Crosslinked polyethylene glycol based anti-icing gel coating, anti-icing gel and preparation method

Abstract

The invention relates to the technical field of anti-icing gel, and provides a cross-linked polyethylene glycol-based anti-icing gel coating, anti-icing gel and a preparation method. The cross-linked polyethylene glycol based anti-icing gel coating provided by the invention comprises the following components: a polyethylene glycol alkenyl polymer, an organic solvent, a sulfydryl cross-linking agent, a photoinitiator and an anti-icing agent, the polyethylene glycol alkenyl polymer is polyethylene glycol diallyl formamide and / or polyethylene glycol diacrylate, and the anti-icing agent is glycol and / or polyethylene glycol. The coating provided by the invention can form anti-icing gel after being photo-cured, a matrix of the anti-icing gel is cross-linked polyethylene glycol, and embedded micromolecular glycol and / or polyethylene glycol, and through crystallization-melting of a polyethylene glycol network in the matrix, glycol and / or polyethylene glycol can be released at a low temperature and resorbed at a high temperature; meanwhile, by controlling the molecular weight of the polyethylene glycol alkenyl polymer, the release temperature of ethylene glycol and / or polyethylene glycol can be controlled below 0 DEG C, so that intelligent anti-icing is realized.

Description

Technical Field

[0001] The present invention relates to the technical field of anti-icing gel, and in particular to a cross-linked polyethylene glycol-based anti-icing gel coating, an anti-icing gel and a preparation method thereof. Background Art

[0002] When water vapor in the air contacts the surface of a material with a temperature below the freezing point, a phase change occurs to form frost. Ice formation in a low-temperature environment seriously affects the operation and safety of equipment and causes significant losses to the national economy. For example, ice on the surface of refrigeration equipment can reduce the heat transfer efficiency of the equipment or even cause it to fail; ice on the surface of an aircraft can change the aerodynamic shape of the aircraft and affect flight safety.

[0003] At present, the common anti-icing methods are active anti-icing and passive anti-icing. Active anti-icing refers to removing ice crystals from the surface of objects through electric heating, vibration, etc. to prevent the ice layer from thickening, but this method is inefficient and costly. Passive anti-icing is to change the surface properties of objects through anti-icing materials to prevent the formation and adhesion of ice crystals.

[0004] Organogels have been developed as a strategy to reduce ice adhesion in recent years, because the liquid small molecules introduced into them have low surface energy and are easy to shear, which can effectively reduce ice adhesion. However, current anti-icing gels lack intelligent response capabilities, and the liquid small molecules inside the gel cannot actively migrate. How to make the liquid small molecules inside the gel actively migrate to the surface to resist ice under icing conditions is still a major challenge facing this field. Summary of the invention

[0005] In view of this, the present invention provides a cross-linked polyethylene glycol-based anti-icing gel coating, an anti-icing gel, and a preparation method. The cross-linked polyethylene glycol-based anti-icing gel coating provided by the present invention forms an anti-icing gel after curing, and the liquid small molecules inside the anti-icing gel can actively migrate to the surface under icing conditions, thereby realizing intelligent anti-icing.

[0006] In order to achieve the above-mentioned object of the invention, the present invention provides the following technical solutions:

[0007] A cross-linked polyethylene glycol-based anti-icing gel coating comprising the following components:

[0008] Polyethylene glycol alkenyl polymer, organic solvent, mercapto crosslinking agent, photoinitiator and anti-icing agent; the polyethylene glycol alkenyl polymer is polyethylene glycol diallyl formamide and / or polyethylene glycol diacrylate; the polyethylene glycol diallyl formamide has a weight average molecular weight of 1066.18 to 1466.18; the polyethylene glycol diacrylate has a weight average molecular weight of 900 to 1300;

[0009] The anti-icing agent is glycol and / or polyglycol;

[0010] The molar ratio of the thiol group in the thiol cross-linking agent to the double bond functional group in the polyethylene glycol olefin polymer is (1-4):(2-3); the mass of the photoinitiator is 1-5% of the mass of the polyethylene glycol olefin polymer; the mass of the anti-icing agent is 30-65% of the total mass of the anti-icing agent and the polyethylene glycol olefin polymer.

