CN115558275A - Preparation method of high-strength temperature-sensitive color-changing hydrogel light-adjusting bent glass - Google Patents
Preparation method of high-strength temperature-sensitive color-changing hydrogel light-adjusting bent glass Download PDFInfo
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- CN115558275A CN115558275A CN202211292138.4A CN202211292138A CN115558275A CN 115558275 A CN115558275 A CN 115558275A CN 202211292138 A CN202211292138 A CN 202211292138A CN 115558275 A CN115558275 A CN 115558275A
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/075—Macromolecular gels
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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
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
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- C—CHEMISTRY; METALLURGY
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- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
- C08J3/246—Intercrosslinking of at least two polymers
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- E04B2/00—Walls, e.g. partitions, for buildings; Wall construction with regard to insulation; Connections specially adapted to walls
- E04B2/88—Curtain walls
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Abstract
The application is a divisional application with the application number of 2022111677123 and the patent name of 'a high-strength temperature-sensitive allochroic hydrogel'. The application discloses the field of preparation of dimming glass, and particularly discloses a preparation method of high-strength temperature-sensitive color-changing hydrogel dimming bent glass, which comprises the steps of S1, S2, S3 and S4, wherein the step of S1: adding the temperature-sensitive polymer, the gel compound, the antifreezing agent, the temperature regulator, the organic cross-linking agent and the infrared absorption functional particles into water for dissolving to obtain a mixed solution A; s2: adding an initiator into the mixed solution A, and uniformly mixing to obtain a mixed solution B; s3, adhering adhesive tapes around each two pieces of glass to establish a cavity space and arranging a reserved opening; s4: and injecting the mixed solution B into the glass cavity through a pipeline, adjusting the glass angle every 3-5 minutes to enable the mixed solution B to be uniformly distributed, sealing the reserved opening, and curing. The bent glass prepared by the method has sensitive heat-sensitive performance, high strength and long service life.
Description
The application is a divisional application with the patent number of 2022111677123, and the patent name is 'a high-strength temperature-sensitive color-changing hydrogel'.
Technical Field
The application relates to the field of glass preparation, in particular to a preparation method of high-strength temperature-sensitive color-changing hydrogel light-adjusting bending glass.
Background
In China, building energy consumption accounts for over 27% of total energy consumption, and is increasing at a rate of 1% per year. The statistics of the construction department show that the area of a newly built house in urban and rural construction in China is nearly 20 hundred million square meters every year, wherein more than 80 percent of the buildings are high-energy-consumption buildings; the existing buildings are about 400 hundred million square meters, and more than 95 percent of the buildings are high-energy-consumption buildings. The proportion of building energy consumption to total national energy consumption is rapidly increased from 27.6 percent to more than 33 percent at present. The new buildings in China are basically designed according to the energy-saving standard, the proportion is as high as 95.7%, and the proportion of the energy-saving design standard executed in the construction stage is only 53.8%.
The energy-saving glass building materials include electric control dimming glass, temperature control dimming glass, light control dimming glass and the like. Temperature control dimming glass is also named as thermotropic dimming glass, and is a glass system which is applied to building curtain walls and has a sun-shading function. When sunlight irradiates the temperature control dimming glass, the sunlight heats the glass, and the dimming glass gradually atomizes after the temperature reaches the set temperature, so that the sun-shading function is realized. When the sunlight is weakened, the temperature of the temperature control dimming glass is reduced, and the glass is restored to be transparent, which is the same as common glass. The process is repeatedly reversible, and no external energy or special person is needed for management. In the prior art, a great deal of research is carried out on the temperature control glass gel, for example, documents report that poly-N-isopropylacrylamide temperature-sensitive gel has higher temperature sensitivity but insufficient weather resistance, and cannot generate a sun-shading effect under the condition that the environment temperature is lower than the response temperature of a temperature-sensitive material but the burning sensation of sunlight is strong. In order to solve the above problems, researchers have found that a temperature-sensitive polymer, such as a polyvinyl acetal gel, which responds at a specific temperature, can be realized by modifying the water-soluble property of polyvinyl alcohol by introducing a hydrophobic group into the molecular chain of polyvinyl alcohol.
Because the temperature control dimming glass has a sun-shading function, other internal and external sun-shading measures are not required to be additionally added, the building facade and the top surface are really simple and transparent, the space is saved, and the temperature control dimming glass is rich in aesthetic feeling and modern sense, more possibilities are created for the design of modern buildings, and wide application requirements are brought, for example, future buildings of Shenzhen Ke institute, kunming national plant museum, chongqing Dongshui bridge sightseeing elevator sun-shading facilities and the like. These requirements are certainly not sufficient to achieve the technical effects of temperature-sensitive and energy-saving, but require longer service lives, which include the recoverability of the temperature-sensitive material and the mechanical properties of the glass structure. Otherwise, as frequent iterative updates generate much garbage which cannot be recycled, the environmental pollution is caused, and the cost for replacing glass of the building is also very considerable.
Disclosure of Invention
The high-strength temperature-sensitive color-changing hydrogel is also called a temperature-sensitive gel system or temperature-sensitive gel, and is a composition of all compounds for preparing temperature-sensitive color-changing hydrogel dimming glass, which is formed by temperature-sensitive polymeric materials, gel compounds and other auxiliary agents.
The gel compound referred to herein is a compound having carboxyl, hydroxyl, amino groups and water and an ionic crosslinking agent which affect the structure of the gel network, excluding initiators and organic crosslinking agents.
The temperature-sensitive polymer is also called as a temperature-sensitive polymeric material, and is specifically a triblock polymer formed by polyoxyethylene and polyoxypropylene or polyoxyethylene and polyoxybutylene, the molecular weight of the triblock polymer is 1000-8500, the HLB value of the triblock polymer is 3-30, and both ends of the triblock polymer are polyoxyethylene.
The product temperature control precision is also called sensitivity, and the specific detection method is a product temperature control precision detection method.
In order to solve the problems, the application provides the temperature-sensitive color-changing hydrogel dimming glass with high strength, long service life and high sensitivity and precision of +/-1 ℃ and the preparation method thereof.
In a first aspect, the application provides a high-strength, long-life, temperature-sensitive, color-changing hydrogel light control glass, which adopts the following technical scheme:
a high-strength temperature-sensitive color-changing hydrogel is prepared from the following raw materials: 0.5-15wt% of temperature-sensitive polymer, 5-15wt% of gel compound, 5-30wt% of antifreezing agent, 0.1-1wt% of temperature regulator, 0.01-0.2wt% of organic cross-linking agent, 0.01-0.1wt% of infrared absorption functional particles, 0.01-0.5wt% of initiator and the balance of water,
the temperature-sensitive polymeric material is a triblock polymer formed by polyoxyethylene and polyoxypropylene or polyoxyethylene and polyoxybutylene, the molecular weight of the triblock polymer is 1000-8500, the HLB value of the triblock polymer is 3-30, and both ends of the triblock polymer are polyoxyethylene;
the gel compound consists of A, B and three components C:
the component A is agar or chitosan;
the component B is sodium carboxymethyl cellulose or acrylic acid or a mixture of the sodium carboxymethyl cellulose and the acrylic acid;
the component C is acrylamide monomer or polyacrylamide or gelatin, and when the component B is acrylic acid, the component C is not acrylamide monomer;
the other components are water and an ionic crosslinking agent;
the ionic crosslinking agent is Fe dissolved in water 3+ Salt or Ca 2+ And (3) salt.
