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CN115246908B - Preparation method and application of acidic pH response type hydrogel - Google Patents

Preparation method and application of acidic pH response type hydrogel Download PDF

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CN115246908B
CN115246908B CN202111575449.7A CN202111575449A CN115246908B CN 115246908 B CN115246908 B CN 115246908B CN 202111575449 A CN202111575449 A CN 202111575449A CN 115246908 B CN115246908 B CN 115246908B
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CN115246908A (en
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刘爱萍
许为中
李嘉欣
程琳
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Zhejiang Sci Tech University ZSTU
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Abstract

The invention relates to preparation and application of an acidic pH response hydrogel, which comprises the following steps: (1) Sequentially adding a monomer, a chemical crosslinking agent and a photoinitiator into deionized water, and stirring and dissolving under a light-shielding condition to obtain a clear hydrogel precursor liquid; (2) Sequentially placing dust-free paper with proper size and a silicon rubber gasket with variable thickness which are cut in advance on a glass plate, and sealing a die by using another glass plate; (3) Injecting the precursor solution into a mold, placing the mold in an ice-water bath, and carrying out in-situ radical polymerization reaction by ultraviolet irradiation to finally obtain the hydrogel driver with the hydrogel-paper double-layer structure. The acidic pH response hydrogel driver has the advantages of high sensitivity, wide pH response range and the like, and can be used for various types of valve applications such as single-pass valve, double-pass valve and the like.

Description

一种酸性pH响应型水凝胶的制备方法及其应用Preparation method and application of acidic pH-responsive hydrogel

技术领域Technical field

本发明属于水凝胶驱动器领域,尤其涉及一种酸性pH响应水凝胶的制备及其在驱动阀门领域的应用。The invention belongs to the field of hydrogel actuators, and in particular relates to the preparation of an acidic pH-responsive hydrogel and its application in the field of driving valves.

背景技术Background technique

水凝胶是一类由亲水高分子链通过物理或化学的方式组成三维网络结构并含有大量水的高分子材料。智能水凝胶是一类具有广泛应用前景的功能高分子材料,其采用功能性单体制备,能够感知外界环境的微小变化或者刺激(如ph值、温度、磁场等),产生结构或者化学性质的变化,通常表现是体积的相变。Hydrogel is a type of polymer material composed of hydrophilic polymer chains that form a three-dimensional network structure through physical or chemical means and contains a large amount of water. Smart hydrogel is a type of functional polymer material with broad application prospects. It is prepared from functional monomers and can sense small changes or stimuli in the external environment (such as pH value, temperature, magnetic field, etc.) and produce structural or chemical properties. The change is usually manifested as a phase change in volume.

酸性pH响应型水凝胶可以在不同酸性pH刺激下表现出预先设计好的行为(如弯曲、折叠、扭转等),而被认为在生物医学和软机器人领域具有广阔的应用前景。Acidic pH-responsive hydrogels can exhibit pre-designed behaviors (such as bending, folding, twisting, etc.) under different acidic pH stimuli, and are considered to have broad application prospects in the fields of biomedicine and soft robotics.

发明内容Contents of the invention

为扩大水凝胶的使用范围,本发明通过调节水凝胶的制备工艺,得到一种酸性pH响应水凝胶,并可应用在阀门驱动中,该酸性pH响应水凝胶的制备方法简单,使用能耗低。In order to expand the scope of use of hydrogel, the present invention obtains an acidic pH-responsive hydrogel by adjusting the preparation process of the hydrogel, and can be used in valve driving. The preparation method of the acidic pH-responsive hydrogel is simple. Low energy consumption.