[0011] Preferably, the weight average molecular weight of the polyethylene glycol diallylformamide is 1166.18; and the weight average molecular weight of the polyethylene glycol diacrylate is 1000.

[0012] Preferably, the preparation method of polyethylene glycol diallylformamide comprises:

[0013] Polyethylene glycol, allyl isocyanate, a solvent and a catalyst are mixed for addition reaction to obtain the polyethylene glycol diallyl formamide; the weight average molecular weight of the polyethylene glycol is 900-1300.

[0014] Preferably, the molar ratio of the polyethylene glycol to allyl isocyanate is 1:(2-3); the catalyst is an organic tin catalyst or an organic bismuth catalyst; the mass of the catalyst is 0.5-2% of the mass of the polyethylene glycol;

[0015] The temperature of the addition reaction is 75-95° C. and the time is 4-6 hours.

[0016] Preferably, the organic solvent is a chlorinated alkane; the mass ratio of the organic solvent to the polyethylene glycol olefin polymer is (2-4):1;

[0017] The mercapto crosslinking agent includes one or more of trimethylolpropane tris(3-mercaptopropionate) and pentaerythritol tetrathioglycolate; the photoinitiator is photoinitiator 651; and the polyglycol is one or more of diethylene glycol, triethylene glycol, tetraethylene glycol, pentaethylene glycol, hexaethylene glycol and heptaethylene glycol.

[0018] The present invention also provides a method for preparing the cross-linked polyethylene glycol-based anti-icing gel coating described in the above scheme, comprising the following steps:

[0019] The cross-linked polyethylene glycol-based anti-icing gel coating is obtained by mixing polyethylene glycol olefin-based polymer, organic solvent, mercapto cross-linking agent, photoinitiator and anti-icing agent.

[0020] The present invention also provides a cross-linked polyethylene glycol-based anti-icing gel, which is obtained by photocuring the cross-linked polyethylene glycol-based anti-icing gel coating described in the above scheme.

[0021] The present invention also provides a method for preparing the cross-linked polyethylene glycol-based anti-icing gel described in the above scheme, comprising the following steps:

[0022] The cross-linked polyethylene glycol-based anti-icing gel coating is coated and then light-cured to obtain the cross-linked polyethylene glycol-based anti-icing gel.

[0023] Preferably, the photocuring is ultraviolet light curing; the main wavelength of the ultraviolet light used in the ultraviolet light curing is 315-450nm, and the main wavelength is 365nm; the photocuring is to perform double-sided curing on the coating obtained by coating, and the curing time of each side is independently 1-4 minutes.

[0024] Preferably, after the UV curing is completed, the obtained solidified material is further subjected to desolventizing, and the desolventizing temperature is 50°C.

