CN113235308A - 一种缓解肌肉关节疼痛的蚕丝及其制备方法和应用 - Google Patents
一种缓解肌肉关节疼痛的蚕丝及其制备方法和应用 Download PDFInfo
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- CN113235308A CN113235308A CN202110499185.5A CN202110499185A CN113235308A CN 113235308 A CN113235308 A CN 113235308A CN 202110499185 A CN202110499185 A CN 202110499185A CN 113235308 A CN113235308 A CN 113235308A
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Abstract
本发明公开了一种缓解肌肉关节疼痛的蚕丝及其制备方法和应用,先以柠檬酸和偏锗酸钠为原料制备锗掺杂碳量子点;然后以山金车、盐肤木、白芥子、细辛、香柏和甘草为原料,得到水提液和提取油;再将变性淀粉、低聚果糖、聚甘油脂肪酸酯、锗掺杂碳量子点加入水提液中,作为水相;接着将镭石粉、高纯氮化镓粉末混合研磨成混合粉,之后将混合粉利用3‑(七氟异丙氧基)丙基三乙氧基硅烷进行表面改性,得到改性混合粉,再将改性混合粉加入提取油中,制得油相;再将油相和水相制成微囊分散液;最后将预膨化蚕丝原料加入微囊分散液中,超声波浸渍处理,取出后烘干,得到一种蚕丝产品。该蚕丝产品具有缓解肌肉关节疼痛的保健效果,具有极好的应用前景。
Description
技术领域
本发明属于功能性蚕丝制备技术领域,特别是涉及一种缓解肌肉关节疼痛的蚕丝及其制备方法和应用。
背景技术
现代人的生活压力增大,越来越多的人处于亚健康的状态。特别是随着电脑、智能手机的普及,人们日常伏案工作或保持低头姿势的时间越来越长,肌肉关节,尤其是肩颈部和腰部的肌肉关节长时间处于紧张的状态,造成劳损;久之则发展成为肩周炎、颈椎病、腰肌劳损,诸如此类的肌肉关节疼痛让人难以忍受,严重影响人们的日常工作和生活质量。
肌肉关节疼痛是常见的自觉症状,通常由风湿、骨质增生、铁打损伤等原因引起的疼痛,常见于肌肉、经脉、韧带和皮下组织。主要表现是肌肉收缩、血管痉挛、乳酸堆积、发炎物质堆积、神经兴奋不已,促使肌肉血管无法缓解,制造更多的代谢产物,血流也不足以带走这些发炎物质,持续循环终于使肌肉收缩及代谢功能变差,身体就会感觉到酸、痛、胀、麻等不适感。
蚕丝是自然界中集轻、柔、细为一体的天然纤维,主要成分为纯天然动物蛋白纤维,含有人体必需的多种氨基酸,有保暖、保湿、安神、滋养及平衡人体肌肤的功效。蚕丝具有滑爽、透气、轻柔、吸湿、不刺痒及抗静电等特点,利用蚕丝加工成的蚕丝被,具有贴身保暖、蓬松轻柔、透气保健等优点。倘若在蚕丝被加工过程中引入可以缓解肌肉关节疼痛的功能性成分,那么就可以在人们盖蚕丝被睡眠过程中获得相应的保健功效。
专利CN102772082B公开了一种蚕丝被褥的生产方法,先将蚕丝从蚕层内部脱离,对蚕丝进行第一次脱水,浸泡,脱水后的蚕丝放进浸泡池内进行浸泡24小时,将浸泡的蚕丝取出,并对蚕丝进行第二次脱水,漂白,第三次脱水,制成蚕丝被褥,烘干。该专利技术获得的蚕丝被褥没有特殊功效,不能满足睡眠过程中肌肉关节疼痛的缓解。
发明内容
本发明的目的就是要提供一种缓解肌肉关节疼痛的蚕丝及其制备方法和应用,本发明所制备的蚕丝可以缓解肌肉关节疼痛,应用前景广阔。
为实现上述目的,本发明是通过如下方案实现的:
一种缓解肌肉关节疼痛的蚕丝的制备方法,具体步骤如下:
(1)先以柠檬酸和偏锗酸钠为原料制备锗掺杂碳量子点;
(2)然后以山金车、盐肤木、白芥子、细辛、香柏和甘草为原料,利用水提取,得到水提液和残渣,接着将残渣经超临界CO2萃取,得到提取油;
(3)再将变性淀粉、低聚果糖、聚甘油脂肪酸酯、锗掺杂碳量子点加入水提液中,30~40℃搅拌30~40分钟,作为水相;接着将镭石粉、高纯氮化镓粉末混合研磨成300~400目的混合粉,之后将混合粉利用3-(七氟异丙氧基)丙基三乙氧基硅烷进行表面改性,得到改性混合粉,再将改性混合粉加入提取油中,50~60℃搅拌30~40分钟,即得油相;再将油相均匀缓慢加入水相中,乳化,均质化,得到微囊分散液;
(4)最后将预膨化蚕丝原料加入微囊分散液中,超声波浸渍处理,取出后烘干,即得所述的蚕丝。
优选的,以重量份计,步骤(1)的具体方法如下:将1份柠檬酸和0.1~0.2份偏锗酸钠加入15~20份水中,搅拌至完全溶解,150~160℃搅拌反应2~3小时,自然冷却至室温,离心取上清,透析,干燥,即得锗掺杂碳量子点。
