A soft anti-freezing elastic mastic coating and a preparation method thereof

By introducing modified multi-walled carbon nanotubes into acrylic emulsions, the problems of insufficient tensile strength and water resistance of acrylic adhesive coatings were solved, and high-performance preparation of soft, antifreeze, and elastic adhesives was achieved.

CN118326725BActive Publication Date: 2025-11-04JIANGMEN CAIGE ENVIRONMENTAL PROTECTION TECH IND
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Patent Information

Application Number
CN202410516071.0
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-04-27
Publication Date
2025-11-04
Estimated Expiration
2044-04-27

AI Technical Summary

Technical Problem

Existing acrylic ester adhesive coatings have poor tensile strength, poor water resistance, and poor resilience, which affects their performance.

Method used

By adding modified multi-walled carbon nanotubes to acrylate emulsions, the tensile strength and water resistance of the adhesive can be improved by utilizing the double bonds and hydrophobic tert-carbonate groups of the modified multi-walled carbon nanotubes, thus preparing a soft, antifreeze, elastic adhesive coating.

Benefits of technology

The addition of modified multi-walled carbon nanotubes improves the tensile strength and resilience of the adhesive, enhances its water resistance, and strengthens its stability and performance.

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Abstract

The present application relates to the field of glue mortar paint, disclose a kind of soft anti-freeze elastic glue mortar paint and preparation method thereof, the glue mortar paint includes the following raw materials according to weight parts: acrylate emulsion 35~65 parts, defoaming agent 1~3 parts, antifreeze 0.5~5 parts, thickening agent 0.2~0.5 parts;Acrylate emulsion includes the following weight parts component: methyl methacrylate 35~55 parts, butyl acrylate 30~45 parts, acrylic acid 2~4 parts, glycidyl methacrylate 3.5~5 parts, modified multi-walled carbon nanotube 1~5 parts, emulsifier 1~3 parts, pH buffer 0.5~1 part, initiator 1.2~1.5 parts, purified water 75~100 parts, the modified multi-walled carbon nanotube of surface introduction double bond and tertiary carbon acid hydrophobic group is added in the preparation process of acrylate emulsion by the present application, and stable acrylate emulsion is prepared, and the glue mortar is endowed with excellent tensile property, and its resilience and water resistance are improved.
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Description

Technical Field

[0001] This invention belongs to the field of adhesive coating technology, specifically relating to a soft, antifreeze, elastic adhesive coating and its preparation method. Background Technology

[0002] Plastisol printing is a chemical coating used for surface finishing and functionalization of textiles. It is primarily transferred to the surface of textiles through screen printing. In the textile coating printing process, plastisol is applied to the fabric via screen printing to create text and patterns in various colors. As a form of screen printing, plastisol printing has gained rapid popularity due to its good pattern coverage, allowing light colors to be printed on dark clothing, and its ability to provide a certain gloss and three-dimensional effect, making garments look more upscale.

[0003] Printing paste is relatively thick and viscous. The quality of the printing paste directly affects the quality of the printed coating on the fabric. Existing printing pastes can generally be divided into two categories: acrylic pastes and polyurethane pastes. Among them, acrylic pastes have strong adhesion and good fastness, and are widely used. However, they have poor tensile strength, poor water resistance, and poor film resilience, which affects their performance. Therefore, a soft, antifreeze, elastic printing paste coating and its preparation method are proposed. Summary of the Invention

[0004] To address the shortcomings mentioned in the background art, the present invention aims to provide a soft, antifreeze, elastic adhesive coating and its preparation method. By adding modified multi-walled carbon nanotubes with double bonds and tertiary carbonate hydrophobic groups introduced on the surface, the modified multi-walled carbon nanotubes participate in the preparation process of acrylic emulsion, thereby obtaining a stable acrylic emulsion. This imparts excellent tensile properties to the adhesive coating, and its resilience and water resistance are also improved.