[0025] The invention provides a cross-linked polyethylene glycol-based anti-icing gel coating, comprising the following components: a polyethylene glycol alkenyl polymer, an organic solvent, a thiol cross-linking agent, a photoinitiator and an anti-icing agent; the polyethylene glycol alkenyl polymer is polyethylene glycol diallyl formamide and / or polyethylene glycol diacrylate; the polyethylene glycol diallyl formamide has a weight average molecular weight of 1066.18 to 1466.18; the polyethylene glycol diacrylate has a weight average molecular weight of 900 to 1300; the anti-icing agent is glycol and / or polyglycol; the molar ratio of the thiol in the thiol cross-linking agent to the double bond functional group in the polyethylene glycol alkenyl polymer is (1 to 4):(2 to 3); the mass of the photoinitiator is 1 to 5% of the mass of the polyethylene glycol alkenyl polymer; the mass of the anti-icing agent is 30 to 65% of the total mass of the anti-icing agent and the polyethylene glycol alkenyl polymer. The cross-linked polyethylene glycol-based anti-icing gel coating provided by the present invention can form an anti-icing gel after photocuring. The matrix of the anti-icing gel is cross-linked polyethylene glycol and embedded small molecule glycol and / or polyglycol. Through the crystallization-melting of the polyethylene glycol network in the matrix, the glycol and / or polyglycol can be released at low temperature and reabsorbed at high temperature. The glycol and / or polyglycol have an anti-icing effect. By utilizing their reversible appearance at the interface, anti-ice adhesion performance and delayed frosting performance can be obtained. In addition, the present invention can control the release temperature of glycol and / or polyglycol to below 0°C by controlling the molecular weight of the polyethylene glycol olefinic polymer, so that it is suitable for icing conditions and realizes intelligent anti-icing. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] Figure 1 This is a diagram demonstrating the reversible release performance of the anti-icing agent of the anti-icing gel in Example 1;

[0027] Figure 2 The secretion efficiency of the gel obtained in Example 1 and Comparative Example 1 varies with temperature;

[0028] Figure 3 The test results of the anti-ice adhesion performance of the gels obtained in Example 1 and Comparative Example 3;

[0029] Figure 4The delayed frosting performance test results of the gels prepared in Example 1 and Comparative Example 1 are shown. DETAILED DESCRIPTION

[0030] The present invention provides a cross-linked polyethylene glycol-based anti-icing gel coating, comprising the following components:

[0031] Polyethylene glycol alkenyl polymer, organic solvent, mercapto crosslinking agent, photoinitiator and anti-icing agent; the polyethylene glycol alkenyl polymer is polyethylene glycol diallyl formamide and / or polyethylene glycol diacrylate; the polyethylene glycol diallyl formamide has a weight average molecular weight of 1066.18 to 1466.18; the polyethylene glycol diacrylate has a weight average molecular weight of 900 to 1300;

[0032] The anti-icing agent is glycol and / or polyglycol;

[0033] The molar ratio of the thiol group in the thiol cross-linking agent to the double bond functional group in the polyethylene glycol olefin polymer is (1-4):(2-3); the mass of the photoinitiator is 1-5% of the mass of the polyethylene glycol olefin polymer; the mass of the anti-icing agent is 30-65% of the total mass of the anti-icing agent and the polyethylene glycol olefin polymer.

[0034] Unless otherwise specified, all raw materials / components used in the present invention are commercially available.

[0035] The cross-linked polyethylene glycol-based anti-icing gel coating provided by the present invention includes polyethylene glycol alkenyl polymers. In the present invention, the polyethylene glycol alkenyl polymers are polyethylene glycol diallyl formamide and / or polyethylene glycol diacrylate; the polyethylene glycol diallyl formamide has a weight average molecular weight of 1066.18 to 1466.18, preferably 1166.18; the polyethylene glycol diacrylate has a weight average molecular weight of 900 to 1300, preferably 1000.

[0036] In the present invention, the preparation method of the polyethylene glycol diallylformamide preferably comprises: mixing polyethylene glycol, allyl isocyanate, a solvent and a catalyst for addition reaction to obtain the polyethylene glycol diallylformamide; the weight average molecular weight of the polyethylene glycol is 900 to 1300, preferably 1000.

[0037] In the present invention, the molar ratio of the polyethylene glycol and allyl isocyanate is preferably 1:(2-3); the catalyst is preferably an organic tin catalyst or an organic bismuth catalyst, the organic tin catalyst is preferably dibutyltin dilaurate (DBTDL), and the organic bismuth catalyst is preferably DY-20; the mass of the catalyst is 0.5-2% of the mass of the polyethylene glycol, specifically 0.5%, 1%, 1.5% or 2%; the solvent is preferably N,N-dimethylformamide (DMF); the temperature of the addition reaction is preferably 75-95°C, specifically 75°C, 80°C, 90°C or 95°C, the time of the addition reaction is preferably 4-6h, specifically 4h, 5h or 6h; the addition reaction is preferably carried out under nitrogen protection; the present invention uses allyl isocyanate to end-cap polyethylene glycol through an addition reaction to obtain polyethylene glycol diallylformamide. After the addition reaction is completed, the present invention preferably adds the obtained reaction liquid into n-heptane, washes the precipitated precipitate and then dries it to obtain polyethylene glycol diallylformamide.