进一步优选的,透析的具体方法为:200Da透析袋透析2天,每5小时换一次水。
优选的,步骤(2)中,山金车、盐肤木、白芥子、细辛、香柏和甘草的质量比为10:7~8:5~6:3~4:1~2:0.3~0.4。
优选的,步骤(2)中,水提取的具体方法为:将山金车、盐肤木、白芥子、细辛、香柏和甘草加入它们总重量5~7倍的水中,加热至沸腾,保温提取40~50分钟,过滤,得到水提液和残渣。
优选的,步骤(2)中,超临界CO2萃取的工艺条件为:采用无水乙醇作为夹带剂,萃取压力28~32MPa,萃取温度40~50℃,萃取时间2~3小时,CO2流量为28~30L/h。
优选的,步骤(3)中,变性淀粉、低聚果糖、聚甘油脂肪酸酯、锗掺杂碳量子点、水提液的质量比为1:4~6:0.06~0.08:0.05~0.07:10~12。
优选的,步骤(3)中,镭石粉、高纯氮化镓粉末的质量比为1:0.1~0.2。
优选的,步骤(3)中,以重量份计,改性混合粉的制备方法如下:先将1份3-(七氟异丙氧基)丙基三乙氧基硅烷加入30~40份无水乙醇中,搅拌分散均匀,接着加入0.25~0.35份混合粉,搅拌分散均匀,滴加冰醋酸调节pH=3~5,300~500W超声波振荡50~60分钟,加热至45~55℃,保温搅拌4~5小时,旋蒸除去乙醇,即得所述的改性混合粉。
优选的,步骤(3)中,改性混合粉与提取油的质量比为1:4~5,油相与水相的质量比为1:8~10。
优选的,步骤(3)中,油相均匀加入水相的时间为30分钟,乳化的工艺条件为:18000~20000r/min剪切乳化30~40分钟;均质化的工艺条件为:70~90MPa条件下均质化2~3次。
优选的,步骤(4)中,膨化处理的蚕丝原料与微囊分散液的质量比为1:3~4;超声波浸渍处理的工艺条件为:300~500W超声波浸渍2~3小时。
优选的,步骤(4)中,以重量份计,所述膨化处理的蚕丝原料的制备方法如下:先将1份清洗后的蚕茧加入100份蛋白酶溶液中,30~40℃浸泡40~45小时,然后转移至清水中,撕开茧层,去掉蚕蛹,套环,丝套,接着转移至50~60份含有2-十一烷基-N-羧甲基-N-羟乙基咪唑啉的碳酸氢钠水溶液中,80~90℃蒸煮6~8分钟,取出后洗涤至中性,烘干,即得所述的预膨化蚕丝原料;其中,蛋白酶溶液中含有:质量浓度0.1%碱性蛋白酶,质量浓度0.1%木瓜蛋白酶,余量为水;所述碳酸氢钠水溶液中含有:质量浓度0.3%2-十一烷基-N-羧甲基-N-羟乙基咪唑啉,质量浓度0.7%碳酸氢钠,余量为水。
另外,本发明还要求保护利用上述制备方法制得的的一种缓解肌肉关节疼痛的蚕丝。
本发明还保护上述一种缓解肌肉关节疼痛的蚕丝在蚕丝被加工中的应用。
本发明还保护一种缓解肌肉关节疼痛的蚕丝被,是利用上述蚕丝加工而成的。
本发明还保护上述一种缓解肌肉关节疼痛的蚕丝被的加工方法,是将前述蚕丝扯松、叠加后,按照重量和尺寸规格加工而得。
与现有技术相比,本发明的有益效果是:
(1)本发明先以柠檬酸和偏锗酸钠为原料制备锗掺杂碳量子点;然后以山金车、盐肤木、白芥子、细辛、香柏和甘草为原料,利用水提取,得到水提液和残渣,接着将残渣经超临界CO2萃取,得到提取油;再将变性淀粉、低聚果糖、聚甘油脂肪酸酯、锗掺杂碳量子点加入水提液中,搅拌混匀,作为水相;接着将镭石粉、高纯氮化镓粉末混合研磨成混合粉,之后将混合粉利用3-(七氟异丙氧基)丙基三乙氧基硅烷进行表面改性,得到改性混合粉,再将改性混合粉加入提取油中,搅拌混匀,即得油相;再将油相均匀缓慢加入水相中,乳化,均质化,得到微囊分散液;最后将预膨化蚕丝原料加入微囊分散液中,超声波浸渍处理,取出后烘干,得到一种蚕丝产品。该蚕丝产品具有缓解肌肉关节疼痛的保健效果,具有极好的应用推广价值。
(2)本发明将预膨化蚕丝原料加入微囊分散液,在超声波浸渍过程中,微囊分散液中的微囊成分嵌入蚕丝孔隙中,实现对蚕丝的修饰,从而赋予其良好的肌肉关节疼痛缓解效果。
(3)本发明中微囊分散液是通过油相加入水相中,经乳化、均质化处理而得。其中,水相的主要成分是山金车、盐肤木、白芥子、细辛、香柏和甘草经水提所得水提液以及锗掺杂碳量子点;油相的主要成分为镭石粉、高纯氮化镓粉末以及山金车、盐肤木、白芥子、细辛、香柏和甘草经超临界CO2萃取所得提取油。在水相中通过变性淀粉、低聚果糖、聚甘油脂肪酸酯的协同作用,改善乳化效果,在油相中通过混合粉的表面改性,3-(七氟异丙氧基)丙基三乙氧基硅烷水解,并在混合粉表面通过硅氧烷分子之间的水解结合,形成长的硅氧烷分子链缠绕在表面,使得混合粉均匀分散于提取油中。
