CN115246263A - Preparation of dust-free paper induced double-layer hydrogel driver - Google Patents
Preparation of dust-free paper induced double-layer hydrogel driver Download PDFInfo
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- B32B38/00—Ancillary operations in connection with laminating processes
- B32B38/08—Impregnating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B38/00—Ancillary operations in connection with laminating processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B38/00—Ancillary operations in connection with laminating processes
- B32B38/0004—Cutting, tearing or severing, e.g. bursting; Cutter details
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B38/00—Ancillary operations in connection with laminating processes
- B32B38/16—Drying; Softening; Cleaning
- B32B38/164—Drying
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F120/00—Homopolymers 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 a salt, anhydride, ester, amide, imide or nitrile thereof
- C08F120/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
- C08F2/48—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light
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Abstract
The invention provides a preparation method of a dust-free paper induced double-layer hydrogel driver, and belongs to the field of hydrogel drivers. Stirring the mixed solution of the synthesized magnesium lithium silicate, N-isopropylacrylamide (NIPAM), 1-hydroxycyclohexyl phenyl ketone and methanol to obtain a clear and transparent hydrogel precursor solution, forming a mold by a glass plate, dust-free paper and a silica gel pad, performing in-situ polymerization by light initiation after injection molding to obtain a double-layer hydrogel driver, and performing bending behavior design by using the double-layer hydrogel driver. The hydrogel driver has the advantages of excellent driving performance, good mechanical property, simple preparation method, numerical control of process parameters, low cost and high repeatability.
Description
Technical Field
The invention belongs to the field of hydrogel drivers, and particularly relates to a preparation method of a dust-free paper-induced double-layer hydrogel driver.
Background
Hydrogels are three-dimensional networks of cross-linked hydrophilic polymer chains with high water content, are highly elastic and soft materials. If these hydrogels contain stimuli-responsive polymers, they can undergo a dramatic change in volume due to environmental stimuli. With the continuous progress of artificial intelligence and soft body robotics, hydrogel drivers with infinite freedom become more and more important for the development of future intelligent devices and biomedical devices, and are one of the research hotspots in the fields of materials, machinery, biology and medicine nowadays. Despite the research results at home and abroad, although the research on the hydrogel driver has made great progress through the development in recent years, the problems that the response speed and the mechanical strength of the hydrogel driver are not compatible and the recovery speed is slow still remain the most outstanding problems to be solved at present. Therefore, the current state of the art hydrogel actuators have not yet been able to meet the current practical application requirements in various fields. In recent years, the thermo-sensitive N-isopropyl acrylamide hydrogel driver has good and stable stimulation corresponding performance and is widely concerned by researchers, but the thermo-sensitive N-isopropyl acrylamide hydrogel driver is generally complex in preparation method, low in driving speed, poor in cycle stability and single in action. Therefore, it is still a great challenge to develop a simple method to prepare a hydrogel actuator with fast response and recovery speed, excellent stability and capability of performing complex motions.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of a double-layer hydrogel driver based on dustless paper induction, and the preparation method is simple and easy to implement, controllable in process parameters, adjustable in hydrogel driver, low in cost and high in repeatability.
