技术领域technical field
本发明涉及功能材料，尤其是电刺激-近红外双重响应高强度水凝胶的制备。The invention relates to a functional material, especially the preparation of a high-strength hydrogel with dual responses of electrical stimulation and near-infrared.
背景技术Background technique
刺激响应水凝胶由于其结构中具有一定比例的亲水和疏水基团，外界刺激可以影响这些基团的亲/疏水作用或大分子链间的氢键作用，从而改变水凝胶的网络结构，产生体积和形状的变化。因此，其在药物控释系统、记忆元件开关、人造肌肉、化工分离等领域具有广泛的潜在价值，其中温度响应水凝胶是最受关注的水凝胶之一。Stimuli-responsive hydrogels have a certain proportion of hydrophilic and hydrophobic groups in their structure, and external stimuli can affect the hydrophilic/hydrophobic interactions of these groups or the hydrogen bonds between macromolecular chains, thereby changing the network structure of the hydrogel. , resulting in volume and shape changes. Therefore, it has a wide range of potential values in the fields of controlled drug release systems, memory element switches, artificial muscles, and chemical separation, among which temperature-responsive hydrogels are one of the most concerned hydrogels.
然而传统的温度响应水凝胶温度的变化受制于外界环境，刺激响应方式单一以及刺激响应灵敏度不佳，并且机械性能差，在一定程度上制约了水凝胶的应用。为克服传统的温度响应水凝胶的缺点，我们提出了一种新思路：通过向温度响应水凝胶中引入刺激响应生热的物质，以不同刺激源从水凝胶内部控制其的温度变化，从而实现水凝胶的温度响应。聚吡咯具有导电性和近红外响应性，将其与温度响应水凝胶结合，可以赋予水凝胶导电性和近红外吸收效应，能有效扩大水凝胶的应用范围。However, the temperature change of traditional temperature-responsive hydrogels is limited by the external environment, the stimulus response method is single, the stimulus response sensitivity is not good, and the mechanical properties are poor, which restricts the application of hydrogels to a certain extent. In order to overcome the shortcomings of traditional temperature-responsive hydrogels, we propose a new idea: by introducing stimuli-responsive thermogenic substances into the temperature-responsive hydrogels, the temperature changes can be controlled from the inside of the hydrogels with different stimuli. , so as to realize the temperature response of the hydrogel. Polypyrrole has electrical conductivity and near-infrared responsiveness. Combining it with temperature-responsive hydrogels can endow hydrogels with electrical conductivity and near-infrared absorption effects, which can effectively expand the application range of hydrogels.
发明内容Contents of the invention
本发明的目的是提供一种电刺激-近红外双重响应高强度水凝胶的制备方法，该方法制备的水凝胶具有电刺激/近红外的双重响应性，能够通过生物传感有效地控制其体积和形状的变化。其次，该水凝胶具有良好的机械性能和生物相容性。The purpose of the present invention is to provide a method for preparing high-strength hydrogel with dual response of electrical stimulation and near-infrared. The hydrogel prepared by this method has dual responsiveness of electrical stimulation and near-infrared, and can effectively control Changes in its size and shape. Second, the hydrogel has good mechanical properties and biocompatibility.