(4)本发明中山金车可以刺激白血细胞生产,消除瘀血和促进液体释放毒素,减少肌肉酸痛;盐肤木清热解毒,散瘀止血;白芥子温肺豁痰利气,乳腺散结通络止痛,用于寒痰喘咳,胸胁胀痛,痰滞经络,关节麻木、疼痛,痰湿流注,阴疽肿毒;细辛有祛风,散寒,行水,开窍等功效,常用于风冷头痛,鼻渊,齿痛,痰饮咳逆,风湿痹痛;香柏具有清热利湿,散瘀止血之功效。用于痢疾,肠风便血,水肿,风湿痹痛,麻风病。本发明以山金车为君药,盐肤木、白芥子为臣药,细辛、香柏为佐药,甘草为使药,协同作用,起到缓解肌肉关节疼痛的作用。
(5)本发明中镭石粉可释放负离子、发射远红外,氮化镓具有压电效应,对镭石粉负离子和远红外的产生具有增强作用,锗掺杂碳量子点的加入具协同作用,进一步促进负离子和远红外的产生,并促进对人体有益电磁波的产生,可以促进人体血液循环,并且,负离子的产生可以带着前述中药成分进入人体内,发挥药效,进一步改善肌肉关节疼痛缓解效果。
具体实施方式
下面将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。
实施例1
一种缓解肌肉关节疼痛的蚕丝的制备方法,具体步骤如下:
(1)先以柠檬酸和偏锗酸钠为原料制备锗掺杂碳量子点;
(2)然后以山金车、盐肤木、白芥子、细辛、香柏和甘草为原料,利用水提取,得到水提液和残渣,接着将残渣经超临界CO2萃取,得到提取油;
(3)再将变性淀粉、低聚果糖、聚甘油脂肪酸酯、锗掺杂碳量子点加入水提液中,30℃搅拌40分钟,作为水相;接着将镭石粉、高纯氮化镓粉末混合研磨成300目的混合粉,之后将混合粉利用3-(七氟异丙氧基)丙基三乙氧基硅烷进行表面改性,得到改性混合粉,再将改性混合粉加入提取油中,60℃搅拌30分钟,即得油相;再将油相均匀缓慢加入水相中,乳化,均质化,得到微囊分散液;
(4)最后将预膨化蚕丝原料加入微囊分散液中,超声波浸渍处理,取出后烘干,即得所述的蚕丝。
步骤(1)的具体方法如下:将1份柠檬酸和0.2kg偏锗酸钠加入15kg水中,搅拌至完全溶解,160℃搅拌反应2小时,自然冷却至室温,离心取上清,透析,干燥,即得锗掺杂碳量子点。
透析的具体方法为:200Da透析袋透析2天,每5小时换一次水。
步骤(2)中,山金车、盐肤木、白芥子、细辛、香柏和甘草的质量比为10:8:5:4:1:0.4。
步骤(2)中,水提取的具体方法为:将山金车、盐肤木、白芥子、细辛、香柏和甘草加入它们总重量5倍的水中,加热至沸腾,保温提取40分钟,过滤,得到水提液和残渣。
步骤(2)中,超临界CO2萃取的工艺条件为:采用无水乙醇作为夹带剂,萃取压力32MPa,萃取温度40℃,萃取时间3小时,CO2流量为28L/h。
步骤(3)中,变性淀粉、低聚果糖、聚甘油脂肪酸酯、锗掺杂碳量子点、水提液的质量比为1:6:0.06:0.07:10。
步骤(3)中,镭石粉、高纯氮化镓粉末的质量比为1:0.2。
步骤(3)中,改性混合粉的制备方法如下:先将1kg 3-(七氟异丙氧基)丙基三乙氧基硅烷加入30kg无水乙醇中,搅拌分散均匀,接着加入0.35kg混合粉,搅拌分散均匀,滴加冰醋酸调节pH=3,500W超声波振荡50分钟,加热至55℃,保温搅拌4小时,旋蒸除去乙醇,即得所述的改性混合粉。
步骤(3)中,改性混合粉与提取油的质量比为1:5,油相与水相的质量比为1:8。
步骤(3)中,油相均匀加入水相的时间为30分钟,乳化的工艺条件为:20000r/min剪切乳化30分钟;均质化的工艺条件为:90MPa条件下均质化2次。
步骤(4)中,膨化处理的蚕丝原料与微囊分散液的质量比为1:4;超声波浸渍处理的工艺条件为:300W超声波浸渍3小时。
步骤(4)中,所述膨化处理的蚕丝原料的制备方法如下:先将1kg清洗后的蚕茧加入100kg蛋白酶溶液中,30℃浸泡45小时,然后转移至清水中,撕开茧层,去掉蚕蛹,套环,丝套,接着转移至50kg含有2-十一烷基-N-羧甲基-N-羟乙基咪唑啉的碳酸氢钠水溶液中,90℃蒸煮6分钟,取出后洗涤至中性,烘干,即得所述的预膨化蚕丝原料;其中,蛋白酶溶液中含有:质量浓度0.1%碱性蛋白酶,质量浓度0.1%木瓜蛋白酶,余量为水;所述碳酸氢钠水溶液中含有:质量浓度0.3%2-十一烷基-N-羧甲基-N-羟乙基咪唑啉,质量浓度0.7%碳酸氢钠,余量为水。
实施例2
一种缓解肌肉关节疼痛的蚕丝的制备方法,具体步骤如下:
(1)先以柠檬酸和偏锗酸钠为原料制备锗掺杂碳量子点;
(2)然后以山金车、盐肤木、白芥子、细辛、香柏和甘草为原料,利用水提取,得到水提液和残渣,接着将残渣经超临界CO2萃取,得到提取油;
