A cross-linked polyethylene glycol-based anti-icing gel coating, an anti-icing gel, and a method of preparation

Abstract

The present application relates to the technical field of anti-icing gel, and 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 application comprises the following components: polyethylene glycol alkenyl polymer, organic solvent, mercapto cross-linking agent, photoinitiator and 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 polyglycol.The coating provided by the present application can form an anti-icing gel after photocuring, the matrix of the anti-icing gel is cross-linked polyethylene glycol, and small-molecule glycol and / or polyglycol are embedded in the matrix; through 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; meanwhile, by controlling the molecular weight of the polyethylene glycol alkenyl polymer, the release temperature of the glycol and / or polyglycol can be controlled below 0 DEG C, so that intelligent anti-icing is realized.

Description

TECHNICAL FIELD

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

[0002] When water vapor in the air contacts the surface of a material with a temperature lower than the freezing point, 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 formation on the surface of refrigeration equipment can reduce the heat transfer efficiency of the equipment or even cause it to fail, and ice formation on the surface of an aircraft can change the aerodynamic shape of the aircraft and affect flight safety.

[0003] Currently, common anti-icing methods mainly include active anti-icing and passive anti-icing, wherein active anti-icing refers to removing ice crystals from the surface of an object by means of electric heating, vibration or the like to prevent the ice layer from thickening, but this method has low efficiency and high cost. Passive anti-icing refers to changing the properties of the surface of an object by means of an anti-icing material to prevent the formation and adhesion of ice crystals.

[0004] Organic gels have been developed in recent years as a strategy for reducing ice adhesion because the liquid small molecules introduced therein have low surface energy and are easy to shear, which can effectively reduce the adhesion of ice. However, current anti-icing gels lack intelligent response capability, and the liquid small molecules in the gel cannot be actively migrated, and how to make the liquid small molecules in the gel actively migrate to the surface to resist ice under icing conditions is still a major challenge in the field. SUMMARY

[0005] Therefore, the present application 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 application forms an anti-icing gel after curing, and the liquid small molecules in the anti-icing gel can actively migrate to the surface under icing conditions, thereby achieving intelligent anti-icing.

[0006] In order to achieve the above-mentioned application purposes, the present application provides the following technical solutions:

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

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

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

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

[0011] Preferably, the polyethylene glycol diallyl formamide has a weight average molecular weight of 1166.18; and the polyethylene glycol diacrylate has a weight average molecular weight of 1000.

[0012] Preferably, the method for preparing the polyethylene glycol diallyl formamide comprises the following steps:

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

[0014] Preferably, the molar ratio of the polyethylene glycol and the allyl isocyanate is 1:(2-3); the catalyst is an organic tin catalyst or an organic bismuth catalyst; and 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℃, and the time is 4-6h.

[0016] Preferably, the organic solvent is a chloroalkane; and the mass ratio of the organic solvent and the polyethylene glycol alkenyl polymer is (2-4):1.

[0017] The thiol crosslinking agent comprises one or more of trimethylolpropane tris(3-mercaptopropionate) and pentaerythritol tetramercaptoacetate; 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 application further provides a preparation method of the crosslinked polyethylene glycol-based anti-icing gel coating as described in the above scheme, comprising the following steps:

[0019] The polyethylene glycol alkenyl polymer, organic solvent, thiol crosslinking agent, photoinitiator and anti-icing agent are mixed to obtain the crosslinked polyethylene glycol-based anti-icing gel coating.

[0020] The application further provides a crosslinked polyethylene glycol-based anti-icing gel obtained by photocuring the crosslinked polyethylene glycol-based anti-icing gel coating as described in the above scheme.

[0021] The application further provides a preparation method of the crosslinked polyethylene glycol-based anti-icing gel as described in the above scheme, comprising the following steps:

[0022] The cross-linked polyethylene glycol-based anti-icing gel coating is obtained by light curing after coating the cross-linked polyethylene glycol-based anti-icing gel coating.