[0005] The objective of this invention can be achieved through the following technical solutions:

[0006] A soft, antifreeze, elastic adhesive coating, by weight, comprises the following raw materials: 35-65 parts acrylic emulsion, 1-3 parts defoamer, 0.5-5 parts antifreeze, and 0.2-0.5 parts thickener;

[0007] The acrylate emulsion comprises the following components in parts by weight: methyl methacrylate 35-55 parts, butyl acrylate 30-45 parts, acrylic acid 2-4 parts, glycidyl methacrylate 3.5-5 parts, modified multi-walled carbon nanotubes 1-5 parts, emulsifier 1-3 parts, pH buffer 0.5-1 part, initiator 1.2-1.5 parts, and purified water 75-100 parts;

[0008] The modified multi-walled carbon nanotubes are prepared by grafting hydroxypropyl acrylate and glycidyl neodecanoate onto the surface of oxidized multi-walled carbon nanotubes.

[0009] Preferably, the method for preparing the acrylate emulsion includes the following steps: mixing parts by weight of methyl methacrylate, butyl acrylate, acrylic acid, glycidyl methacrylate, modified multi-walled carbon nanotubes, emulsifier and purified water, stirring evenly, raising the temperature to 80-90°C, continuing to add parts by weight of initiator and pH buffer, keeping warm and stirring for 6-9 hours, cooling and discharging to prepare the acrylate emulsion.

[0010] Preferably, the defoamer is one of fatty alcohol polyoxyethylene ether or alkylphenol polyoxyethylene ether; the antifreeze is one or more of glycerol, propylene glycol, ethanol, and ethylene glycol; the thickener is one or more of hydroxyethyl methylcellulose, hydroxypropyl methylcellulose, and polydimethylsiloxane; the emulsifier is one of sodium dodecyl sulfate or sodium dodecylbenzene sulfonate; the pH buffer is sodium bicarbonate; and the initiator is ammonium persulfate.

[0011] Preferably, the method for preparing the modified multi-walled carbon nanotubes includes the following steps:

[0012] A. Place multi-walled carbon nanotubes in a mixture of concentrated sulfuric acid and concentrated nitric acid with a volume ratio of 3:1, sonicate at room temperature for 20-30 min, stir in an oil bath at 75-90℃ for 4-6 h, filter and wash the product until neutral, and then dry under vacuum to prepare oxidized multi-walled carbon nanotubes.

[0013] B. Place isophorone diisocyanate in a reactor, add butyl acetate and stir until uniform, then add dibutyltin dilaurate, heat to 35-50℃, then add hydroxypropyl acrylate, react for 5-6 hours to prepare isocyanate-based hydroxypropyl acrylate.

[0014] C. Oxygenated multi-walled carbon nanotubes were placed in butyl acetate, ultrasonically dispersed, and then transferred to a reactor. The temperature was raised to 55-80℃, and dibutyltin dilaurate was added. Hydroxypropyl isocyanate-based acrylate and butyl acetate were mixed evenly and added to the reactor. The reaction was carried out at a constant temperature for 10-12 hours. After the reaction was completed, the mixture was filtered, washed, and dried to prepare a multi-walled carbon nanotube intermediate containing double bonds.

[0015] D. Dissolve the multi-walled carbon nanotube intermediate in butyl acetate, disperse it by ultrasonication, transfer it to a reactor, add triphenylphosphine and hydroquinone, stir and mix, heat to 95-105℃, add glycidyl neodecanoate, and react at a constant temperature for 10-14 hours. After the reaction is completed, filter, wash and dry to prepare modified multi-walled carbon nanotubes.

[0016] Preferably, in step B, the mass ratio of isophorone diisocyanate, dibutyltin dilaurate, and hydroxypropyl acrylate is 10:0.02-0.05:4-8.

[0017] Preferably, in step C, the mass ratio of oxidized multi-walled carbon nanotubes, dibutyltin dilaurate, and isocyanate-based hydroxypropyl acrylate is 3–7: 0.01–0.05: 5–10.

