CN113024893A - Temperature-sensitive cellulose intelligent window - Google Patents
Temperature-sensitive cellulose intelligent window Download PDFInfo
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- CN113024893A CN113024893A CN202110334454.2A CN202110334454A CN113024893A CN 113024893 A CN113024893 A CN 113024893A CN 202110334454 A CN202110334454 A CN 202110334454A CN 113024893 A CN113024893 A CN 113024893A
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
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- E—FIXED CONSTRUCTIONS
- E06—DOORS, WINDOWS, SHUTTERS, OR ROLLER BLINDS IN GENERAL; LADDERS
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- E06B9/00—Screening or protective devices for wall or similar openings, with or without operating or securing mechanisms; Closures of similar construction
- E06B9/24—Screens or other constructions affording protection against light, especially against sunshine; Similar screens for privacy or appearance; Slat blinds
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- C—CHEMISTRY; METALLURGY
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- C08J2333/00—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
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- C08J2433/00—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
- C08J2433/02—Homopolymers or copolymers of acids; Metal or ammonium salts thereof
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Abstract
The invention discloses a temperature-sensitive cellulose intelligent window which is prepared by the following specific processes: dissolving a certain mass of temperature-sensitive cellulose in deionized water, and slowly stirring until the temperature-sensitive cellulose is completely dissolved, wherein the solution is in a transparent state; adding polyacrylic acid and/or polyacrylate into the cellulose solution to prepare temperature-sensitive cellulose/polyacrylic acid and/or polyacrylate mixed sol, then adding acid or alkali into the mixed sol to adjust the pH value of the solution so as to regulate the lowest critical temperature to be close to the room temperature, finally injecting the mixed sol into the middle of two glass or flexible polymer films, and sealing to prepare the temperature-sensitive cellulose intelligent window with the sandwich structure.
Description
Technical Field
The invention relates to the field of thermochromic intelligent windows, in particular to a temperature-sensitive cellulose intelligent window.
Background
Cellulose is a natural polymer, belongs to renewable resources, and is nontoxic and biodegradable. In recent years, cellulose has been widely used in various fields such as medical fields, photo-thermal devices and food processing due to the demand for environmentally friendly, non-toxic and renewable materials in various countries. The temperature-sensitive cellulose is water-soluble cellulose ether with amphiphilic groups, is mainly prepared by chemically modifying natural cellulose, and is mainly represented by hydroxypropyl cellulose and hydroxypropyl methyl cellulose. When the environmental temperature is lower than the lowest critical temperature, a large number of hydrogen bonds can be formed between hydrophilic groups of the temperature-sensitive cellulose and water molecules, molecular chains stretch, and the solution is in a transparent state; when the environmental temperature is higher than the lowest critical temperature, the hydrophobic effect of the hydrophobic groups of the cellulose molecular chains is enhanced, and the hydrogen bonds with water molecules can be broken, so that the molecular chains are curled and collapsed into small balls, the separation of a polymer phase and a water phase occurs, and the solution is in an opaque state. The thermo-sensitive cellulose can regulate and control the transmittance of sunlight before and after phase change, and the thermochromic property enables the thermo-sensitive cellulose to be applied to thermochromic intelligent windows. However, the optimal phase transition temperature of the thermochromic intelligent window is near room temperature, and the phase transition temperature of the temperature-sensitive cellulose is higher than room temperature, for example, the phase transition temperature of the hydroxypropyl cellulose is 42 ℃ and the phase transition temperature of the hydroxypropyl methyl cellulose is 60 ℃, so that the phase transition temperature is especially critical when the thermochromic intelligent window is applied to the thermochromic intelligent window.
The literature (RSCAV, 2016,6, 61449; Nanomaterials 2019,9,970) reports that the lowest critical temperature of temperature-sensitive cellulose can be greatly reduced by a metal ion salt effect or a chemical grafting modification method. However, the problem of salting-out cannot be avoided with a decrease in temperature; although stable temperature-sensitive cellulose can be obtained by chemical modification, the regulation and control means are complex and full of uncertainty. Therefore, the lowest critical temperature of the temperature-sensitive cellulose is effectively reduced to be close to the room temperature by adopting a mild regulation and control means, the stability of the material is not influenced, and the application of the intelligent window is expanded, so that the method has important significance.