(3)再将变性淀粉、低聚果糖、聚甘油脂肪酸酯、锗掺杂碳量子点加入水提液中,40℃搅拌30分钟,作为水相;接着将镭石粉、高纯氮化镓粉末混合研磨成400目的混合粉,之后将混合粉利用3-(七氟异丙氧基)丙基三乙氧基硅烷进行表面改性,得到改性混合粉,再将改性混合粉加入提取油中,50℃搅拌40分钟,即得油相;再将油相均匀缓慢加入水相中,乳化,均质化,得到微囊分散液;
(4)最后将预膨化蚕丝原料加入微囊分散液中,超声波浸渍处理,取出后烘干,即得所述的蚕丝。
步骤(1)的具体方法如下:将1份柠檬酸和0.1kg偏锗酸钠加入20kg水中,搅拌至完全溶解,150℃搅拌反应3小时,自然冷却至室温,离心取上清,透析,干燥,即得锗掺杂碳量子点。
透析的具体方法为:200Da透析袋透析2天,每5小时换一次水。
步骤(2)中,山金车、盐肤木、白芥子、细辛、香柏和甘草的质量比为10:7:6:3:2:0.3。
步骤(2)中,水提取的具体方法为:将山金车、盐肤木、白芥子、细辛、香柏和甘草加入它们总重量7倍的水中,加热至沸腾,保温提取40~50分钟,过滤,得到水提液和残渣。
步骤(2)中,超临界CO2萃取的工艺条件为:采用无水乙醇作为夹带剂,萃取压力28MPa,萃取温度50℃,萃取时间2小时,CO2流量为30L/h。
步骤(3)中,变性淀粉、低聚果糖、聚甘油脂肪酸酯、锗掺杂碳量子点、水提液的质量比为1:4:0.08:0.05:12。
步骤(3)中,镭石粉、高纯氮化镓粉末的质量比为1:0.1。
步骤(3)中,改性混合粉的制备方法如下:先将1kg 3-(七氟异丙氧基)丙基三乙氧基硅烷加入40kg无水乙醇中,搅拌分散均匀,接着加入0.25kg混合粉,搅拌分散均匀,滴加冰醋酸调节pH=5,300W超声波振荡60分钟,加热至45℃,保温搅拌5小时,旋蒸除去乙醇,即得所述的改性混合粉。
步骤(3)中,改性混合粉与提取油的质量比为1:4,油相与水相的质量比为1:10。
步骤(3)中,油相均匀加入水相的时间为30分钟,乳化的工艺条件为:18000r/min剪切乳化40分钟;均质化的工艺条件为:70MPa条件下均质化3次。
步骤(4)中,膨化处理的蚕丝原料与微囊分散液的质量比为1:3;超声波浸渍处理的工艺条件为:500W超声波浸渍2小时。
步骤(4)中,所述膨化处理的蚕丝原料的制备方法如下:先将1kg清洗后的蚕茧加入100kg蛋白酶溶液中,40℃浸泡40小时,然后转移至清水中,撕开茧层,去掉蚕蛹,套环,丝套,接着转移至60kg含有2-十一烷基-N-羧甲基-N-羟乙基咪唑啉的碳酸氢钠水溶液中,80℃蒸煮8分钟,取出后洗涤至中性,烘干,即得所述的预膨化蚕丝原料;其中,蛋白酶溶液中含有:质量浓度0.1%碱性蛋白酶,质量浓度0.1%木瓜蛋白酶,余量为水;所述碳酸氢钠水溶液中含有:质量浓度0.3%2-十一烷基-N-羧甲基-N-羟乙基咪唑啉,质量浓度0.7%碳酸氢钠,余量为水。
实施例3
一种缓解肌肉关节疼痛的蚕丝的制备方法,具体步骤如下:
(1)先以柠檬酸和偏锗酸钠为原料制备锗掺杂碳量子点;
(2)然后以山金车、盐肤木、白芥子、细辛、香柏和甘草为原料,利用水提取,得到水提液和残渣,接着将残渣经超临界CO2萃取,得到提取油;
(3)再将变性淀粉、低聚果糖、聚甘油脂肪酸酯、锗掺杂碳量子点加入水提液中,35℃搅拌35分钟,作为水相;接着将镭石粉、高纯氮化镓粉末混合研磨成400目的混合粉,之后将混合粉利用3-(七氟异丙氧基)丙基三乙氧基硅烷进行表面改性,得到改性混合粉,再将改性混合粉加入提取油中,55℃搅拌35分钟,即得油相;再将油相均匀缓慢加入水相中,乳化,均质化,得到微囊分散液;
(4)最后将预膨化蚕丝原料加入微囊分散液中,超声波浸渍处理,取出后烘干,即得所述的蚕丝。
步骤(1)的具体方法如下:将1份柠檬酸和0.15kg偏锗酸钠加入18kg水中,搅拌至完全溶解,155℃搅拌反应2.5小时,自然冷却至室温,离心取上清,透析,干燥,即得锗掺杂碳量子点。
透析的具体方法为:200Da透析袋透析2天,每5小时换一次水。
步骤(2)中,山金车、盐肤木、白芥子、细辛、香柏和甘草的质量比为10:7.5:5.5:3.5:1.5:0.35。
步骤(2)中,水提取的具体方法为:将山金车、盐肤木、白芥子、细辛、香柏和甘草加入它们总重量6倍的水中,加热至沸腾,保温提取45分钟,过滤,得到水提液和残渣。
步骤(2)中,超临界CO2萃取的工艺条件为:采用无水乙醇作为夹带剂,萃取压力30MPa,萃取温度45℃,萃取时间2.5小时,CO2流量为29L/h。
步骤(3)中,变性淀粉、低聚果糖、聚甘油脂肪酸酯、锗掺杂碳量子点、水提液的质量比为1:5:0.07:0.06:11。
步骤(3)中,镭石粉、高纯氮化镓粉末的质量比为1:0.15。