[0018] Preferably, in step D, the mass ratio of the multi-walled carbon nanotube intermediate, triphenylphosphine, hydroquinone, and glycidyl neodecanoate is 3–5: 0.005–0.01: 0.001–0.005: 35–40.

[0019] The preparation method of the soft, antifreeze, elastic adhesive coating as described above includes the following steps:

[0020] (1) Pour the acrylic emulsion, defoamer and antifreeze in parts by weight into the mixer, stir and mix evenly, let stand to defoam, and form a premix.

[0021] (2) Mix the thickener and premixed materials by weight to prepare a soft, antifreeze elastic adhesive coating.

[0022] The beneficial effects of this invention are:

[0023] This invention involves adding modified multi-walled carbon nanotubes with double bonds and tertiary carbonate hydrophobic groups to the surface of the acrylic emulsion, thereby preparing a stable acrylic emulsion that imparts excellent tensile properties to the adhesive, while also improving its resilience and water resistance. This invention first utilizes concentrated sulfuric acid and concentrated nitric acid to oxidize multi-walled carbon nanotubes, resulting in oxidized multi-walled carbon nanotubes with hydroxyl, carboxyl, and carbonyl groups on their surface. This process also facilitates the dispersion of multi-walled carbon nanotubes in emulsions. Simultaneously, this invention utilizes the highly reactive isocyanate group in isophorone diisocyanate, directly linked to the cyclohexane ring, to react with the hydroxyl groups on the surface of hydroxypropyl acrylate. Hydroxypropyl acrylate is then semi-blocked with isophorone diisocyanate. Next, another isocyanate group in the isophorone diisocyanate reacts with the hydroxyl groups on the surface of the oxidized multi-walled carbon nanotubes to prepare a multi-walled carbon nanotube intermediate. This introduces double bonds on the surface of the oxidized multi-walled carbon nanotubes, serving as a bridge for polymerization with acrylate monomers. Furthermore, this invention modifies the oxidized multi-walled carbon nanotubes using glycidyl neodecanoate. The carboxyl groups on the surface of the oxidized multi-walled carbon nanotubes react with the epoxy groups on the surface of the glycidyl neodecanoate, thereby introducing tertiary carbonate hydrophobic groups onto the surface of the multi-walled carbon nanotube intermediate. Multi-walled carbon nanotubes (MWCNTs) possess excellent elastic modulus. Their large aspect ratio gives them very high axial tensile strength, while their unique microscopic tubular structure and atomic configuration endow them with extremely high flexural strength. The addition of MWCNTs enhances both the tensile properties and resilience of the adhesive. Detailed Implementation

[0024] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0025] Example 1: A soft, antifreeze, elastic adhesive coating, comprising the following raw materials by weight: 35 parts acrylic emulsion, 1 part defoamer fatty alcohol polyoxyethylene ether, 0.5 parts antifreeze glycerin, and 0.2 parts thickener hydroxyethyl methyl cellulose;

[0026] The preparation method of the above-mentioned soft, antifreeze, elastic adhesive coating includes the following steps:

[0027] (1) Pour the acrylic emulsion, defoamer fatty alcohol polyoxyethylene ether and antifreeze glycerin into the mixer by weight, stir and mix evenly, let stand to defoam, and form a premix.

[0028] (2) The thickener hydroxyethyl methyl cellulose in parts by weight is mixed with the premix to prepare a soft, antifreeze elastic adhesive coating.

[0029] The preparation method of the acrylate emulsion includes the following steps:

[0030] 35 parts of methyl methacrylate, 30 parts of butyl acrylate, 2 parts of acrylic acid, 3.5 parts of glycidyl methacrylate, 1 part of modified multi-walled carbon nanotubes, 1 part of sodium dodecyl sulfate emulsifier, and 75 parts of purified water were mixed and stirred evenly. The temperature was raised to 80°C, and 1.2 parts of ammonium persulfate initiator and 0.5 parts of sodium bicarbonate pH buffer were added. The mixture was kept at this temperature and stirred for 6 hours. The mixture was then cooled and discharged to prepare an acrylic emulsion.