Disclosure of Invention
The invention aims to provide a temperature-sensitive cellulose intelligent window. The basic principle is that polyacrylic acid or polyacrylate is added into temperature sensitive cellulose solution, the pH value of the system is adjusted through hydrochloric acid or sodium hydroxide solution, and deprotonation of carboxyl of the polyacrylic acid or polyacrylate is inhibited to form a polymer containing a large number of intermolecular hydrogen bonds. The polymer has the lowest adjustable critical temperature, and the method only needs to simply blend the temperature-sensitive cellulose and polyacrylic acid or polyacrylate without complex cross-linking polymerization reaction.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a temperature-sensitive cellulose intelligent window comprises the following steps:
mixing the temperature-sensitive cellulose solution with polyacrylic acid and/or polyacrylate, adjusting the pH value to 0.1-10 to control the lowest critical temperature value to be 0-50 ℃ to obtain mixed sol, injecting the mixed sol between two pieces of glass or flexible polymer films, and sealing to obtain the temperature-sensitive cellulose intelligent window.
Preferably, the temperature-sensitive cellulose comprises one or more of hydroxypropyl cellulose, methyl cellulose and hydroxypropyl methyl cellulose.
Preferably, the temperature-sensitive cellulose solution is prepared by adding temperature-sensitive cellulose into deionized water and slowly stirring until the temperature-sensitive cellulose is completely dissolved, and the solution is transparent.
Preferably, the molecular weight of the temperature-sensitive cellulose is 80-120K.
More preferably, the temperature-sensitive cellulose has molecular weights of 80K, 86K, 90K, 100K and 120K.
Preferably, the mass concentration of the temperature-sensitive cellulose is 0.1-5%.
More preferably, the mass concentration of the temperature-sensitive cellulose is 0.5%.
Preferably, the polyacrylate comprises one or both of potassium polyacrylate and sodium polyacrylate.
Preferably, the polyacrylic acid or polyacrylate has a molecular weight of 1-100K.
More preferably, the polyacrylic acid or polyacrylate has a molecular weight of 3000.
More preferably, the polyacrylic acid or polyacrylate has a mass concentration of 0.5%.
Preferably, the acid used for adjusting the pH is one or more of hydrochloric acid, acetic acid, sulfuric acid, nitric acid and phosphoric acid; the alkali used for adjusting the pH is one or more of sodium hydroxide, potassium carbonate, sodium bicarbonate, potassium bicarbonate, sodium hydrogen phosphate, potassium hydrogen phosphate, sodium dihydrogen phosphate and potassium dihydrogen phosphate.
Preferably, the pH is adjusted to 1-3 to control the lowest critical temperature value to be between 10 and 38 ℃.
Preferably, the mass ratio of the temperature-sensitive cellulose to the polyacrylic acid or polyacrylate is (0.5-2): 1.
More preferably, the mass ratio of the temperature-sensitive cellulose to the polyacrylic acid or polyacrylate is 1: 1.
The invention also provides the temperature-sensitive cellulose intelligent window prepared by the preparation method.
Compared with the prior art, the invention has the beneficial effects that:
the thermochromic material playing a key role in the invention can be prepared by directly and simply mixing the temperature-sensitive cellulose and the polyacrylic acid or polyacrylate without complex polymerization reaction, does not relate to other reaction solvents, chemical raw materials and complex chemical reaction containers, and has simple and rapid mixing process.
The thermochromic intelligent window prepared by the method has mild phase change temperature regulation and control means of the temperature-sensitive cellulose/polyacrylic acid or polyacrylate complex, and can be accurately regulated and controlled by adopting a mode of regulating the pH value of a system.