[0023] Preferably, the light curing is ultraviolet light curing; the main wave band of the ultraviolet light used in the ultraviolet light curing is 315-450 nm, and the main wavelength is 365 nm; the light curing is double-sided curing of the obtained coating, and the curing time of each side is independently 1-4 min.

[0024] Preferably, after the ultraviolet curing is completed, the obtained cured product is further subjected to solvent removal, and the temperature of the solvent removal is 50℃.

[0025] The present application provides a cross-linked polyethylene glycol-based anti-icing gel coating, comprising the following components: polyethylene glycol alkenyl polymer, organic solvent, mercapto cross-linking agent, photoinitiator and anti-icing agent; the polyethylene glycol alkenyl polymer is polyethylene glycol diallyl formamide and / or polyethylene glycol diacrylate; the weight average molecular weight of the polyethylene glycol diallyl formamide is 1066.18-1466.18; the weight average molecular weight of the polyethylene glycol diacrylate is 900-1300; the anti-icing agent is glycol and / or polyglycol; the molar ratio of mercapto groups in the mercapto cross-linking agent to double bond functional groups in the polyethylene glycol alkenyl polymer is (1-4):(2-3); the mass of the photoinitiator is 1-5% of the mass of the polyethylene glycol alkenyl polymer; and the mass of the anti-icing agent is 30-65% 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 application can form an anti-icing gel after light curing. The matrix of the anti-icing gel is cross-linked polyethylene glycol, with small molecule glycol and / or polyglycol embedded therein. 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 has an anti-icing effect, and by virtue of its reversible appearance at the interface, anti-icing adhesion and delayed frosting performance can be obtained. Furthermore, by controlling the molecular weight of the polyethylene glycol alkenyl polymer, the present application can control the release temperature of the glycol and / or polyglycol to be below 0℃, so as to be applicable to icing conditions and realize intelligent anti-icing. BRIEF DESCRIPTION OF DRAWINGS

[0026] Figure 1 The anti-icing agent reversible release performance demonstration diagram of the anti-icing gel in Example 1;

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

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

[0029] Figure 4The results of the delayed frosting performance test of the gel prepared for Example 1 and Comparative Example 1. DETAILED DESCRIPTION

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

[0031] polyethylene glycol alkenyl polymer, organic solvent, mercapto cross-linking 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 1066.18-1466.18; the polyethylene glycol diacrylate has a weight average molecular weight of 900-1300;

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

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

[0034] As no special instructions are given, each raw material / component used in the present application is commercially available.

[0035] The cross-linked polyethylene glycol-based anti-icing gel coating provided by the present application comprises a polyethylene glycol alkenyl polymer. In the present application, 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 1066.18-1466.18, preferably 1166.18; the polyethylene glycol diacrylate has a weight average molecular weight of 900-1300, preferably 1000.

[0036] In the present application, the preparation method of the polyethylene glycol diallyl formamide preferably comprises: mixing polyethylene glycol, allyl isocyanate, a solvent and a catalyst to perform an addition reaction, thereby obtaining the polyethylene glycol diallyl formamide; the polyethylene glycol has a weight average molecular weight of 900-1300, preferably 1000.

[0037] In the present application, the molar ratio of the polyethylene glycol and the 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 dibutyl tin 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, and can be 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, and can be specifically 75°C, 80°C, 90°C, or 95°C; the time of the addition reaction is preferably 4-6h, and can be specifically 4h, 5h, or 6h; the addition reaction is preferably carried out under nitrogen protection; the present application uses allyl isocyanate to cap polyethylene glycol through an addition reaction to obtain polyethylene glycol diallyl formamide. After the addition reaction is completed, the present application preferably adds the obtained reaction liquid into n-heptane, washes and dries the precipitate separated out to obtain polyethylene glycol diallyl formamide.