为达到上述技术目的,本发明采用如下技术方案:In order to achieve the above technical objectives, the present invention adopts the following technical solutions:

一种酸性pH响应水凝胶的制备方法,所述方法包括:A method for preparing acidic pH-responsive hydrogel, the method comprising:

(1)水凝胶前驱体溶液的制备:将单体、化学交联剂和光引发剂按一定的比例溶解于去离子水中,避光条件下搅拌得到澄清的水凝胶前驱液;(1) Preparation of hydrogel precursor solution: Dissolve monomers, chemical cross-linking agents and photoinitiators in deionized water in a certain proportion, and stir under light-proof conditions to obtain a clear hydrogel precursor solution;

(2)注模:将无尘纸延表面条纹90°的方向裁剪备用,将无尘纸和可变厚且中间掏空面积的硅橡胶垫片依次放置在玻璃板上,用另一块玻璃杯密封模具,将前驱液注入模具内,注入过程应避免产生气泡;(2) Injection molding: Cut the dust-free paper along the 90° direction of the surface stripes for later use. Place the dust-free paper and the silicone rubber gasket that can be thickened and hollowed out in the middle on the glass plate in sequence, and use another glass cup. Seal the mold and inject the precursor liquid into the mold. Bubbles should be avoided during the injection process;

(3)交联:将步骤(2)中的模具置于冰水浴下,在距离模具一定距离采用波长365nm,功率250W紫外灯照射交联反应一段时间,脱模即可得到P(AAm-co-VI)水凝胶-纸双层结构;(3) Cross-linking: Place the mold in step (2) under an ice-water bath, use a UV lamp with a wavelength of 365nm and a power of 250W at a certain distance from the mold to irradiate the cross-linking reaction for a period of time, and demold to obtain P(AAm-co -VI) Hydrogel-paper double-layer structure;

(4)酸性PH下P(AAm-co-VI)水凝胶的响应:所得P(AAm-co-VI)水凝胶置于酸性环境下,测试弯曲性能和驱动行为。(4) Response of P(AAm-co-VI) hydrogel under acidic pH: The obtained P(AAm-co-VI) hydrogel was placed in an acidic environment to test the bending performance and driving behavior.

进一步地,所述单体包括丙烯酰胺和1-乙烯基咪唑,所述交联剂为N,N'-亚甲基双丙烯酰胺、所述引发剂为偶氮二异丁脒盐酸盐。Further, the monomers include acrylamide and 1-vinylimidazole, the cross-linking agent is N,N'-methylenebisacrylamide, and the initiator is azobisisobutylamidine hydrochloride.

进一步地,步骤(3)中紫外灯距离模具的距离为10~20nm。Further, in step (3), the distance between the ultraviolet lamp and the mold is 10 to 20 nm.

进一步地,所述紫外灯照射交联时间为2~10min。Further, the ultraviolet lamp irradiation cross-linking time is 2 to 10 minutes.

进一步地,所述酸性环境为PH=1~6。Further, the acidic environment is pH=1-6.

一种如上述所述方法制备的酸性PH响应型水凝胶驱动阀门,在酸性环境下处于打开状态,在中性或酸性环境下处于关闭状态,实现P(AAm-co-VI)水凝胶在酸性环境下的应用。An acidic pH-responsive hydrogel-driven valve prepared by the method described above is in an open state in an acidic environment and in a closed state in a neutral or acidic environment, realizing P(AAm-co-VI) hydrogel Applications in acidic environments.

本发明具有以下优点:通过选取耐酸性的合成水凝胶原料,再结合交联工艺,制备出酸性pH响应水凝胶,该制备方法简单易行,控制工艺参数可控,成本低廉,可重复性高。该酸性pH响应水凝胶具有灵敏度高和ph响应范围广等优点,且可用于阀门、水下抓手等。The invention has the following advantages: by selecting acid-resistant synthetic hydrogel raw materials and combining it with a cross-linking process, an acidic pH-responsive hydrogel is prepared. The preparation method is simple and easy to implement, the process parameters are controllable, the cost is low, and it is repeatable. High sex. The acidic pH-responsive hydrogel has the advantages of high sensitivity and wide pH response range, and can be used in valves, underwater grippers, etc.

附图说明Description of the drawings

图1为酸性pH响应水凝胶在不同pH下的驱动性能;Figure 1 shows the driving performance of acidic pH-responsive hydrogel at different pH;

图2为酸性pH响应水凝胶的SEM图;Figure 2 is an SEM image of acidic pH-responsive hydrogel;

图3为水凝胶的动力学示意图;Figure 3 is a schematic diagram of the dynamics of hydrogel;

图4为酸性pH响应水凝胶驱动阀门的开关过程示意图。Figure 4 is a schematic diagram of the switching process of the acidic pH-responsive hydrogel-driven valve.