According to the thermochromic intelligent window prepared by the method, the pH value of the temperature-sensitive cellulose/polyacrylic acid or polyacrylate complex is directly regulated and controlled by adding acid and alkali, so that the salting-out defect caused by the modulation of the traditional buffer salt solution is avoided.
The invention strictly controls the molecular weight of the temperature-sensitive cellulose and the polyacrylic acid and/or polyacrylate, avoids the problem that the dissolution difficulty is increased due to overlarge molecular weight, causes bubbles to be generated, reduces the visible light transmittance, and otherwise avoids the problem that the solar energy regulation efficiency of the intelligent window is influenced due to the overlow molecular weight. Meanwhile, the dosage ratio of the temperature-sensitive cellulose to polyacrylic acid and/or polyacrylate is strictly controlled, and the effective regulation and control of the phase transition temperature of the temperature-sensitive cellulose are realized.
The invention strictly controls the concentration of the temperature-sensitive cellulose, and avoids the phenomena that the concentration is too high, the viscosity is too high, and the gel loses fluidity too quickly to be poured.
Drawings
FIG. 1 is a graph showing the visible light transmittance effect of the temperature-sensitive cellulose smart window prepared in example 1 at 20 ℃ and 40 ℃;
FIG. 2 is a graph of the lowest critical temperature of the temperature sensitive cellulose smart window prepared in example 1 as a function of pH;
FIG. 3 is an energy-saving simulation test chart of the temperature-sensitive cellulose smart window prepared in example 1;
FIG. 4 is a graph of the temperature-sensitive cellulose smart window cycle stability test prepared in example 1;
FIG. 5 is a spectrum of hydroxypropyl methylcellulose/sodium polyacrylate prepared in example 2 at 300-2600 nm;
FIG. 6 is a spectrum of hydroxypropyl methylcellulose/potassium polyacrylate prepared in example 3 at 300-2600 nm.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. Further, for numerical ranges in this disclosure, it is understood that each intervening value, between the upper and lower limit of that range, is also specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference herein for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. The specification and examples are exemplary only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including, but not limited to.
The mass concentration of polyacrylic acid or polyacrylate in the following examples is 0.5%.
Example 1
1) Dissolving 0.5g of hydroxypropyl cellulose with the molecular weight of 100K in 100mL of deionized water, wherein the mass concentration is 0.5%, slowly stirring until the hydroxypropyl cellulose is completely dissolved, and the solution is in a transparent state to obtain a hydroxypropyl cellulose solution;
2) adding polyacrylic acid with the molecular weight of 3000 into the prepared hydroxypropyl cellulose solution, and controlling the mass ratio of the hydroxypropyl cellulose to the polyacrylic acid to be 1:1, preparing hydroxypropyl cellulose/polyacrylic acid mixed sol;
3) 5mol/L hydrochloric acid is added into the mixed sol to adjust the pH value to 2.5.
Adding hydroxypropyl cellulose/polyacrylic acid mixed sol with pH of 2.5 into the middle of two pieces of glass, and sealing to obtain intermediate sol with thickness of 0.5mm and area of 30.5 × 26cm2The temperature-sensitive cellulose intelligent window.
The temperature-sensitive cellulose intelligent window prepared in the embodiment is tested, and a visible light transmission effect graph (as shown in fig. 1) of the temperature-sensitive cellulose intelligent window at 20 ℃ and 40 ℃ is verified. It can be seen from fig. 1 that, when the external temperature is higher than the minimum critical temperature, the whole smart window is in an opaque state, and the temperature-sensitive cellulose smart window prepared according to the embodiment can be obtained, and has a good effect of blocking infrared ray from being injected when the external temperature is higher than 25 ℃.
The relationship between the lowest critical temperature and the pH value of the hydroxypropyl cellulose/polyacrylic acid mixed sol shown in figure 2 is obtained by adjusting different pH values by using hydrochloric acid and sodium hydroxide. As can be seen from the figure, when the pH is 2.5, the lowest critical temperature corresponding to the mixed sol is 26.5 ℃, which shows that the lowest critical temperature can be flexibly regulated within the range of 20-45 ℃ by adjusting the pH value of the mixed sol system, and particularly, the lowest critical temperature is close to the room temperature when the system has an acidic pH of 2.5.
