WO2020011240A1 - 一种双敏感性纤维素基气凝胶的制备方法 - Google Patents
一种双敏感性纤维素基气凝胶的制备方法 Download PDFInfo
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- C08J2333/14—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing halogen, nitrogen, sulfur, or oxygen atoms in addition to the carboxy oxygen
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Definitions
- the invention belongs to a method for modifying natural polymer materials, and particularly relates to a method for preparing a dual-sensitivity cellulose-based aerogel.
- the purpose of the present invention is to overcome the shortcomings of the prior art, provide a method for preparing a dual-sensitivity cellulose-based aerogel, and solve the problems in the background art described above.
- the technical solution adopted by the present invention to solve its technical problem is to provide a method for preparing a dual-sensitivity cellulose-based aerogel, including the following steps:
- DAC cellulose and IO 4 - donor are thoroughly mixed at a molar ratio of 1: 0.2-2.0%, stirred at 25-75 ° C in the dark for 0.5-48h, washed with deionized water, and dialyzed to obtain DAC, molecular weight Is 5000-20000;
- the step (1) further comprises preparing a DAC aqueous dispersion: adding the DAC to deionized water, and reacting at 70-150 ° C for 0.5h-4h at a stirring speed of 200-1000rpm, and centrifuging After concentration, a transparent DAC aqueous dispersion was obtained.
- the cellulose includes natural biomass cellulose and cellulose chemicals, and the natural biomass cellulose includes cellulose extracted from bamboo, wood, and cotton; and the cellulose Chemicals include microcrystalline cellulose and nanocellulose.
- the IO 4 - donors include periodic acid, sodium periodate, potassium periodate.
- a reducing agent is added in the step (3), and the reducing agent includes at least one of lithium aluminum hydride, potassium borohydride, sodium borohydride, and sodium cyanoborohydride.
- the preparation method of the invention has simple operation, low raw material price, wide source, environmental protection, low cost, good biocompatibility, and meets the requirements of sustainable development.
- the cellulose aerogel prepared by the present invention has small density, light weight, small toxic and side effects, good pH and temperature sensitivity, and can specifically deliver drugs into the stomach or intestine, thereby improving drug efficiency and Targeting, suitable for drug sustained release, medical dressings, etc., has broad application prospects in biomedical materials.
- a method for preparing a dual-sensitivity cellulose-based aerogel is prepared by using biomass cellulose as a raw material, and includes the following steps:
- Pretreatment-preparation of cellulose suspension 200g of pulp (or bamboo pulp) is immersed in water for 1 to 2 hours, and mechanical stirring at a speed of less than 100 rpm is used for 2 to 5 hours; then an ultrafine mill is used at a speed of 1000 to 2000 rpm , The disc gap gradually decreased from 2mm to 0 ⁇ m or even lower. The pulp was fibrillated by means of cyclic feeding. Finally, the dispersion was homogenized 10 to 30 times using a high-pressure homogenization method, and then concentrated to a certain degree by rotary evaporation A cellulose suspension with good stability is obtained (pulp concentration is 0.55 wt% and bamboo pulp concentration is 0.48 wt%);
- DAC dialdehyde cellulose
- PDMAEMA is a temperature- and pH-sensitive polymer.
- hydrophilic tertiary amine groups, carbonyl groups, and hydrophobic alkyl groups are present.
- the two types of groups are in spatial structure with each other. match.
- step (1) Take 10 ml of the homogeneous dispersion of the copolymer obtained in step (1) to rapidly mold in liquid nitrogen at -196 ° C, and then put it into a freeze-drying chamber for 12 hours to obtain the product.
- microcrystalline cellulose which is a cellulose chemical purchased on the market.
- the cellulose suspension without the step (0) is used as a raw material to prepare a cellulose suspension.
