CN113304324A - Preparation method of piezoelectric hydrogel and product - Google Patents
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- CN113304324A CN113304324A CN202110350059.3A CN202110350059A CN113304324A CN 113304324 A CN113304324 A CN 113304324A CN 202110350059 A CN202110350059 A CN 202110350059A CN 113304324 A CN113304324 A CN 113304324A
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- 239000000017 hydrogel Substances 0.000 title claims abstract description 69
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000000243 solution Substances 0.000 claims abstract description 57
- 239000000463 material Substances 0.000 claims abstract description 39
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims abstract description 34
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 32
- 230000008014 freezing Effects 0.000 claims abstract description 17
- 238000007710 freezing Methods 0.000 claims abstract description 17
- 239000000499 gel Substances 0.000 claims abstract description 13
- 239000000203 mixture Substances 0.000 claims abstract description 11
- 230000018044 dehydration Effects 0.000 claims abstract description 10
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000007864 aqueous solution Substances 0.000 claims abstract description 7
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 12
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 12
- 239000002033 PVDF binder Substances 0.000 claims description 11
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 11
- 230000035484 reaction time Effects 0.000 claims description 9
- 238000010257 thawing Methods 0.000 claims description 8
- 230000000694 effects Effects 0.000 claims description 4
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 claims description 3
- KDXKERNSBIXSRK-UHFFFAOYSA-N Lysine Natural products NCCCCC(N)C(O)=O KDXKERNSBIXSRK-UHFFFAOYSA-N 0.000 claims description 3
- 239000004472 Lysine Substances 0.000 claims description 3
- 108010020346 Polyglutamic Acid Proteins 0.000 claims description 3
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 claims description 3
- 229910002113 barium titanate Inorganic materials 0.000 claims description 3
- 229920002643 polyglutamic acid Polymers 0.000 claims description 3
- 239000004814 polyurethane Substances 0.000 claims description 3
- 229920002635 polyurethane Polymers 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 1
- 230000007547 defect Effects 0.000 abstract description 11
- 230000009471 action Effects 0.000 abstract description 6
- 230000000638 stimulation Effects 0.000 abstract description 5
- 239000000047 product Substances 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 6
- 230000012010 growth Effects 0.000 description 5
- 239000011148 porous material Substances 0.000 description 5
- 210000001519 tissue Anatomy 0.000 description 5
- 230000005012 migration Effects 0.000 description 4
- 238000013508 migration Methods 0.000 description 4
- 239000012467 final product Substances 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 125000004122 cyclic group Chemical group 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 230000033458 reproduction Effects 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 210000000988 bone and bone Anatomy 0.000 description 1
- 210000000845 cartilage Anatomy 0.000 description 1
- 230000010261 cell growth Effects 0.000 description 1
- 230000012292 cell migration Effects 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 230000004936 stimulating effect Effects 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 230000017423 tissue regeneration Effects 0.000 description 1
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- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
- A61L27/52—Hydrogels or hydrocolloids
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/14—Macromolecular materials
- A61L27/26—Mixtures of macromolecular compounds
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- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
- A61L27/56—Porous materials, e.g. foams or sponges
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Abstract
The preparation method of the piezoelectric hydrogel comprises the following steps: step 1: dissolving a base material with both mechanical property and biocompatibility in a 90 ℃ aqueous solution to form a solution A; dissolving a piezoelectric material in a dimethyl sulfoxide solution at 75 ℃ to form a solution B; step 2: rapidly mixing the solution A and the solution B obtained in the step 1, pouring the mixture into a mold, then putting the mold into a refrigerator with the temperature of-20 ℃ for freezing, and performing freezing and unfreezing cycle operation for three times to obtain piezoelectric gel; and step 3: and (3) unfreezing the piezoelectric hydrogel obtained in the step (2), putting the piezoelectric hydrogel into an ethanol gradient solution for dehydration, and removing residual dimethyl sulfoxide to obtain a piezoelectric hydrogel product. The invention can adapt to the mechanical strength of different defect parts, and finally achieves the purpose of repairing the defect parts through the combined action of the physiological microenvironment simulated by the hydrogel and the piezoelectric stimulation. The invention also discloses a piezoelectric hydrogel product prepared by the method.