By adopting the technical scheme, the hydrogel generally forms a network structure of the hydrogel through chemical crosslinking, physical crosslinking and chemical physical crosslinking. Chemically crosslinked hydrogels refer to permanent and irreversible network structures formed by chemical crosslinking, e.g., covalent or ionic, that have high strength and toughness but cannot be repaired once they are destroyed. And physically crosslinked hydrogels are bonded to the crosslinked polymer network by van der waals forces, electrostatic interactions, hydrogen bonding, hydrophobic associations, or combinations of these interactions between molecular chains. The physical crosslinking network has reversibility under certain conditions, and can enable the hydrogel to have a self-recovery function, a plastic function and the like.
The gel compound contains three groups of-OH, -NH2 and-COOH, more specifically, the carboxyl-containing sodium carboxymethyl cellulose or acrylic acid, the amino-containing polyacrylamide or other amide-type high-molecular polymers capable of forming amide bonds with carboxyl, such as Acrylamide (AM) monomer or polyacrylamide or gelatin, and the hydroxyl-containing agar or chitosan. The carboxyl and the hydroxyl can form ester, and can also form amide with amino, namely three gel compounds form chemical crosslinking of ester or amide through covalent bonds, the gel system also contains iron ions and/or calcium ions, so that ion complex chemical crosslinking is formed, and simultaneously strong molecular chain entanglement is generated due to the same van der Waals force, electrostatic interaction, hydrogen bond interaction (such as NH2-OH or OH-OH hydrogen bond), hydrophobic association interaction, electrostatic interaction or combination of the interactions in the high-strength temperature-sensitive color-changing hydrogel system, so that the gel prepared by the application has certain strength and toughness and has a plastic function and a self-recovery function, and the service life of the temperature-sensitive color-changing hydrogel dimming glass is prolonged; compared with sodium alginate, the technical effect of adopting carboxymethyl cellulose is better, particularly, the carboxymethyl cellulose is artificially modified cellulose, and the introduction amount of carboxymethyl is convenient to control. Most importantly, compared with sodium alginate, carboxymethyl cellulose of different manufacturers has no influence on the quality stability of the high-strength temperature-sensitive color-changing hydrogel, but different sodium algin cannot ensure the quality stability of the final temperature-sensitive color-changing hydrogel, possibly caused by different reactions of the impurity content of the sodium alginate of different manufacturers or slight difference (such as carboxyl content difference) of the sodium alginate per se to the system. Meanwhile, the gel compound also comprises agar or chitosan, so that more intramolecular cross-links are formed by carboxyl, namely, hydroxyl of the agar is cross-linked with hydroxyl or amino of the chitosan, carboxyl and hydroxyl cross-links in carboxymethyl cellulose molecules are relatively less, and an amide bond, an ester bond, a hydrogen bond and other staggered network structures are formed, so that the chain length is prolonged, and the ionic cross-linking points are increased, so that the strength and toughness of the hydrogel are increased, and the service life of the temperature-sensitive allochroic hydrogel is further prolonged;
in addition, the temperature-sensitive polymeric material in the application can expand and contract freely along with the temperature change in the hydrogel network structure, and finally appears in the temperature control precision of the product, the temperature control precision of the product in the prior art is +/-2 ℃ or higher, and the temperature control precision of the temperature-sensitive allochroic hydrogel light-adjusting glass in the application is +/-1 ℃. The reason for this is probably because, on the one hand, molecular chains in the temperature-sensitive color-changing hydrogel system are not only entangled with each other but also repel each other, and a cavity with a certain aperture is formed due to intermolecular repulsion, so that the temperature-sensitive material is deformed more freely. On the other hand, the temperature-sensitive polymer material is dissolved in the water of the temperature-sensitive color-changing hydrogel, and is dispersed and dissolved in the water when the temperature is lower, and is aggregated and separated out when the temperature is higher, so that the temperature control precision is high.
Preferably, the polymerization degree of the sodium carboxymethyl cellulose is 200-300, the etherification degree is 0.6-0.7, and 2-3mmol of carboxymethyl is introduced into 1g of dry weight of cellulose on average.
By adopting the technical scheme, 2-3mmol of carboxymethyl is introduced into 1g of dry weight of cellulose, so that the solubility of carboxymethyl cellulose is better.
Preferably, the ionic crosslinking agent contains Ca 2+ A salt.
By adopting the technical scheme, when the gel compound adopts carboxymethyl cellulose, calcium ions are preferentially selected as the ionic crosslinking agent. Same Fe 3+ Compared with the temperature-sensitive color-changing hydrogel dimming glass prepared by taking calcium ions as an ionic cross-linking agent, the temperature control precision is higher, which is probably because Ca 2+ The network gel grid has larger aperture, and is more favorable for the temperature-sensitive polymerization to freely stretch along with the temperature change when the chain length of the temperature-sensitive polymerization is longer.
Preferably, the mass ratio of the component A, the component B and the component C is (0.1-0.5): (0.2-2): (1-5).
By adopting the technical scheme, within the mass ratio range, the crosslinking conditions of various components are good, the strength, toughness, sensitivity and heat gain coefficient of the prepared temperature-sensitive allochroic hydrogel can achieve the optimal effect, and the specific expression is that no broken glass appears in 5 groups of experiments, the sensitivity is +/-1 ℃, the heat gain coefficient is not higher than 0.12, and the service life is more than 35 years.
Preferably, the pH value of the high-strength temperature-sensitive color-changing hydrogel is 6-8.
Preferably, the use temperature of the high-strength temperature-sensitive color-changing hydrogel is-20 ℃ to 80 ℃.
Preferably, the polyacrylamide has an average molecular weight of 50 to 100 ten thousand; the average molecular weight of the gelatin is 5-7 ten thousand; the average molecular weight of the agar is 10-15 ten thousand; the average molecular weight of the chitosan is 3-5 ten thousand.
By adopting the technical scheme, the molecular weight of the gel compound formed by the compound with the average molecular weight is proper, the molecular weight of the gel compound is too large, the strength and the toughness of the prepared temperature-sensitive allochroic hydrogel are strong, but the sensitivity is reduced, the molecular weight of the gel compound is too small, and the strength and the toughness of the prepared temperature-sensitive allochroic hydrogel are insufficient. This is probably because when the molecular weight of the gel compound is too large, the crosslinked state is more dense, resulting in too small pore diameters of the lattice structure, and conversely, when the molecular weight of the gel compound is too small, too few network crosslinks, resulting in a decrease in strength or toughness.