[0038] The cross-linked polyethylene glycol-based anti-icing gel paint provided by the present application comprises an organic solvent; the organic solvent is preferably a chloroalkane; the chloroalkane is preferably one or more of dichloromethane, trichloromethane, and trichloroethane; and the mass ratio of the organic solvent to the polyethylene glycol alkenyl polymer is preferably (2-4):1, and can be specifically 2:1, 2.5:1, 3:1, or 4:1.

[0039] The cross-linked polyethylene glycol-based anti-icing gel paint provided by the present application comprises a mercapto cross-linking agent. In the present application, the molar ratio of the mercapto groups in the mercapto cross-linking agent to the double bond functional groups in the polyethylene glycol alkenyl polymer is (1-4):(2-3), and can be specifically 4:3, 1:2, 1:3, 4:2, 3:2, 3:3, or 4:2.5; and the mercapto cross-linking agent preferably comprises one or both of trimethylolpropane tris(3-mercaptopropionate) (TMPMP) and pentaerythritol tetramercaptoacetate.

[0040] The cross-linked polyethylene glycol-based anti-icing gel paint provided by the present application comprises a photoinitiator. In the present application, the mass of the photoinitiator is 1-5% of the mass of the polyethylene glycol alkenyl polymer, and can be specifically 1%, 2%, 3%, 4%, or 5%; and the photoinitiator is preferably photoinitiator 651.

[0041] The cross-linked polyethylene glycol-based anti-icing gel paint provided by the present application comprises an anti-icing agent. In the present application, 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; and the mass of the anti-icing agent is preferably 30-65% of the total mass of the anti-icing agent and the polyethylene glycol alkenyl polymer, and can be specifically 30%, 40%, 45%, 55%, or 65%.

[0042] The application further provides a preparation method of the cross-linked polyethylene glycol-based anti-icing gel coating as described in the above scheme, comprising the following steps:

[0043] The polyethylene glycol alkene polymer, the organic solvent, the mercapto cross-linking agent, the photoinitiator and the anti-icing agent are mixed to obtain the cross-linked polyethylene glycol-based anti-icing gel coating.

[0044] In specific embodiments of the application, the polyethylene glycol alkene polymer is preferably dissolved in the organic solvent first, and then the mercapto cross-linking agent, the photoinitiator and the anti-icing agent are added and mixed; or the polyethylene glycol alkene polymer, the mercapto cross-linking agent, the photoinitiator and the anti-icing agent are directly added into the organic solvent and mixed.

[0045] The application further provides a cross-linked polyethylene glycol-based anti-icing gel obtained by photo-curing the cross-linked polyethylene glycol-based anti-icing gel coating as described in the above scheme. In the application, the cross-linked polyethylene glycol-based anti-icing gel can be attached to the surface of a 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 application further provides a preparation method of the cross-linked polyethylene glycol-based anti-icing gel as described in the above scheme, comprising the following steps:

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

[0048] In the application, the photo-curing is preferably ultraviolet light curing; the main wave band of the ultraviolet light used for the ultraviolet light curing is 315-450 nm, and the main wavelength is 365 nm; in specific embodiments of the application, an ultraviolet lamp is preferably used for the ultraviolet light curing, and the power of the ultraviolet lamp is preferably 25 W; the photo-curing is double-sided curing of the obtained coating, and the curing time of each side is independently preferably 1-4 min; in laboratory embodiments of the application, the cross-linked polyethylene glycol-based anti-icing gel coating can be poured into an open petri dish, and the open side is cured under the ultraviolet lamp first, and then the other side is cured by inversion; the double-sided curing in the application can eliminate the cross-linking gradient as much as possible.

[0049] In other specific embodiments of the application, the coating can be directly coated on a substrate and then photo-cured, so as to obtain an anti-icing gel coating on the surface of the substrate, and the substrate is specifically glass or aluminum material, etc.; or the coating can be coated on the surface of a polytetrafluoroethylene substrate and then photo-cured, and then the cured film is removed to obtain a separate anti-icing gel film.