本发明为实现其发明目的，所采用的技术方案是，一种电刺激-近红外效应双重响应高强度水凝胶的制备方法，其具体步骤如下：In order to achieve the purpose of the invention, the present invention adopts a technical solution that is a method for preparing a high-strength hydrogel with double response of electric stimulation-near-infrared effect, and its specific steps are as follows:
A、水凝胶的制备：A, the preparation of hydrogel:
将温敏性聚合物单体和天然高分子单体溶于去离子水中，二者浓度范围分别为5～30wt.％和1～20wt.％，充分搅拌形成混合溶液。然后向混合溶液中依次加入交联剂和助剂，交联剂的用量范围是总单体量的0.1～9.0wt.％，助剂的用量范围为0.1～3.0wt.％。向溶液中通入惰性气体，以去除溶液中的氧气，再快速加入引发剂，引发剂的用量范围是总单体量的1.0～10.0wt.％，在室温的条件下引发聚合得到具有半互穿网络结构的水凝胶。The temperature-sensitive polymer monomer and the natural polymer monomer are dissolved in deionized water, and the concentration ranges of the two are 5-30wt.% and 1-20wt.%, and they are fully stirred to form a mixed solution. Then add a cross-linking agent and an auxiliary agent to the mixed solution in sequence, the amount of the cross-linking agent ranges from 0.1 to 9.0 wt.% of the total monomer amount, and the amount of the auxiliary agent ranges from 0.1 to 3.0 wt.%. Feed an inert gas into the solution to remove the oxygen in the solution, then quickly add the initiator, the amount of the initiator is 1.0-10.0wt.% of the total monomer amount, and initiate polymerization at room temperature to obtain a semi-reciprocal Hydrogel through the network structure.
B、氧化剂的吸附：B. Adsorption of oxidants:
将A步中所制备的水凝胶置于氧化剂溶液中浸泡10～30h，得到吸附了氧化剂的水凝胶。其中，氧化剂溶液中氧化剂的质量与C步中吡咯溶液中吡咯单体的质量之比为0.5:1～3:1。Soak the hydrogel prepared in step A in the oxidizing agent solution for 10-30 hours to obtain the hydrogel adsorbed with the oxidizing agent. Wherein, the ratio of the mass of the oxidizing agent in the oxidizing agent solution to the mass of the pyrrole monomer in the pyrrole solution in step C is 0.5:1˜3:1.
C、吡咯单体的吸附及氧化：C. Adsorption and oxidation of pyrrole monomer:
将B步中吸附了氧化剂的水凝胶浸泡在吡咯溶液中，吡咯单体的质量是水凝胶总单体量质量的1～20wt.％，在冰浴条件下避光放置10～30h,使吡咯单体充分渗入水凝胶网络中并被氧化形成聚吡咯，从而得到目标物电刺激-近红外双重响应高强度水凝胶。Soak the hydrogel with the oxidant adsorbed in step B in the pyrrole solution, the mass of the pyrrole monomer is 1-20wt.% of the total monomer mass of the hydrogel, and place it in the dark under ice bath conditions for 10-30h, The pyrrole monomer is fully infiltrated into the hydrogel network and oxidized to form polypyrrole, so as to obtain a high-strength hydrogel with dual response to electrical stimulation and near infrared.
与现有技术相比，本发明的有益效果是：Compared with prior art, the beneficial effect of the present invention is:
一、在本发明制备的水凝胶中，由于聚吡咯的引入，使其具有导电性和近红外响应性，即当处于通电状态或者在受到近红外光照时，该水凝胶温度升高，致使体系中的温敏性聚合物网络收缩，产生体积和形状变化，实现光、电双刺激响应。附图1为本发明实施例所得产物近红外光照射30s前后的形态对比，水凝胶产生显著的体积收缩和形状变化，并且水凝胶的轮廓线明显被晕染，这说明水凝胶中释放出了液体(中部深色部分为水凝胶；外部浅色部分为用红色水笔画的水凝胶轮廓线)。1. In the hydrogel prepared by the present invention, due to the introduction of polypyrrole, it has conductivity and near-infrared responsiveness, that is, when it is in an electrified state or is subjected to near-infrared light, the temperature of the hydrogel increases, As a result, the temperature-sensitive polymer network in the system shrinks, resulting in volume and shape changes, and realizes both light and electrical stimulation responses. Accompanying drawing 1 is the morphological comparison before and after 30s irradiation of near-infrared light of the product obtained in the embodiment of the present invention, and hydrogel produces remarkable volume shrinkage and shape change, and the outline line of hydrogel is obviously blurred, and this shows that in hydrogel The liquid was released (the dark part in the middle is the hydrogel; the light part outside is the outline of the hydrogel drawn with a red pen).