To achieve the above technical object, the present invention provides a method for manufacturing a dust-free paper-induced double-layer hydrogel actuator, the method comprising:
(1) Preparation of raw materials: purification of N-isopropylacrylamide (NIPAM) monomer: recrystallizing N-isopropylacrylamide (NIPAM) in an acetone/N-hexane mixed solvent for three times to obtain a white acicular purified N-isopropylacrylamide (NIPAM) monomer, and drying in vacuum at room temperature for 6-16 h for later use; magnesium lithium silicate: vacuum drying the synthesized magnesium lithium silicate for later use;
(2) Preparing a hydrogel precursor solution: adding synthetic magnesium lithium silicate into deionized water, magnetically stirring until the synthetic magnesium lithium silicate is completely dispersed to obtain clear liquid, then adding NIPAM into the clear liquid, stirring until the NIPAM is completely dissolved, finally adding a mixed solution of 1-hydroxycyclohexyl phenyl ketone and methanol, stirring to obtain a clear and transparent hydrogel precursor solution, and keeping nitrogen gas introduction in the whole process to avoid air oxidation and stirring in a dark place;
(3) Preparing the dust-free paper: soaking the dust-free paper in the modifying liquid for a certain time, then carrying out vacuum drying for 6-10 h at the temperature of 50-70 ℃, cutting the dust-free paper into a certain shape, and enabling the surface stripes and the longer edges to form a certain included angle;
(4) Preparation of the bilayer hydrogel based actuator: sequentially placing the dustless paper cut in the step (3) and the silicone rubber gasket with variable thickness and a hollowed surface in the middle on a glass plate, sealing the mold by using another glass cup, injecting the precursor liquid in the step (2) into the mold, wherein bubbles are prevented from being generated in the injection process, and then carrying out in-situ polymerization under the irradiation of ultraviolet light to prepare a double-layer hydrogel-based driver;
(5) Demolding of the double-layer hydrogel-based actuator: and (3) taking down the glass plate and the silica gel pad, wherein the dust-free paper can be adhered to the surface of one side of the hydrogel due to the viscosity of the hydrogel, the hydrogel forms a double-layer structure at the moment, the lower layer is PNIPAM hydrogel, and the upper layer is the dust-free paper with a surface stripe structure.
Further, the modifying solution of the dust-free paper is hydrochloric acid (HCl), N-methylpyrrolidone (NMP), ethanol (Ethanol), polyvinyl alcohol (PVA) solution or Chitosan Solution (CS).
Furthermore, the concentrations of hydrochloric acid (HCl), N-methylpyrrolidone (NMP) and Ethanol (Ethanol) solutions of the modification liquid of the dust-free paper are all 0.2-2 mol/L, and the concentration of the polyvinyl alcohol solution (PVA) or the Chitosan Solution (CS) is 5-30 g/L.
Further, the soaking time of the dust-free paper is 2-10 h.
Further, the volume ratio of the acetone/n-hexane mixed solvent in the step (1) is 1:0.5 to 10.
Further, the synthetic lithium magnesium silicate is dried in vacuum at 90-150 ℃ for 4-12 h.
Further, the included angle between the surface stripes and the longer sides of the dust-free paper is 0-90 degrees.
Furthermore, the dust-free paper is cut into different shapes, and the prepared double-layer hydrogel can realize corresponding shapes in hot water.
Further, cutting the dust-free paper into "Z", "S", "T" and "U" letter drivers, constructing a two-layer hydrogel letter driver can achieve deformation of "Z", "S", "T" and "U" in water at 60 ℃.
The invention has the beneficial effects that:
(1) The method further processes the raw materials, improves the quality of the hydrogel precursor solution, and enables the response performance of the prepared dust-free paper induced double-layer hydrogel to be better changed;
(2) The method adopts different modification liquids to treat the dust-free paper to obtain the dust-free paper induced double-layer hydrogel with different mechanical properties and driving properties, and realizes the regulation and control of the dust-free paper induced double-layer hydrogel driving properties through the modification of the dust-free paper;
(3) The invention realizes the regulation and control of the driving behavior of the double-layer hydrogel by preparing the dust-free paper with different stripe angles.
(4) The method for preparing the double-layer hydrogel is simple and easy to implement, the cost is low, and the prepared double-layer hydrogel has good driving performance and mechanical performance.
Drawings
FIG. 1 is an SEM image of a piece of dust-free paper modified by different treatment modes;
FIG. 2 shows the mechanical properties of the dust-free paper modified by different treatment methods;
FIG. 3 shows the driving performance of the dust-free paper modified by different treatment methods;
FIG. 4 is a pictorial view of a two-layer hydrogel actuator at different stripe angles;
FIG. 5 is a process of bending a bi-layer hydrogel actuator at different stripe angles;
FIG. 6 is a letter deformation detail plan view of a bilayer hydrogel actuator;
figure 7 is a letter deformation bending process for a two-layer hydrogel actuator.