[0050] In the present application, after the photo-curing is completed, the obtained cured product is preferably further subjected to solvent removal, and the temperature for the solvent removal is preferably 50°C; in the laboratory examples of the present application, after the solvent removal, the gel is demolded from the open petri dish, and the cross-linked polyethylene glycol-based anti-icing gel is obtained; in the present application, 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 polyglycol, the obtained anti-icing gel is recorded as polyglycol / cross-linked polyethylene glycol-based anti-icing gel.

[0051] The technical solutions in the present application will be clearly and completely described below in combination with the examples in the present application. Obviously, the described examples are only a part of the examples of the present application, rather than all the examples. Based on the examples in the present application, all the other examples obtained by those skilled in the art without creative labor fall within the protection scope of the present application.

[0052] Example 1

[0053] Synthesis of polyethylene glycol diallyl formamide: 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, then 1.83 g of allyl isocyanate and 3 g of DBTDL were added, nitrogen was introduced, and the reaction was carried out under magnetic stirring at 90°C for 5 h. The post-reaction liquid was precipitated in n-heptane, and the obtained precipitate was washed and dried to obtain polyethylene glycol diallyl formamide.

[0054] Synthesis of polyglycol / cross-linked polyethylene glycol-based anti-icing gel: 2 g of polyethylene glycol diallyl formamide, 0.4557 g of TMPMP, and 0.1 g of photoinitiator 651 were dissolved in 2 g of triethylene glycol and 4.67 g of trichloroethane. The obtained solution was poured into an open petri dish, the open surface was placed under an ultraviolet lamp for curing for 3 min, then the other surface was cured for 3 min by inverting. Then, trichloroethane was removed at 50°C to obtain the polyglycol / cross-linked polyethylene glycol-based anti-icing gel.

[0055] Example 2

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

[0057] Synthesis of polyglycol / 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, and 0.1 g of photoinitiator 651 were dissolved in 2 g of triethylene glycol and 4.67 g of trichloroethane. The obtained solution was poured into an open petri dish, the open surface was placed under an ultraviolet lamp for curing for 3 min, then the other surface was cured for 3 min by inverting. Then, trichloroethane was removed at 50°C to obtain the polyglycol / cross-linked polyethylene glycol-based anti-icing gel.

[0058] Example 3

[0059] The triethylene glycol was replaced with hexaethylene glycol compared to Example 1. The procedure was as follows:

[0060] Polyethylene glycol diallyl formamide synthesis: 10 g of polyethylene glycol with a weight average molecular weight of 1000 was placed in a three-necked flask, 18 g of DMF was added to dissolve, 1.83 g of allyl isocyanate was added, 3 g of DBTDL was added, nitrogen was bubbled, and the reaction was stirred magnetically at 90 °C for 5 h. The reaction solution was precipitated in n-heptane, and the obtained precipitate was washed and dried to obtain polyethylene glycol diallyl formamide.

[0061] Synthesis of multi-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 obtained solution was poured into an open petri dish, and the open surface was placed under a UV lamp for curing for 3 min, and then the other surface was cured for 3 min by inverting. After that, the trichloroethane was removed at 50 °C to obtain the multi-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 procedure was as follows:

[0064] Polyethylene glycol diallyl formamide synthesis: 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 was added, 3 g of DBTDL was added, nitrogen was bubbled, and the reaction was stirred magnetically at 90 °C for 5 h. The reaction solution was precipitated in n-heptane, and the obtained precipitate was washed and dried to obtain polyethylene glycol diallyl formamide.

[0065] Synthesis of multi-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 obtained solution was poured into an open petri dish, and the open surface was placed under a UV lamp for curing for 3 min, and then the other surface was cured for 3 min by inverting. After that, the trichloroethane was removed at 50 °C to obtain the multi-glycol / cross-linked polyethylene glycol-based anti-icing gel.

