CN113930966B - 一种耐黄变软片及其制备方法 - Google Patents
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- 238000004383 yellowing Methods 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title abstract description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 24
- 235000021355 Stearic acid Nutrition 0.000 claims abstract description 21
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 21
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000008117 stearic acid Substances 0.000 claims abstract description 21
- 239000013067 intermediate product Substances 0.000 claims abstract description 14
- 229960000583 acetic acid Drugs 0.000 claims abstract description 12
- 239000012362 glacial acetic acid Substances 0.000 claims abstract description 12
- VAYGXNSJCAHWJZ-UHFFFAOYSA-N dimethyl sulfate Chemical compound COS(=O)(=O)OC VAYGXNSJCAHWJZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 9
- NSOXQYCFHDMMGV-UHFFFAOYSA-N Tetrakis(2-hydroxypropyl)ethylenediamine Chemical compound CC(O)CN(CC(C)O)CCN(CC(C)O)CC(C)O NSOXQYCFHDMMGV-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 4
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
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- 238000002844 melting Methods 0.000 claims description 4
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- ONJQDTZCDSESIW-UHFFFAOYSA-N polidocanol Chemical compound CCCCCCCCCCCCOCCOCCOCCOCCOCCOCCOCCOCCOCCO ONJQDTZCDSESIW-UHFFFAOYSA-N 0.000 claims description 3
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims description 2
- 229910052740 iodine Inorganic materials 0.000 claims description 2
- 239000011630 iodine Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000005886 esterification reaction Methods 0.000 abstract description 5
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- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 150000003141 primary amines Chemical class 0.000 description 3
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- 239000004902 Softening Agent Substances 0.000 description 2