Detailed Description
Example 1
(1) Preparation of raw materials: n-isopropylacrylamide (NIPAM) was added in a volume ratio of 1:1, recrystallizing for three times in an acetone/N-hexane mixed solvent to obtain a white acicular purified N-isopropylacrylamide (NIPAM) monomer, and drying for 12 hours at room temperature in vacuum for later use; the synthesized lithium magnesium silicate is dried in vacuum for 8 hours at 130 ℃ for standby;
(2) Preparing a hydrogel precursor solution: adding 0.2285g of synthetic lithium magnesium silicate into 10mL of deionized water, magnetically stirring for 4 hours until the synthetic lithium magnesium silicate is completely dispersed to obtain clear liquid, then adding 1.13g of NIPAM into the clear liquid, stirring for 30 minutes until the clear liquid is completely dissolved, finally adding a mixed solution of 2.26mg of 1-hydroxycyclohexyl phenyl ketone and 100 mu L of methanol, and stirring to obtain a clear and transparent hydrogel precursor solution, wherein nitrogen is introduced in the whole process to avoid the oxidation of air, and stirring in a dark place;
(3) Preparing the dust-free paper: soaking the dust-free paper in 1mol/L hydrochloric acid (HCl) solution for 3h, then drying the dust-free paper in vacuum at 50 ℃ for 10h, cutting the dust-free paper to enable the size of the dust-free paper to be 40mm multiplied by 10mm and enabling surface stripes and longer sides to form an included angle of 90 degrees;
(4) Preparation of the bilayer hydrogel based actuator: sequentially placing the dustless paper cut in the step (3) and the silicone rubber gasket with variable thickness and a hollow area of 40mm multiplied by 10mm in the middle on a glass plate, sealing the mold by using another glass cup, injecting the precursor solution in the step (2) into the mold, wherein bubbles are prevented from being generated in the injection process, and then carrying out in-situ polymerization under the irradiation of ultraviolet light to prepare a double-layer hydrogel-based driver;
(5) Demolding of the bilayer hydrogel-based actuator: and (3) taking down the glass plate and the silica gel pad, wherein the dust-free paper can be adhered to the surface of one side of the hydrogel due to the viscosity of the hydrogel, the hydrogel forms a double-layer structure at the moment, the lower layer is PNIPAM hydrogel, and the upper layer is the dust-free paper with a surface stripe structure.
Examples 2-5 compared to example 1, the procedure was the same as in example 1 except that the process for preparing the dust-free paper in step (3) was different.
Example 2
Preparing the dust-free paper: the dust-free paper is soaked in 1mol/L N-methyl pyrrolidone (NMP) solution for 12h, then dried in vacuum at 50 ℃ for 10h, and cut to have the size of 40mm multiplied by 10mm, and the included angle of 90 degrees is formed between the surface stripes and the longer sides.
Example 3
Preparing the dust-free paper: soaking the dust-free paper in 1mol/L ethanol solution for 12h, then drying the dust-free paper in vacuum at 50 ℃ for 10h, cutting the dust-free paper to enable the size of the dust-free paper to be 40mm multiplied by 10mm, and enabling surface stripes and longer sides to form an included angle of 90 degrees.
Example 4
Preparing the dust-free paper: the dust-free paper was soaked in 10mg/mL polyvinyl alcohol (PVA) solution for 12h, then vacuum dried at 50 ℃ for 10h, cut to 40mm x 10mm in size and have surface stripes with a 90 DEG included angle with the longer sides.
Example 5
Preparing the dust-free paper: the dust-free paper was soaked in 10mg/mL Chitosan Solution (CS) for 12h, then vacuum dried at 50 ℃ for 10h, cut to 40mm by 10mm in size and have surface stripes with a 90 ° included angle with the longer sides.