[0038] The cross-linked polyethylene glycol-based anti-icing gel coating provided by the present invention comprises an organic solvent; the organic solvent is preferably a chlorinated alkane; the chlorinated alkane is preferably one or more of dichloromethane, chloroform and trichloroethane; the mass ratio of the organic solvent to the polyethylene glycol olefin polymer is preferably (2-4):1, specifically 2:1, 2.5:1, 3:1 or 4:1.

[0039] The cross-linked polyethylene glycol-based anti-icing gel coating provided by the present invention includes a thiol cross-linking agent. In the present invention, the molar ratio of the thiol group in the thiol cross-linking agent to the double bond functional group in the polyethylene glycol olefin polymer is (1-4): (2-3), specifically 4:3, 1:2, 1:3, 4:2, 3:2, 3:3 or 4:2.5; the thiol cross-linking agent preferably includes one or two of trimethylolpropane tris (3-mercaptopropionate) (TMPMP) and pentaerythritol tetrathioglycolate.

[0040] The cross-linked polyethylene glycol-based anti-icing gel coating provided by the present invention includes a photoinitiator. In the present invention, the mass of the photoinitiator is 1-5% of the mass of the polyethylene glycol olefin polymer, specifically 1%, 2%, 3%, 4% or 5%; the photoinitiator is preferably photoinitiator 651.

[0041] The cross-linked polyethylene glycol-based anti-icing gel coating provided by the present invention includes an anti-icing agent. In the present invention, the anti-icing agent is glycol and / or polyglycol; the polyglycol is preferably one or more of diethylene glycol, triethylene glycol, tetraethylene glycol, pentaethylene glycol, hexaethylene glycol and heptaethylene glycol; the mass of the anti-icing agent is preferably 30-65% of the total mass of the anti-icing agent and the polyethylene glycol olefin polymer, specifically 30%, 40%, 45%, 55% or 65%.

[0042] The present invention also provides a method for preparing the cross-linked polyethylene glycol-based anti-icing gel coating described in the above scheme, comprising the following steps:

[0043] The cross-linked polyethylene glycol-based anti-icing gel coating is obtained by mixing polyethylene glycol olefin-based polymer, organic solvent, mercapto cross-linking agent, photoinitiator and anti-icing agent.

[0044] In a specific embodiment of the present invention, it is preferred to first dissolve the polyethylene glycol olefin polymer in an organic solvent, and then add a thiol cross-linking agent, a photoinitiator and an anti-icing agent for mixing; or, the polyethylene glycol olefin polymer, the thiol cross-linking agent, the photoinitiator and the anti-icing agent are directly added to the organic solvent for mixing.

[0045] The present invention also provides a cross-linked polyethylene glycol-based anti-icing gel, which is obtained by photocuring the cross-linked polyethylene glycol-based anti-icing gel coating described in the above scheme. In the present invention, the cross-linked polyethylene glycol-based anti-icing gel can be attached to the surface of the substrate as a coating, or can be used in the form of an anti-icing gel film, which will be described in detail later.

[0046] The present invention also provides a method for preparing the cross-linked polyethylene glycol-based anti-icing gel described in the above scheme, comprising the following steps:

[0047] The cross-linked polyethylene glycol-based anti-icing gel coating is coated and then light-cured to obtain the cross-linked polyethylene glycol-based anti-icing gel.

