CA3130987C

CA3130987C - Water-based low-temperature heat transfer printing adhesive and preparation method thereof

Info

Publication number: CA3130987C
Application number: CA3130987A
Authority: CA
Inventors: Qingmei Zhu; Kunbin Wu; Hongcun Huang
Original assignee: Hainan BNK Water Based New Materials Co Ltd
Current assignee: Hainan BNK Water Based New Materials Co Ltd
Priority date: 2021-04-13
Filing date: 2021-05-07
Publication date: 2023-09-26
Anticipated expiration: 2041-05-07
Also published as: CA3130987A1

Abstract

This disclosure relates to the technical field of printing materials, and specifically is directed to a water-based low-temperature heat transfer printing adhesive. The adhesive is prepared from raw materials comprising in parts by weight 20-30 parts of an ethylene acrylic acid resin, 3-10 parts of an alkaline neutralizing agent, 0.3-0.5 part of a leveling agent, 1-5 parts of a wax emulsion, 1-3 parts of a plasticizer, 0.01-0.05 part of a defoamer, and 65-80 parts of water. Such raw materials containing these components at specified contents render the adhesive excellent performances, which has improved the existing heat transfer printing adhesives that yield unsatisfactory transfer printing image-text in respects of scratch resistance, levelling property, water resistance, high-temperature resistance, and the completeness of the transfer printing image-text at low temperature.

Description

WATER-BASED LOW-TEMPERATURE HEAT TRANSFER PRINTING ADHESIVE
AND PREPARATION METHOD THEREOF
[0001]
FIELD

[0002] The present disclosure relates to the technical field of printing materials, and more specifically to a water-based low-temperature heat transfer printing adhesive and a preparation method thereof.
BACKGROUND

[0003] Heat transfer printing is to directly contact a transfer printing film having patterns with a substrate, so that the image-text layer on the transfer printing film is dissolved and transferred to the substrate. A heat transfer printing film includes a carrier layer, a release layer, a protective layer, an ink layer, and an adhesive layer. Each of the layers is closely contacted and interacts with each other. Among them, the adhesive layer is used as a substrate adhesive to bond the ink information layer with various materials, so it is required to have high adhesion, high temperature resistance, scratch resistance, water resistance, and cooking resistance. In the existing technology, the heat transfer printing adhesives have problems that cause unsatisfactory transfer printing image-text in scratch resistance, levelling property, water resistance, high-temperature resistance, and the completeness of the transfer printing image-text at low temperature.

[0004] The Chinese Patent with Publication No. CN 103289611A discloses a heat transfer printing adhesive of acrylic resins and a method of preparing the same, which is prepared from Date recue/Date received 2023-03-10 from the following raw materials in parts by weight: 25-28 parts of acrylic resin (AR-1520), 12-15 parts of polyisobutylene, 3-6 parts of aminopropyltriethoxysilane, 3-5 parts of methyltriethoxysilane, 2-3 parts of dicumyl peroxide, 12-15 parts of dibutyl maleate, 4-6 parts of dodecyl mercaptan, 5-8 parts of rosin, 1-2 parts of a crosslinking agent TAC, 3-5 parts of dioctyl ester, 1-2 parts of 1-hydroxyethy1-2-oley1 imidazoline, 2-3 parts of p-phenylenediamine, 55-60 parts of acetone, and 40-45 parts of xylene, and has the properties of firm bonding, not easy to break, fall off, and yellowing. The Chinese Patent with Publication No. CN 109517566A discloses a water-based heat transfer printing PP adhesive, comprising the following components in mass fraction: 5-15 parts of a water-based acrylic emulsion, 20-40 parts of a water-based polyurethane dispersion, 5-15 parts of polyvinyl alcohol, 5-15 parts of water-based coumarone resin, 0-5 parts of a water-based adhesion promoter, 0-1 parts of fumed silica, 10-20 parts of ethanol, 10-20 parts of distilled water, 0-0.001 parts of a leveling agent, and 0-0.001 parts of a defoamer, which has high adhesion and high shearing property. However, the levelling property, water resistance, scratch resistance and the completeness of the transfer printing image-text at low temperature of the products disclosed in the prior art still have not been improved, and the raw materials are not eco-friendly.
SUMMARY

[0005] In view of this, an object of the present disclosure is to provide a water-based low-temperature heat transfer printing adhesive and preparation method thereof. The water-based low-temperature heat transfer printing adhesive provided by the present disclosure has good levelling property, water resistance, and scratch resistance, and a good completeness of the transfer printing image-text at low temperature, and it is a pure water-based material, eco-friendly, and pollution-free.