In a second aspect, the application provides a high-strength temperature-sensitive color-changing hydrogel light-adjusting glass with high strength and long service life, which adopts the following technical scheme:
the heat gain coefficient of the temperature-sensitive color-changing hydrogel light-adjusting glass prepared from the temperature-sensitive color-changing hydrogel is less than or equal to 0.12.
Preferably, the heat coefficient is 0.108 or more.
Preferably, the service life of the temperature-sensitive color-changing hydrogel light-adjusting glass is as long as 35 years.
In a third aspect, the application provides a preparation method of high-strength temperature-sensitive color-changing hydrogel light-adjusting glass, which adopts the following technical scheme:
a preparation method of high-strength temperature-sensitive color-changing hydrogel dimming glass comprises the following preparation steps:
s1: adding a temperature-sensitive polymer, a gel compound, an antifreezing agent, a temperature regulator, an organic cross-linking agent and infrared absorption functional particles into water for dissolving to obtain a mixed solution A;
s2: adding an initiator into the mixed solution A, and uniformly mixing to obtain a mixed solution B;
s3, adhering adhesive tapes around each two pieces of glass to establish a cavity space and arrange a reserved opening, and then adjusting the distance between each two pieces of glass to be 1.5-2.5cm through pressure;
s4: and (3) the mixed solution B is deeply injected into the glass cavity far away from the reserved opening through a pipeline, the injection flow rate is 2.0-2.5L/min, the reserved opening is sealed, the temperature is heated to 30-70 ℃, and the high-strength temperature-sensitive color-changing hydrogel dimming glass is obtained after 1-1.5 h.
The temperature-sensitive color-changing hydrogel is poured into the glass cavity through the glue injection process to form the temperature-controlled glass, so that the following technical effects can be achieved:
1. the solar heat gain coefficient SHGC is not higher than 0.12;
2. product temperature control precision: plus or minus 1 ℃;
service life: for more than 35 years.
Preferably, the reserved opening in the step S3 is one and is arranged on the side surface of the temperature-sensitive color-changing hydrogel light modulation glass, and the length of the reserved opening is 3.5-6.0cm.
Preferably, in step S4, mixed liquor B is injected through a pipeline to a position 10-30cm far away from the reserved opening.
Preferably, the diameter of the pipe in step S4 is 1.5-2.5cm.
Preferably, the sealing reserved opening in the step S4 is sealed by using a glue sealing method.
When the glass is the bent toughened glass, the preferable step S4 is to deeply insert the mixed liquid B into the reserved opening through a pipeline and inject the mixed liquid B into the glass cavity, adjust the glass angle every 3-5 minutes to enable the mixed liquid B to be uniformly distributed, seal the reserved opening, heat the mixed liquid B for 30-70 ℃ and obtain the high-strength temperature-sensitive gel bent glass after 1-1.5 hours.
By adopting the technical scheme, the inventor also unexpectedly discovers that the heat gain coefficient of the dimming glass prepared from the temperature-sensitive color-changing hydrogel is further reduced to 0.108 and is far lower than the approved value of a relevant local standard by 0.18 in the experimental process, and proves that the temperature-sensitive color-changing hydrogel and the glue injection process have the technical effects of keeping the glass structure complete and having better environment-friendly and energy-saving effects.
In summary, the present application has the following beneficial effects:
1. the gel compound simultaneously contains three groups of-OH, -NH2 and-COOH, carboxyl and hydroxyl can form ester and can also form amide with amino, namely the three gel compounds form chemical crosslinking of ester or amide through covalent bonds, the gel system also contains iron ions and/or calcium ions, so that ion complexing chemical crosslinking is formed, and meanwhile, van der Waals force, electrostatic interaction, hydrogen bond interaction (such as NH2-OH or OH-OH hydrogen bonds), hydrophobic association, electrostatic interaction or combination of the interactions also exist in the temperature-sensitive color-changing hydrogel system, so that stronger entanglement of molecular chains is generated, and therefore the gel prepared by the method has certain strength and toughness, and also has a plastic function and a self-recovery function, so that the service life of the temperature-sensitive color-changing hydrogel dimming glass is prolonged;
2. the technical effect of adopting the carboxymethyl cellulose is better, and the carboxymethyl cellulose is matched with the agar or the chitosan, so that more sufficient and stable intramolecular cross-links are formed by carboxyl, namely, hydroxyl of the agar is cross-linked with hydroxyl or amino of the chitosan, carboxyl and hydroxyl cross-links in carboxymethyl cellulose molecules are relatively less, an amide bond, an ester bond, a hydrogen bond and other staggered network structures are formed, the chain length is prolonged, and an ionic cross-linking point is increased, so that the strength and the toughness of the hydrogel are improved, and the service life of the temperature-sensitive color-changing hydrogel dimming glass is further prolonged.
3. The temperature-sensitive polymeric material in the hydrogel network structure can stretch and contract more freely along with the temperature change, and finally appears in the temperature control precision of a product, the temperature control precision of the product in the prior art is +/-2 ℃ or higher, and the temperature control precision of the temperature-sensitive allochroic hydrogel light-adjusting glass is +/-1 ℃; the heat coefficient of the temperature-sensitive dimming glass prepared from the temperature-sensitive color-changing hydrogel is not more than 0.12, and is further reduced to 0.108 by the improved glue injection process, and is far lower than the approved value of the relevant local standard by 0.18, so that the temperature-sensitive color-changing hydrogel and the glue injection process thereof both improve the sun-shading effect of the existing temperature-sensitive color-changing hydrogel dimming glass.
Drawings
FIG. 1 is a flow chart of the process for laminating the temperature-sensitive color-changing hydrogel light control glass according to the present application;
FIG. 2 is a flow chart of the process for light-bending glass laminating of the temperature-sensitive color-changing hydrogel.
Detailed Description
Performance detection test: each detection index is provided with 5 groups of experiments, and each group of experiments is provided with 6 glass experiments.
1. The heat gain coefficient is detected by a GB50189-20152.0.4 Solar Heat Gain Coefficient (SHGC) detection method.
2. The durability detection method comprises the following steps:
2.1 color change cycle durability: the temperature control dimming glass is kept for 5 minutes in an environment with the temperature of not higher than 25 ℃, then the sample is placed in a drying oven with the temperature of 65 ℃ and kept for 5 minutes, after the circulation is carried out for more than 3000 times, the sample is placed in an environment with the temperature of 23 +/-2 ℃ for 24 hours, and then observation is carried out, the sample cannot generate bubbles, blooms and the like, the change value of the visible light transmittance before and after the experiment is less than or equal to 3%, and the change value of the sun shading coefficient is less than or equal to 0.05. If the test sample is circulated 3000 times, the test sample can not generate bubbles, bloom and other phenomena, the change value of the visible light transmittance before and after the test is less than or equal to 3%, and the change value of the shading coefficient is less than or equal to 0.05, the service life is defined as 15 years, if the test sample is circulated 4000 times, the test sample can not generate bubbles, bloom and other phenomena, the change value of the visible light transmittance before and after the test is less than or equal to 3%, and the change value of the shading coefficient is less than or equal to 0.05, the service life is 20 years, and so on, if the test sample is circulated 7000 times, the test sample can not generate bubbles, bloom and other phenomena, and the change value of the visible light transmittance before and after the test is less than or equal to 3%, and the change value of the shading coefficient is less than or equal to 0.05, the service life is 35 years.