[0048] In the present invention, the light curing is preferably ultraviolet light curing; the main band of ultraviolet light used for the ultraviolet light curing is 315-450nm, and the main wavelength is 365nm; in a specific embodiment of the present invention, ultraviolet lamp is preferably used for ultraviolet light curing, and the power of the ultraviolet lamp is preferably 25W; the light curing is to perform double-sided curing on the coating obtained by coating, and the curing time of each side is independently preferably 1-4min; in a laboratory embodiment of the present invention, the cross-linked polyethylene glycol-based anti-icing gel coating can be poured into an open culture dish, the open surface is first placed under an ultraviolet lamp for curing, and then the other side is inverted for curing; the present invention can eliminate the cross-linking gradient as much as possible through double-sided curing.

[0049] In other specific embodiments of the present invention, the coating can be directly coated on a substrate and then photocured to obtain an anti-icing gel coating on the substrate surface, and the substrate can be glass or aluminum. Alternatively, the coating can be coated on a polytetrafluoroethylene-based substrate surface and then photocured, and then the cured film can be removed to obtain a separate anti-icing gel film.

[0050] In the present invention, after the photocuring is completed, it is preferred that the obtained solidified material is desolvated, and the temperature of the desolvation is preferably 50°C; in the laboratory embodiment of the present invention, the gel is demolded from the open culture dish after the desolvation to obtain the cross-linked polyethylene glycol-based anti-icing gel; in the present invention, when the anti-icing agent is glycol, the obtained anti-icing gel is recorded as glycol / cross-linked polyethylene glycol-based anti-icing gel; when the anti-icing agent is polyethylene glycol, the obtained anti-icing gel is recorded as polyethylene glycol / cross-linked polyethylene glycol-based anti-icing gel.

[0051] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0052] Example 1

[0053] Synthesis of polyethylene glycol diallylformamide: 10 g of polyethylene glycol with a weight average molecular weight of 1000 was weighed into a three-necked flask, 18 g of DMF solvent was added to dissolve the polyethylene glycol, and then 1.83 g of allyl isocyanate and 3 g of DBTDL were added, nitrogen was passed through, and the reaction was carried out at 90°C with magnetic stirring for 5 h. The reaction liquid was precipitated in n-heptane, and the obtained precipitate was washed and dried to obtain polyethylene glycol diallylformamide.

[0054] Synthesis of poly(ethylene glycol) / cross-linked polyethylene glycol)-based anti-icing gel: 2 g of polyethylene glycol diallyl formamide, 0.4557 g of TMPMP, 0.1 g of photoinitiator 651, and 2 g of triethylene glycol were dissolved in 4.67 g of trichloroethane. The resulting solution was poured into an open petri dish, and the open side was placed under a UV lamp for curing for 3 min, and then the other side was inverted for curing for 3 min. Then the trichloroethane was removed at 50°C to obtain a poly(ethylene glycol) / cross-linked polyethylene glycol-based anti-icing gel.

[0055] Example 2

[0056] Compared with Example 1, polyethylene glycol diallyl formamide is replaced with polyethylene glycol diacrylate having a weight average molecular weight of 1000, as follows:

[0057] Synthesis of poly(ethylene glycol) / cross-linked polyethylene glycol)-based anti-icing gel: 2 g of polyethylene glycol diacrylate with a weight average molecular weight of 1000, 0.4557 g of TMPMP, 0.1 g of photoinitiator 651, and 2 g of triethylene glycol were dissolved in 4.67 g of trichloroethane. The resulting solution was poured into an open petri dish, and the open side was placed under a UV lamp for curing for 3 min, and then the other side was inverted for curing for 3 min. After that, the trichloroethane was removed at 50°C to obtain a poly(ethylene glycol) / cross-linked polyethylene glycol-based anti-icing gel.