Control group
Preparing the dust-free paper: the dust-free paper was vacuum dried at 50 ℃ for 10h, cut to 40mm x 10mm and have surface stripes at 90 ° angles to the longer sides.
SEM images of the dust-free papers of examples 1-5 and the control are shown in FIG. 1, and it is known from FIG. 1 that the microstructure of the dust-free paper is changed by modifying the dust-free paper, and the main influence is the structure of the cellulose fibers. The untreated dust-free paper presents a rough and wavy fiber structure, and the dust-free paper treated by HCl and NMP has certain corrosivity to cellulose fibers, so that large fibers are gradually and partially decomposed into small nano fibers, the mechanical performance is reduced due to the corrosion action, the deformation resistance of the paper layer is reduced, and the driving performance of a hydrogel driver is increased; the structure of the fiber is not changed because the ethanol is non-corrosive, and the mechanical property of the modified dust-free paper is not greatly changed; according to the dust-free paper treated by the PVA and CS solutions, a polymer chain is spread on the surface of a fiber to form a polymer film, so that more concave-convex fluctuation exists on the surface of the fiber, the mechanical property of the modified dust-free paper is increased, the resistance of a paper layer is increased, and the driving performance of a hydrogel driver is reduced.
Tensile stress strain tests and driving performance tests were performed on two-layer hydrogel drivers with different modified dust-free papers, and the results are shown in fig. 2 and 3. The maximum stress of pure dust-free paper after ethanol modification, HCl modification, NMP modification, PVA modification and CS solution modification is 2.48MPa, 2.56MPa, 1.60MPa, 2.07MPa, 2.88MPa and 3.59MPa respectively, the corresponding strain is 186.01 percent, 181.93 percent, 183.99 percent, 190.48 percent, 162.59 percent and 127.70 percent respectively, and the Young modulus is 4.28MPa, 4.62MPa, 2.14MPa, 3.26MPa, 9.2MPa and 17.84MPa respectively.
As shown in fig. 2 and 3, the HCl-soaked hydrogel driver of the dust-free paper reaches the maximum bending amplitude within 30s, and the bending amplitudes of the pure dust-free paper, the ethanol-modified hydrogel driver, the HCl-modified hydrogel driver and the NMP-modified hydrogel driver 30s are 608.6 °, 433.6 °, 850.0 ° and 666.1 °; the bending amplitudes of the hydrogel actuators of the dust-free paper modified with PVA and CS solutions at 60s were 355.9 ° and 141.1 °, respectively. The hydrogel driver soaked by HCl and placed in cold water can recover to a straight state within 2min, and reversely bend to-479.5 degrees within 5 min; the dust-free paper is subjected to a hydrogel driver soaked by NMP, and the dust-free paper returns to be straight after being in cold water for about 2.5min and is reversely bent to-371.5 degrees after 9 min; the reverse bending amplitudes of pure dust-free paper in cold water after ethanol modification, PVA modification and CS solution modification are respectively 902.807 degrees, 950.1 degrees, 492.0 degrees and 577.3 degrees; the reverse bending rates in cold water of the pure dust-free paper, the paper modified by ethanol, the paper modified by PVA and the paper modified by CS solution are respectively 0.94 DEG/s, 0.79 DEG/s, 0.27 DEG/s and 0.08 DEG/s.
As can be seen from the experiments of examples 1 to 5 and a control group, the double-layer hydrogel driver can obtain different bending properties and driving properties by adopting different methods for treatment, and the driving properties of the double-layer hydrogel driver can be adjusted and controlled by adjusting the treatment method of the dust-free paper.