[0006] The present disclosure provides a water-based low-temperature heat transfer printing adhesive, prepared from raw materials comprising the following components:

[0007] 20-30 parts by weight of an ethylene acrylic acid resin,

[0008] 3-10 parts by weigh of an alkaline neutralizing agent, Date Recue/Date Received 2021-09-15

[0009] 0.3-0.5 part by weight of a leveling agent,

[0010] 1-5 parts by weigh of a wax emulsion,

[0011] 1-3 parts by weight of a plasticizer,

[0012] 0.01-0.05 part by weight of a defoamer, and

[0013] 65-80 parts by weight of water,

[0014] wherein the plasticizer is one or more selected from glycerin, dioctyl adipate and di octyl sebacate.

[0015] Preferably, the ethylene acrylic acid resin has a melt index of 300-1300, and a melting point of 75 C-78 C.

[0016] Preferably, the alkaline neutralizing agent is one or more selected from ammonia liqour, KOH, NaOH and triethylamine.

[0017] Preferably, the leveling agent is one or more selected from Glide 410, Wet KL 245 and Glide 496.

[0018] Preferably, the wax emulsion is one or more selected from palm wax, polyethylene wax, oxidized polyethylene wax and micronized wax.

[0019] The present disclosure further provides a method of preparing the water-based low-temperature heat transfer printing adhesive described in the above technical solutions, comprising the following steps:

[0020] a) under stirring conditions, mixing a first amount of water, a second amount of an alkaline neutralizing agent and a plasticizer, and then adding an ethylene acrylic acid resin to perform a first reaction; then adding the remaining alkaline neutralizing agent dropwise at a rate of 4 g/s-6 g/s to perform a second reaction; after that, adding the remaining water at a rate of 45 g/s-55 g/s to perform a third reaction; and after cooling, adding and well mixing a defoamer and a leveling agent, and finally adding a wax emulsion, to obtain a water-based low-temperature heat transfer printing adhesive.

[0021] Preferably, in step a), the stiffing is carried out at a rotation rate of 100 r/min-500 r/min; the first amount of water, the second amount of the alkaline neutralizing agent and the Date Recue/Date Received 2021-09-15 plasticizer are mixed for a duration of 1 min-10 min.

[0022] Preferably, in step a) the first amount of water accounts for 70-90 wt%
of the total amount of water; the second amount of the alkaline neutralizing agent accounts for 70-80 wt%
of the total amount of the alkaline neutralizing agent.

[0023] Preferably, in step a) the first reaction is carried out at a temperature of 90 C-100 C
for a duration of 1 h-2 h;

[0024] the second reaction is carried out at a temperature of 90 C-100 C for a duration of 0.5 h-1 h; and

[0025] the third reaction is carried out at a temperature of 90 C-100 C for a duration of 1 h-2 h.

[0026] Preferably, in step a), a temperature of cooling is 20 C-30 C.

[0027] The present disclosure provides a water-based low-temperature heat transfer printing adhesive, prepared from raw materials comprising the following components: 20-30 parts by weight of an ethylene acrylic acid resin, 3-10 parts by weight of an alkaline neutralizing agent, 0.3-0.5 part by weight of a leveling agent, 1-5 parts by weight of a wax emulsion, 1-3 parts by weight of a plasticizer, 0.01-0.05 part by weight of a defoamer, and 65-80 parts by weight of water, wherein the plasticizer is one or more selected from glycerin, dioctyl adipate and dioctyl sebacate. Compared with the prior art, the water-based low-temperature heat transfer printing adhesive provided by the present disclosure is prepared from specific contents of components and achieves a better overall interaction, and the product has better levelling property, water resistance, scratch resistance, and excellent completeness of the transfer printing image-text at low temperature, and it is a pure water-based material, eco-friendly, and pollution-free. The experimental results have shown that the water-based low-temperature heat transfer printing adhesive provided in the present application has good levelling property, .. the formed coating does not whiten and swell after being washed in water at a temperature of 45 C-60 C for 1 h; the coating appearance remains intact after being scratched; the coating can be stretched for 2-2.6 times without breaking; the transfer printing image-text at low temperature of 110 C-125 C is intact, and it shows a good printing performanc, can make ink not fall off and show bright color.