具体实施方式Detailed ways

下面结合具体实施例对本发明进行详细说明。以下实施例将有助于本领域的技术人员进一步理解本发明,但不以任何形式限制本发现。应当指出的是,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。The present invention will be described in detail below with reference to specific embodiments. The following examples will help those skilled in the art to further understand the present invention, but do not limit the present invention in any form. It should be noted that, for those of ordinary skill in the art, several modifications and improvements can be made without departing from the concept of the present invention. These all belong to the protection scope of the present invention.

实施例1Example 1

一种酸性PH响应型水凝胶的制备方法,包括如下制备步骤:A method for preparing acidic pH-responsive hydrogel, including the following preparation steps:

(1)水凝胶前驱体溶液的制备:将0.890g的丙烯酰胺、0.133g的1-乙烯基咪唑、0.035g的N,N'-亚甲基双丙烯酰胺、0.045g的偶氮二异丁脒盐酸盐加入8.897g的水中,磁力搅拌下依次加入直至各组分完全溶解,得到澄清的水凝胶前驱液,避光搅拌保存;(1) Preparation of hydrogel precursor solution: 0.890g acrylamide, 0.133g 1-vinylimidazole, 0.035g N,N'-methylenebisacrylamide, 0.045g azobisiso Add butamidine hydrochloride to 8.897g of water, and add it in sequence under magnetic stirring until each component is completely dissolved to obtain a clear hydrogel precursor, which should be stored in the dark while stirring;

(2)注模:将无尘纸使裁剪为尺寸40mm×10mm、表面条纹为90°备用,将无尘纸和可变厚且中间掏空面积为40mm×10mm的硅橡胶垫片依次放置在玻璃板上,用另一块玻璃杯密封模具,将前驱液注入模具内,注入过程应避免产生气泡;(2) Injection molding: Cut the dust-free paper into a size of 40mm × 10mm, with surface stripes at 90° for later use. Place the dust-free paper and a silicone rubber gasket that can be thickened and has a hollow area of 40mm × 10mm in sequence. On the glass plate, seal the mold with another glass cup and inject the precursor liquid into the mold. Bubbles should be avoided during the injection process;

(3)交联:将步骤(2)中的模具置于冰水浴下,在距离模具15cm的位置采用波长365nm,功率250W紫外灯照射交联6min,脱模即可得到P(AAm-co-VI)水凝胶-纸双层结构;(3) Cross-linking: Place the mold in step (2) under an ice water bath, use a UV lamp with a wavelength of 365nm and a power of 250W at a position 15cm away from the mold to irradiate cross-linking for 6 minutes, and demold to obtain P(AAm-co- VI) Hydrogel-paper double-layer structure;

(4)酸性PH时水凝胶的响应:所得P(AAm-co-VI)水凝胶在置于pH=2的溶液中,80s就可以实现360°的弯曲,最大在420s实现649.748°超大弯曲;所得置于pH=4的溶液中,110s就可以实现360°的弯曲,最大在380s实习459.452°超大弯曲;所得P(AAm-co-VI)/纸复合水凝胶置于pH=6的溶液中,在180s可以实现360°的弯曲,最大在460s实习440.74°超大弯曲,如图1-3所示。(4) Response of the hydrogel at acidic pH: The resulting P(AAm-co-VI) hydrogel can achieve 360° bending in 80 s when placed in a solution with pH = 2, and can achieve a maximum of 649.748° in 420 s. Bending; the obtained P(AAm-co-VI)/paper composite hydrogel can be placed in a solution of pH=4, and 360° bending can be achieved in 110s, with a maximum bending of 459.452° in 380s; the obtained P(AAm-co-VI)/paper composite hydrogel can be placed in a solution of pH=6 In the solution, 360° bending can be achieved in 180s, and the maximum bending is 440.74° in 460s, as shown in Figure 1-3.

