CN107903410B - 一种异丁烯-马来酸酐交替共聚物/海藻酸钠水凝胶及其制备方法 - Google Patents
一种异丁烯-马来酸酐交替共聚物/海藻酸钠水凝胶及其制备方法 Download PDFInfo
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- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 235000010413 sodium alginate Nutrition 0.000 title claims abstract description 36
- 239000000661 sodium alginate Substances 0.000 title claims abstract description 36
- 229940005550 sodium alginate Drugs 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000000017 hydrogel Substances 0.000 title claims abstract description 24
- 229920005603 alternating copolymer Polymers 0.000 title claims abstract description 23
- RPOCFUQMSVZQLH-UHFFFAOYSA-N furan-2,5-dione;2-methylprop-1-ene Chemical compound CC(C)=C.O=C1OC(=O)C=C1 RPOCFUQMSVZQLH-UHFFFAOYSA-N 0.000 title claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000003755 preservative agent Substances 0.000 claims abstract description 14
- 230000002335 preservative effect Effects 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims description 14
- 239000002994 raw material Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- PASHVRUKOFIRIK-UHFFFAOYSA-L calcium sulfate dihydrate Chemical compound O.O.[Ca+2].[O-]S([O-])(=O)=O PASHVRUKOFIRIK-UHFFFAOYSA-L 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 235000019832 sodium triphosphate Nutrition 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 abstract description 11
- 239000003431 cross linking reagent Substances 0.000 abstract description 9
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- 239000000084 colloidal system Substances 0.000 abstract description 4
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- 230000001815 facial effect Effects 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- VQTUBCCKSQIDNK-UHFFFAOYSA-N Isobutene Chemical compound CC(C)=C VQTUBCCKSQIDNK-UHFFFAOYSA-N 0.000 abstract 2
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 30
- 239000000499 gel Substances 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 8
- 150000001768 cations Chemical class 0.000 description 6
- 159000000007 calcium salts Chemical group 0.000 description 5
- ZOMBKNNSYQHRCA-UHFFFAOYSA-J calcium sulfate hemihydrate Chemical compound O.[Ca+2].[Ca+2].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O ZOMBKNNSYQHRCA-UHFFFAOYSA-J 0.000 description 5
- 159000000003 magnesium salts Chemical class 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical group [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 description 4
- 235000019982 sodium hexametaphosphate Nutrition 0.000 description 4
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 4