二、在A步中天然高分子与温敏性聚合物网络以相互缠结的方式形成半互穿网络结构，在B步中天然高分子中的活性基团与氧化剂中的金属离子产生络合作用，这种半互穿网络结构和络合作用的协同效应使水凝胶具有良好的机械性能。2. In step A, the natural polymer and the temperature-sensitive polymer network form a semi-interpenetrating network structure by intertwining each other, and in step B, the active groups in the natural polymer and the metal ions in the oxidant are complexed The synergistic effect of this semi-interpenetrating network structure and complexation endows the hydrogel with good mechanical properties.
三、在本发明制备的水凝胶中，半互穿网络结构增加了水凝胶的孔隙率，有利于氧化剂和吡咯单体的吸附，并且天然高分子的氨基和羟基与聚吡咯产生的氢键作用将聚吡咯固定在凝胶网络中，因此水凝胶中聚吡咯的分散稳定且均匀，从而使水凝胶具有良好的刺激响应灵敏度。3. In the hydrogel prepared by the present invention, the semi-interpenetrating network structure increases the porosity of the hydrogel, which is conducive to the adsorption of oxidants and pyrrole monomers, and the amino groups and hydroxyl groups of natural polymers and the hydrogen produced by polypyrrole The bonding effect fixes the polypyrrole in the gel network, so the dispersion of polypyrrole in the hydrogel is stable and uniform, which makes the hydrogel have good stimuli-response sensitivity.
附图说明Description of drawings
图1本发明目标产物在近红外光照射30s后的形体变化对比图；(a)为照射前；(b)为照射后。Fig. 1 is a comparison diagram of the shape change of the target product of the present invention after 30s of near-infrared light irradiation; (a) is before irradiation; (b) is after irradiation.
具体实施方式Detailed ways
实施例1Example 1
A、水凝胶的制备：A, the preparation of hydrogel:
将浓度范围为0.226g的N-异丙基丙烯酰胺(NIPAM)和浓度范围为0.1g的可溶性壳聚糖溶于2ml去离子水，充分搅拌。然后向混合溶液中依次加入2mg交联剂N，N-亚甲基双丙烯酰胺(Bis)，10μl TMEDA。向溶液中通入氮气，以去除溶液中的氧气，再快速加入10mg过硫酸铵(APS)，在室温条件下聚合10h，得到具有半互穿网络结构的水凝胶。Dissolve N-isopropylacrylamide (NIPAM) with a concentration range of 0.226 g and soluble chitosan with a concentration range of 0.1 g in 2 ml of deionized water, and stir thoroughly. Then, 2 mg of cross-linking agent N,N-methylenebisacrylamide (Bis) and 10 μl of TMEDA were sequentially added to the mixed solution. Nitrogen was blown into the solution to remove oxygen in the solution, and then 10 mg of ammonium persulfate (APS) was quickly added, and polymerized at room temperature for 10 h to obtain a hydrogel with a semi-interpenetrating network structure.
B、吸附氧化剂：B. Adsorption of oxidants:
将A步中所制备的水凝胶置于5ml浓度为0.06g/ml的氯化三铁溶液中浸泡10h，得到吸附了氧化剂的水凝胶。Soak the hydrogel prepared in step A for 10 hours in 5 ml ferric chloride solution with a concentration of 0.06 g/ml to obtain a hydrogel adsorbed with an oxidant.
C、吡咯单体的吸附及氧化：C. Adsorption and oxidation of pyrrole monomer:
将B步中吸附了氧化剂的水凝胶浸泡在4ml质量分数为1％的吡咯溶液中，在冰浴条件下避光放置24h,使吡咯单体充分渗入水凝胶网络中并被氧化形成聚吡咯，从而得到具有电刺激-近红外双重响应的水凝胶。Soak the hydrogel that has absorbed the oxidizing agent in step B in 4ml of pyrrole solution with a mass fraction of 1%, and place it in the dark for 24 hours under ice bath conditions, so that the pyrrole monomer can fully penetrate into the hydrogel network and be oxidized to form a polymer. pyrrole, thus obtaining a hydrogel with dual responses of electrical stimulation and near-infrared.