实施例2Example 2

一种酸性PH响应型水凝胶驱动阀门的制备方法,包括如下步骤:A preparation method for an acidic pH-responsive hydrogel-driven valve, including the following steps:

(1)水凝胶前驱体溶液的制备:将0.890g的丙烯酰胺、0.133g的1-乙烯基咪唑、0.035g的N,N'-亚甲基双丙烯酰胺、0.045g的偶氮二异丁脒盐酸盐加入8.897g的水中,磁力搅拌下依次加入直至各组分完全溶解,得到澄清的水凝胶前驱液,避光搅拌保存;(2)注模:将无尘纸使裁剪为尺寸40mm×10mm、表面条纹为90°备用,将无尘纸和可变厚且中间掏空面积为40mm×10mm的硅橡胶垫片依次放置在玻璃板上,用另一块玻璃杯密封模具,将前驱液注入模具内,注入过程应避免产生气泡;(1) Preparation of hydrogel precursor solution: 0.890g acrylamide, 0.133g 1-vinylimidazole, 0.035g N,N'-methylenebisacrylamide, 0.045g azobisiso Add butamidine hydrochloride to 8.897g of water, and add it in sequence under magnetic stirring until each component is completely dissolved to obtain a clear hydrogel precursor, which should be protected from light and stored under stirring; (2) Injection molding: cut the dust-free paper into The size is 40mm × 10mm and the surface stripes are 90°. Place the dust-free paper and the silicone rubber gasket that can be thickened and have a hollow area of 40mm × 10mm on the glass plate in sequence. Seal the mold with another glass cup. The precursor liquid is injected into the mold, and bubbles should be avoided during the injection process;

(3)交联:将步骤(2)中的模具置于冰水浴下,在距离模具15cm的位置采用波长365nm,功率250W紫外灯照射交联6min,脱模即可得到P(AAm-co-VI)水凝胶-纸双层结构。如图2所示,a、b、c分别为P(AAm-co-VI)水凝胶的正面、反面、横截面的SEM图。该水凝胶呈开孔状,结构均匀,孔径在50μm左右。d、e、f分别为P(AAm-co-VI)/纸复合水凝胶的整体及局部横截面的SEM图。水凝胶网络和纸的纤维结构互相嵌入,得到紧密结合的双层结构。(3) Cross-linking: Place the mold in step (2) under an ice water bath, use a UV lamp with a wavelength of 365nm and a power of 250W at a position 15cm away from the mold to irradiate cross-linking for 6 minutes, and demold to obtain P(AAm-co- VI) Hydrogel-paper bilayer structure. As shown in Figure 2, a, b, and c are the SEM images of the front, back, and cross sections of P(AAm-co-VI) hydrogel, respectively. The hydrogel is open-pored, has a uniform structure, and has a pore size of about 50 μm. d, e, and f are SEM images of the overall and partial cross-sections of P(AAm-co-VI)/paper composite hydrogel, respectively. The hydrogel network and the fiber structure of the paper are embedded in each other, resulting in a tightly coupled two-layer structure.

(4)酸性PH响应型水凝胶驱动阀门制备:采用P(AAm-co-VI)水凝胶制备阀门,得到的阀门在1mol/l HCl环境下实验,在水通过时关闭,在酸通过时打开,响应速度为90s,如图4所示。(4) Preparation of acidic pH-responsive hydrogel-driven valve: P(AAm-co-VI) hydrogel was used to prepare the valve. The obtained valve was tested in a 1mol/l HCl environment. It closed when water passed through and closed when acid passed through. When opened, the response speed is 90s, as shown in Figure 4.

对比例:Comparative ratio:

P(AAm-co-VI)水凝胶制备步骤(1)和(2)都与实施例1相同,步骤(3)如下:The preparation steps (1) and (2) of P(AAm-co-VI) hydrogel are the same as those in Example 1, and step (3) is as follows:

交联:将模具置于室温水中,在距离模具15cm的位置采用波长365nm,功率250W紫外灯照射交联6min,脱模即可得到P(AAm-co-VI)水凝胶-纸双层结构。Cross-linking: Place the mold in room temperature water, use a UV lamp with a wavelength of 365nm and a power of 250W at a distance of 15cm from the mold to irradiate cross-linking for 6 minutes. After demoulding, the P(AAm-co-VI) hydrogel-paper double-layer structure can be obtained. .