2.2 durability at high temperature and high humidity: the temperature control dimming glass is placed in an environment with the temperature of 85 ℃ and the humidity of 85% for preventing 2500 hours, and then is placed in an environment with the temperature of 23 +/-2 ℃ for 24 hours, and then observation is carried out, so that the phenomena of bubbles, flowering and the like cannot be generated on a sample, the change value of the visible light transmittance before and after the experiment is less than or equal to 3%, and the change value of the shading coefficient is less than or equal to 0.05.
3. The product temperature control precision detection method comprises the following steps: the detection method adopted by the application comprises the following steps: and (3) placing the temperature control dimming glass in an oven with a set temperature, and carrying out visible light transmittance test after heat preservation of each temperature point for 30min (the temperature of the product reaches the set temperature of the oven). The difference value Delta T of the visible light transmittance measured by two adjacent temperature points with the difference of 1 DEG C Transparent film As a criterion, Δ T Penetrate through ＝T2 Transparent film -T1 Transparent film Wherein T2 Transparent film The visible light transmittance measured at the temperature point T2; t1 Transparent film The visible light transmittance measured at the temperature point T1; when Δ T Penetrate through And when the temperature is more than or equal to 5 percent, judging the T2 as the color-changing temperature point. When the temperature of T2-T1=1 ℃, the temperature control precision of the product is +/-1 ℃.
4. Detection indexes of the glue-pouring glass are as follows: the adhesive for bonding the glass and the supporting material is smooth and free from adhesive seepage and overflow. No air bubble with the diameter larger than 1.5mm is generated after glue pouring.
5. Method for detecting mechanical strength and toughness
Falling ball impact peeling performance test: 5 sets of experiments are set, each set of experiments is set with 6 glass tests, the glass tests are detected according to the method GB 15763.3-20097.11, and the number of damaged glass blocks is calculated according to GB15763.3-20096.10 and 8.3.5, and finally the number of the glass which is broken and the intermediate layer is exposed due to chip stripping is counted.
All listed gel preparations in this application are considered as variant components and, for the sake of clarity and brief description of the inventive process of this application, the components common to the various preparations are described in the way stated. In addition, in all gel preparation examples, after a gel system and a temperature-sensitive polymer are mixed, the temperature-sensitive color-changing hydrogel dimming glass is prepared by different preparation methods, and then the mechanical strength, the sensitivity, the haze, the transparency, the heat gain coefficient and the like are detected and investigated according to the detection method and the standard of the temperature-controlled glass at the temperature of-20-80 ℃. The application also simultaneously investigates the influence of different pH values on the temperature-sensitive gel system with the same components. The present application only lists the beneficial effects distinguished from the prior art, and the processes and effects of the present invention are briefly described, and the examination items which are not different from the prior art are omitted.
When all the preparations in the present application are used as test samples, at least 5 groups are set for statistical analysis under each test condition in each preparation.
The technical solution of the present application will be further described in detail with reference to specific embodiments.
Example 1 investigation of the effect of carboxyl groups on the gel system:
example 1 was prepared from preparations 1.A, 1.B and 1.C, respectively, using a gel compound.
All the gel compounds and the content ratios thereof are shown in preparation examples 1A-1C, and mainly a plurality of common carboxyl-containing carboxymethyl cellulose, acrylic acid and sodium alginate are examined.
Preparation examples 1.A1 to 1.A4
The component A is agar, the component B is sodium carboxymethylcellulose, the component C is polyacrylamide, the ionic cross-linking agent is ferric sulfate and water to prepare a gel compound, and the components A, B and C, the cross-linking agent and water are proportioned according to the following table 1A:
TABLE 1 component ratios of gel Compounds
Preparation examples 1.B1-1.B4
Different from preparation 1.A, component B is sodium alginate, and the compounding ratio is specifically as shown in table 1B:
TABLE 1B component ratios of gel compounds
Preparation examples 1.C1 to 1.C4
Different from preparation 1.A, component B is acrylic acid, specifically in the following ratio in table 1C:
TABLE 1C component ratios of gel Compounds
Example 1A preparation of a high-strength temperature-sensitive color-changing hydrogel privacy glass comprises the following steps:
s1: adding 0.5kg of temperature-sensitive polymer, 5kg of gel compound, 5kg of antifreezing agent, 0.1kg of temperature regulator, 0.01kg of organic cross-linking agent and 0.01kg of infrared absorption functional particles into 89.37kg of water for dissolving to obtain a mixed solution A;
s2: adding 0.01kg of initiator into the mixed solution, and uniformly mixing to obtain a mixed solution B;
s3: adhering adhesive tapes around each two pieces of glass to establish a cavity space and arranging 2 reserved openings, wherein the length of each reserved opening is 3.5-6.0cm, the smaller the glass is, the smaller the reserved opening is, and then adjusting the distance between each piece of glass to be 1.5-2.5cm through pressure;
s4: before the mixed liquid B is injected into the glass cavity, the liquid injection pipe is deeply inserted to a position which is 10cm-30cm far away from the reserved opening, the specific test is carried out on the glass size, the smaller the glass is, the shorter the penetration distance is, the pipe diameter of the peristaltic pump is 1.5cm, the speed and the flow rate of the peristaltic pump are adjusted to be 2.0L/min, the mixed liquid B is injected into the glass cavity, the reserved opening is sealed in a plug mode, and the high-strength temperature-sensitive color-changing hydrogel dimming glass is obtained after heating for 1h at the temperature of 30 ℃.