- the specific steps are as follows:
- Example 6 also uses a commercially available cellulose chemical to prepare a cellulose suspension without using the cellulose of step (0) as a raw material:
- a reducing agent is added in the step (3), and the reducing agent includes hydrogenation At least one of lithium aluminum, potassium borohydride, sodium borohydride, and sodium cyanoborohydride.
- the invention provides a method for preparing a dual-sensitivity cellulose-based aerogel, which solves the traditional pharmaceutical preparations that usually have many side effects, including the side effects of the gastrointestinal tract or kidney. Moreover, most drugs have a short half-life and must be taken several times a day to maintain therapeutic blood level problems, which has good industrial applicability.
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Abstract
本发明公开了一种双敏感性纤维素基气凝胶的制备方法,先后制备二醛纤维素、二醛纤维素/甲基丙烯酸二甲胺乙酯共聚物、二醛纤维素/甲基丙烯酸二甲胺乙酯/聚乙烯亚胺共聚物,然后进行冷冻干燥,即得产物;所述产物为双敏感性纤维素基气凝胶,其累积吸附量达250mg/g,其在0.2%NaC(pH<3),0.05mol/L NaH2PO4(pH=3-8)或NaOH(pH>8)的溶液中的累积释放量达63~90%,所得产物具有质量轻、生物相容性好、孔隙度高和pH/温度双敏感性等优点,可作为生物医用材料,如药物缓释、创口敷料等方面有广阔的应用前景。
Description
本发明属于天然高分子材料改性方法,具体涉及一种双敏感性纤维素基气凝胶的制备方法。
传统的药物制剂通常存在很多副作用,包括胃肠道或肾脏的副作用。而且,大多数药物半衰期较短,必须每日多次剂量服用,才能维持治疗性血液水平。因此,针对药物释放、药物作用强度和药效持续时间等已成为相关学科研究的主题。
目前,已经开发了一些聚合物来实现药物缓释从而增加药效持续时间。然而,大多数药物制剂,如Pe、PP和PDMS是化学合成的且非生物降解的。目前,天然多糖或其衍生物因具有可生物降解性、可再生性和低毒性成为载药制剂研究的首选。特别是纤维素在众多天然多糖中显示出的独特性质,如较大的比表面积,高强度和刚度,易化学修饰等优势引起各研究领域的广泛关注。
常用的药物传递系统包括离子交换树脂,薄膜,微球,凝胶等。气凝胶作为一种特殊的高孔材料,引起生物医学和医药应用领域的广泛兴趣。然而,对于原始纤维素,药物负载能力很低。因此,纤维素的化学改性成为提高其实用性的重要一步。聚乙烯亚胺(PEI)含有大量的伯胺和仲胺基在分子上,表现出优异的给药性能。聚甲基丙烯酸二甲胺乙酯(PDMAEMA)含有对H