Example 6
(1) Preparation of raw materials: n-isopropyl acrylamide is prepared by mixing N-isopropyl acrylamide and N-isopropyl acrylamide in a volume ratio of 1:1, recrystallizing for three times in an acetone/N-hexane mixed solvent to obtain a white needle-shaped purified N-isopropylacrylamide (NIPAM) monomer, and drying for 12 hours at room temperature in vacuum for later use; the synthesized magnesium lithium silicate is dried for 8 hours at 130 ℃ in vacuum for standby;
(2) Preparation of hydrogel precursor solution: adding 0.2285g of synthetic lithium magnesium silicate into 10mL of deionized water, magnetically stirring for 4 hours until the synthetic lithium magnesium silicate is completely dispersed to obtain clear liquid, then adding 1.13g of NIPAM into the clear liquid, stirring for 30 minutes until the clear liquid is completely dissolved, finally adding a mixed solution of 2.26mg of 1-hydroxycyclohexyl phenyl ketone and 100 mu L of methanol, and stirring to obtain a clear and transparent hydrogel precursor solution, wherein nitrogen is introduced in the whole process to avoid the oxidation of air, and stirring in a dark place;
(3) Preparing the dust-free paper: selecting dust-free paper which is not soaked in the solution, cutting the dust-free paper into 40mm multiplied by 10mm, and enabling surface stripes to be 0 degree, 30 degrees, 45 degrees, 60 degrees and 90 degrees respectively;
(4) Preparation of the bilayer hydrogel based actuator: sequentially placing the dustless paper cut in the step (3) and a silicone rubber gasket which has variable thickness and a middle hollowed area of 40mm multiplied by 10mm on a glass plate, injecting the precursor liquid in the step (2) into a mold, sealing the mold by using another glass cup during the injection process, and then carrying out in-situ polymerization under the irradiation of ultraviolet light to prepare a double-layer hydrogel base driver;
(5) Demolding of the bilayer hydrogel-based actuator: and (3) taking down the glass plate and the silica gel pad, wherein the dust-free paper can be adhered to the surface of one side of the hydrogel due to the viscosity of the hydrogel, the hydrogel forms a double-layer structure at the moment, the lower layer is PNIPAM hydrogel, and the upper layer is the dust-free paper with a surface stripe structure.
The two-layer hydrogel actuators with different stripe angles prepared in this example 6 were placed in hot water at 60 ℃ as shown in fig. 4, and the two-layer hydrogel actuators with surface stripes of 0 °, 30 °, 45 °, 60 ° and 90 °, respectively, exhibited bending behavior in which the hydrogel was bent in a direction perpendicular to the stripes as shown in fig. 5, and exhibited different actuation behaviors at different stripe angles, and the hydrogel actuators could reach the maximum bending amplitude at 10 s. From example 6, it can be seen that adjusting the stripe angle of the dust-free paper realizes regulating the driving behavior of the double-layer hydrogel driver.
Example 7
The two-layer hydrogel actuator prepared using the method in example 1, which was cut into letter actuators, was constructed to achieve the deformation of "Z", "S", "T" and "U" in water at 60 ℃, as shown in fig. 6 and 7.
The double-layer PNIPAM hydrogel based on the induction of the dust-free paper can purposefully design the controlled deformation of the temperature response driver by adjusting the processing method, the angle, the position and the length of the stripes of the dust-free paper, realize the local bending of the double-layer hydrogel driver and control the bending direction. As shown in fig. 6, the bilayer hydrogel actuator can achieve deformation of "Z", "S", "T", and "U" within 45S.
The above examples are intended to illustrate the invention, but not to limit it. Any modifications and variations of the present invention, which fall within the spirit of the present invention and the scope of the appended claims, are also included.