[0058] Example 3

[0059] Compared with Example 1, triethylene glycol is replaced with hexaethylene glycol. The details are as follows:

[0060] Synthesis of polyethylene glycol diallylformamide: Weigh 10 g of polyethylene glycol with a weight average molecular weight of 1000 in a three-necked flask, add 18 g of DMF to dissolve, add 1.83 g of allyl isocyanate and 3 g of DBTDL, pass nitrogen, and react at 90°C with magnetic stirring for 5 hours. The reaction liquid is precipitated in n-heptane, washed and dried to obtain polyethylene glycol diallylformamide.

[0061] Synthesis of poly(ethylene glycol) / cross-linked polyethylene glycol)-based anti-icing gel: 2 g of polyethylene glycol diallyl formamide, 0.4557 g of TMPMP, 0.1 g of photoinitiator 651, and 2 g of hexaethylene glycol were dissolved in 4.67 g of trichloroethane. The resulting solution was poured into an open petri dish, and the open side was placed under a UV lamp for curing for 3 min, and then the other side was inverted for curing for 3 min. After that, trichloroethane was removed at 50°C to obtain a poly(ethylene glycol) / cross-linked polyethylene glycol-based anti-icing gel.

[0062] Comparative Example 1

[0063] The polyethylene glycol with a weight average molecular weight of 1000 in Example 1 was replaced with polyethylene glycol with a weight average molecular weight of 4000. The specific steps are as follows:

[0064] Synthesis of polyethylene glycol diallylformamide: 10 g of polyethylene glycol with a weight average molecular weight of 4000 was placed in a three-necked flask, 18 g of DMF was added to dissolve, 0.52 g of allyl isocyanate and 3 g of DBTDL were added, nitrogen was passed through, and the reaction was carried out at 90°C with magnetic stirring for 5 h. The reaction solution was precipitated in n-heptane, and the obtained precipitate was washed and dried to obtain polyethylene glycol diallylformamide.

[0065] Synthesis of poly(ethylene glycol) / cross-linked polyethylene glycol)-based anti-icing gel: 2 g of polyethylene glycol diallyl formamide, 0.1276 g of TMPMP, 0.1 g of photoinitiator 651, and 2 g of triethylene glycol were dissolved in 4.67 g of trichloroethane. The resulting solution was poured into an open petri dish, and the open side was placed under a UV lamp for curing for 3 min, and then the other side was inverted for curing for 3 min. After that, trichloroethane was removed at 50°C to obtain a poly(ethylene glycol) / cross-linked polyethylene glycol-based anti-icing gel.

[0066] Comparative Example 2

[0067] The other conditions were the same as those in Example 1, except that photocuring was not performed. The results showed that the obtained system had no reversible release effect, which further explained the importance of photocuring for the system to achieve a reversible release effect.

[0068] Comparative Example 3

[0069] The other conditions were the same as those in Example 1, except that triethylene glycol was not added. The results showed that the obtained system had no reversible release effect, and thus no delayed frosting performance, and exhibited great ice adhesion, proving the importance of the anti-icing agent (ethylene glycol / polyethylene glycol) in the system to achieve anti-icing performance.

[0070] Performance Testing

[0071] Performance Test:

[0072] 1. Reversible release performance test

[0073] Figure 1 This is a demonstration diagram of the reversible release performance of the anti-icing agent of the anti-icing gel in Example 1. Figure 1 It can be seen that after the anti-icing gel of the present invention is kept at -10°C for 1 hour, triethylene glycol is released from the surface. After being kept at -10°C for 7 hours, the triethylene glycol released to the surface increases significantly. After the temperature is raised to 60°C, the triethylene glycol is absorbed back into the anti-icing gel, indicating that the anti-icing gel of the present invention has the performance of reversibly releasing the anti-icing agent.