步骤(3)中,改性混合粉的制备方法如下:先将1kg 3-(七氟异丙氧基)丙基三乙氧基硅烷加入35kg无水乙醇中,搅拌分散均匀,接着加入0.3kg混合粉,搅拌分散均匀,滴加冰醋酸调节pH=4,400W超声波振荡55分钟,加热至50℃,保温搅拌4.5小时,旋蒸除去乙醇,即得所述的改性混合粉。
步骤(3)中,改性混合粉与提取油的质量比为1:4.5,油相与水相的质量比为1:9。
步骤(3)中,油相均匀加入水相的时间为30分钟,乳化的工艺条件为:19000r/min剪切乳化35分钟;均质化的工艺条件为:80MPa条件下均质化2次。
步骤(4)中,膨化处理的蚕丝原料与微囊分散液的质量比为1:3.5;超声波浸渍处理的工艺条件为:400W超声波浸渍2.5小时。
步骤(4)中,所述膨化处理的蚕丝原料的制备方法如下:先将1kg清洗后的蚕茧加入100kg蛋白酶溶液中,35℃浸泡42小时,然后转移至清水中,撕开茧层,去掉蚕蛹,套环,丝套,接着转移至55kg含有2-十一烷基-N-羧甲基-N-羟乙基咪唑啉的碳酸氢钠水溶液中,85℃蒸煮7分钟,取出后洗涤至中性,烘干,即得所述的预膨化蚕丝原料;其中,蛋白酶溶液中含有:质量浓度0.1%碱性蛋白酶,质量浓度0.1%木瓜蛋白酶,余量为水;所述碳酸氢钠水溶液中含有:质量浓度0.3%2-十一烷基-N-羧甲基-N-羟乙基咪唑啉,质量浓度0.7%碳酸氢钠,余量为水。
对比例1
一种缓解肌肉关节疼痛的蚕丝的制备方法,具体步骤如下:
(1)先以山金车、盐肤木、白芥子、细辛、香柏和甘草为原料,利用水提取,得到水提液和残渣,接着将残渣经超临界CO2萃取,得到提取油;
(2)再将变性淀粉、低聚果糖、聚甘油脂肪酸酯加入水提液中,30℃搅拌40分钟,作为水相;接着将镭石粉、高纯氮化镓粉末混合研磨成300目的混合粉,之后将混合粉利用3-(七氟异丙氧基)丙基三乙氧基硅烷进行表面改性,得到改性混合粉,再将改性混合粉加入提取油中,60℃搅拌30分钟,即得油相;再将油相均匀缓慢加入水相中,乳化,均质化,得到微囊分散液;
(3)最后将预膨化蚕丝原料加入微囊分散液中,超声波浸渍处理,取出后烘干,即得所述的蚕丝。
步骤(1)中,山金车、盐肤木、白芥子、细辛、香柏和甘草的质量比为10:8:5:4:1:0.4。
步骤(1)中,水提取的具体方法为:将山金车、盐肤木、白芥子、细辛、香柏和甘草加入它们总重量5倍的水中,加热至沸腾,保温提取40分钟,过滤,得到水提液和残渣。
步骤(1)中,超临界CO2萃取的工艺条件为:采用无水乙醇作为夹带剂,萃取压力32MPa,萃取温度40℃,萃取时间3小时,CO2流量为28L/h。
步骤(2)中,变性淀粉、低聚果糖、聚甘油脂肪酸酯、水提液的质量比为1:6:0.06:10。
步骤(2)中,镭石粉、高纯氮化镓粉末的质量比为1:0.2。
步骤(2)中,改性混合粉的制备方法如下:先将1kg 3-(七氟异丙氧基)丙基三乙氧基硅烷加入30kg无水乙醇中,搅拌分散均匀,接着加入0.35kg混合粉,搅拌分散均匀,滴加冰醋酸调节pH=3,500W超声波振荡50分钟,加热至55℃,保温搅拌4小时,旋蒸除去乙醇,即得所述的改性混合粉。
步骤(2)中,改性混合粉与提取油的质量比为1:5,油相与水相的质量比为1:8。
步骤(2)中,油相均匀加入水相的时间为30分钟,乳化的工艺条件为:20000r/min剪切乳化30分钟;均质化的工艺条件为:90MPa条件下均质化2次。
步骤(3)中,膨化处理的蚕丝原料与微囊分散液的质量比为1:4;超声波浸渍处理的工艺条件为:300W超声波浸渍3小时。
步骤(3)中,所述膨化处理的蚕丝原料的制备方法如下:先将1kg清洗后的蚕茧加入100kg蛋白酶溶液中,30℃浸泡45小时,然后转移至清水中,撕开茧层,去掉蚕蛹,套环,丝套,接着转移至50kg含有2-十一烷基-N-羧甲基-N-羟乙基咪唑啉的碳酸氢钠水溶液中,90℃蒸煮6分钟,取出后洗涤至中性,烘干,即得所述的预膨化蚕丝原料;其中,蛋白酶溶液中含有:质量浓度0.1%碱性蛋白酶,质量浓度0.1%木瓜蛋白酶,余量为水;所述碳酸氢钠水溶液中含有:质量浓度0.3%2-十一烷基-N-羧甲基-N-羟乙基咪唑啉,质量浓度0.7%碳酸氢钠,余量为水。
对比例2
一种缓解肌肉关节疼痛的蚕丝的制备方法,具体步骤如下:
(1)先以柠檬酸和偏锗酸钠为原料制备锗掺杂碳量子点;
(2)然后以山金车、盐肤木、细辛、香柏和甘草为原料,利用水提取,得到水提液和残渣,接着将残渣经超临界CO2萃取,得到提取油;
(3)再将变性淀粉、低聚果糖、聚甘油脂肪酸酯、锗掺杂碳量子点加入水提液中,30℃搅拌40分钟,作为水相;接着将镭石粉、高纯氮化镓粉末混合研磨成300目的混合粉,之后将混合粉利用3-(七氟异丙氧基)丙基三乙氧基硅烷进行表面改性,得到改性混合粉,再将改性混合粉加入提取油中,60℃搅拌30分钟,即得油相;再将油相均匀缓慢加入水相中,乳化,均质化,得到微囊分散液;