Wherein the temperature-sensitive polymeric material is a triblock polymer formed by polyoxyethylene and polyoxypropylene, the molecular weight of the triblock polymer is between 1000 and 8500, the HLB value of the triblock polymer is between 3 and 30, and both ends of the triblock polymer are polyoxyethylene;
in the application document, the polymerization degree of the sodium polycarboxymethyl cellulose is 200-300, the etherification degree is 0.6-0.7, 2-3mmol of carboxymethyl is introduced into cellulose per 1g of dry weight on average, the average molecular weight of polyacrylamide is 50-100 ten thousand, the average molecular weight of gelatin is 5-7 ten thousand, the average molecular weight of agar is 10-15 ten thousand, and the average molecular weight of chitosan is 3-5 ten thousand;
the antifreezing agent is ethylene glycol; the temperature regulator is sodium dodecyl sulfate, and the organic cross-linking agent is N, N ' -methylene bisacrylamide and N, N, N ', N ' -tetramethyl ethylenediamine; the infrared absorption functional particles are vanadium dioxide; the initiator is sodium bisulfite, potassium bisulfite and ammonium persulfate;
in the range of-20 ℃ to 80 ℃, the thermal coefficient groups and the groups of the temperature-sensitive allochroic hydrogel light-adjusting glass prepared in the preparation examples 1.A, 1.B and 1.C have no significant difference, and the average thermal coefficient is 0.114; the temperature control precision of the product does not have significant difference between groups, and the temperature control precision of the product is +/-1 ℃; when the cycle times of the color-changing cycle durability experiment reach 7000 times, the sample does not generate bubbles, blossoming and other phenomena, the change value of the visible light transmittance before and after the experiment is less than or equal to 3 percent, and the change value of the shading coefficient is less than or equal to 0.05; in the experimental detection process of mechanical strength and toughness, two batches of sodium alginate from different sources are unexpectedly found to have significant difference, which is specifically shown in that one group of the preparation example 1.B is broken in a ball drop test, then the two batches of sodium alginate are respectively adopted to carry out repeated verification at the temperature of 0 ℃, 25 ℃ and 40 ℃ according to four mixture ratios of the preparation example 1.B, and similar results are obtained, and the conclusion is probably caused by different reactions of the system due to the impurity content of the sodium alginate of different manufacturers or slight difference (such as carboxyl content difference) of the sodium alginate. Therefore, in order to ensure the stability of the mechanical strength of the temperature-sensitive gel, sodium carboxymethyl cellulose and acrylic acid are preferably used as donors of carboxyl.
The embodiment 1B is different from the embodiment 1A in that 1 reserved opening is arranged in the step S3 and is arranged on the side surface of the temperature-sensitive color-changing hydrogel light modulation glass, and the reserved opening is sealed in a glue sealing manner. In the range of-20 ℃ to 80 ℃, the heat gain coefficients of the temperature-sensitive allochroic hydrogel dimming glass prepared by the preparation examples 1.A, 1.B and 1.C are respectively in 1.A, 1.B and 1.C groups, and no significant difference exists among the groups, and the average heat gain coefficient is 0.108; compared with the example 1A, the example 1B has significant difference, which is significantly better than the example 1A, and shows that the preparation method has significant influence on the temperature-sensitive effect of the temperature-sensitive color-changing hydrogel dimming glass.
Example 2 the effect of amino groups on temperature sensitive gel systems was mainly examined.
The gel compounds used in example 2 were from preparations 2.A, 2.B, 2.C and 2.D, respectively.
Preparation examples 2.A1 to 2.A4
The component A is agar, the component B is sodium carboxymethylcellulose, the component C is an acrylamide monomer, the components A, B and C, an ionic crosslinking agent and water are used in the following amount according to the proportion in a table 2A:
TABLE 2 component proportions of gel Compounds
Preparation example 2.B1-2.B4
The component A is agar, the component B is acrylic acid, the component C is an acrylamide monomer, and the components A, B and C, the ionic crosslinking agent and the water are proportioned according to the following table 2B:
TABLE 2B component ratios of gel compounds
Preparation examples 2.C1-2.C4
The component A is agar, the component B is acrylic acid, the component C is an acrylamide monomer, a cross-linking agent and water form a gel compound, and the components A, B and C, an ionic cross-linking agent and water are proportioned according to the following dosage in a table 2C:
TABLE 2C component ratios of gel Compounds
Preparation examples 2.D1-2.D4
The component A is agar, the component B is sodium carboxymethylcellulose, the component C is gelatin, and the components A, B and C, the ionic crosslinking agent and water are proportioned according to the following dosage in a table 2D:
TABLE 2 component proportions of gel Compounds
The difference between the embodiment 2A and the embodiment 1A is that the dosage of each raw material for preparing the high-strength temperature-sensitive color-changing hydrogel light-adjusting glass is different, and the parameters of S3 are different, specifically:
s1: adding 10kg of temperature-sensitive polymer, 10kg of gel compound, 10kg of antifreezing agent, 0.5kg of temperature regulator, 0.1kg of organic cross-linking agent and 0.05kg of infrared absorption functional particles into 69.35kg of water for dissolving to obtain a mixed solution A;
s2: adding 0.2kg of initiator into the mixed solution, and uniformly mixing to obtain a mixed solution B;
s3: adhering adhesive tapes around each two pieces of glass to establish a cavity space and arranging 2 reserved openings, wherein the diameter of each reserved opening is 3.5-6.0cm, the smaller the glass is, the smaller the reserved opening is, and then adjusting the distance between each piece of glass to be 1.5-2.5cm through pressure;
s4: before the mixed liquid B is injected into the glass cavity, the liquid injection pipe is deeply far away from the reserved opening by about 10cm-30cm, the specific glass size is determined, the smaller the glass is, the shorter the deep distance is, the pipe diameter of the peristaltic pump is 2.5cm, the speed and the flow rate of the peristaltic pump are adjusted by 2.5L/min, the mixed liquid B is injected into the glass cavity, the reserved opening is sealed in a plug mode, and the high-strength temperature-sensitive color-changing hydrogel dimming glass is obtained after heating at 50 ℃ for 1.5 h.
In the experimental detection process of the mechanical strength and toughness of the temperature-sensitive color-changing hydrogel dimming glass at the temperature of-20-80 ℃, in the ball drop test, 2 groups of experimental glass at 0 ℃ are broken, and 5 groups of experimental glass at 20 ℃ are broken, and then the temperature-sensitive color-changing hydrogel dimming glass prepared in the preparation example 2B is repeatedly verified at 0 ℃ and-20 ℃ to obtain similar results, and the conclusion is that the acrylic acid-acrylamide chemical crosslinking fails probably because the polymerization of acrylic acid and acrylamide monomers is reversely carried out towards the direction of raw materials at a low temperature, and finally the gel network structure is loose. Therefore, in order to secure mechanical strength of the temperature-sensitive color-changing hydrogel, when the B component is acrylic acid, the C component is not acrylamide. Statistical analysis is carried out on the coefficient of heat gain in and among the temperature-sensitive color-changing hydrogel light-adjusting glass groups prepared in the preparation examples 2A, 2C and 2D, no significant difference exists, and the average coefficient of heat gain is 0.116; the temperature control precision of the product does not have significant difference between groups, and the temperature control precision of the product is +/-1 ℃; when the cycle times of the color-changing cycle durability experiment reach 7200 times, the sample does not generate bubbles, blooms and the like, the change value of the visible light transmittance before and after the experiment is less than or equal to 3 percent, the change value of the sun-shading coefficient is less than or equal to 0.05, namely the service life is more than 35 years.
Statistical analysis was performed on the glass samples prepared in examples 1A and 2A except for the glass samples prepared in preparation examples 1B and 2B, and there was no significant difference in the average heat gain coefficient, service life, mechanical strength and toughness, and sensitivity among the five other preparation examples.