[0074] 2. Quantitative test of release performance

[0075] The mass of poly(ethylene glycol) released from the anti-icing gel at different temperatures was tested by weighing method, and then its mass percentage of the total poly(ethylene glycol) was calculated, which is the secretion efficiency. The specific test method is: weigh the mass of the anti-icing gel sample, recorded as m0, then the total mass M of poly(ethylene glycol) in the sample is m0×w, where w is the mass percentage of poly(ethylene glycol) in the anti-icing gel, and the calculation method is: w=m 防 / m 总 ×100%, where m 防 Indicates the mass of the anti-icing agent, m 总 represents the total mass of the anti-icing agent and polyethylene glycol olefin polymer. The anti-icing gel sample was then placed at the release temperature for 12 h, and the polyethylene glycol released on the interface was subsequently removed with a non-woven fabric, and the remaining mass was weighed and recorded as m1; the mass of polyethylene glycol released on the surface was m0-m1; and the secretion efficiency was (m0-m1) / (m0×w).

[0076] Figure 2 The secretion efficiency of the gels obtained in Example 1 and Comparative Example 1 varies with temperature, wherein PEG1000 represents the anti-icing gel prepared in Example 1, and PEG4000 represents the gel prepared in Comparative Example 1. Figure 2 It can be seen that the release temperature range of triethylene glycol is related to the molecular weight of polyethylene glycol olefin polymer. When the polyethylene glycol diallyl formamide is synthesized, the polyethylene glycol molecular weight (M w=1000), the obtained anti-icing gel starts to release triethylene glycol at around 0°C, and the release amount increases first and then decreases as the temperature decreases; while the polyethylene glycol molecular weight (M w =4000), the obtained anti-icing gel starts to release triethylene glycol only when the temperature is above 0°C; the above content shows that the anti-icing gel prepared by using low molecular weight polyethylene glycol olefin polymer is suitable for anti-icing conditions and can realize intelligent anti-icing.

[0077] 3. Anti-ice adhesion performance test

[0078] Test method 1: Place ice cubes on a 2 cm×2 cm anti-icing gel sample, then place it in a low temperature environment of -20°C, and test the ice adhesion after 24 hours.

[0079] Test method 2: After placing the anti-icing gel sample at -20°C for 24 hours, place ice cubes on it to test ice adhesion.

[0080] Figure 3 The test results of the anti-ice adhesion performance of the gels obtained in Example 1 and Comparative Example 3 are as follows: Figure 3 Wherein CPEG / 3EG is the anti-icing gel prepared in Example 1, and CPEG is the gel prepared in Example 3; Figure 3 It can be seen that the anti-icing gel prepared in Example 1 of the present invention exhibits low ice adhesion under both test methods, the ice adhesion under the first test method is about 3 kPa, and the ice adhesion under the second test method is about 7 kPa; while the ice adhesion of the gel prepared in Comparative Example 3 reaches more than 110 kPa.

[0081] 4. Delayed frosting performance test

[0082] The anti-icing gel sample was placed on a cold platform at -20°C and water mist was continuously sprayed with an air humidifier. The water mist was condensed to form frost on the surface of the sample, and the frosting performance of the sample was observed.

[0083] Figure 4 The test results of the delayed frosting performance of the gel prepared in Example 1 and Comparative Example 1, wherein CPEG / 3EG is the anti-icing gel prepared in Example 1, and CPEG is the gel prepared in Example 3. The test results show that the gel prepared in Comparative Example 3 can completely cover the surface with frost after being placed in a -20°C high humidity environment for 8 minutes. However, no surface frost was observed on the anti-icing gel in Example 1 within 8 minutes. After removing the water deposited on the surface sample and the released glycol, the frosting performance was tested again. A small amount of frost appeared on the edge of the sample in Example 1 because triethylene glycol was lost in the system. At this time, triethylene glycol was replenished in a swelling manner, and the sample regained the ability to delay frosting. After being placed in a -20°C high humidity environment for 15 minutes, obvious frost was observed on the sample.

[0084] The anti-icing gels prepared in Examples 2 and 3 were subjected to a reversible release performance test, a release performance quantitative test, an anti-ice adhesion performance test, and a delayed frosting performance test, and showed similar effects to those in Example 1.