+和OH
-敏感的基团,对外界pH和温度的变化有较敏锐的感知。可以作为智能材料递送载体使药物靶向性直达病灶部位,进而提高药物疗效,是目前给药系统发展的一种趋势。
发明内容
本发明的目的在于克服现有技术的不足之处,提供了一种双敏感性纤维素基气凝胶的制备方法,解决了上述背景技术中的问题。
本发明解决其技术问题所采用的技术方案是:提供了一种双敏感性纤维素基气凝胶的制备方法,包括如下步骤:
(1)制备DAC:将纤维素和IO
4
-供体以1:0.2~2.0%的摩尔比充分混合,25~75℃ 避光搅拌0.5~48h,经去离子水洗涤、透析得DAC,分子量为5000-20000;
(2)制备DAC/PDMAEMA共聚物:将步骤(1)产物和PDMAEMA加入到去离子水中,N
2氛围下搅拌均匀,得到混合液;调节混合液的pH≤3,并向混合液中加入CAN,在N
2保护下搅拌至少5h,经透析,得到DAC/PDMAEMA共聚物,分子量为5000-20000;其中,DAC、PDMAEMA和CAN的质量比为DAC:PDMAEMA:CAN=1.0g:5.0~50.0mg:0.5~5.0mg;
(3)制备DAC/PDMAEMA/PEI共聚物:将DAC/PDMAEMA共聚物与分子量小于10000的PEI以1:0.5~5.0的质量比充分混合,室温下搅拌进行接枝共聚,然后进行透析,即得DAC/PDMAEMA/PEI共聚物,分子量为5000-20000;
(4)制备气凝胶:取DAC/PDMAEMA/PEI共聚物的悬浮液快速冷冻,然后进行冷冻干燥,即得产物;所述产物为pH/温度双敏感性纤维素基气凝胶,其累积吸附量达250mg/g,其在0.05mol/L NaH
2PO
4(pH=3-8)或0.2%NaCl(pH<3)或NaOH(pH>8)溶液中的累积释放量达63~90%。
在本发明一较佳实施例中,所述步骤(1)还包括制备DAC水分散体:将DAC加入去离子水中,于200~1000rpm的搅拌速度下70~150℃反应0.5h~4h,离心、浓缩后得到透明DAC水分散体。
在本发明一较佳实施例中,所述纤维素包括天然生物质纤维素和纤维素化学品,所述天然生物质纤维素包括从竹子、木材、棉花提取的纤维素;所述的纤维素化学品包括微晶纤维素、纳米纤维素。
在本发明一较佳实施例中,所述的IO
4
-供体包括高碘酸、高碘酸钠、高碘酸钾。
在本发明一较佳实施例中,所述步骤(3)中加入还原剂,所述还原剂包括氢化铝锂、硼氢化钾、硼氢化钠、氰基硼氢化钠中的至少一种。
在本发明一较佳实施例中,所述步骤(4)中将产物在NaSA溶液中搅拌22~26h,测吸附量;然后在0.05mol/L、pH=7.4的NaH
2PO
4溶液或质量分数为0.2%、pH=2的NaCl溶液中测最高释放量。
本技术方案与背景技术相比,它具有如下优点:
1.本发明制备方法操作简单,原料价格低廉、来源广泛、环保,成本低,具有良好的生物相容性,符合可持续发展的要求。
2.本发明所制备的纤维素气凝胶密度小,质量轻,毒副作用小,具有较好的pH、温度敏感性,能够将药物特异性递送到胃内或肠内,从而提高药物效率和靶向性,适合用于药物缓释,医用敷料等方面,在生物医用材料方面具有广阔的应用前景。
实施例1
本实施例的一种双敏感性纤维素基气凝胶的制备方法,采用生物质纤维素为原料进行制备,包括如下步骤:
(0)前处理-制备纤维素悬浮液:将200g的纸浆(或竹浆)在水中浸泡1~2h,采用转速小于100rpm的机械搅拌2~5h;然后使用超微研磨机在转速1000~2000rpm,磨盘间隙从2mm逐渐降到0μm甚至更低,通过循环加料的方式对纸浆进行开纤化处理;最后采用高压均质法将分散液均质10~30次,再经一定程度的旋蒸浓缩得到稳定性良好的纤维素悬浮液(纸浆浓度为0.55wt%、竹浆浓度为0.48wt%);
(1)制备DAC(二醛纤维素):取上述100mL 0.55wt%木浆或竹浆纤维素和1.5g NaIO