[0066] Comparative Example 2

[0067] The other conditions were the same as in Example 1, except that no light curing was performed. The results showed that the obtained system had no reversible release effect, which further illustrated the importance of light curing for the system to achieve the reversible release effect.

[0068] Comparative Example 3

[0069] Other conditions and Example 1 are the same, only not to join the triethylene glycol. The results show that the resulting system no irreversible release effect, and then no delay frosting performance, and show a great ice adhesion. Prove the importance of anti-icing agent (glycol / polyglycol) in the system to achieve anti-icing performance.

[0070] Performance test

[0071] Performance test:

[0072] 1. Reversible release performance test

[0073] Figure 1 For the anti-icing gel of Example 1, the anti-icing agent reversible release performance demonstration figure, according to Figure 1 It can be seen that the anti-icing gel of the present application has a reversible release of anti-icing agent performance.

[0074] 2. Quantitative test of release performance

[0075] The weighing method is used to test the mass of polyglycol released on the interface of the anti-icing gel at different temperatures, and then the mass percentage of the total polyglycol is calculated, that is, the secretion efficiency. The specific test method is: weigh the mass of the anti-icing gel sample, denoted as m0, then the total polyglycol mass M in the sample is m0xw, wherein w is the mass percentage of polyglycol in the anti-icing gel, the calculation method is: w = m 防 / m 总 x 100%, wherein m 防 represents the mass of the anti-icing agent, and m 总 represents the total mass of the anti-icing agent and the polyethylene glycol alkenyl polymer. Then place the anti-icing gel sample at the release temperature for 12 h, and then remove the polyglycol released on the interface with non-woven fabric, and weigh the remaining mass as m1; the mass of the polyglycol released on the surface is m0-m1; the secretion efficiency is (m0-m1) / (m0xw).

[0076] Figure 2 For the secretion efficiency of the gel obtained from Example 1 and Comparative Example 1 with temperature, wherein PEG1000 represents the anti-icing gel prepared in Example 1, and PEG4000 represents the gel prepared in Comparative Example 1. According to Figure 2 It can be seen that the release temperature range of triethylene glycol is related to the molecular weight of polyethylene glycol alkenyl polymer. When synthesizing polyethylene glycol diallyl formamide, the molecular weight of polyethylene glycol is lower (M wWhen the molecular weight of the polyethylene glycol is 1000, the anti-icing gel begins to release triethylene glycol at about 0℃, and the release amount first increases and then decreases with the decrease of temperature; when the molecular weight of the polyethylene glycol is 4000, the anti-icing gel begins to release triethylene glycol at above 0℃; the above contents show that the anti-icing gel prepared by using the polyethylene glycol alkylene polymer with low molecular weight is suitable for the working condition of anti-icing, and can realize intelligent anti-icing. w When the molecular weight of the polyethylene glycol is 1000, the anti-icing gel begins to release triethylene glycol at about 0℃, and the release amount first increases and then decreases with the decrease of temperature; when the molecular weight of the polyethylene glycol is 4000, the anti-icing gel begins to release triethylene glycol at above 0℃; the above contents show that the anti-icing gel prepared by using the polyethylene glycol alkylene polymer with low molecular weight is suitable for the working condition of anti-icing, and can realize intelligent anti-icing.

[0077] 3. Anti-icing adhesion performance test

[0078] Test method one: ice blocks are placed on the anti-icing gel sample with a size of 2cm*2cm, and then placed in a low-temperature environment at-20℃, and the ice adhesion is tested after 24h.

[0079] Test method two: the anti-icing gel sample is placed at-20℃ for 24h, and then ice blocks are placed thereon to test the ice adhesion.

[0080] Figure 3 The anti-icing adhesion performance test results of the gels obtained in Example 1 and Comparative Example 3, Figure 3 CPEG / 3EG is the anti-icing gel prepared in Example 1, and CPEG is the gel prepared in Example 3; according to the test method one, the ice adhesion of the gel prepared in Example 1 is about 3kPa, and the ice adhesion of the gel prepared in Comparative Example 3 is more than 110kPa. Figure 3 It can be seen that the anti-icing gel prepared in Example 1 has low ice adhesion under the two test methods, and the ice adhesion under the first test method is about 3kPa, and the ice adhesion under the second test method is about 7kPa; and the ice adhesion of the gel prepared in Comparative Example 3 reaches more than 110kPa.