Description
Technical Field
The invention relates to the technical field of hydrogel, in particular to a preparation method and a product of piezoelectric hydrogel.
Background
Hydrogels, which are materials having an internal structure very similar to that of biological tissues, have been widely used in biomedical engineering, such as artificial skin, biosensors, and scaffold materials in tissue engineering. Particularly in the self-repairing field of tissue engineering, the hydrogel provides physiological microenvironments such as cell migration, growth and reproduction by virtue of a unique network pore structure in the hydrogel, thereby achieving the purposes of promoting tissue repair and the like. However, simple hydrogels have limited their application in certain specific tissues, such as bone and cartilage defects, due to their poor mechanical properties and single repair action. Therefore, the preparation of the intelligent hydrogel with excellent mechanical properties and the functions of stimulating the growth and the reproduction of tissue cells has important significance.
Disclosure of Invention
The invention mainly aims to provide a preparation method of piezoelectric hydrogel and a product thereof, and aims to solve the technical problems of poor mechanical property and single repairing effect of the hydrogel in the prior art.
In order to achieve the above object, according to one aspect of the present invention, there is provided a method for preparing a piezoelectric hydrogel, comprising the steps of:
step 1: dissolving a base material with both mechanical property and biocompatibility in a 90 ℃ aqueous solution to form a solution A; dissolving a piezoelectric material in a dimethyl sulfoxide solution at 75 ℃ to form a solution B;
step 2: rapidly mixing the solution A and the solution B obtained in the step 1, pouring the mixture into a mold, then putting the mold into a refrigerator with the temperature of-20 ℃ for freezing, and performing freezing and unfreezing cycle operation for three times to obtain piezoelectric gel;
and step 3: and (3) unfreezing the piezoelectric hydrogel obtained in the step (2), putting the piezoelectric hydrogel into an ethanol gradient solution for dehydration, and removing residual dimethyl sulfoxide to obtain a piezoelectric hydrogel product.
When the piezoelectric hydrogel is prepared, the ratio of the base material to the doped material is adjusted, so that the size of the internal network pore diameter of the material can be adjusted to adapt to the growth and migration of different cells, and the output size of the piezoelectric voltage of the material can be adjusted; meanwhile, the mechanical strength of different defect parts can be adapted according to the proportion of dehydrated ethanol, and finally the defect parts can be repaired under the combined action of the physiological microenvironment simulated by the hydrogel and piezoelectric stimulation.
Further, the matrix material is one or a mixture of more than one of polyvinyl alcohol, acrylonitrile, polyglutamic acid and lysine.
Further, the piezoelectric material is one or a mixture of more than one of barium titanate, polyvinylidene fluoride and polyurethane with piezoelectric effect.
Further, the mass fractions of the components adopted in the step 1 are as follows: 10% -20% of base material, 10% -20% of piezoelectric material and water solution: 40 to 60 percent.
Further, the reaction time of step 1 is 8 h.
Further, in the step 2, the solution B is firstly poured into the solution A for mixing, and then is quickly poured into a mold.
Further, the freezing time in the step 2 is 18h, and the thawing time is 4 h.
Further, the volume ratio of the total amount of ethanol in the step 3 to the volume ratio of the piezoelectric gel thawed in the step 2 is more than or equal to 30:1, and the dehydration time is more than or equal to 24 hours.
Further, the mould is a culture dish or a test tube.
The invention also provides a piezoelectric hydrogel which is a product prepared by the preparation method of the piezoelectric hydrogel.
Therefore, when the piezoelectric hydrogel is prepared, the ratio of the base material to the doped material is adjusted, so that the size of the internal network pore diameter of the material can be adjusted to adapt to the growth and migration of different cells, and the output size of the piezoelectric voltage of the material can be adjusted; meanwhile, the mechanical strength of different defect parts can be adapted according to the proportion of dehydrated ethanol, and finally the defect parts can be repaired under the combined action of the physiological microenvironment simulated by the hydrogel and piezoelectric stimulation. The invention is further described with reference to the following figures and detailed description. Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to assist in understanding the invention, and are included to explain the invention and their equivalents and not limit it unduly. In the drawings:
FIG. 1 is a graph showing the compressive stress curves of examples 1-4 of the present invention.