4于250ml锥形瓶中,室温下避光搅拌6h,然后经离心、去离子水洗涤、透析得到0.42g/g的DAC水分散体;
(2)~(3)制备共聚物:取1g所得的DAC水分散体和50mg可聚合单体 PDMAEMA(聚甲基丙烯酸二甲胺乙酯,分子式:C
8H
15NO
2,分子量157.21)加入到盛有去离子水的三口烧瓶中在N
2氛围下搅拌均匀,用70%的HNO
3调节溶液的pH=3,向混合液中加入5mg CAN(硝酸铈铵)继续搅拌6h,透析,即得DAC/PDMAEMA共聚物。取1g上述所得的共聚物与2.5g PEI(Mw=600)充分混合,室温下搅拌12h,然后进行透析,并调节悬浮液浓度至约0.1%,得DAC/PDMAEMA/PEI共聚物;
其中,PDMAEMA是一种具有温度和pH敏感性的高分子,其分子结构单元中同时存在亲水性的叔胺基、羰基和疏水性的烷基基团,两类基团在空间结构上互相匹配。
(4)制备气凝胶:取10mlDAC/PDMAEMA/PEI共聚物的均匀分散液在-196℃的液氮中快速成型,然后将其放入冷冻干燥室12h,即得产物;
称取0.1g上述产物,在0.2M NaSA溶液中搅拌24h,吸附量达到95mg/g;在0.2%NaCl(pH=2)溶液中最高释放量达到近60%。
实施例2
实施例2与实施例1的区别在于:
(1)取2g实施例1步骤(1)的DAC水分散体于盛有100ml去离子水的圆底烧瓶中,100℃下搅拌2h,离心得浓度为3.2mg/mL的DAC水溶液。
(2)~(3):取50ml所得的DAC水溶液和20mg可聚合单体PDMAEMA加入到盛有去离子水的三口烧瓶中在N
2氛围下搅拌均匀,用70%的HNO
3调节溶液的pH<3,向混合液中加入5mg CAN继续搅拌6h,透析,即得DAC/PDMAEMA共聚物;取0.1g上述所得的共聚物与0.5g PEI(Mw=600)充分混合,室温下搅拌12h,然后进行透析,并调节悬浮液浓度至约0.1%,得DAC/PDMAEMA/PEI共聚物。
(4)取10mlDAC/PDMAEMA/PEI共聚物均匀分散液在-196℃的液氮中快速成型, 然后将其放入冷冻干燥室12h,即得产物。
称取0.1g产物,在0.1M NaSA溶液中搅拌24h,吸附量达到80mg/g;在0.05mol/L NaH
2PO
4(pH=7.4)溶液中最高释放量达到近90%。
实施例3
(1)取100mL 0.48wt%竹浆纤维素和1.75g NaIO
4于250ml锥形瓶中,室温下避光搅拌48h,然后经离心、去离子水洗涤、透析得到0.35g/g的DAC水分散体;
(2)~(3):取1g所得的DAC水分散体和50mg可聚合单体PDMAEMA加入到盛有去离子水的三口烧瓶中在N
2氛围下搅拌均匀,用70%的HNO
3调节溶液的pH=1,向混合液中加入3mg CAN继续搅拌12h,透析,即得DAC/PDMAEMA共聚物。取1g上述所得的共聚物与5.0g PEI(Mw=1800)充分混合,室温下搅拌12h,然后进行透析,并调节悬浮液浓度至约0.1%,得DAC/PDMAEMA/PEI共聚物。
(4)取10ml DAC/PDMAEMA/PEI共聚物均匀分散液在-196℃的液氮中快速成型,然后将其放入冷冻干燥室12h,即得产物。
(3)称取0.1g产物,在0.5M NaSA溶液中搅拌24h,吸附量达到90mg/g;在0.2%NaCl(pH=2)溶液中最高释放量达到近63%。
实施例4
(1)取2g实施例3中得到的DAC水分散体于盛有100ml去离子水的圆底烧瓶中,100℃下搅拌2h,离心得浓度为2.1mg/mL的DAC水溶液。
(2)~(3)取50ml所得的DAC水溶液和20mg可聚合单体PDMAEMA加入到盛有去离子水的三口烧瓶中在N
2氛围下搅拌均匀,用70%的HNO