[0031] The preparation method of modified multi-walled carbon nanotubes includes the following steps:

[0032] A. Take 3g of multi-walled carbon nanotubes and place them in 118mL of a mixture of concentrated sulfuric acid and concentrated nitric acid with a volume ratio of 3:1. Sonicate at room temperature for 25min, stir in an oil bath at 80℃ for 6h, and filter and wash the product until neutral. Then, vacuum dry to prepare oxidized multi-walled carbon nanotubes.

[0033] B. Place 10g of isophorone diisocyanate in a reactor, add 50mL of butyl acetate and stir until homogeneous, then add 0.02g of dibutyltin dilaurate, heat to 45℃, then add 5g of hydroxypropyl acrylate, react for 5h to prepare isocyanate-based hydroxypropyl acrylate.

[0034] C. Take 3g of oxidized multi-walled carbon nanotubes in 50mL of butyl acetate, disperse them by ultrasonication, transfer them to a reactor, heat to 70℃, add 0.01g of dibutyltin dilaurate, take 7g of isocyanate-based hydroxypropyl acrylate and 10mL of butyl acetate, mix them evenly and add them to the reactor, react at a constant temperature for 11h, filter, wash and dry after the reaction is completed to prepare the multi-walled carbon nanotube intermediate containing double bonds;

[0035] D. Dissolve 5g of multi-walled carbon nanotube intermediate in 50mL of butyl acetate, disperse by ultrasonication, transfer to a reactor, add 0.007g of triphenylphosphine and 0.002g of hydroquinone and stir to mix, heat to 98℃, add 38g of glycidyl neodecanoate, and react at a constant temperature for 12h. After the reaction is completed, filter, wash and dry to prepare modified multi-walled carbon nanotubes.

[0036] Example 2: A soft, antifreeze, elastic adhesive coating, comprising the following raw materials by weight: 45 parts acrylic emulsion, 2 parts alkylphenol polyoxyethylene ether defoamer, 2 parts propylene glycol antifreeze, and 0.3 parts hydroxypropyl methylcellulose thickener;

[0037] The preparation method of the above-mentioned soft, antifreeze, elastic adhesive coating includes the following steps:

[0038] (1) Pour the acrylic emulsion, defoamer alkylphenol polyoxyethylene ether and antifreeze propylene glycol into a mixer, stir and mix evenly, let stand to defoam, and form a premix.

[0039] (2) Mix the thickener hydroxypropyl methylcellulose with the premix to prepare a soft, antifreeze elastic adhesive coating.

[0040] The preparation method of the acrylate emulsion includes the following steps:

[0041] 40 parts of methyl methacrylate, 35 parts of butyl acrylate, 3 parts of acrylic acid, 4 parts of glycidyl methacrylate, 3 parts of modified multi-walled carbon nanotubes, 2 parts of sodium dodecylbenzenesulfonate emulsifier, and 85 parts of purified water were mixed and stirred evenly. The temperature was raised to 85°C, and 1.4 parts of ammonium persulfate initiator and 0.7 parts of sodium bicarbonate pH buffer were added. The mixture was kept at this temperature and stirred for 8 hours. The mixture was then cooled and discharged to prepare an acrylate emulsion.

[0042] The preparation method of the modified multi-walled carbon nanotubes is the same as in Example 1.

[0043] Example 3: A soft, antifreeze, elastic adhesive coating, comprising the following raw materials by weight: 62 parts acrylic emulsion, 3 parts alkylphenol polyoxyethylene ether defoamer, 5 parts ethylene glycol antifreeze, and 0.5 parts polydimethylsiloxane thickener;

[0044] The preparation method of the above-mentioned soft, antifreeze, elastic adhesive coating includes the following steps:

[0045] (1) Pour the acrylic emulsion, defoamer alkylphenol polyoxyethylene ether and antifreeze ethylene glycol into a mixer, stir and mix evenly, let stand to defoam, and form a premix.