(4)最后将预膨化蚕丝原料加入微囊分散液中,超声波浸渍处理,取出后烘干,即得所述的蚕丝。
步骤(1)的具体方法如下:将1份柠檬酸和0.2kg偏锗酸钠加入15kg水中,搅拌至完全溶解,160℃搅拌反应2小时,自然冷却至室温,离心取上清,透析,干燥,即得锗掺杂碳量子点。
透析的具体方法为:200Da透析袋透析2天,每5小时换一次水。
步骤(2)中,山金车、盐肤木、细辛、香柏和甘草的质量比为10:8:4:1:0.4。
步骤(2)中,水提取的具体方法为:将山金车、盐肤木、细辛、香柏和甘草加入它们总重量5倍的水中,加热至沸腾,保温提取40分钟,过滤,得到水提液和残渣。
步骤(2)中,超临界CO2萃取的工艺条件为:采用无水乙醇作为夹带剂,萃取压力32MPa,萃取温度40℃,萃取时间3小时,CO2流量为28L/h。
步骤(3)中,变性淀粉、低聚果糖、聚甘油脂肪酸酯、锗掺杂碳量子点、水提液的质量比为1:6:0.06:0.07:10。
步骤(3)中,镭石粉、高纯氮化镓粉末的质量比为1:0.2。
步骤(3)中,改性混合粉的制备方法如下:先将1kg 3-(七氟异丙氧基)丙基三乙氧基硅烷加入30kg无水乙醇中,搅拌分散均匀,接着加入0.35kg混合粉,搅拌分散均匀,滴加冰醋酸调节pH=3,500W超声波振荡50分钟,加热至55℃,保温搅拌4小时,旋蒸除去乙醇,即得所述的改性混合粉。
步骤(3)中,改性混合粉与提取油的质量比为1:5,油相与水相的质量比为1:8。
步骤(3)中,油相均匀加入水相的时间为30分钟,乳化的工艺条件为:20000r/min剪切乳化30分钟;均质化的工艺条件为:90MPa条件下均质化2次。
步骤(4)中,膨化处理的蚕丝原料与微囊分散液的质量比为1:4;超声波浸渍处理的工艺条件为:300W超声波浸渍3小时。
步骤(4)中,所述膨化处理的蚕丝原料的制备方法如下:先将1kg清洗后的蚕茧加入100kg蛋白酶溶液中,30℃浸泡45小时,然后转移至清水中,撕开茧层,去掉蚕蛹,套环,丝套,接着转移至50kg含有2-十一烷基-N-羧甲基-N-羟乙基咪唑啉的碳酸氢钠水溶液中,90℃蒸煮6分钟,取出后洗涤至中性,烘干,即得所述的预膨化蚕丝原料;其中,蛋白酶溶液中含有:质量浓度0.1%碱性蛋白酶,质量浓度0.1%木瓜蛋白酶,余量为水;所述碳酸氢钠水溶液中含有:质量浓度0.3%2-十一烷基-N-羧甲基-N-羟乙基咪唑啉,质量浓度0.7%碳酸氢钠,余量为水。
对比例3
一种缓解肌肉关节疼痛的蚕丝的制备方法,具体步骤如下:
(1)先以柠檬酸和偏锗酸钠为原料制备锗掺杂碳量子点;
(2)然后以山金车、盐肤木、白芥子、细辛、香柏和甘草为原料,利用水提取,得到水提液和残渣,接着将残渣经超临界CO2萃取,得到提取油;
(3)再将变性淀粉、低聚果糖、聚甘油脂肪酸酯、锗掺杂碳量子点加入水提液中,30℃搅拌40分钟,作为水相;接着将镭石粉研磨至300目,之后利用3-(七氟异丙氧基)丙基三乙氧基硅烷进行表面改性,得到改性镭石粉,再将改性镭石粉加入提取油中,60℃搅拌30分钟,即得油相;再将油相均匀缓慢加入水相中,乳化,均质化,得到微囊分散液;
(4)最后将预膨化蚕丝原料加入微囊分散液中,超声波浸渍处理,取出后烘干,即得所述的蚕丝。
步骤(1)的具体方法如下:将1份柠檬酸和0.2kg偏锗酸钠加入15kg水中,搅拌至完全溶解,160℃搅拌反应2小时,自然冷却至室温,离心取上清,透析,干燥,即得锗掺杂碳量子点。
透析的具体方法为:200Da透析袋透析2天,每5小时换一次水。
步骤(2)中,山金车、盐肤木、白芥子、细辛、香柏和甘草的质量比为10:8:5:4:1:0.4。
步骤(2)中,水提取的具体方法为:将山金车、盐肤木、白芥子、细辛、香柏和甘草加入它们总重量5倍的水中,加热至沸腾,保温提取40分钟,过滤,得到水提液和残渣。
步骤(2)中,超临界CO2萃取的工艺条件为:采用无水乙醇作为夹带剂,萃取压力32MPa,萃取温度40℃,萃取时间3小时,CO2流量为28L/h。
步骤(3)中,变性淀粉、低聚果糖、聚甘油脂肪酸酯、锗掺杂碳量子点、水提液的质量比为1:6:0.06:0.07:10。
步骤(3)中,改性镭石粉的制备方法如下:先将1kg 3-(七氟异丙氧基)丙基三乙氧基硅烷加入30kg无水乙醇中,搅拌分散均匀,接着加入0.35kg镭石粉,搅拌分散均匀,滴加冰醋酸调节pH=3,500W超声波振荡50分钟,加热至55℃,保温搅拌4小时,旋蒸除去乙醇,即得所述的改性镭石粉。
步骤(3)中,改性镭石粉与提取油的质量比为1:5,油相与水相的质量比为1:8。