3调节溶液的pH=2, 向混合液中加入2mg CAN继续搅拌24h,透析,即得DAC/PDMAEMA共聚物。取0.1g上述所得的共聚物与0.5g PEI(Mw=1800)充分混合,室温下搅拌12h,然后进行透析,并调节悬浮液浓度至约0.1%,得DAC/PDMAEMA/PEI共聚物。
(4)取10ml步骤(1)所得的共聚物均匀分散液在-196℃的液氮中快速成型,然后将其放入冷冻干燥室12h,即得产物。
称取0.1g产物,在2.0M NaSA溶液中搅拌24h,吸附量达到64mg/g;在0.2%NaCl(pH=2)溶液中最高释放量达到近50%。
实施例5
本实施例采用的是微晶纤维素,为购置于市面的纤维素化学品,无需经步骤(0)的生物质纤维素为原料制备纤维素悬浮液,具体步骤如下:
(1)取1g微晶纤维素和0.5g NaIO
4于250ml锥形瓶中,室温下避光搅拌6h,然后经离心、去离子水洗涤、透析得到0.51g/g的DAC水分散体;
(2)取1g所得的DAC水分散体和30mg可聚合单体PDMAEMA加入到盛有去离子水的三口烧瓶中在N
2氛围下搅拌均匀,用70%的HNO
3调节溶液的pH=2,向混合液中加入5mg CAN继续搅拌12h,透析,即得DAC/PDMAEMA共聚物。
(3)取1g上述所得的共聚物与0.5g PEI(Mw=600)充分混合,室温下搅拌12h,然后进行透析,并调节悬浮液浓度至约0.1%,得DAC/PDMAEMA/PEI共聚物。
(4)取10ml DAC/PDMAEMA/PEI共聚物均匀分散液在-196℃的液氮中快速成型,然后将其放入冷冻干燥室12h,即得产物。
称取0.1g产物,在1.0M NaSA溶液中搅拌24h,吸附量达到82mg/g;在NaOH(pH=10.0)溶液中最高释放量达到近87%。
实施例6
实施例6同样采用购置于市面的纤维素化学品,无需经步骤(0)的生物质纤维素为原料制备纤维素悬浮液:
(1)取1g纳米纤维素和2.0g NaIO
4于250ml锥形瓶中,室温下避光搅拌6h,然后经离心、去离子水洗涤、透析得到0.44g/g的DAC水分散体;
(2)取1g所得的DAC水分散体和5mg可聚合单体PDMAEMA加入到盛有去离子水的三口烧瓶中在N
2氛围下搅拌均匀,用HNO
3调节溶液的pH=2,向混合液中加入5mg CAN继续搅拌6h,透析,即得DAC/PDMAEMA共聚物。
(3)取1g上述所得的共聚物与5.0g PEI(Mw=10000)充分混合,室温下搅拌12h,然后进行透析,并调节悬浮液浓度至约0.1%,得DAC/PDMAEMA/PEI共聚物。
(4)取10ml DAC/PDMAEMA/PEI共聚物均匀分散液在-196℃的液氮中快速成型,然后将其放入冷冻干燥室12h,即得产物。
称取0.1g产物,在0.01M NaSA溶液中搅拌24h,吸附比例为56%;在0.05mol/L NaH
2PO
4(pH=5.7)溶液中最高释放量达到近60%。
实施例7
(1)取1g纳米纤维素和1.0g NaIO
4于250ml锥形瓶中,室温下避光搅拌60h,然后经离心、去离子水洗涤、透析得到0.37g/g的DAC水分散体;
(2)取1g所得的DAC水分散体和50mg可聚合单体PDMAEMA加入到盛有去离子水的三口烧瓶中在N
2氛围下搅拌均匀,用HNO
3调节溶液的pH=2,向混合液中加入5mg CAN继续搅拌12h,透析,即得DAC/PDMAEMA共聚物。
(3)取1g上述所得的共聚物与2.5g PEI(Mw=1800)充分混合,添加室温下搅拌12h,然后进行透析,并调节悬浮液浓度至约0.1%,得DAC/PDMAEMA/PEI共聚物。
(4)取10ml DAC/PDMAEMA/PEI共聚物均匀分散液在-196℃的液氮中快速成型,然后将其放入冷冻干燥室12h,即得产物。