Embodiment 2B is different from embodiment 2A in that the number of the reserved openings in step S3 is set to 1, and the reserved openings are arranged on the side surface of the temperature-sensitive color-changing hydrogel light control glass, and are sealed by using a glue sealing method. In the range of-20 ℃ to 80 ℃, no significant difference exists between the heat coefficient groups and between the temperature-sensitive color-changing hydrogel light-adjusting glass prepared by the preparation examples 2A and 2C, and the average heat coefficient is 0.110; the example 2B is significantly different from the example 2A and is significantly better than the example 2A, which indicates that the preparation method has a significant influence on the temperature-sensitive effect of the temperature-sensitive color-changing hydrogel light control glass.
Statistical analysis is carried out on the temperature-sensitive color-changing hydrogel light-regulating glasses prepared in the embodiments 1B and 2B except the temperature-sensitive color-changing hydrogel light-regulating glasses prepared in the preparation examples 1B and 2B, and the average heat gain coefficient, the service life, the mechanical strength, the toughness and the sensitivity of the temperature-sensitive color-changing hydrogel light-regulating glasses prepared in the other five groups of preparation examples except the preparation examples 1B and 2B are not significant.
Example 3 the effect of hydroxyl groups on temperature sensitive color changing hydrogel systems was mainly examined.
Example 3 was from preparations 3.A, 3.B, 3.C and 3D, respectively, using gel compounds.
Preparation examples 3.A1 to 3.A4
The component A is chitosan, the component B is carboxymethyl cellulose, the component C is polyacrylamide, a cross-linking agent and water form a gel compound, and the components A, B and C, the cross-linking agent and water are combined according to the proportion in a table 3A:
TABLE 3 component ratios of gel Compounds
Preparation examples 3.B1 to 3.B4
The component A, the component B, the component C, the cross-linking agent and water form a gel compound, and the components A, B and C, the cross-linking agent and water are proportioned according to the following table 3:
TABLE 3B component ratios of gel compounds
Preparation examples 3.C1 to 3.C4
The gel compound is formed by the component A, the component B, the component C, the cross-linking agent and water, and the components A, B and C, the cross-linking agent and water are combined according to the proportion in the following table 3C:
TABLE 3C component ratios of gel Compounds
Preparation examples 3.D1-3. D4
The gel compound is formed by the component A, the component B, the component C, the cross-linking agent and water, and the components A, B and C, the cross-linking agent and water are combined according to the proportion in the following table 3:
TABLE 3 component ratios of gel Compounds
The embodiment 3A is different from the embodiment 1A in that the amount of each raw material for preparing the high-strength temperature-sensitive color-changing hydrogel light control glass is different, and specifically comprises the following steps:
s1: adding 15kg of temperature-sensitive polymer, 15kg of gel compound, 30kg of antifreezing agent, 1kg of temperature regulator, 0.1kg of organic cross-linking agent and 0.05kg of infrared absorption functional particles into 38.65kg of water for dissolving to obtain a mixed solution A;
s2: adding 0.2kg of initiator into the mixed solution, and uniformly mixing to obtain a mixed solution B;
s3: adhering adhesive tapes around each two pieces of glass to establish a cavity space and arranging 2 reserved openings, wherein the diameter of each reserved opening is 3.5-6.0cm, the smaller the glass is, the smaller the reserved opening is, and then adjusting the distance between each piece of glass to be 1.5-2.5cm through pressure;
s4: before the mixed liquid B is injected into the glass cavity, the liquid injection pipe is deeply far away from the reserved opening by about 10-30cm, and the smaller the glass is, the shorter the deep distance is; and (3) adjusting the pipe diameter of the peristaltic pump to be 2.0cm, adjusting the speed and the flow rate of the peristaltic pump to be 2.5L/min, injecting the mixed solution B into the glass cavity, sealing the reserved opening in a plugging mode, and heating at 70 ℃ for 1.5h to obtain the dimming glass containing the high-strength temperature-sensitive color-changing hydrogel.
In the experimental detection process of the mechanical strength and toughness of the temperature-sensitive color-changing hydrogel light-adjusting glass at the temperature of-20-80 ℃, the experimental glass breakage condition of the temperature-sensitive color-changing hydrogel light-adjusting glass prepared in the preparation example 3B group and the preparation example 3D group in the ball drop test is shown in Table 3E, and the inference is that the strength is reduced probably because the adjacent hydroxyl groups are far away compared with the adjacent hydroxyl groups of the polyvinyl alcohol and the chitosan or agar, so the acting force between the hydroxyl groups and the carboxyl groups, between the hydroxyl groups and the amide groups, and between the hydroxyl groups and the hydroxyl groups is weakened.
TABLE 3E CRASHING OF TEMPERATURE-SENSITIVE COLOUR-CHANGING HYDROGEL LIGHT REGULATING GLASS PREPARED BY PREPARATIVE EXAMPLE 3B GROUP AND PREPARATIVE EXAMPLE 3D GROUP
Statistical analysis is carried out on the heat gain coefficients of the preparation example 3A and the preparation example 3C in the range of-20 ℃ to 80 ℃ in a group and between groups, no significant difference exists, and the average heat gain coefficient is 0.119; the temperature control precision of the product does not have significant difference between groups, and the temperature control precision of the product is +/-1 ℃; when the cycle times of the color-changing cycle durability experiment reach 7500 times, the sample does not generate bubbles, blossoming and other phenomena, the change value of the visible light transmittance before and after the experiment is less than or equal to 3 percent, the change value of the sun-shading coefficient is less than or equal to 0.05, namely the service life is more than 35 years.
Statistical analysis was performed on the temperature-sensitive color-changing hydrogel light-adjusting glasses prepared in examples 1A, 2A and 3A except for the temperature-sensitive color-changing hydrogel light-adjusting glasses prepared in preparation examples 1B, 2B, 3B and 3D, and there was no significance in the differences among the average heat gain coefficient, the service life, the mechanical strength, the toughness and the sensitivity of the temperature-sensitive color-changing hydrogel light-adjusting glasses prepared in the other 7 preparation examples.
Embodiment 3B is different from embodiment 3A in that the number of the reserved openings in the step S3 is set to 1, and the reserved openings are arranged on the side surface of the temperature-sensitive color-changing hydrogel light modulation glass and sealed by using a glue sealing method. In the range of-20 ℃ to 80 ℃, the heat obtaining coefficients of the temperature-sensitive color-changing hydrogel light-adjusting glass prepared by the preparation examples 3A and 3C do not have significant difference in groups and among groups respectively, and the average heat obtaining coefficient is 0.111; compared with example 3A, the temperature-sensitive hydrogel dimming glass has significant difference, is significantly superior to example 3A, and shows that the preparation method has significant influence on the temperature-sensitive effect of the temperature-sensitive color-changing hydrogel dimming glass.
Statistical analysis was performed on the temperature-sensitive color-changing hydrogel light-adjusting glasses prepared in examples 1B, 2B, 3B and 3B except for the temperature-sensitive color-changing hydrogel light-adjusting glasses prepared in preparation examples 1B, 2B, 3B and 3D, and there was no significance in the differences among the average heat gain coefficient, the service life, the mechanical strength, the toughness and the sensitivity of the temperature-sensitive color-changing hydrogel light-adjusting glasses prepared in the other 7 preparation examples.