- 150000003751 zinc Chemical class 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 2
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- -1 polysaccharide carbohydrate Chemical class 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- AEMOLEFTQBMNLQ-AZLKCVHYSA-N (2r,3s,4s,5s,6r)-3,4,5,6-tetrahydroxyoxane-2-carboxylic acid Chemical compound O[C@@H]1O[C@@H](C(O)=O)[C@@H](O)[C@H](O)[C@@H]1O AEMOLEFTQBMNLQ-AZLKCVHYSA-N 0.000 description 1
- AEMOLEFTQBMNLQ-SYJWYVCOSA-N (2s,3s,4s,5s,6r)-3,4,5,6-tetrahydroxyoxane-2-carboxylic acid Chemical compound O[C@@H]1O[C@H](C(O)=O)[C@@H](O)[C@H](O)[C@@H]1O AEMOLEFTQBMNLQ-SYJWYVCOSA-N 0.000 description 1
- 229920001817 Agar Polymers 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 239000004971 Cross linker Substances 0.000 description 1
- 241000199919 Phaeophyceae Species 0.000 description 1
- 241000195474 Sargassum Species 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000008272 agar Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- FUFJGUQYACFECW-UHFFFAOYSA-L calcium hydrogenphosphate Chemical compound [Ca+2].OP([O-])([O-])=O FUFJGUQYACFECW-UHFFFAOYSA-L 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- 230000009920 chelation Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 235000019700 dicalcium phosphate Nutrition 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 description 1
- 235000019818 tetrasodium diphosphate Nutrition 0.000 description 1
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Abstract
本发明涉及一种异丁烯/马来酸酐交替共聚物/海藻酸钠水凝胶及其制备方法。所述水凝胶由海藻酸钠，固化剂，缓凝剂，交联剂，防腐剂，余量为水组成。本发明所得水凝胶，胶体性能稳定，耐温性能好，60度高温稳定性好，‑20度低温均不析水，制备工艺简单，条件温和，是一种性能优越的载体，可用于空气清新剂，面膜等日化领域。
Description
技术领域
本品涉及日用化工产品领域，特别涉及一种异丁烯-马来酸酐交替共聚物/海藻酸钠水凝胶及其制备方法。
背景技术
海藻酸钠(Sodium Alginate,NaAlg,简称AGS)是从褐藻类的海带或马尾藻中提取的一种多糖碳水化合物，其分子由β-D-甘露糖醛酸(β-D-mannuronic，M)和α-L-古洛糖醛酸(α-L-guluronic，G)按(1→4)键连接而成。海藻酸钠的分子中含有-COO－基团，当向海藻酸钠的水溶液中添加二价阳离子时，G单元中的Na+会与这些二价阳离子发生交换，使海藻酸钠溶液向凝胶转变。但单纯的海藻酸钠凝胶，交联方式单一，在低温条件下，析水严重，这极大的限制了海藻酸钠凝胶在低温条件下的使用。现有专利技术CN105601950A公布一种海藻酸钠琼脂双网络高强度天然水凝胶材料的制备方法，此法工艺较为复杂，所得凝胶强度虽高，但不能解决其高温稳定性能和低温条件下析水严重的问题。
鉴于现有海藻酸钠凝胶在低温下使用存在明显的析水现象，高温下不稳定的缺点，本发明旨在提供一种制备工艺简单，条件温和，凝胶强度大，耐温性能好的海藻酸钠水凝胶。
发明内容
在一个实施方案中，本发明提供了一种异丁烯-马来酸酐交替共聚物/海藻酸钠水凝胶，其特征在于，水凝胶包含：
a)海藻酸钠；b)交联剂；c)固化剂；d)缓凝剂；e)防腐剂；f)水；
其中，所述交联剂为酰胺-铵盐型异丁烯-马来酸酐交替共聚物；
所述固化剂为钙盐、镁盐或锌盐。
在一个实施方案中，本发明提供一种异丁烯-马来酸酐交替共聚物/海藻酸钠水凝胶，以重量百分比计，所述水凝胶包含：
0.2％-10％海藻酸钠，0.1％-8％交联剂，0.5％-10％固化剂，0.3％-8％缓凝剂，，0.2％-1％防腐剂，余量为水组成。
在另一个实施方案中，以重量百分比计，所述水凝胶包含：
0.8％-8％海藻酸钠，0.8％-6％交联剂，1.2％-6％固化剂，1％-6％缓凝剂，0.2％-1％防腐剂，余量为水组成。
在一些实施方案中，所述固化剂为钙盐、镁盐或锌盐，所述钙盐为半水硫酸钙，二水硫酸钙，磷酸氢钙中的一种或几种。
在一些实施方案中，所述缓凝剂为磷酸盐，所述磷酸盐为六偏磷酸钠，焦磷酸四钠，三聚磷酸钠。
在另一个实施方案中，本发明提供一种异丁烯-马来酸酐交替共聚物/海藻酸钠水凝胶的制备方法，包括以下步骤：
(1)A相溶液的制备：室温下，将海藻酸钠溶于适量的水中，搅拌至完全溶解，成透明溶液；