实施例2Example 2
A、水凝胶的制备：A, the preparation of hydrogel:
将300ml甲基丙烯酸-N,N-二甲氨基乙酯(DMAEMA)和0.1g海藻酸钠溶于2ml去离子水，充分搅拌。然后向混合溶液中依次加入2mg交联剂N，N-亚甲基双丙烯酰胺(Bis)，10μlTMEDA。向溶液中通入氮气，以去除溶液中的氧气，再快速加入20mg过硫酸铵(APS)和10mg亚硫酸钠，在室温条件下聚合10h，得到具有半互穿网络结构的水凝胶。Dissolve 300ml of N,N-dimethylaminoethyl methacrylate (DMAEMA) and 0.1g of sodium alginate in 2ml of deionized water and stir well. Then, 2 mg of the cross-linking agent N,N-methylenebisacrylamide (Bis) and 10 μl of TMEDA were sequentially added to the mixed solution. Nitrogen was blown into the solution to remove the oxygen in the solution, and then 20 mg of ammonium persulfate (APS) and 10 mg of sodium sulfite were quickly added, and polymerized at room temperature for 10 h to obtain a hydrogel with a semi-interpenetrating network structure.
B、吸附氧化剂：B. Adsorption of oxidants:
将A步中所制备的水凝胶置于5ml浓度为0.06g/ml的过硫酸钾溶液中浸泡10h，得到吸附了氧化剂的水凝胶。Soak the hydrogel prepared in step A in 5ml of potassium persulfate solution with a concentration of 0.06g/ml for 10h to obtain a hydrogel with adsorbed oxidant.
C、吸附吡咯以及吡咯的氧化：C. Adsorption of pyrrole and oxidation of pyrrole:
将B步中吸附了氧化剂的水凝胶浸泡在4ml质量分数为1％的吡咯溶液中，在冰浴的条件下避光放置24h,使吡咯单体充分渗入水凝胶网络中并被氧化形成聚吡咯，从而得到具有电刺激-近红外双重响应水凝胶。Soak the hydrogel with the oxidant adsorbed in step B in 4ml of pyrrole solution with a mass fraction of 1%, and place it in the dark for 24 hours in an ice bath, so that the pyrrole monomer can fully penetrate into the hydrogel network and be oxidized to form Polypyrrole, so as to obtain a hydrogel with electrical stimulation-near infrared dual response.
实施例3Example 3
本例的操作与实施例1基本相同，只是将实施例1中所使用的天然高分子单体换成海藻酸钠。The operation of this example is basically the same as that of Example 1, except that the natural macromolecular monomer used in Example 1 is replaced by sodium alginate.
实施例4Example 4
本例的操作与实施例1基本相同，只是将实施例1中所使用的天然高分子单体换成透明质酸。The operation of this example is basically the same as that of Example 1, except that the natural macromolecular monomer used in Example 1 is replaced by hyaluronic acid.
实施例5Example 5
A、水凝胶的制备：A, the preparation of hydrogel:
将0.226g N-异丙基丙烯酰胺(NIPAM)和0.2g水溶性壳聚糖溶于2ml去离子水，充分搅拌。然后向混合溶液中依次加入2ml PEGDMA，10μl TMEDA。向溶液中通入氮气，以去除溶液中的氧气，再快速加入40mg过硫酸钾(KPS)，在室温条件下聚合10h，得到具有半互穿网络结构的水凝胶。Dissolve 0.226g of N-isopropylacrylamide (NIPAM) and 0.2g of water-soluble chitosan in 2ml of deionized water and stir thoroughly. Then, 2 ml PEGDMA and 10 μl TMEDA were sequentially added to the mixed solution. Nitrogen was blown into the solution to remove oxygen in the solution, and then 40 mg of potassium persulfate (KPS) was quickly added, and polymerized at room temperature for 10 h to obtain a hydrogel with a semi-interpenetrating network structure.