称取0.1g产物,在0.02M NaSA溶液中搅拌24h,吸附比例为70%;在0.2%NaCl(pH=2)溶液中最高释放量达到近55%。
实施例8
(1)取1g纳米纤维素和1.0g NaIO
4于250ml锥形瓶中,室温下避光搅拌60h,然后经离心、去离子水洗涤、透析得到0.37g/g的DAC水分散体;
(2)取1g所得的DAC水分散体和50mg可聚合单体PDMAEMA加入到盛有去离子水的三口烧瓶中在N
2氛围下搅拌均匀,用HNO
3调节溶液的pH=2,向混合液中加入5mg CAN继续搅拌12h,透析,即得DAC/PDMAEMA共聚物。
(3)取1g上述所得的共聚物与2.5g PEI(Mw=600)充分混合,添加0.1g的硼氢化钠室温下搅拌2h,然后进行透析,并调节悬浮液浓度至约0.1%,得DAC/PDMAEMA/PEI共聚物。
(2)取10ml DAC/PDMAEMA/PEI共聚物均匀分散液在-196℃的液氮中快速成型,然后将其放入冷冻干燥室12h,即得产物。
称取0.1g产物,在0.05M NaSA溶液中搅拌24h,吸附量达到91mg/g;在0.05mol/L NaH
2PO
4(pH=7.4)溶液中最高释放量达到近70%。
本领域技术人员可知,当本发明的技术参数在如下范围内变化时,可以预期得到与上述实施例相同或相近的技术效果:所述步骤(3)中加入还原剂,所述还原剂包括氢化铝锂、硼氢化钾、硼氢化钠、氰基硼氢化钠中的至少一种。
以上所述,仅为本发明较佳实施例而已,故不能依此限定本发明实施的范围,即依本发明专利范围及说明书内容所作的等效变化与修饰,皆应仍属本发明涵盖的范围内。
本发明提供了一种双敏感性纤维素基气凝胶的制备方法,解决了传统的药物制剂通常存在很多副作用,包括胃肠道或肾脏的副作用。而且,大多数药物半衰期较短,必须每日多次剂量服用,才能维持治疗性血液水平的问题,具有良好的工业实用性。
Claims (8)
- 一种双敏感性纤维素基气凝胶的制备方法,其特征在于,包括如下步骤:(1)制备DAC:将纤维素和IO 4 -供体以1:0.2~2.0%的摩尔比混合,25~75℃避光搅拌0.5~48h,经去离子水洗涤、透析得DAC,分子量为5000-20000;(2)制备DAC/PDMAEMA共聚物:将步骤(1)产物和PDMAEMA加入到去离子水中,N 2氛围下搅拌均匀,得到混合液;调节混合液的pH≤3,并向混合液中加入CAN,在N 2保护下搅拌至少5h,经透析,得到DAC/PDMAEMA共聚物,分子量为5000-20000;其中,DAC、PDMAEMA和CAN的质量比为DAC:PDMAEMA:CAN=1.0g:5.0~50.0mg:0.5~5.0mg;(3)制备DAC/PDMAEMA/PEI共聚物:将DAC/PDMAEMA共聚物与分子量小于10000的PEI以1:0.5~5.0的质量比混合,室温下搅拌进行接枝共聚,然后进行透析,即得DAC/PDMAEMA/PEI共聚物,分子量为5000-20000;(4)制备气凝胶:取DAC/PDMAEMA/PEI共聚物的悬浮液快速冷冻,然后进行冷冻干燥,即得产物;所述产物为pH/温度双敏感性纤维素基气凝胶,其累积吸附量达250mg/g,其在0.05mol/L NaH 2PO 4(pH=3-8)或0.2%NaCl(pH<3)或NaOH(pH>8)的累积释放量达63~90%。
- 根据权利要求1所述的一种双敏感性纤维素基气凝胶的制备方法,其特征在于,所述步骤(1)还包括制备DAC水分散体:将DAC加入去离子水中,于200~1000rpm的搅拌速度下70~150℃反应0.5h~4h,离心、浓缩后得到透明DAC水分散体。
- 根据权利要求1所述的一种双敏感性纤维素基气凝胶的制备方法,其特征在于:所述纤维素包括天然生物质纤维素和纤维素化学品,所述天然生物质纤维素包括从竹子、木材、棉花提取的纤维素;所述的纤维素化学品包括微晶纤维素、纳米纤维素。