[0046] (2) Mix the thickener polydimethylsiloxane with the premix to prepare a soft, antifreeze elastic adhesive coating.

[0047] The preparation method of the acrylate emulsion includes the following steps:

[0048] 55 parts of methyl methacrylate, 45 parts of butyl acrylate, 4 parts of acrylic acid, 5 parts of glycidyl methacrylate, 5 parts of modified multi-walled carbon nanotubes, 3 parts of sodium dodecylbenzenesulfonate emulsifier, and 100 parts of purified water were mixed and stirred evenly. The temperature was raised to 90°C, and 1.5 parts of ammonium persulfate initiator and 1 part of sodium bicarbonate pH buffer were added. After stirring at this temperature for 9 hours, the mixture was cooled and discharged to prepare an acrylate emulsion.

[0049] The preparation method of the modified multi-walled carbon nanotubes is the same as in Example 1.

[0050] Comparative Example 1: A soft, antifreeze, elastic adhesive coating, comprising the following raw materials by weight: 50 parts acrylic emulsion, 1 part defoamer fatty alcohol polyoxyethylene ether, 1 part antifreeze glycerin, and 0.3 parts thickener hydroxyethyl methyl cellulose.

[0051] The preparation method of the above-mentioned soft, antifreeze, elastic adhesive coating includes the following steps:

[0052] (1) Pour the acrylic emulsion, defoamer fatty alcohol polyoxyethylene ether and antifreeze glycerin into the mixer by weight, stir and mix evenly, let stand to defoam, and form a premix.

[0053] (2) The thickener hydroxyethyl methyl cellulose in parts by weight is mixed with the premix to prepare a soft, antifreeze elastic adhesive coating.

[0054] The preparation method of the acrylate emulsion includes the following steps:

[0055] 45 parts of methyl methacrylate, 45 parts of butyl acrylate, 2 parts of acrylic acid, 3.5 parts of glycidyl methacrylate, 2 parts of sodium dodecyl sulfate emulsifier, and 95 parts of purified water were mixed and stirred evenly. The temperature was raised to 80°C, and 1.2 parts of ammonium persulfate initiator and 1 part of sodium bicarbonate pH buffer were added. The mixture was kept warm and stirred for 8 hours, then cooled and discharged to prepare an acrylic emulsion.

[0056] Comparative Example 2: A soft, antifreeze, elastic adhesive coating, comprising the following raw materials by weight: 52 parts acrylic emulsion, 2 parts alkylphenol polyoxyethylene ether defoamer, 3 parts propylene glycol antifreeze, and 0.5 parts hydroxypropyl methylcellulose thickener.

[0057] The preparation method of the above-mentioned soft, antifreeze, elastic adhesive coating includes the following steps:

[0058] (1) Pour the acrylic emulsion, defoamer alkylphenol polyoxyethylene ether and antifreeze propylene glycol into a mixer, stir and mix evenly, let stand to defoam, and form a premix.

[0059] (2) Mix the thickener hydroxypropyl methylcellulose with the premix to prepare a soft, antifreeze elastic adhesive coating.

[0060] The preparation method of the acrylate emulsion includes the following steps:

[0061] 42 parts of methyl methacrylate, 40 parts of butyl acrylate, 3 parts of acrylic acid, 4 parts of glycidyl methacrylate, 5 parts of multi-walled carbon nanotubes, 2 parts of sodium dodecylbenzenesulfonate emulsifier, and 90 parts of purified water were mixed and stirred evenly. The temperature was raised to 85°C, and 1.4 parts of ammonium persulfate initiator and 0.9 parts of sodium bicarbonate pH buffer were added. The mixture was kept at this temperature and stirred for 8 hours. After cooling, the mixture was discharged to prepare an acrylate emulsion.