The energy-saving simulation test is performed on the temperature-sensitive cellulose intelligent window prepared in the embodiment, and the result is shown in fig. 3. Compared with the intelligent window with the temperature-sensitive cellulose sandwich structure, which is prepared by the embodiment, the light intensity of the simulated house designed according to the American military standard is 700w/m after 1 hour2The indoor temperature of the simulated room provided with the common glass is 10 ℃ higher than that of the intelligent temperature-sensitive fiber window prepared by the embodiment, and the indoor temperature of the simulated room provided with the water-sandwiched double-layer glass is 5 ℃ higher than that of the intelligent temperature-sensitive fiber window prepared by the embodiment.
The result of the cycle stability test on the temperature-sensitive cellulose intelligent window prepared in the embodiment is shown in fig. 4, and it can be found from fig. 4 that the visible light transmittance is still maintained above 90% after 100 times of cold and heat cycles, the solar energy regulation efficiency is still maintained at 50%, and no obvious attenuation is generated, which indicates that the temperature-sensitive cellulose intelligent window prepared in the embodiment has excellent stability.
Example 2
1) Dissolving 0.4g of hydroxypropyl methyl cellulose with the molecular weight of 100K in 100mL of deionized water, wherein the mass concentration is 0.4%, slowly stirring until the cellulose is completely dissolved, and the solution is in a transparent state to obtain a hydroxypropyl methyl cellulose solution;
2) adding sodium polyacrylate with molecular weight of 5100 into the prepared cellulose solution, and controlling the mass ratio of hydroxypropyl methyl cellulose to sodium polyacrylate to be 1: 0.5, preparing hydroxypropyl methyl cellulose/sodium polyacrylate mixed sol;
3) 4mol/L hydrochloric acid is added into the mixed sol to adjust the pH value to 2.5.
Adding hydroxypropyl methylcellulose/sodium polyacrylate mixed sol with pH of 2.5 into the middle of two pieces of glass, and sealing to obtain intermediate layer sol with thickness of 0.5mm and area of 30.5 × 26cm2The temperature-sensitive cellulose intelligent window.
Fig. 5 is a spectrum diagram of the hydroxypropyl methylcellulose/sodium polyacrylate mixed sol prepared in the embodiment at a wavelength band of 300-2600nm, and it can be seen from the diagram that the visible light transmittance of the hydroxypropyl methylcellulose/sodium polyacrylate sol is 79.6%, and the solar energy regulation efficiency is 9.4%.
Example 3
1) Dissolving 0.3g of hydroxypropyl methyl cellulose with the molecular weight of 100K in 100mL of deionized water, wherein the mass concentration is 0.3%, slowly stirring until the cellulose is completely dissolved, and obtaining the hydroxypropyl methyl cellulose when the solution is in a transparent state;
2) adding potassium polyacrylate into a hydroxypropyl methyl cellulose solution, and controlling the mass ratio of hydroxypropyl methyl cellulose to potassium polyacrylate to be 1:1, preparing hydroxypropyl methyl cellulose/potassium polyacrylate mixed sol;
3) 3mol/L hydrochloric acid is added into the mixed sol to adjust the pH value to 2.5.
Adding hydroxypropyl methyl cellulose/potassium polyacrylate mixed sol with pH of 2.5 into the middle of two pieces of glass, and sealing to obtain intermediate layer sol with thickness of 0.5mm and area of 30.5 × 26cm2The temperature-sensitive cellulose intelligent window.
Fig. 6 is a spectrum diagram of the hydroxypropyl methylcellulose/potassium polyacrylate mixed sol prepared in the embodiment at a wavelength band of 300-2600nm, and it can be seen from the diagram that the visible light transmittance of the hydroxypropyl methylcellulose/potassium polyacrylate sol is 89.4% and the solar energy control efficiency is 15.0%.