- 根据权利要求1所述的一种双敏感性纤维素基气凝胶的制备方法,其特征在于:所述的IO 4 -供体包括高碘酸、高碘酸钠、高碘酸钾。
- 根据权利要求1所述的一种双敏感性纤维素基气凝胶的制备方法,其特征在于:所述步骤(3)中加入还原剂,所述还原剂包括氢化铝锂、硼氢化钾、硼氢化钠、氰基硼氢化钠中的至少一种。
- 根据权利要求1所述的一种双敏感性纤维素基气凝胶的制备方法,其特征在于:所述步骤(4)中将产物在NaSA溶液中搅拌22~26h,测吸附量;然后在0.05mol/L、pH=7.4的NaH 2PO 4溶液或质量分数为0.2%、pH=2的NaCl溶液中测最高释放量。
- 一种双敏感性纤维素基气凝胶的制备方法,其特征在于,包括如下步骤:(1)制备DAC:将纤维素和IO 4 -供体以1:0.2~2.0%的摩尔比混合,25~75℃避光搅拌0.5~48h,经去离子水洗涤、透析得DAC,分子量为5000-20000;(2)制备DAC/PDMAEMA共聚物:将步骤(1)产物和PDMAEMA加入到去离子水中,N 2氛围下搅拌均匀,得到混合液;调节混合液的pH≤3,并向混合液中加入CAN,在N 2保护下搅拌至少5h,经透析,得到DAC/PDMAEMA共聚物,分子量为5000-20000;其中,DAC、PDMAEMA和CAN的质量比为DAC:PDMAEMA:CAN=1.0g:5.0~50.0mg:0.5~5.0mg;(3)制备DAC/PDMAEMA/PEI共聚物:将DAC/PDMAEMA共聚物与分子量小于10000的PEI以1:0.5~5.0的质量比混合,室温下搅拌进行接枝共聚,然后进行透析,即得DAC/PDMAEMA/PEI共聚物,分子量为5000-20000;(4)制备气凝胶:取DAC/PDMAEMA/PEI共聚物的悬浮液快速冷冻,然后进行冷冻干燥,即得产物。
- 根据权利要求7所述的一种双敏感性纤维素基气凝胶的制备方法,其特征在 于:所述产物为pH/温度双敏感性纤维素基气凝胶,其累积吸附量达250mg/g,其在0.05mol/L NaH 2PO 4(pH=3-8)或0.2%NaCl(pH<3)或NaOH(pH>8)的累积释放量达63~90%。
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| CN109881489B (zh) * | 2019-01-30 | 2021-04-13 | 广西大学 | 一种多重响应性智能纳米纤维功能材料及其制备方法和应用 |
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| CN112911920B (zh) * | 2021-02-08 | 2022-09-02 | 浙江环龙新材料科技有限公司 | 一种MXene-碳气凝胶/TPU复合材料的制备方法 |
| CN119331305A (zh) * | 2024-12-19 | 2025-01-21 | 浙江农林大学 | 一种兼具吸湿和光热解吸的生物质气凝胶及其制备方法 |
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| Publication number | Publication date |
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| US12146042B2 (en) | 2024-11-19 |
| US20210130567A1 (en) | 2021-05-06 |
| CN109134914A (zh) | 2019-01-04 |
| CN109134914B (zh) | 2020-04-21 |
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