Claims (9)
1. A method of making a non-dusting paper-induced dual-layer hydrogel actuator, the method comprising:
(1) Preparation of raw materials: purification of N-isopropylacrylamide (NIPAM) monomer: recrystallizing N-isopropylacrylamide (NIPAM) in an acetone/N-hexane mixed solvent for three times to obtain a white acicular purified N-isopropylacrylamide (NIPAM) monomer, and drying in vacuum for 6-16 h at room temperature for later use; magnesium lithium silicate: vacuum drying the synthesized magnesium lithium silicate for later use;
(2) Preparing a hydrogel precursor solution: adding synthetic magnesium lithium silicate into deionized water, magnetically stirring until the synthetic magnesium lithium silicate is completely dispersed to obtain clear liquid, then adding NIPAM into the clear liquid, stirring until the NIPAM is completely dissolved, finally adding a mixed solution of 1-hydroxycyclohexyl phenyl ketone and methanol, stirring to obtain a clear and transparent hydrogel precursor solution, and keeping nitrogen gas introduction in the whole process to avoid air oxidation and stirring in a dark place;
(3) Preparing the dust-free paper: soaking the dust-free paper in the modifying liquid for a certain time, then carrying out vacuum drying for 6-10 h at the temperature of 50-70 ℃, cutting the dust-free paper into a certain shape, and enabling the surface stripes and the longer edges to form a certain included angle;
(4) Preparation of the bilayer hydrogel based actuator: sequentially placing the dustless paper cut in the step (3) and the silicone rubber gasket with variable thickness and a hollow middle on a glass plate, sealing the mold by using another glass cup, injecting the precursor liquid in the step (2) into the mold, wherein bubbles are avoided in the injection process, and then carrying out in-situ polymerization under ultraviolet irradiation to prepare a double-layer hydrogel-based driver;
(5) Demolding of the double-layer hydrogel-based actuator: and (3) taking down the glass plate and the silica gel pad, wherein the dust-free paper can be adhered to the surface of one side of the hydrogel due to the viscosity of the hydrogel, the hydrogel forms a double-layer structure at the moment, the lower layer is PNIPAM hydrogel, and the upper layer is the dust-free paper with a surface stripe structure.
2. The method for preparing a non-dusting paper-induced double-layer hydrogel actuator as claimed in claim 1, wherein the modifying solution of the non-dusting paper is one or more of hydrochloric acid (HCl), N-methylpyrrolidone (NMP), ethanol (Ethanol), polyvinyl alcohol (PVA), or Chitosan Solution (CS).
3. The method for preparing a non-dusting paper-induced double-layer hydrogel actuator as claimed in claim 2, wherein the concentrations of the hydrochloric acid (HCl), N-methylpyrrolidone (NMP) and Ethanol (Ethanol) are 0.2-2 mol/L, and the concentration of the polyvinyl alcohol solution (PVA) or Chitosan Solution (CS) is 5-30 g/L.
4. The method for preparing a dust-free paper-induced double-layer hydrogel actuator according to claim 3, wherein the soaking time of the dust-free paper is 2-10 h.
5. The method for preparing a non-dusting paper-induced double-layer hydrogel actuator as claimed in claim 4, wherein the included angle between the surface stripes and the longer sides of the non-dusting paper is 0-90 °.
6. The method for preparing a non-dusting paper-induced double-layer hydrogel actuator as claimed in claim 1, wherein the volume ratio of the acetone/n-hexane mixed solvent in the step (1) is 1:0.5 to 10.
7. The method for preparing a dust-free paper-induced double-layer hydrogel actuator according to claim 1, wherein the synthetic lithium magnesium silicate is dried at 90-150 ℃ in vacuum for 4-12 h.
8. The method for preparing a non-dusting paper-induced double-layer hydrogel actuator as claimed in any one of claims 1 to 7, wherein the non-dusting paper is cut into different shapes, and the prepared double-layer hydrogel can realize the corresponding shapes in hot water.
9. The method for manufacturing a dust-free paper-induced double-layer hydrogel actuator as claimed in claim 5, wherein the dust-free paper is cut into "Z", "S", "T" and "U" letter actuators, and the double-layer hydrogel letter actuator is constructed to realize the deformation of "Z", "S", "T" and "U" in water at 60 ℃.
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