Example 4
The difference from example 1 is that hydroxypropylcellulose has a molecular weight of 80K.
As a result, the performance of the prepared temperature-sensitive cellulose intelligent window is basically consistent with that of the comparison document 1.
Example 5
The difference from example 1 is that polyacrylic acid and sodium polyacrylate are added simultaneously.
Example 6
The difference from example 1 is that polyacrylic acid, potassium polyacrylate and sodium polyacrylate are added simultaneously.
Example 7
The difference from example 1 is that the pH is adjusted to 2.5 with sulfuric acid.
Example 8
The difference from example 1 is that glass was replaced with a flexible polymer film.
Example 9
The difference from example 1 is that the pH is adjusted to 9.
Comparative example 1
The difference from example 1 is that hydroxypropylcellulose has a molecular weight of 130K.
Comparative example 2
The difference from example 1 is that the mass ratio of the temperature-sensitive cellulose to the polyacrylic acid or polyacrylate is 1: 2.
comparative example 3
The difference from example 1 is that the hydroxypropyl cellulose mass concentration is 7%.
Comparative example 4
The difference from example 1 is that the molecular weight of polyacrylic acid is 110K.
The temperature-sensitive cellulose intelligent windows prepared in examples 4-9 and comparative examples 1-4 were subjected to 100 cycles of cooling and heating, and the visible light transmittance and the solar energy regulation rate were measured, and the results are shown in table 1.
TABLE 1
| Case(s) | Visible light transmittance (%) | Solar control efficiency (%) |
| Example 4 | 90.2 | 48.2 |
| Example 5 | 87.3 | 42.9 |
| Example 6 | 89.8 | 46.5 |
| Example 7 | 89.3 | 49.1 |
| Example 8 | 91.4 | 47.3 |
| Example 9 | 86.0 | 39.4 |
| Comparative example | 78.2 | 38.7 |
| Comparative example 2 | 87.5 | 41.0 |
| Comparative example 3 | 76.6 | 39.8 |
| Comparative example 4 | 87.3 | 42.4 |
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included therein.
Claims (9)
1. The preparation method of the temperature-sensitive cellulose intelligent window is characterized by comprising the following steps:
mixing the temperature-sensitive cellulose solution with polyacrylic acid and/or polyacrylate, adjusting the pH value to 0.1-10 to obtain mixed sol, injecting the mixed sol between two glass or flexible polymer films, and sealing to obtain the temperature-sensitive cellulose intelligent window.
2. The method for preparing according to claim 1, wherein the temperature-sensitive cellulose includes one or more of hydroxypropyl cellulose, methyl cellulose, and hydroxypropylmethyl cellulose.
3. The method according to claim 2, wherein the temperature-sensitive cellulose has a molecular weight of 80 to 120K.
4. The method according to claim 2, wherein the mass concentration of the temperature-sensitive cellulose is 0.1 to 5%.
5. The method of claim 1, wherein the polyacrylate comprises one or both of potassium polyacrylate and sodium polyacrylate.
6. The method of claim 5, wherein the polyacrylic acid or polyacrylate has a molecular weight of 1-100K.
7. The method according to claim 1, wherein the acid for adjusting the pH is one or more of hydrochloric acid, acetic acid, sulfuric acid, nitric acid, and phosphoric acid; the alkali used for adjusting the pH is one or more of sodium hydroxide, potassium carbonate, sodium bicarbonate, potassium bicarbonate, sodium hydrogen phosphate, potassium hydrogen phosphate, sodium dihydrogen phosphate and potassium dihydrogen phosphate.
8. The preparation method according to claim 1, wherein the mass ratio of the temperature-sensitive cellulose to the polyacrylic acid or polyacrylate is (0.5-2): 1.
9. A temperature-sensitive cellulose smart window prepared according to the preparation method of any one of claims 1-8.
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| CN113896908B (en) * | 2021-10-11 | 2023-06-23 | 上海大学 | Composite hydrogel, preparation method thereof, thermoelectric dual-drive composite hydrogel intelligent window and preparation method thereof |
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