FIG. 2 is a graph showing tensile stress curves of examples 1-4 of the present invention.
FIG. 3 is a schematic of the piezoelectric voltage output of example 6 of the present invention.
FIG. 4 is a schematic scanning view of the piezoelectric hydrogel obtained in example 1 of the present invention.
FIG. 5 is a schematic scanning view of the piezoelectric hydrogel obtained in example 2 of the present invention.
FIG. 6 is a schematic scanning view of the piezoelectric hydrogel obtained in example 3 of the present invention.
Detailed Description
The invention will be described more fully hereinafter with reference to the accompanying drawings. Those skilled in the art will be able to implement the invention based on these teachings. Before the present invention is described in detail with reference to the accompanying drawings, it is to be noted that:
the technical solutions and features provided in the present invention in the respective sections including the following description may be combined with each other without conflict.
Moreover, the embodiments of the present invention described in the following description are generally only some embodiments of the present invention, and not all embodiments. Therefore, all other embodiments obtained by a person of ordinary skill in the art based on the embodiments of the present invention without any creative effort shall fall within the protection scope of the present invention.
With respect to terms and units in the present invention. The terms "comprising," "having," and any variations thereof in the description and claims of this invention and the related sections are intended to cover non-exclusive inclusions.
In one aspect of the present invention, a method for preparing a piezoelectric hydrogel is provided, which comprises the following steps:
step 1: dissolving a base material with both mechanical property and biocompatibility in a 90 ℃ aqueous solution to form a solution A; dissolving a piezoelectric material in a dimethyl sulfoxide solution at 75 ℃ to form a solution B;
step 2: rapidly mixing the solution A and the solution B obtained in the step 1, pouring the mixture into a mold, then putting the mold into a refrigerator with the temperature of-20 ℃ for freezing, and performing freezing and unfreezing cycle operation for three times to obtain piezoelectric gel;
and step 3: and (3) unfreezing the piezoelectric hydrogel obtained in the step (2), putting the piezoelectric hydrogel into an ethanol gradient solution for dehydration, and removing residual dimethyl sulfoxide to obtain a piezoelectric hydrogel product.
When the piezoelectric hydrogel is prepared, the ratio of the base material to the doped material is adjusted, so that the size of the internal network pore diameter of the material can be adjusted to adapt to the growth and migration of different cells, and the output size of the piezoelectric voltage of the material can be adjusted; meanwhile, the mechanical strength of different defect parts can be adapted according to the proportion of dehydrated ethanol, and finally the defect parts can be repaired under the combined action of the physiological microenvironment simulated by the hydrogel and piezoelectric stimulation.
The matrix material is one or a mixture of more than one of polyvinyl alcohol, acrylonitrile, polyglutamic acid and lysine.
The piezoelectric material is one or a mixture of more than one of barium titanate, polyvinylidene fluoride and polyurethane with piezoelectric effect.
The mass fraction of the components adopted in the step 1 is as follows: 10% -20% of base material, 10% -20% of piezoelectric material and water solution: 40 to 60 percent.
The reaction time of the step 1 is 8 h.
In the step 2, the solution B is poured into the solution A to be mixed, and then the mixture is quickly poured into a mold.
The freezing time in the step 2 is 18h, and the unfreezing time is 4 h.
The volume ratio of the total amount of the ethanol in the step 3 to the volume ratio of the piezoelectric gel thawed in the step 2 is more than or equal to 30:1, and the dehydration time is more than or equal to 24 hours.
The mould is a culture dish or a test tube.
The piezoelectric hydrogel is a product prepared by the preparation method of the piezoelectric hydrogel.
Therefore, when the piezoelectric hydrogel is prepared, the ratio of the base material to the doped material is adjusted, so that the size of the internal network pore diameter of the material can be adjusted to adapt to the growth and migration of different cells, and the output size of the piezoelectric voltage of the material can be adjusted; meanwhile, the mechanical strength of different defect parts can be adapted according to the proportion of dehydrated ethanol, and finally the defect parts can be repaired under the combined action of the physiological microenvironment simulated by the hydrogel and piezoelectric stimulation.