Date Recue/Date Received 2021-09-15

[0028] In addition, the preparation method provided by the present disclosure has simple process with mild and easy-to-control conditions, and broad application prospects.
DETAILED DESCRIPTION

[0029] Hereinafter the technical solutions in the embodiments of the present disclosure will be described clearly and completely. Obviously, the embodiments to be described are only a part of the embodiments of the present disclosure, rather than all of them.
Based on these embodiments in the present disclosure, all the other embodiments obtained by a person having ordinary skill in the art without creative labor should fall within the protection scope of the present disclosure.

[0030] The present disclosure provides a water-based low-temperature heat transfer printing adhesive, prepared from raw materials comprising the following components:

[0031] 20-30 parts by weight of an ethylene acrylic acid resin,

[0032] 3-10 parts by weigh of an alkaline neutralizing agent,

[0033] 0.3-0.5 part by weight of a leveling agent,

[0034] 1-5 parts by weigh of a wax emulsion,

[0035] 1-3 parts by weight of a plasticizer,

[0036] 0.01-0.05 part by weight of a defoamer, and

[0037] 65-80 parts by weight of water,

[0038] wherein the plasticizer is one or more selected from glycerin, dioctyl adipate and dioctyl sebacate .

[0039] In the present disclosure, the water-based low-temperature heat transfer printing adhesive is prepared from the raw materials including ethylene acrylic acid resin, an alkaline neutralizing agent, a leveling agent, a wax emulsion, a plasticizer, a defoamer and water, and preferably prepared from ethylene acrylic acid resin, an alkaline neutralizing agent, a leveling agent, a wax emulsion, a plasticizer, a defoamer and water.

[0040] In the present disclosure, the ethylene acrylic acid resin preferably has a melt index Date Recue/Date Received 2021-09-15 of 300-1300, and preferably a melting point of 75 C-78 C. In the present disclosure, the source of the ethylene acrylic acid resin is not particularly limited. Either the commercially available products well-known to these skilled in the art or self-made products can be used.
For example, the products can be prepared by using ethylene-vinyl acetate copolymer, behenyl methacrylate, and methyl methacrylate as main ingredients, which are well known to these skilled in the art, as long as the EAA parameters meet the above-mentioned raw material requirements. In the present disclosure, the water-based low-temperature heat transfer printing adhesive comprises 20-30 parts by weight, and preferably 20-28 parts by weight of ethylene acrylic acid resin.
.. [0041] In the present disclosure, the alkaline neutralizing agent is preferably one or more selected from ammonia liqour, KOH, NaOH and triethylamine, and more preferably one or two selected from ammonia liqour, KOH, NaOH and triethylamine. In the present disclosure, the source of the alkaline neutralizing agent is not particularly limited. The commercially available products of the above ammonia liqour, KOH, NaOH and trimethylamine, which are well known to these skilled in the art, can be used.
[0042] In the present disclosure, the leveling agent is preferably one or more selected from Glide 410, Wet KL 245 and Glide 496, and more preferably is Glide 410, Wet KL
245 or Glide 496. In the present disclosure, the source of the leveling agent is not particularly limited.
The commercially available products of the above Glide 410, Wet KL 245 and Glide 496, which are well known to these skilled in the art, can be used.
[0043] In the present disclosure, the wax emulsion is preferably one or more selected from palm wax, polyethylene wax, oxidized polyethylene wax and micronized wax, and more preferably is palm wax, polyethylene wax, oxidized polyethylene wax or micronized wax. In the present disclosure, the source of the wax emulsion is not particularly limited. The commercially available products of the above palm wax, polyethylene wax, oxidized polyethylene wax and micronized wax, which are well known to these skilled in the art, can be used. In the present disclosure, the water-based low-temperature heat transfer printing adhesive contains 1-5 parts by weight, and preferably 2-5 parts by weight of the wax emulsion.