B、吸附氧化剂：B. Adsorption of oxidants:
将A步中所制备的水凝胶置于10ml浓度为0.03g/ml的过硫酸钾溶液中浸泡10h，得到吸附了氧化剂的水凝胶。Soak the hydrogel prepared in step A in 10ml of potassium persulfate solution with a concentration of 0.03g/ml for 10h to obtain a hydrogel with adsorbed oxidant.
C、吸附吡咯以及吡咯的氧化：C. Adsorption of pyrrole and oxidation of pyrrole:
将B步中吸附了氧化剂的水凝胶浸泡在4ml质量分数为2.5％的吡咯溶液中，在避光的环境下放置24h,使吡咯单体充分渗入水凝胶网络中并被氧化形成聚吡咯，从而得到具有电刺激-近红外双重响应水凝胶。Soak the hydrogel with the oxidant adsorbed in step B in 4ml of pyrrole solution with a mass fraction of 2.5%, and place it in a dark environment for 24 hours, so that the pyrrole monomer can fully penetrate into the hydrogel network and be oxidized to form polypyrrole , so as to obtain a hydrogel with electrical stimulation-near infrared dual response.
实施例6Example 6
本例的操作与实施例5基本相同，只是将实施例5中所使用引发剂改为过硫酸钾(KPS)。The operation of this example is substantially the same as in Example 5, except that the initiator used in Example 5 is changed into potassium persulfate (KPS).
实施例7Example 7
本例的操作与实施例5基本相同，只是将实施例5中所使用氧化剂改为碘酸钾。The operation of this example is substantially the same as in Example 5, except that the oxidizing agent used in Example 5 is changed into potassium iodate.
实施例8Example 8
A、水凝胶的制备：A, the preparation of hydrogel:
将0.3g N-异丙基丙烯酰胺(NIPAM)和0.2g明胶溶于2ml去离子Dissolve 0.3 g of N-isopropylacrylamide (NIPAM) and 0.2 g of gelatin in 2 ml of deionized
水，充分搅拌。然后向混合溶液中依次加入4ml PEGDMA，20μl TMEDA。向溶液中通入氮气，以去除溶液中的氧气，再快速加入40mg过硫酸铵(APS)，在室温条件下聚合10h，得到具有半互穿网络结构的水凝胶。water, stir well. Then, 4 ml PEGDMA and 20 μl TMEDA were sequentially added to the mixed solution. Nitrogen was blown into the solution to remove oxygen in the solution, and then 40 mg of ammonium persulfate (APS) was quickly added, and polymerized at room temperature for 10 h to obtain a hydrogel with a semi-interpenetrating network structure.
B、吸附氧化剂：B. Adsorption of oxidants:
将A步中所制备的水凝胶置于5ml浓度为0.048g/ml的氯化三铁溶液浸泡10h，得到吸附了氧化剂的水凝胶。The hydrogel prepared in step A was soaked in 5 ml ferric chloride solution with a concentration of 0.048 g/ml for 10 hours to obtain a hydrogel adsorbed with an oxidant.
C、吸附吡咯以及吡咯的氧化：C. Adsorption of pyrrole and oxidation of pyrrole:
将B步中吸附了氧化剂的水凝胶浸泡在5ml质量分数为1.6％的吡咯溶液中，在避光的环境下放置24h,使吡咯单体充分渗入水凝胶网络中并被氧化形成聚吡咯，从而得到具有电刺激-近红外双重响应水凝胶。Soak the hydrogel with the oxidant adsorbed in step B in 5ml of pyrrole solution with a mass fraction of 1.6%, and place it in a light-proof environment for 24 hours, so that the pyrrole monomer can fully penetrate into the hydrogel network and be oxidized to form polypyrrole , so as to obtain a hydrogel with electrical stimulation-near infrared dual response.
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