[0085] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principle of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims

1. A cross-linked polyethylene glycol-based anti-icing gel coating, characterized in that: Includes the following components: Polyethylene glycol alkenyl polymer, organic solvent, mercapto crosslinking agent, photoinitiator and anti-icing agent; the polyethylene glycol alkenyl polymer is polyethylene glycol diallyl formamide and / or polyethylene glycol diacrylate; the polyethylene glycol diallyl formamide has a weight average molecular weight of 1066.18 to 1466.18; the polyethylene glycol diacrylate has a weight average molecular weight of 900 to 1300; The anti-icing agent is glycol and / or polyglycol; The molar ratio of the thiol group in the thiol cross-linking agent to the double bond functional group in the polyethylene glycol olefin polymer is (1-4):(2-3); the mass of the photoinitiator is 1-5% of the mass of the polyethylene glycol olefin polymer; the mass of the anti-icing agent is 30-65% of the total mass of the anti-icing agent and the polyethylene glycol olefin polymer.

2. The cross-linked polyethylene glycol-based anti-icing gel coating according to claim 1, characterized in that: The weight average molecular weight of the polyethylene glycol diallylformamide is 1166.18; the weight average molecular weight of the polyethylene glycol diacrylate is 1000.

3. The cross-linked polyethylene glycol-based anti-icing gel coating according to claim 1 or 2, characterized in that: The preparation method of the polyethylene glycol diallylformamide comprises: Polyethylene glycol, allyl isocyanate, a solvent and a catalyst are mixed for addition reaction to obtain the polyethylene glycol diallyl formamide; the weight average molecular weight of the polyethylene glycol is 900-1300.

4. The cross-linked polyethylene glycol-based anti-icing gel coating according to claim 3, characterized in that: The molar ratio of the polyethylene glycol to allyl isocyanate is 1:(2-3); the catalyst is an organic tin catalyst or an organic bismuth catalyst; the mass of the catalyst is 0.5-2% of the mass of the polyethylene glycol; The temperature of the addition reaction is 75-95° C. and the time is 4-6 hours.

5. The cross-linked polyethylene glycol-based anti-icing gel coating according to claim 1, characterized in that: The organic solvent is a chlorinated alkane; the mass ratio of the organic solvent to the polyethylene glycol olefin polymer is (2-4):1; The mercapto crosslinking agent includes one or two of trimethylolpropane tris(3-mercaptopropionate) and pentaerythritol tetrathioglycolate; the photoinitiator is photoinitiator 651; and the polyglycol is one or more of diethylene glycol, triethylene glycol, tetraethylene glycol, pentaethylene glycol, hexaethylene glycol and heptaethylene glycol.

6. The method for preparing the cross-linked polyethylene glycol-based anti-icing gel coating according to any one of claims 1 to 5, characterized in that: The following steps are involved: The cross-linked polyethylene glycol-based anti-icing gel coating is obtained by mixing polyethylene glycol olefin-based polymer, organic solvent, mercapto cross-linking agent, photoinitiator and anti-icing agent.

7. A cross-linked polyethylene glycol-based anti-icing gel, characterized in that: The anti-icing gel coating is obtained by photocuring the cross-linked polyethylene glycol-based anti-icing gel coating according to any one of claims 1 to 5.

8. The method for preparing the cross-linked polyethylene glycol-based anti-icing gel according to claim 7, characterized in that: The following steps are involved: The cross-linked polyethylene glycol-based anti-icing gel coating is coated and then light-cured to obtain the cross-linked polyethylene glycol-based anti-icing gel.

9. The preparation method according to claim 8, characterized in that: The light curing is ultraviolet light curing; the main wavelength of ultraviolet light used in the ultraviolet light curing is 315-450nm, and the main wavelength is 365nm; the light curing is to perform double-sided curing on the coating obtained by coating, and the curing time of each side is independently 1-4 minutes.

10. The preparation method according to claim 7, characterized in that: After the UV curing is completed, the obtained solidified material is subjected to desolventizing, and the desolventizing temperature is 40-100°C.

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