Example 4 the effect of pH on the gel system was mainly examined.
Examples 1-3 no deliberate adjustment of the pH of the gel system, the pH of the system being close to neutral between 6 and 8, it is well known to those skilled in the art that sodium carboxymethylcellulose is more stable under alkaline conditions and that the hydroxyl groups of sodium carboxymethylcellulose more readily form complexes with ferric ions under alkaline conditions, but from this consideration it is meant that the strength of the gel system is stronger under alkaline conditions when carboxymethylcellulose is the donor of the carboxyl groups, and therefore design example 4 was made to look at the pH of the gel system. Meanwhile, the prior art shows that the stability of carboxymethyl cellulose is inversely proportional to viscosity, the stability is poorer when the viscosity is larger, and the viscosity is larger when the concentration is higher.
In addition, as is well known to those skilled in the art, polyacrylamide, chitosan, gelatin and the like are unstable under acidic conditions, so that influence factors of a gel system are investigated without setting a low pH value.
Example 4A is different from example 3A in that the preparation step S1 is to add 15kg of the temperature sensitive polymer, 15kg of the gel compound, 30kg of the antifreeze, 1kg of the temperature regulator, 0.1kg of the organic crosslinking agent and 0.05kg of the infrared absorbing functional particles to 38.65kg of water for dissolution and to adjust the pH to 10 to obtain a mixed solution a.
At 25 ℃, the average obtained thermal coefficient is 0.119; mechanical strength and toughness experimental test example 4A did not show significant differences from the gel system obtained in example 3A; the temperature control sensitivity of the product is +/-2 ℃, and the product has a significant difference from the product in example 3A, probably because the grid structure is too tight when the pH is 10, so that the temperature-sensitive polymer and the gel grid are mutually entangled, and the shrinkage of the temperature-sensitive polymer is influenced when the temperature changes.
Embodiment 4B is different from embodiment 4A in that 1 reserved opening is arranged in the step S3 and is arranged on the side surface of the temperature-sensitive color-changing hydrogel light control glass, and the reserved opening is sealed by using a glue sealing method. In the range of-20 ℃ to 80 ℃, the heat obtaining coefficients of the temperature-sensitive color-changing hydrogel light-adjusting glass prepared in the embodiment 4B do not have significant difference in the group, and the average heat obtaining coefficient is 0.111; compared with the example 4A, the temperature-sensitive hydrogel dimming glass has significant difference and is significantly better than the example 4A, which shows that the preparation method has significant influence on the temperature-sensitive effect of the temperature-sensitive color-changing hydrogel dimming glass.
Example 5 the effect on the gel system was mainly examined when the polymer was a triblock polymer of polyoxyethylene and polyoxybutylene.
Example 5A the gel compound of preparation 3A was used, except that the temperature sensitive polymer was replaced with a triblock polymer of polyoxyethylene and polyoxybutylene, and both ends were polyoxyethylene, and the remaining steps were the same as in example 3A.
At 25 ℃, the average obtained thermal coefficient is 0.115; the mechanical strength and toughness test does not show that the gel system has no significant difference with the gel system obtained in the preparation example 3A; the temperature control precision of the product does not have significant difference between groups, and the temperature control precision of the product is +/-1 ℃; when the cycle times of the color-changing cycle durability experiment reach 7800 times, the sample does not generate bubbles, blossoming and other phenomena, the change value of the visible light transmittance before and after the experiment is less than or equal to 3 percent, the change value of the sun-shading coefficient is less than or equal to 0.05, namely the service life is more than 35 years.
The embodiment 5B is different from the embodiment 5A in that the number of the reserved openings in the step S3 is set to 1, the reserved openings are arranged on the side surface of the temperature-sensitive color-changing hydrogel dimming glass, and the reserved openings are sealed in a glue sealing manner. In the range of-20 ℃ to 80 ℃, the heat obtaining coefficients of the temperature-sensitive color-changing hydrogel light-adjusting glass prepared in the embodiment 5B do not have significant difference in the group, and the average heat obtaining coefficient is 0.109; compared with the example 5A, the temperature-sensitive hydrogel dimming glass has significant difference and is significantly better than the example 5A, which shows that the preparation method has significant influence on the temperature-sensitive effect of the temperature-sensitive color-changing hydrogel dimming glass.
Example 6 the effect on the gel system was mainly examined when the polymer was a triblock polymer of polyoxyethylene and polyoxypentene.
Example 6A the gel compound of preparation 3A was used, except that the temperature sensitive polymer was replaced with a triblock polymer of polyoxyethylene and polyoxypentene, and both ends were polyoxyethylene, and the remaining steps were the same as in example 3A.
At 25 ℃, the average obtained thermal coefficient is 0.121; the mechanical strength and toughness test does not show that the gel system has no significant difference with the gel system obtained in the preparation example 3A; the temperature control sensitivity of the product is +/-2 ℃, and the obvious difference exists between the temperature control sensitivity of the product and the preparation example 3A, probably because the polyoxypentene chain structure is long, the temperature-sensitive polymer grid structure is wound too tightly, so that the shrinkage of the temperature-sensitive polymer is influenced when the temperature changes, and the sensitivity is reduced.
When the cycle times of the color-changing cycle durability experiment reach 7800 times, the sample does not generate bubbles, blossoming and other phenomena, the change value of the visible light transmittance before and after the experiment is less than or equal to 3 percent, the change value of the sun-shading coefficient is less than or equal to 0.05, namely the service life is more than 35 years.
Embodiment 6B is different from embodiment 6A in that the number of the reserved openings in step S3 is set to 1, and the reserved openings are arranged on the side surface of the temperature-sensitive color-changing hydrogel light control glass and sealed by using a glue sealing method. In the range of-20 ℃ to 80 ℃, the heat obtaining coefficients of the temperature-sensitive color-changing hydrogel light-adjusting glass prepared in the embodiment 6B do not have significant difference in the group, and the average heat obtaining coefficient is 0.113; compared with example 6A, the temperature-sensitive hydrogel light control glass has significant difference, is significantly superior to example 6A, and shows that the preparation method has significant influence on the temperature-sensitive effect of the temperature-sensitive color-changing hydrogel light control glass.
Example 7 the effect of calcium ions on the gel system was mainly examined.
Example 7A differs from example 6A in that the ionic cross-linking agent, ferric sulphate, was replaced with calcium chloride and the remaining steps were the same.
At 25 ℃, the average obtained thermal coefficient is 0.118; the mechanical strength and toughness test shows no significant difference from the gel system obtained in example 6; the temperature control sensitivity of the product is +/-1 ℃, and the product has a significant difference from the temperature control sensitivity of the product in example 6, and probably iron ions can be complexed with three hydroxyl groups, calcium ions can be complexed with two hydroxyl groups, the chain structure of the polyoxypentene is long, and the calcium ions and the polyoxypentene are in the same gel polymer system, so that the winding density of the temperature-sensitive polymer grid structure is reduced, and the sensitivity is improved.