[0062] Performance testing

[0063] The acrylate emulsions prepared in Examples 1-3 and Comparative Examples 1-2 were poured into polytetrafluoroethylene plates and allowed to dry naturally at room temperature. After the surface was dry, the plates were placed in an electric heating drying oven and dried at 40°C for 24 hours to obtain a film with a thickness of approximately 1 mm. The adhesion of the film was determined using the cross-cut test according to GB / T 9286-2021; the water contact angle was tested using a PZ-200SD contact angle meter; and the pencil hardness of the film was determined according to GB / T6739-2022. The data results are shown in Table 1.

[0064] Table 1 Results of film performance testing

[0065]

[0066] As can be seen from the data in Table 1, the acrylate emulsions prepared in Examples 1-3 of this invention exhibit strong adhesion, high pencil hardness, and water contact angles greater than 110°, indicating a hydrophobic surface. In Comparative Example 1, no modified multi-walled carbon nanotubes were added, resulting in a significant decrease in both water contact angle and pencil hardness. In Comparative Example 2, no modification treatment was applied to the multi-walled carbon nanotubes, leading to lower water contact angles and pencil hardness compared to Examples 1-3. This may be due to the aggregation of the multi-walled carbon nanotubes, resulting in reduced pencil hardness, and the absence of grafted tert-carbonic acid hydrophobic groups, leading to a lower water contact angle compared to Examples 1-3.

[0067] The adhesive coatings prepared in Examples 1-3 and Comparative Examples 1-2 were printed on standard fabrics using a conventional table screen printing process, including three steps: printing, pre-baking (60℃×3min), and baking (120~130℃×3min), to obtain printed products. Elongation was tested according to GB / T 3923.1-2013; resilience was tested according to industry standard FZT 70006-2004; and wash fastness was determined according to GB / T 8629-2017. The data results are shown in Table 2.

[0068] Table 2 Performance test results of printed products

[0069]

[0070] As can be seen from the data in Table 2, the elongation, resilience, and wash fastness of the adhesive coatings prepared in Examples 1-3 of this invention are better than those in Comparative Examples 1-2. In Comparative Example 1, no modified multi-walled carbon nanotubes were added, and the measured maximum elongation and resilience were significantly reduced. In Comparative Example 2, no modification treatment was performed on the multi-walled carbon nanotubes, and the wash fastness and storage stability of the adhesive coating were significantly reduced, possibly due to the lack of grafting of double bonds and tertiary carbonate hydrophobic groups. Furthermore, its maximum elongation and resilience were slightly worse than those in Examples 1-3, possibly due to the aggregation of multi-walled carbon nanotubes, which reduced its performance.

[0071] In the description of this specification, references to terms such as "an embodiment," "example," "specific example," etc., indicate that a specific feature, structure, material, or characteristic described in connection with that embodiment or example is included in at least one embodiment or example of the invention. In this specification, illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples.

[0072] The foregoing has shown and described the basic principles, main features, and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited to the above embodiments. The embodiments and descriptions in the specification are merely illustrative of the principles of the invention. Various changes and modifications can be made to the invention without departing from its spirit and scope, and all such changes and modifications fall within the scope of the claimed invention.