步骤(3)中,油相均匀加入水相的时间为30分钟,乳化的工艺条件为:20000r/min剪切乳化30分钟;均质化的工艺条件为:90MPa条件下均质化2次。
步骤(4)中,膨化处理的蚕丝原料与微囊分散液的质量比为1:4;超声波浸渍处理的工艺条件为:300W超声波浸渍3小时。
步骤(4)中,所述膨化处理的蚕丝原料的制备方法如下:先将1kg清洗后的蚕茧加入100kg蛋白酶溶液中,30℃浸泡45小时,然后转移至清水中,撕开茧层,去掉蚕蛹,套环,丝套,接着转移至50kg含有2-十一烷基-N-羧甲基-N-羟乙基咪唑啉的碳酸氢钠水溶液中,90℃蒸煮6分钟,取出后洗涤至中性,烘干,即得所述的预膨化蚕丝原料;其中,蛋白酶溶液中含有:质量浓度0.1%碱性蛋白酶,质量浓度0.1%木瓜蛋白酶,余量为水;所述碳酸氢钠水溶液中含有:质量浓度0.3%2-十一烷基-N-羧甲基-N-羟乙基咪唑啉,质量浓度0.7%碳酸氢钠,余量为水。
对比例4
一种缓解肌肉关节疼痛的蚕丝的制备方法,具体步骤如下:
(1)先以柠檬酸和偏锗酸钠为原料制备锗掺杂碳量子点;
(2)然后以山金车、盐肤木、白芥子、细辛、香柏和甘草为原料,利用水提取,得到水提液和残渣,接着将残渣经超临界CO2萃取,得到提取油;
(3)再将变性淀粉、低聚果糖、聚甘油脂肪酸酯、锗掺杂碳量子点加入水提液中,30℃搅拌40分钟,作为水相;接着将镭石粉、高纯氮化镓粉末混合研磨成300目的混合粉,之后将混合粉加入提取油中,60℃搅拌30分钟,即得油相;再将油相均匀缓慢加入水相中,乳化,均质化,得到微囊分散液;
(4)最后将预膨化蚕丝原料加入微囊分散液中,超声波浸渍处理,取出后烘干,即得所述的蚕丝。
步骤(1)的具体方法如下:将1份柠檬酸和0.2kg偏锗酸钠加入15kg水中,搅拌至完全溶解,160℃搅拌反应2小时,自然冷却至室温,离心取上清,透析,干燥,即得锗掺杂碳量子点。
透析的具体方法为:200Da透析袋透析2天,每5小时换一次水。
步骤(2)中,山金车、盐肤木、白芥子、细辛、香柏和甘草的质量比为10:8:5:4:1:0.4。
步骤(2)中,水提取的具体方法为:将山金车、盐肤木、白芥子、细辛、香柏和甘草加入它们总重量5倍的水中,加热至沸腾,保温提取40分钟,过滤,得到水提液和残渣。
步骤(2)中,超临界CO2萃取的工艺条件为:采用无水乙醇作为夹带剂,萃取压力32MPa,萃取温度40℃,萃取时间3小时,CO2流量为28L/h。
步骤(3)中,变性淀粉、低聚果糖、聚甘油脂肪酸酯、锗掺杂碳量子点、水提液的质量比为1:6:0.06:0.07:10。
步骤(3)中,镭石粉、高纯氮化镓粉末的质量比为1:0.2。
步骤(3)中,混合粉与提取油的质量比为1:5,油相与水相的质量比为1:8。
步骤(3)中,油相均匀加入水相的时间为30分钟,乳化的工艺条件为:20000r/min剪切乳化30分钟;均质化的工艺条件为:90MPa条件下均质化2次。
步骤(4)中,膨化处理的蚕丝原料与微囊分散液的质量比为1:4;超声波浸渍处理的工艺条件为:300W超声波浸渍3小时。
步骤(4)中,所述膨化处理的蚕丝原料的制备方法如下:先将1kg清洗后的蚕茧加入100kg蛋白酶溶液中,30℃浸泡45小时,然后转移至清水中,撕开茧层,去掉蚕蛹,套环,丝套,接着转移至50kg含有2-十一烷基-N-羧甲基-N-羟乙基咪唑啉的碳酸氢钠水溶液中,90℃蒸煮6分钟,取出后洗涤至中性,烘干,即得所述的预膨化蚕丝原料;其中,蛋白酶溶液中含有:质量浓度0.1%碱性蛋白酶,质量浓度0.1%木瓜蛋白酶,余量为水;所述碳酸氢钠水溶液中含有:质量浓度0.3%2-十一烷基-N-羧甲基-N-羟乙基咪唑啉,质量浓度0.7%碳酸氢钠,余量为水。
对上述实施例和对比例所制备的蚕丝的性能进行评价:
按照重量为3kg,尺寸为180cm×200cm的规格,采用人工分别将实施例1~3和对比例1~4所得蚕丝扯松、叠加,加工成蚕丝被。
选择160例志愿者进行蚕丝被进行功效实验考察,志愿者参考《中医病症诊断疗效标准》进行诊断,肌肉、关节酸痛僵硬,有沉重感,天气改变及劳累后可使症状加重,年龄30~50岁,男女各半,平均分为8组,其中1组作为对照组,每晚睡眠时间使用市场上的普通蚕丝被,其余7组分别使用实施例1~3和对比例1~4所得蚕丝加工成的蚕丝被。连续使用60天后考察使用效果。
评价标准:
痊愈,肌肉关节酸痛感完全消失,没有沉重感,天气改变及劳累后没有酸痛症状;
显效,肌肉关节酸痛感消失,没有沉重感,天气改变及劳累后有酸痛感;
有效,肌肉关节酸痛感减弱,略有沉重感,天气改变及劳累后有酸痛感;
无效,肌肉关节酸痛感明显,有沉重感,天气改变及劳累后有酸痛感。
表1.蚕丝被使用效果考察
痊愈(例) | 显效(例) | 有效(例) | 无效(例) | |