When the cycle times of the color-changing cycle durability experiment reach 7800 times, the sample does not generate bubbles, blossoming and other phenomena, the change value of the visible light transmittance before and after the experiment is less than or equal to 3 percent, the change value of the sun-shading coefficient is less than or equal to 0.05, namely the service life is more than 35 years.
Embodiment 7B is different from embodiment 7A in that the number of the reserved openings in the step S3 is set to 1, and the reserved openings are arranged on the side surface of the temperature-sensitive color-changing hydrogel light modulation glass, and are sealed by using a glue seal. In the range of-20 ℃ to 80 ℃, the heat gain coefficients of the temperature-sensitive color-changing hydrogel light control glass prepared in the embodiment 7B do not have significant difference in the group, and the average heat gain coefficient is 0.113; compared with example 7A, the temperature-sensitive hydrogel light-adjusting glass has significant difference and is significantly better than example 7A, which shows that the preparation method has significant influence on the temperature-sensitive effect of the temperature-sensitive color-changing hydrogel light-adjusting glass.
EXAMPLE 8 temperature-sensitive gel-bending glass
Example 8A
The gel compound is prepared from 1.A, the preparation process is the same as that in example 1B, after the temperature-sensitive color-changing hydrogel light-adjusting bent glass is prepared, in 30 glass blocks in five groups, the gel is uneven, and 17 glass blocks in total with wrinkles are directly judged to be unqualified products; the other 9 blocks have a large amount of bubbles larger than 1.5mm, and are directly judged as unqualified products by visual inspection; there are two, more than 1.5mm bubbles are within 10, but the diameter between 5mm-10mm is respectively 5 and 8; and the final two blocks are tested by the glue-pouring glass if the test result is unqualified, and the results are shown in table 8A:
example 8B
The difference from the embodiment 8A is that the step S4 is that the mixed solution B is deeply injected into the glass cavity through the pipeline, the glass angle is adjusted every 3 to 5 minutes to ensure that the mixed solution B is uniformly distributed, the reserved opening is sealed, and the high-strength temperature-sensitive color-changing hydrogel light-adjusting bent glass is obtained after heating for 1 hour at the temperature of 30 ℃.
At 25 ℃, the average heat gain coefficient of the obtained temperature-sensitive color-changing hydrogel light-adjustable bent glass is 0.110, and the obtained glass has no significant difference from that of the glass obtained in the embodiment 1B; the mechanical strength and toughness test does not show that the gel system has no significant difference with the gel system obtained in preparation example 1.A; the temperature control sensitivity of the product is +/-1 ℃; and the detection of the glue-pouring glass meets the specification.
Comparing examples 8A and 8B, in the curved steel glass glue injection process, adjusting the glass angle every 3-5 minutes to make the mixed solution B uniformly distributed is a necessary step for preparing the qualified temperature-sensitive color-changing hydrogel light-adjusting curved steel glass.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (10)
1.A preparation method of high-strength temperature-sensitive color-changing hydrogel light-adjusting bent glass comprises the steps of preparing S1 mixed solution A, preparing S2 mixed solution B, bonding butyl rubber strips around S3 two pieces of glass, adjusting the space between the two pieces of glass to set a glass cavity and a reserved opening, and injecting the solution B into the glass cavity for post-curing by S4, and is characterized in that:
and S1: adding a temperature-sensitive polymer, a gel compound, an antifreezing agent, a temperature regulator, an organic cross-linking agent and infrared absorption functional particles into water for dissolving to obtain a mixed solution A;
and S2: adding an initiator into the mixed solution A, and uniformly mixing to obtain a mixed solution B;
s3, adhering adhesive tapes around each two pieces of glass to establish a cavity space and set a reserved opening, and then adjusting the distance between each two pieces of glass to be 1.5-2.5cm through pressure;
and S4: and (3) deeply penetrating the mixed liquid B into the glass cavity far away from the reserved opening through a pipeline, adjusting the glass angle to ensure that the mixed liquid B is uniformly distributed every 3-5 minutes, sealing the reserved opening, heating to 30-70 ℃ for 1-1.5 hours to obtain the high-strength temperature-sensitive color-changing hydrogel light-adjusting bending glass.
2. The preparation method of the high-strength temperature-sensitive color-changing hydrogel light-dimming bent glass according to claim 1, which is characterized in that: and S3, setting the number of the reserved ports to be 1 or two.
3. The preparation method of the high-strength temperature-sensitive color-changing hydrogel light-dimming bent glass according to claim 1, which is characterized in that: the length of the reserved opening is 3.5-6.0cm.
4. The method for preparing the high-strength temperature-sensitive color-changing hydrogel light-dimming bent glass according to claim 1, characterized in that: the diameter of the pipeline in the S4 is 1.5-2.5cm.
5. The preparation method of the high-strength temperature-sensitive color-changing hydrogel light-dimming bent glass according to claim 1, which is characterized in that: in the step S4, the mixed liquor B is deeply injected to a position 10-30cm away from the reserved opening through a pipeline.
6. The preparation method of the high-strength temperature-sensitive color-changing hydrogel light-dimming bent glass according to claim 1, which is characterized in that: and in the step S4, the sealing reserved opening is sealed in a glue sealing mode.
7. The preparation method of the high-strength temperature-sensitive color-changing hydrogel light-dimming bent glass according to claim 1, which is characterized in that: the S1 medium temperature-sensitive polymer is a triblock polymer formed by polyoxyethylene and polyoxypropylene or polyoxyethylene and polyoxybutylene, the molecular weight of the triblock polymer is 1000-8500, the HLB value of the triblock polymer is 3-30, and two ends of the triblock polymer are polyoxyethylene.
8. The method for preparing the high-strength temperature-sensitive color-changing hydrogel light-dimming bent glass according to claim 1, characterized in that: the gel compound in S1 consists of A, B and C:
the component A is agar or chitosan,
the component B is sodium carboxymethyl cellulose or acrylic acid or a mixture of the sodium carboxymethyl cellulose and the acrylic acid,
the component C is acrylamide monomer or polyacrylamide or gelatin, and when the component B is acrylic acid, the component C is not acrylamide monomer,
the balance of water and ionic crosslinking agent, wherein the ionic crosslinking agent is Fe3+ salt or Ca2+ salt dissolved in water.
9. The method for preparing the high-strength temperature-sensitive color-changing hydrogel light-dimming bent glass according to claim 8, characterized in that: the mass ratio of the component A to the component B to the component C is (0.1-0.5): (0.2-2): (1-5).
10. The utility model provides a curved glass of high strength temperature sensitive color-changing aquogel light modulation which characterized in that: is prepared by the preparation method of any one of claims 1 to 9.
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| CN104086928A (en) * | 2014-07-04 | 2014-10-08 | 苏州珀力玛高分子材料有限公司 | Novel composition for intelligent dimming glass |
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