- LHIJANUOQQMGNT-UHFFFAOYSA-N aminoethylethanolamine Chemical compound NCCNCCO LHIJANUOQQMGNT-UHFFFAOYSA-N 0.000 description 2
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
- D06M13/46—Compounds containing quaternary nitrogen atoms
- D06M13/467—Compounds containing quaternary nitrogen atoms derived from polyamines
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- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
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- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
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Abstract
本发明公开了一种耐黄变软片及其制备方法,所述耐黄变软片按照质量份包括以下原料,硬脂酸150‑180份;N,N,N',N'‑四(2‑羟基丙基)乙二胺20‑35份;亚磷酸1‑3份;硫酸二甲酯2‑5份;乳化剂10‑15份;冰醋酸5‑15份。本发明采用上述结构的一种耐黄变软片及其制备方法,通过硬脂酸和N,N,N',N'‑四(2‑羟基丙基)乙二胺在亚磷酸的催化作用下酯化反应获得中间产物,得到的中间产物在硫酸二甲酯的作用下完成季铵化,再添加乳化剂和冰醋酸得到耐黄变软片,由于原料不存在伯胺和仲胺基团,通过季铵化反应后所得到的软片具有优异的耐黄变性能,且酯化反应得到的产物具有很好的生物降解性和使用安全性。
Description
技术领域
本发明涉及纺织印染助剂技术领域,特别是涉及一种耐黄变软片及其制备方法。
背景技术
在染整加工过程中,由于纤维在各种加工工序中容易受到损伤,从而导致纤维手感粗糙,同时在各种树脂整理后纤维也会损失手感,因此必须加入柔软剂进行整理,以获得柔软、蓬松的手感。目前行业主要使用的柔软剂包括软片和硅油两大类,而软片不仅能够赋予纤维不同的风格手感,同时也可以改进染整工艺,节约能源,降低加工成本;软片具有包装简单、体积小、易储运和成本低等特点,从而深受印染厂欢迎。
市场现有软片主要是采用硬脂酸和二乙烯三胺或羟乙基乙二胺经合成反应得到的。由于硬脂酸和二乙烯三胺在反应中残留的伯胺和仲胺会在高温作用下导致纤维黄变,从而影响了面料的质量;而羟乙基乙二胺在长时间接触后,会对胎儿发育产生不良影响。因此软片的黄变和安全是行业需要解决的长期困难。
发明内容
本发明的目的是提供一种耐黄变软片及其制备方法,以解决现有技术中的软片容易造成纤维黄变和对人体有危害的问题。
为实现上述目的,本发明提供了一种耐黄变软片,所述耐黄变软片按照质量份包括以下原料,
硬脂酸150-180份;
N,N,N',N'-四(2-羟基丙基)乙二胺20-35份;
亚磷酸1-3份;
硫酸二甲酯2-5份;
乳化剂10-15份;
冰醋酸5-15份。
优选的,所述硬脂酸的碘值不大于0.4gI2/100g。
优选的,所述乳化剂为脂肪醇聚氧乙烯醚AEO-7、脂肪醇聚氧乙烯醚AEO-9中至少一种。
优选的,所述冰醋酸的质量浓度不小于98%。
一种耐黄变软片的制备方法,包括以下步骤,
(1)将称量好的硬脂酸在氮气保护下按照2℃/min逐步升温至120℃融化;
(2)将称量好的N,N,N',N'-四(2-羟基丙基)乙二胺和亚磷酸加入上述融化的硬脂酸中,按照1-3℃/min逐步升温至140-160℃,抽真空并保温反应2-4小时至没有水产生,得到初产物;
(3)将上述初产物降温至100-120℃,加入称量好的硫酸二甲酯,保温反应1-3小时得到中间产物;
(4)将上述中间产物降温至80-100℃,加入称量好的乳化剂和冰醋酸,继续保温1-2小时,出料,切片得到耐黄变软片。
因此,本发明采用上述结构的一种耐黄变软片及其制备方法,具有以下有益效果:
1、本发明选用N,N,N',N'-四(2-羟基丙基)乙二胺和硬脂酸反应,不存在伯胺和仲胺基团,通过季铵化反应后所得到的软片具有优异的耐黄变性能;
2、通过酯化反应和季铵化反应即可得到本发明所述的耐黄变软片,制备方法简单,控制方便,流程短易于操作,容易实现工业化;
3、酯化反应得到的产物具有很好的生物降解性和使用安全性。
下面通过实施例,对本发明的技术方案做进一步的详细描述。
具体实施方式
以下将对本发明进行进一步的描述,需要说明的是,本实施例以本技术方案为前提,给出了详细的实施方式和具体的操作过程,但本发明并不限于本实施例。对本领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干变形和改进,这些都属于本发明的保护范围。