Claims

1. A soft, antifreeze, elastic adhesive coating, characterized in that, By weight, it includes the following raw materials: 35-65 parts of acrylic emulsion, 1-3 parts of defoamer, 0.5-5 parts of antifreeze, and 0.2-0.5 parts of thickener; The acrylate emulsion comprises the following components in parts by weight: methyl methacrylate 35-55 parts, butyl acrylate 30-45 parts, acrylic acid 2-4 parts, glycidyl methacrylate 3.5-5 parts, modified multi-walled carbon nanotubes 1-5 parts, emulsifier 1-3 parts, pH buffer 0.5-1 part, initiator 1.2-1.5 parts, and purified water 75-100 parts; The modified multi-walled carbon nanotubes are prepared by grafting hydroxypropyl acrylate and glycidyl neodecanoate onto the surface of oxidized multi-walled carbon nanotubes. The method for preparing the modified multi-walled carbon nanotubes includes the following steps: A. Place multi-walled carbon nanotubes in a mixture of concentrated sulfuric acid and concentrated nitric acid with a volume ratio of 3:1, sonicate at room temperature for 20-30 min, stir in an oil bath at 75-90℃ for 4-6 h, filter and wash the product until neutral, and then vacuum dry to prepare oxidized multi-walled carbon nanotubes. B. Place isophorone diisocyanate in a reactor, add butyl acetate and stir until uniform, then add dibutyltin dilaurate, heat to 35~50℃, then add hydroxypropyl acrylate, react for 5~6h to prepare isocyanate-based hydroxypropyl acrylate. C. Oxygenated multi-walled carbon nanotubes were placed in butyl acetate, ultrasonically dispersed, and then transferred to a reactor. The temperature was raised to 55-80℃, and dibutyltin dilaurate was added. Hydroxypropyl isocyanate-based acrylate and butyl acetate were mixed evenly and added to the reactor. The reaction was carried out at a constant temperature for 10-12 hours. After the reaction was completed, the mixture was filtered, washed, and dried to prepare a multi-walled carbon nanotube intermediate containing double bonds. D. Dissolve the multi-walled carbon nanotube intermediate in butyl acetate, disperse it by ultrasonication, transfer it to a reactor, add triphenylphosphine and hydroquinone, stir and mix, heat to 95~105℃, add glycidyl neodecanoate, and react at a constant temperature for 10~14h. After the reaction is completed, filter, wash and dry to prepare modified multi-walled carbon nanotubes.

2. The soft, antifreeze, elastic adhesive coating according to claim 1, characterized in that, The preparation method of the acrylate emulsion includes the following steps: mixing parts by weight of methyl methacrylate, butyl acrylate, acrylic acid, glycidyl methacrylate, modified multi-walled carbon nanotubes, emulsifier and purified water, stirring evenly, raising the temperature to 80~90℃, continuing to add parts by weight of initiator and pH buffer, keeping warm and stirring for 6~9 hours, cooling and discharging to prepare the acrylate emulsion.

3. The soft, antifreeze, elastic adhesive coating according to claim 1, characterized in that, The defoamer is one of fatty alcohol polyoxyethylene ether or alkylphenol polyoxyethylene ether; the antifreeze is one or more of glycerol, propylene glycol, ethanol, and ethylene glycol; the thickener is one or more of hydroxyethyl methylcellulose, hydroxypropyl methylcellulose, and polydimethylsiloxane; the emulsifier is one of sodium dodecyl sulfate or sodium dodecylbenzene sulfonate; the pH buffer is sodium bicarbonate; and the initiator is ammonium persulfate.

4. The soft, antifreeze, elastic adhesive coating according to claim 1, characterized in that, In step B, the mass ratio of isophorone diisocyanate, dibutyltin dilaurate, and hydroxypropyl acrylate is 10:0.02~0.05:4~8.

5. The soft, antifreeze, elastic adhesive coating according to claim 1, characterized in that, In step C, the mass ratio of oxidized multi-walled carbon nanotubes, dibutyltin dilaurate, and isocyanate-based hydroxypropyl acrylate is 3~7:0.01~0.05:5~10.

6. The soft, antifreeze, elastic adhesive coating according to claim 1, characterized in that, In step D, the mass ratio of the multi-walled carbon nanotube intermediate, triphenylphosphine, hydroquinone, and glycidyl neodecanoate is 3~5:0.005~0.01:0.001~0.005:35~40.

7. The method for preparing the soft, antifreeze, elastic adhesive coating according to claim 1, characterized in that, Includes the following steps: (1) Pour the acrylic emulsion, defoamer and antifreeze in parts by weight into the mixer, stir and mix evenly, let stand to defoam, and form a premix; (2) Mix the thickener and premixed materials by weight to prepare a soft, antifreeze elastic adhesive coating.

Citation Information

Patent Citations

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    CN108676480A

  • Water-based environment-friendly coating and preparation method thereof

    CN115058184A