酸性PH时水凝胶的响应:将上述P(AAm-co-VI)水凝胶分别置于PH=2、4、6的溶液中,弯曲和驱动性能均比实施例1差,将其应用于酸性阀门中,在关闭状态有漏液现在。Response of the hydrogel at acidic pH: The above P(AAm-co-VI) hydrogel was placed in solutions with pH = 2, 4, and 6 respectively. The bending and driving properties were worse than those in Example 1, and they were applied In acidic valves, there is leakage in the closed state.

通过实施例1-2和对比例可知,通过控制交联环境,可实现P(AAm-co-VI)水凝胶在酸性环境下的驱动,扩大应用范围。It can be seen from Examples 1-2 and Comparative Examples that by controlling the cross-linking environment, the driving of P(AAm-co-VI) hydrogel in an acidic environment can be achieved and the application range can be expanded.

上述实例用来解释说明本发明,然而并非限定本发明。在本发明的精神和权利要求的保护范围内,对本发明作出的任何修改和改变,都落入本发明的保护范围。The above examples are used to illustrate the present invention, but do not limit the present invention. Within the spirit of the present invention and the protection scope of the claims, any modifications and changes made to the present invention fall within the protection scope of the present invention.

Claims (5)

1. A method of preparing an acidic pH-responsive hydrogel, the method comprising:
(1) Preparation of hydrogel precursor solution: dissolving a monomer, a chemical crosslinking agent and a photoinitiator in deionized water according to a certain proportion, and stirring under a dark condition to obtain a clear hydrogel precursor liquid; the monomer comprises acrylamide and 1-vinylimidazole, the cross-linking agent is N, N' -methylene bisacrylamide, and the initiator is azobisisobutyltime hydrochloride;
(2) Injection molding: cutting the dust-free paper along the direction of 90 degrees of surface stripes for later use, sequentially placing the dust-free paper and a silicon rubber gasket with variable thickness and hollow middle area on a glass plate, sealing a mould by using another glass cup, and injecting a precursor liquid into the mould, wherein the injection process should avoid generating bubbles;
(3) Crosslinking: placing the die in the step (2) under ice-water bath, irradiating and crosslinking for a period of time at a certain distance from the die by adopting a wavelength 365 and nm and a power 250 and W ultraviolet lamp, and demolding to obtain the P (AAm-co-VI) hydrogel-paper double-layer structure;
(4) Response of P (AAm-co-VI) hydrogels at acidic pH: the resulting P (AAm-co-VI) hydrogels were placed in an acidic environment and tested for flexural properties and driving behavior.
2. The method for preparing an acidic pH responsive hydrogel according to claim 1, wherein the distance from the ultraviolet lamp to the mold in the step (3) is 10-20 nm.
3. The method for preparing the acidic pH response hydrogel according to claim 2, wherein the ultraviolet lamp irradiation crosslinking time is 2-10 min.
4. The method for preparing an acidic pH-responsive hydrogel according to claim 1, wherein the acidic environment is ph=1 to 6.
5. The acidic PH-responsive hydrogel driving valve prepared by the method according to claim 1 is in an open state under an acidic environment and is in a closed state under a neutral or acidic environment, so that the application of the P (AAm-co-VI) hydrogel under the acidic environment is realized.
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CN111533925A (en) * 2020-03-20 2020-08-14 浙江理工大学 A kind of bilayer hydrogel, preparation method and application thereof

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CN109438728A (en) * 2018-10-29 2019-03-08 山东大学 A kind of Thermo-sensitive conductive hydrogel and preparation method thereof of metallic ion coordination effect enhancing
CN111533925A (en) * 2020-03-20 2020-08-14 浙江理工大学 A kind of bilayer hydrogel, preparation method and application thereof

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