对照组 | 0 | 0 | 0 | 20 |
实施例1 | 19 | 1 | 0 | 0 |
实施例2 | 18 | 2 | 0 | 0 |
实施例3 | 20 | 0 | 0 | 0 |
对比例1 | 6 | 6 | 5 | 3 |
对比例2 | 10 | 5 | 3 | 2 |
对比例3 | 8 | 6 | 4 | 2 |
对比例4 | 13 | 4 | 2 | 1 |
由表1可知,与对照组相比,实施例1~3所得蚕丝加工成的蚕丝被对肌肉关节酸痛具有较好的缓解效果。
对于本领域技术人员而言,显然本发明不限于上述示范性实施例的细节,而且在不背离本发明的精神或基本特征的情况下,能够以其他的具体形式实现本发明。因此,无论从哪一点来看,均应将实施例看作是示范性的,而且是非限制性的,本发明的范围由所附权利要求而不是上述说明限定,因此旨在将落在权利要求的等同要件的含义和范围内的所有变化囊括在本发明内。
此外,应当理解,虽然本说明书按照实施方式加以描述,但并非每个实施方式仅包含一个独立的技术方案,说明书的这种叙述方式仅仅是为清楚起见,本领域技术人员应当将说明书作为一个整体,各实施例中的技术方案也可以经适当组合,形成本领域技术人员可以理解的其他实施方式。
Claims (10)
1.一种缓解肌肉关节疼痛蚕丝的制备方法,其特征在于,具体步骤如下:
(1)以柠檬酸和偏锗酸钠为原料制备锗掺杂碳量子点;
(2)以山金车、盐肤木、白芥子、细辛、香柏和甘草为原料,利用水提取,得到水提液和残渣,接着将残渣经超临界CO2萃取,得到提取油;
(3)将变性淀粉、低聚果糖、聚甘油脂肪酸酯、步骤(1)制备的锗掺杂碳量子点加入步骤(2)得到的水提液中,30~40℃搅拌30~40分钟,作为水相;接着将镭石粉、高纯氮化镓粉末混合研磨成300~400目的混合粉,之后将混合粉利用3-(七氟异丙氧基)丙基三乙氧基硅烷进行表面改性,得到改性混合粉,再将改性混合粉加入步骤(2)中的提取油中,50~60℃搅拌30~40分钟,即得油相;再将油相均匀缓慢加入水相中,乳化,均质化,得到微囊分散液;
(4)将预膨化蚕丝原料加入步骤(3)制得的微囊分散液中,超声波浸渍处理,取出后烘干,即得所述的蚕丝。
2.根据权利要求1所述的制备方法,其特征在于,以重量份计,步骤(1)的具体方法如下:将1份柠檬酸和0.1~0.2份偏锗酸钠加入15~20份水中,搅拌至完全溶解,150~160℃搅拌反应2~3小时,自然冷却至室温,离心取上清,透析,干燥,即得锗掺杂碳量子点。
3.根据权利要求1所述的制备方法,其特征在于,步骤(2)中,山金车、盐肤木、白芥子、细辛、香柏和甘草的质量比为10:7~8:5~6:3~4:1~2:0.3~0.4。
4.根据权利要求1所述的制备方法,其特征在于,步骤(2)中,水提取的具体方法为:将山金车、盐肤木、白芥子、细辛、香柏和甘草加入它们总重量5~7倍的水中,加热至沸腾,保温提取40~50分钟,过滤,得到水提液和残渣。
5.根据权利要求1所述的制备方法,其特征在于,步骤(3)中,以重量份计,改性混合粉的制备方法如下:先将1份3-(七氟异丙氧基)丙基三乙氧基硅烷加入30~40份无水乙醇中,搅拌分散均匀,接着加入0.25~0.35份混合粉,搅拌分散均匀,滴加冰醋酸调节pH=3~5,300~500W超声波振荡50~60分钟,加热至45~55℃,保温搅拌4~5小时,旋蒸除去乙醇,即得所述的改性混合粉。
6.根据权利要求1所述的制备方法,其特征在于,步骤(4)中,以重量份计,所述膨化处理的蚕丝原料的制备方法如下:先将1份清洗后的蚕茧加入100份蛋白酶溶液中,30~40℃浸泡40~45小时,然后转移至清水中,撕开茧层,去掉蚕蛹,套环,丝套,接着转移至50~60份含有2-十一烷基-N-羧甲基-N-羟乙基咪唑啉的碳酸氢钠水溶液中,80~90℃蒸煮6~8分钟,取出后洗涤至中性,烘干,即得所述的预膨化蚕丝原料;其中,蛋白酶溶液中含有:质量浓度0.1%碱性蛋白酶,质量浓度0.1%木瓜蛋白酶,余量为水;所述碳酸氢钠水溶液中含有:质量浓度0.3%2-十一烷基-N-羧甲基-N-羟乙基咪唑啉,质量浓度0.7%碳酸氢钠,余量为水。
7.一种利用权利要求1~6中任一项所述制备方法得到的缓解肌肉关节疼痛的蚕丝。
8.一种权利要求1-7中任一项所述缓解肌肉关节疼痛的蚕丝在蚕丝被加工中的应用。
9.一种缓解肌肉关节疼痛的蚕丝被,其特征在于,所述蚕丝被是利用权利要求7所述蚕丝加工而成的。
10.一种权利要求9所述缓解肌肉关节疼痛的蚕丝被的加工方法,其特征在于,将所述蚕丝扯松、叠加后,按照重量和尺寸规格加工而得。
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