(2)B相溶液的制备：60度恒温水浴下，将交联剂溶于适量的水中，搅拌至透明溶液，冷却至室温备用；
(3)C相溶液的制备：将固化剂，缓凝剂、防腐剂用剩余的水溶解搅拌均匀；
(4)将A,B,C相溶液混合均匀后，倒入容器内，静置固化即可。
在另一个实施方案中，本发明提供一种异丁烯-马来酸酐交替共聚物/海藻酸钠水凝胶在制备空气清新剂或面膜中的应用。
在另一个实施方案中，本发明提供一种由异丁烯-马来酸酐交替共聚物/海藻酸钠水凝胶制成的空气清新剂或面膜。
本发明中，海藻酸钠与二价阳离子离子发生化学反应，通过邻近聚合物链上的两个-COO－基团与阳离子形成离子桥或通过每一对聚合物链上的-OH-和-COO－基团同阳离子发生螯合作用而形成凝胶；酰胺-铵盐型异丁烯-马来酸酐交替共聚物是一种水溶液PH值呈中性的高分子聚合物，其作为粘合剂使用，性能非常优越，同时酰胺-铵盐型异丁烯-马来酸酐交替共聚物的水溶液中含有-NH2、NH4 +等活性基团，其加入海藻酸钠溶液后，与其中的-COO－基团也能发生反应，这样即可形成如海藻酸钠-钙离子，海藻酸钠-酰胺-铵盐型异丁烯-马来酸酐交替共聚物双重网络结构的水凝胶，大大提高了水凝胶的强度，稳定性以及水凝胶的耐温性能。
本发明具有如下的优点及有益效果：
(1)选用酰胺-铵盐型异丁烯-马来酸酐交替共聚物和二价阳离子如钙盐、镁盐或锌盐配合使用，形成双重网络结构的水凝胶，提高了水凝胶的强度、稳定性以及耐温性能。
(2)所得凝胶胶体性能稳定，60℃高温不熔化，-20度低温不析水，耐温性能好，可广泛用于空清或面膜等日化产品领域。
(3)反应条件温和，工艺简单，成本可控，可大规模生产。
具体实施方式：
以下对本发明的水凝胶作进一步详细的说明，但本发明并不仅限于以下的实施例。
实施例1：
本发明的一种实施例，包括以下重量百分比的各原料及组份：
8％海藻酸钠，4％半水硫酸钙，5％六偏磷酸钠，6％的酰胺-铵盐型异丁烯-马来酸酐交替共聚物，1.0％防腐剂，余量为水组成。
实施例2：
本发明的一种实施例，包括以下重量百分比的各原料及组份：
5.6％海藻酸钠，3.2％二水硫酸钙，2.8％三聚磷酸钠，3.2％酰胺-铵盐型异丁烯-马来酸酐交替共聚物，0.6％防腐剂，余量为水组成。
实施例3：
本发明的一种实施例，包括以下重量百分比的各原料及组份：
2.5％海藻酸钠，1.8％半水硫酸钙，1.6％六偏磷酸钠，1.8％酰胺-铵盐型异丁烯-马来酸酐交替共聚物，0.3％防腐剂，余量为水组成。
实施例4：
本发明的一种实施例，包括以下重量百分比的各原料及组份：
0.8％海藻酸钠，1.2％磷酸氢钙，1.0％六偏磷酸钠，0.8％酰胺-铵盐型异丁烯-马来酸酐交替共聚物，0.2％防腐剂，余量为水组成。
对比例1：与实施例1相同，区别在于不添加交联剂酰胺-铵盐型异丁烯-马来酸酐交替共聚物，添加10％的半水硫酸钙。
对比例2：与实施例1相同，区别在于不添加固化剂半水硫酸钙，添加10％的酰胺-铵盐型异丁烯-马来酸酐交替共聚物。
其中，实施例1-4包括以下制备步骤：
(1)A相溶液的制备：室温下，将海藻酸钠溶于适量的水中，搅拌至完全溶解，成透明溶液；
(2)B相溶液的制备：60度恒温水浴下，将交联剂溶于适量的水中，搅拌至透明溶液，冷却至室温备用；
(3)C相溶液的制备：将固化剂，缓凝剂，防腐剂用剩余水溶解搅拌均匀；
(4)将A,B,C相溶液混合均匀后，倒入容器内，静置固化即可。
对比例1包括以下制备步骤：
(1)A相溶液的制备：室温下，将海藻酸钠溶于适量的水中，搅拌至完全溶解，成透明溶液；
(2)C相溶液的制备：将固化剂，缓凝剂，防腐剂用剩余水溶解搅拌均匀；
(3)将A,C相溶液混合均匀后，倒入容器内，静置固化即可。
对比例2包括以下制备步骤“
(1)A相溶液的制备：室温下，将海藻酸钠溶于适量的水中，搅拌至完全溶解，成透明溶液；
(2)B相溶液的制备：60度恒温水浴下，将交联剂溶于适量的水中，搅拌至透明溶液，冷却至室温备用；
(3)C相溶液的制备：将缓凝剂，防腐剂用剩余水溶解搅拌均匀；
(4)将A,B,C相溶液混合均匀后，倒入容器内，静置固化即可。
产品性能测试：
a、高温性能测试：
将实施例、对比例配制的样品放置于60度烘箱内加热8小时，记录时间，并分别于1小时，4小时，8小时三个不同时间点，观察胶体性能的稳定情况。
b、低温性能测试：
分别将实施例、对比例配制的样品(约70g)放置于-20度冰箱内冷冻24小时后，从冰箱内拿出，解冻至室温(约4小时)后称重，胶体若有水析出，则将析出的水挤压倒出后，再称重，计算析水量，按以下公式计算析水率。
析水率＝(W0-W1)/W0*100％
式中：W0为初始重量，W1为将析出的水除去后重量
实施例、对比例配制的样品低温性能测试如下表所示：
通过上表可以看出，实施例1-4所得凝胶，高低温下，胶体性能稳定，析水率低，而对比例1-2分别不添加交联剂或固化剂，海藻酸钠凝胶低温下，析水严重，高温下均有少量析水。因此，本发明通过选用酰胺-铵盐型异丁烯-马来酸酐交替共聚物和二价阳离子如钙盐、镁盐或锌盐配合使用，形成双重网络结构的水凝胶，大大提高了水凝胶的耐高低温性能。
以上仅是本发明的优选实施方式，应当指出的是，上述优选实施方式不应视为对本发明的限制，本发明的保护范围应当以权利要求所限定的范围为准。对于本技术领域的普通技术人员来说，在不脱离本发明的精神和范围内，还可以做出若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。
Claims (1)
1.一种水凝胶的制备方法，其特征在于：
所述水凝胶包括以下重量百分比的各原料及组份：
5.6％海藻酸钠，3.2％二水硫酸钙，2.8％三聚磷酸钠，3.2％酰胺-铵盐型异丁烯-马来酸酐交替共聚物，0.6％防腐剂，余量为水组成；
(1)A相溶液的制备：室温下，将海藻酸钠溶于适量的水中，搅拌至完全溶解，成透明溶液；
(2)B相溶液的制备：60度恒温水浴下，将酰胺-铵盐型异丁烯-马来酸酐交替共聚物溶于适量的水中，搅拌至透明溶液，冷却至室温备用；
(3)C相溶液的制备：将二水硫酸钙，三聚磷酸钠，防腐剂用剩余水溶解搅拌均匀；
(4)将A，B，C相溶液混合均匀后，倒入容器内，静置固化即可。
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