实施例1
将150g硬脂酸在氮气保护下按照2℃/min逐步升温至120℃融化;
将20gN,N,N',N'-四(2-羟基丙基)乙二胺和1g亚磷酸加入上述融化的硬脂酸中,按照1℃/min逐步升温至140℃,抽真空并保温反应2小时至没有水产生,得到初产物;
将上述初产物降温至100℃,加入2g硫酸二甲酯,保温反应1小时得到中间产物;
将上述中间产物降温至80℃,加入10g脂肪醇聚氧乙烯醚AEO-7和5g冰醋酸,继续保温1小时,出料,切片得到耐黄变软片。
实施例2
将180g硬脂酸在氮气保护下按照2℃/min逐步升温至120℃融化;
将35gN,N,N',N'-四(2-羟基丙基)乙二胺和3g亚磷酸加入上述融化的硬脂酸中,按照3℃/min逐步升温至160℃,抽真空并保温反应4小时至没有水产生,得到初产物;
将上述初产物降温至120℃,加入5g硫酸二甲酯,保温反应3小时得到中间产物;
将上述中间产物降温至100℃,加入15g脂肪醇聚氧乙烯醚AEO-7和15g冰醋酸,继续保温2小时,出料,切片得到耐黄变软片。
实施例3
将160g硬脂酸在氮气保护下按照2℃/min逐步升温至120℃融化;
将30gN,N,N',N'-四(2-羟基丙基)乙二胺和2g亚磷酸加入上述融化的硬脂酸中,按照2℃/min逐步升温至150℃,抽真空并保温反应3小时至没有水产生,得到初产物;
将上述初产物降温至110℃,加入4g硫酸二甲酯,保温反应2小时得到中间产物;
将上述中间产物降温至90℃,加入12g脂肪醇聚氧乙烯醚AEO-9和10g冰醋酸,继续保温1.6小时,出料,切片得到耐黄变软片。
将上述实施例1-3制备得到的耐黄变软片与现有技术中的软片(硬脂酸和二乙烯三胺反应得到的产物)均配制成10%的水溶液,静置1小时观察水溶液稳定性,然后将上述软片应用于棉针织柔软整理,按照布样质量的3%,浴比1:10,浸渍法处理棉针织面料,工作液温度45℃,时间15分钟,140℃烘干,布样静置回潮3小时后测试白度和手感。白度可通过白度仪测试,可以显示布样的黄变性;手感按照5人小组评价,1级最差,5级最好,将5人评分相加即为手感分数,分数越高手感越好。具体数据如下表1。
表1不同样品的性能测试结果
样品 | 10%水溶液状态 | 稳定性 | 白度 | 手感 |
实施例1 | 白色乳液 | 未分层 | 72.37 | 18 |
实施例2 | 白色乳液 | 未分层 | 74.52 | 23 |
实施例3 | 白色乳液 | 未分层 | 73.16 | 20 |
对比样 | 白色乳液 | 未分层 | 68.94 | 16 |
从上表数据可以看出,本发明实施例1-3所得软片处理后的布样白度值较高,说明软片具有较好的耐黄变性能;此外本发明实施例1-3所得软片处理后的布样手感较好,这是由于本发明的软片结构中分子链更大。
因此,本发明采用上述结构的一种耐黄变软片及其制备方法,通过硬脂酸和N,N,N',N'-四(2-羟基丙基)乙二胺在亚磷酸的催化作用下酯化反应获得中间产物,得到的中间产物在硫酸二甲酯的作用下完成季铵化,再添加乳化剂和冰醋酸得到耐黄变软片,由于原料不存在伯胺和仲胺基团,通过季铵化反应后所得到的软片具有优异的耐黄变性能,且酯化反应得到的产物具有很好的生物降解性和使用安全性。
最后应说明的是:以上实施例仅用以说明本发明的技术方案而非对其进行限制,尽管参照较佳实施例对本发明进行了详细的说明,本领域的普通技术人员应当理解:其依然可以对本发明的技术方案进行修改或者等同替换,而这些修改或者等同替换亦不能使修改后的技术方案脱离本发明技术方案的精神和范围。
Claims (2)
1.一种耐黄变软片,其特征在于:所述耐黄变软片按照质量份包括以下原料,
硬脂酸150-180份;
N,N,N',N'-四(2-羟基丙基)乙二胺20-35份;
亚磷酸1-3份;
硫酸二甲酯2-5份;
乳化剂10-15份;
冰醋酸5-15份;
所述硬脂酸的碘值不大于0.4gI2/100g;
所述乳化剂为脂肪醇聚氧乙烯醚AEO-7、脂肪醇聚氧乙烯醚AEO-9中至少一种;
所述冰醋酸的质量浓度不小于98%。
2.如权利要求1所述的一种耐黄变软片的制备方法,其特征在于:包括以下步骤,
(1)将称量好的硬脂酸在氮气保护下按照2℃/min逐步升温至120℃融化;
(2)将称量好的N,N,N',N'-四(2-羟基丙基)乙二胺和亚磷酸加入上述融化的硬脂酸中,按照1-3℃/min逐步升温至140-160℃,抽真空并保温反应2-4小时至没有水产生,得到初产物;
(3)将上述初产物降温至100-120℃,加入称量好的硫酸二甲酯,保温反应1-3小时得到中间产物;
(4)将上述中间产物降温至80-100℃,加入称量好的乳化剂和冰醋酸,继续保温1-2小时,出料,切片得到耐黄变软片。
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