The invention is further illustrated by the following specific examples.
Example 1
7.5g of polyvinyl alcohol was weighed out and dissolved in 40ml of an aqueous solution and 10ml of a dimethylsulfoxide solution to form a solution A with a mass fraction of 15%. The reaction temperature is 94 ℃ and the reaction time is 8 h.
7.5g of polyvinylidene fluoride is weighed and dissolved in 50ml of dimethyl sulfoxide solution to form a solution B with the mass fraction of 15%. The reaction temperature is 75 ℃, and the reaction time is 8 h.
The solution B was mixed with the solution A and poured quickly into a petri dish with a diameter of 10mm before the gel was formed.
Placing the culture dish containing the mixed solution into a refrigerator at-20 deg.C, freezing for 18h, and thawing at room temperature for 6 h. Thus, three cycles of freezing and thawing were performed to obtain a piezoelectric hydrogel.
The obtained gel was put into a 70% ethanol solution to remove dimethyl sulfoxide. The volume ratio of the ethanol to the hydrogel is 30:1, and the final product, namely the piezoelectric hydrogel, is obtained after dehydration for 24 hours.
Example 2
5g of polyvinyl alcohol 1799 are weighed out and dissolved in 40ml of aqueous solution and 10ml of dimethyl sulfoxide solution to form a solution A with a mass fraction of 10%. The reaction temperature is 94 ℃ and the reaction time is 8 h.
Weighing 10g of polyvinylidene fluoride, and dissolving the polyvinylidene fluoride in 50ml of dimethyl sulfoxide solution to form a solution B with the mass fraction of 20%. The reaction temperature is 75 ℃, and the reaction time is 8 h.
The solution B was mixed with the solution A and poured quickly into a petri dish with a diameter of 10mm before the gel was formed.
Placing the culture dish containing the mixed solution into a refrigerator at-20 deg.C, freezing for 18h, and thawing at room temperature for 6 h. Thus, three cycles of freezing and thawing were performed to obtain a piezoelectric hydrogel.
The obtained gel was put into a 70% ethanol solution to remove dimethyl sulfoxide. The volume ratio of the ethanol to the hydrogel is 30:1, and the final product, namely the piezoelectric hydrogel, is obtained after dehydration for 24 hours.
Example 3
10 portions of polyvinyl alcohol are weighed and dissolved in 40ml of aqueous solution and 10ml of dimethyl sulfoxide solution to form solution A with the mass fraction of 20%. The reaction temperature is 94 ℃ and the reaction time is 8 h.
Weighing 5 parts of polyvinylidene fluoride, and dissolving the polyvinylidene fluoride in 50ml of dimethyl sulfoxide solution to form a solution B with the mass fraction of 10%. The reaction temperature is 75 ℃, and the reaction time is 8 h.
The solution B was mixed with the solution A and poured quickly into a petri dish with a diameter of 10mm before the gel was formed.
Placing the culture dish containing the mixed solution into a refrigerator at-20 deg.C, freezing for 18h, and thawing at room temperature for 6 h. Thus, three cycles of freezing and thawing were performed to obtain a piezoelectric hydrogel.
The obtained gel was put into a 70% ethanol solution to remove dimethyl sulfoxide. The volume ratio of the ethanol to the hydrogel is 30:1, and the final product, namely the piezoelectric hydrogel, is obtained after dehydration for 24 hours.
Example 4
The difference between this example and examples 1 to 3 is that 1788 is polyvinyl alcohol; the content of dehydrated ethanol solution used was 50%.
Example 5
The difference between this example and examples 1 to 3 is that 2699 parts of polyvinyl alcohol; the content of dehydrated ethanol solution used was 90%.
Example 6
Application experiments; a cylindrical sample having a specification of d × h (1mm × 0.1mm) was prepared by the preparation method of example 1, two cross sections thereof were sprayed with gold, then a cyclic force of 10N was continuously applied to the material, and the piezoelectric output voltage of the material at 10N was obtained by a digital source meter to be about 0.15V. As shown in fig. 3, the hydrogel material of example 6 can generate a voltage of about 0.15V under a cyclic load of F ═ 10N.
