MHz,DMSO):δ=0.79-0.88(t,6H,-CH3),1.13-1.37(m,24H),2.64-2.86(s,12H),2.89-3.07(m,4H),3.28-3.36(m,4H);MALDI-TOF-MS(M+Na)+:Calcd.For C42H90Br2N2O4:846.9.Found:847(M+H),869(M+Na);经验证,结构正确。
对比例
在60℃的温度下将30mg实施例1制备的式(A)所示化合物溶于1.5ml水,加入20mgNaCl,得到的溶液在60℃无明显粘度,图1所示。
实施例2、增粘(增稠)体系的制备
称取40mg的实施例1中制得的式(A)所示化合物溶于1.5ml二次水中,加热60°溶解,向溶液中加入10mg NaCl,缓慢搅拌均匀,降至室温,得到粘度增加的溶液。
实施例3、凝胶的制备
在60℃的温度下将40mg实施例1中制得的式(A)所示化合物溶于1.5ml水,加入20mg NaCl,冷却至室温,得到的溶液粘度明显增加(粘度值3343mPa.s),静置后成凝胶,如下图2所示。
实施例4、凝胶的制备
称取40mg的实施例1中制得的式(A)所示化合物溶于1.5ml二次水中,加热60℃溶解,向溶液中加入20mg(1.2%wt)CuCl2,缓慢搅拌均匀,降至室温,得到凝胶体系。
实施例5、考察NaCl的量对溶液粘度的影响
在60℃的温度下将40mg实施例1中制得的式(A)所示化合物溶于1.5ml水(2.59wt%),加入不同质量的NaCl,冷却至室温,考察所得溶液的粘度值。结果如图3所示。由图3可知,式(A)所示化合物的用量为31.5mmol/L或者2.59wt%,随着NaCl浓度的增加,溶液粘度增大,当NaCl浓度为1.2wt%时成凝胶,NaCl浓度增大至1.9wt%时,粘度急剧下降。
实施例6、考察式(A)所示化合物的添加量对溶液粘度的影响
在60℃的温度下配制不同浓度的式(A)所示化合物水溶液,加入质量浓度为1.2wt%的NaCl,冷却至室温,考察所得溶液的粘度值。结果如图4和表1所示。由图4可知,NaCl含量为1.2wt%时,溶液粘度随式(A)所示化合物浓度增加而增加,较低浓度的式(A)所示化合物的增粘效果也很显著。
表1、表面活性剂的用量对溶液粘度的影响
实施例7、不同无机盐种类制得的增粘溶液抗剪切能力的比较
在60℃的温度下配制浓度为2.59wt%的式(A)所示化合物S水溶液,加入不同种类无机盐,无机盐的质量浓度均为1.2wt%,冷却至室温,考察所得溶液的粘度随剪切速率的变化,结果如图5所示。由图5可知,加入1.2wt%的NaCl时,溶液的增稠效果最好,且增稠溶液的粘度有一定的抗剪切能力。
实施例8、凝胶体系的粘弹性考察
在60℃的温度下配制浓度为2.59wt%的式(A)所示化合物水溶液,加入1.2wt%的NaCl,冷却至室温,考察所得溶液的模量随剪切速率的变化,结果图如6所示。
由图6可知,制得的凝胶体系有一定的粘弹性。
以上对本发明进行了详述。对于本领域技术人员来说,在不脱离本发明的宗旨和范围,以及无需进行不必要的实验情况下,可在等同参数、浓度和条件下,在较宽范围内实施本发明。虽然本发明给出了特殊的实施例,应该理解为,可以对本发明作进一步的改进。总之,按本发明的原理,本申请欲包括任何变更、用途或对本发明的改进,包括脱离了本申请中已公开范围,而用本领域已知的常规技术进行的改变。
Claims (9)
1.式(A)所示化合物:
2.制备权利要求1中式(A)所示化合物的方法,包括如下步骤:使得式2所示溴代山梨醇与N,N-二甲基十六胺反应,即得,
3.权利要求1中式(A)所示化合物在制备增稠剂中的应用。
4.一种增稠体系,包括权利要求1中式(A)所示化合物、无机盐及水,
所述增稠体系中,式(A)所示化合物的质量浓度为0.65wt%-3.28wt%;无机盐的质量浓度为0-3wt%,端点值0不可取。
5.根据权利要求4所述的增稠体系,其特征在于,式(A)所示化合物的质量浓度为2.59wt%,无机盐的质量浓度为0.3-2.0wt%。
6.根据权利要求4所述的增稠体系,其特征在于,无机盐的质量浓度为1.2wt%,式(A)所示化合物的质量浓度为0.65wt%-3.28wt%。
7.根据权利要求4所述的增稠体系,其特征在于,所述无机盐选自:氯化钠、氯化镁、氯化铵、溴化钠、溴化钾、氯化钾、氯化镁、氯化铜、氯化锌、硫酸钠、醋酸钠和三氯化铁中至少一种。
8.根据权利要求4所述的增稠体系,其特征在于,式(A)所示化合物的质量浓度大于等于2.59wt%,无机盐的质量浓度为1.2wt%,所得体系为凝胶体系。
9.制备权利要求4-8中任一项所述的增稠体系的方法,包括如下步骤:将权利要求1中式(A)所示化合物溶于水,加热溶解,向所得溶液中加入无机盐,搅拌均匀,冷却至室温,得到增稠体系。
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