[0081] 4. Delayed frosting performance test

[0082] The anti-icing gel sample is placed on a cold table at-20℃, and water mist is continuously sprayed by an air humidifier, the water mist can be condensed to frost on the surface of the sample, and the frosting performance of the sample is observed.

[0083] Figure 4 The delayed frosting performance test results of the gels 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 is completely covered with frost on the surface after being placed in a high-humidity environment at-20℃ for 8min. The anti-icing gel in Example 1 does not have surface frost within 8min. After removing the water deposited on the surface of the sample and the released glycol, the frosting performance is tested again, a small amount of frost appears on the edge of the sample in Example 1, because the triethylene glycol in the system is consumed, at this time, the triethylene glycol is supplemented in a swelling manner, and the sample regains the ability of delayed frosting, and obvious frosting can be observed on the sample after being placed in a high-humidity environment at-20℃ for 15min.

[0084] The anti-icing gels prepared in Examples 2 and 3 were subjected to reversible release performance testing, release performance quantitative testing, anti-icing adhesion performance testing, and delay frosting performance testing, and exhibited similar effects to Example 1.

[0085] The above merely describes the preferred embodiments of the present application, and it should be noted that those of ordinary skill in the art can make several improvements and refinements without departing from the principles of the present application, and these improvements and refinements should also be considered within the protection scope of the present application.

Claims

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

2. The crosslinked polyethylene glycol based anti-icing gel coating of claim 1, wherein, The polyethylene glycol diallyl formamide has a weight average molecular weight of 1166.18; the polyethylene glycol diacrylate has a weight average molecular weight of 1000.

3. The crosslinked polyethylene glycol based anti-icing gel coating of claim 1 or 2, wherein, The preparation method of the polyethylene glycol diallyl formamide comprises: mixing polyethylene glycol, allyl isocyanate, a solvent and a catalyst to perform an addition reaction to obtain the polyethylene glycol diallyl formamide; the polyethylene glycol has a weight average molecular weight of 900-1300.

4. The crosslinked polyethylene glycol based anti-icing gel coating of claim 3, wherein, The molar ratio of the polyethylene glycol to the 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 h.

5. The crosslinked polyethylene glycol based anti-icing gel coating of claim 1, wherein, The organic solvent is a chloroalkane; the mass ratio of the organic solvent to the polyethylene glycol alkenyl polymer is (2-4):1; The mercapto crosslinking agent comprises one or both of trimethylolpropane tris(3-mercaptopropionate) and pentaerythritol tetramercaptoacetate; the photoinitiator is photoinitiator 651; 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 method comprises the following steps: mixing polyethylene glycol alkenyl polymer, organic solvent, mercapto crosslinking agent, photoinitiator and anti-icing agent to obtain the crosslinked polyethylene glycol-based anti-icing gel coating.

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

8. The method for preparing the cross-linked polyethylene glycol-based anti-icing gel according to claim 7, characterized in that: The method comprises the following steps: performing photocuring on the crosslinked polyethylene glycol-based anti-icing gel coating after coating to obtain the crosslinked polyethylene glycol-based anti-icing gel.

9. The production method according to claim 8, characterized by, The photocuring is ultraviolet photocuring; the main wave band of the ultraviolet light used for the ultraviolet photocuring is 315-450 nm, and the main wavelength is 365 nm; the photocuring is double-sided curing of the obtained coating, and the curing time of each side is independently 1-4 min.

10. The method of claim 9, wherein, After the ultraviolet photocuring is completed, the obtained cured product is further subjected to desolventization at a temperature of 40-100°C.

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