As shown in FIGS. 1-2, it can be seen from the graphs of compressive stress and tensile stress that the mechanical properties of the piezoelectric hydrogel are mainly the result of the synergistic effect of PVA and PVDF, the PVA three-dimensional network scaffold plays a role in bearing load, and PVDF plays a role in toughening sites. By changing the content of PVA and PVDF or the degree of polymerization of PVA, the three-dimensional network structure and the degree of crosslinking of the hydrogel are changed, and the compressive and tensile stresses are changed. FIG. 4 is a schematic scanning view of the piezoelectric hydrogel obtained in example 1 of the present invention. FIG. 5 is a schematic scanning view of the piezoelectric hydrogel obtained in example 2 of the present invention. FIG. 6 is a schematic scanning view of the piezoelectric hydrogel obtained in example 3 of the present invention.
The contents of the present invention have been explained above. Those skilled in the art will be able to implement the invention based on these teachings. All other embodiments, which can be derived by a person skilled in the art from the above description without inventive step, shall fall within the scope of protection of the present invention.
Claims (10)
1. The preparation method of the piezoelectric hydrogel is characterized by comprising the following steps:
step 1: dissolving a base material with both mechanical property and biocompatibility in a 90 ℃ aqueous solution to form a solution A; dissolving a piezoelectric material in a dimethyl sulfoxide solution at 75 ℃ to form a solution B;
step 2: rapidly mixing the solution A and the solution B obtained in the step 1, pouring the mixture into a mold, then putting the mold into a refrigerator with the temperature of-20 ℃ for freezing, and performing freezing and unfreezing cycle operation for three times to obtain piezoelectric gel;
and step 3: and (3) unfreezing the piezoelectric hydrogel obtained in the step (2), putting the piezoelectric hydrogel into an ethanol gradient solution for dehydration, and removing residual dimethyl sulfoxide to obtain a piezoelectric hydrogel product.
2. The method for preparing a piezoelectric hydrogel according to claim 1, wherein the base material is one or a mixture of more than one of polyvinyl alcohol, acrylonitrile, polyglutamic acid, and lysine.
3. The method for preparing a piezoelectric hydrogel according to claim 1, wherein the piezoelectric material is one or a mixture of more than one of barium titanate, polyvinylidene fluoride and polyurethane having a piezoelectric effect.
4. The method for preparing a piezoelectric hydrogel according to claim 1, wherein the mass fractions of the components used in step 1 are: 10% -20% of base material, 10% -20% of piezoelectric material and water solution: 40 to 60 percent.
5. The method of preparing a piezoelectric hydrogel according to claim 1, wherein the reaction time of step 1 is 8 hours.
6. The method of preparing a piezoelectric hydrogel according to claim 1, wherein the solution B is mixed with the solution a in step 2, and then rapidly poured into a mold.
7. The method for preparing a piezoelectric hydrogel according to claim 1, wherein the freezing time in step 2 is 18 hours and the thawing time is 4 hours.
8. The preparation method of the piezoelectric hydrogel according to claim 1, wherein the volume ratio of the total amount of ethanol in the step 3 to the piezoelectric gel thawed in the step 2 is not less than 30:1, and the dehydration time is not less than 24 h.
9. The method of preparing a piezoelectric hydrogel according to claim 1, wherein the mold is a petri dish or a test tube.
10. A piezoelectric hydrogel, characterized in that it is a product obtained by the production method of a piezoelectric hydrogel according to any one of claims 1 to 9.
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| CN114015079A (en) * | 2021-12-14 | 2022-02-08 | 四川大学 | Polyvinyl alcohol-based piezoelectric active hydrogel and preparation and forming method thereof |
| CN114306652A (en) * | 2021-12-29 | 2022-04-12 | 华南理工大学 | Injectable piezoelectric hydrogel and preparation and application thereof |
| CN115014591A (en) * | 2022-06-24 | 2022-09-06 | 电子科技大学 | Anti-extravasation monitoring sensor for CT enhanced scanning, preparation method and monitoring equipment |
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