Date Recue/Date Received 2021-09-15 [0044] In the present disclosure, the plasticizer is one or more selected from glycerin, dioctyl adipate and dioctyl sebacate, and preferably is glycerin, dioctyl adipate or dioctyl sebacate. In the present disclosure, the source of the plasticizer is not particularly limited. The commercially available products of the above glycerin, dioctyl adipate and dioctyl sebacate, which are well known to these skilled in the art, can be used. In the present disclosure, the water-based low-temperature heat transfer printing adhesive comprises 1-3 parts by weight, and preferably 1-2 parts by weight of plasticizer.
[0045] In the present disclosure, the defoamer is preferably a polyether modified organosilicon-based defoamer. In the present disclosure, its source is not particularly limited.
The commercially available products well known to these skilled in the art can be used.
[0046] In the present disclosure, the water is the soft water well known to these skilled in the art, and is not particularly limited in the present disclosure. In the present disclosure, the water-based low-temperature heat transfer printing adhesive comprises 65-80 parts by weight, and preferably 72-80 parts by weight of water.
.. [0047] In the present disclosure, the water-based low-temperature heat transfer printing adhesive preferably has a solid content of 20%-30%, and should be stored at low temperature, with protection from light, and sealed.
[0048] The water-based low-temperature heat transfer printing adhesive provided by the present disclosure is prepared from specific contents of components and achieves a better overall interaction, and the product has better levelling, water resistance, scratch resistance, and excellent completeness of the transfer printing image-text at low temperature, and it is a pure water-based material, which is a fully water-based formula without any residue. It meets the market requirements of environmental protection, ease of use and stability, and can be used with confidence. Moreover, the water-based low-temperature heat transfer printing adhesive provided by the present disclosure can be coated on substrates such as release film or release paper, and has a good product adaptability. The experimental results have shown that the water-based low-temperature heat transfer printing adhesive has good levelling property, the formed coating does not whiten and swell after being washed in water at a temperature of 45 C-60 C for 1 h; the appearance remains intact after being scratched; the coating can be Date Recue/Date Received 2021-09-15 stretched for 2-2.6 times without breaking. Compared with 160 C-180 C of a transfer printing temperature of the product with the same solid content, the transfer printing temperature required for the product provided by the present disclosure is 110 C-125 C;
and the transfer printing image-text at low temperature of 110 C-125 C is intact, and it shows a good printing performance, can make ink not fall off and show bright color.
[0049] The present disclosure further provides a method of preparing the water-based low-temperature heat transfer printing adhesive described in the above technical solution, comprising the following steps:
[0050] a) under stirring conditions, mixing a first amount of water, a second amount of an alkaline neutralizing agent and a plasticizer, and then adding an ethylene acrylic acid resin to perform a first reaction; then adding the remaining alkaline neutralizing agent dropwise at a rate of 4 g/s-6 g/s to perform a second reaction; after that, adding the remaining water at a rate of 45 g/s-55 g/s to perform a third reaction; after cooling, adding and well mixing a defoamer and a leveling agent, and finally adding a wax emulsion, to obtain a water-based low-temperature heat transfer printing adhesive.
[0051] In the present disclosure, the water, the alkaline neutralizing agent, the plasticizer, the ethylene acrylic acid resin, the wax emulsion, the defoamer, the leveling agent are the same as that in the above technical solution, and will not be repeated here.
[0052] In the present disclosure, the stirring conditions are continued throughout the preparation method; the stirring is preferably carried out at a rotation rate of 100 r/min-500 r/min. In the present disclosure, the devices used in the preparation method are not particularly limited, and reaction kettles well known to these skilled in the art can be used.
[0053] In the present disclosure, the first amount of water, the second amount of the alkaline neutralizing agent, and the plasticizer are preferably mixed for a duration of 1 min-10 min, and more preferably 5 min.
[0054] In the present disclosure, the first amount of water preferably accounts for 70-90 wt%
of the total amount of water; the second amount of an alkaline neutralizing agent preferably accounts for 70-80 wt% of the total amount of the alkaline neutralizing agent.

Date Recue/Date Received 2021-09-15 [0055] In the present disclosure, the first reaction is preferably carried out at a temperature of 90 C-100 C, and more preferably 90 C-98 C; the first reaction is preferably carried out for a duration of 1 h-2 h.
[0056] In the present disclosure, the second reaction is preferably carried out at a temperature of 90 C-100 C, and more preferably 90 C-98 C; the second reaction is preferably carried out for a duration of 0.5 h-1 h.
[0057] In the present disclosure, the third reaction is preferably carried out at a temperature of 90 C-100 C, and more preferably 95 C-100 C; the third reaction is preferably carried out for a duration of 1 h-2 h.
[0058] In the present disclosure, a temperature of cooling is preferably 20 C-30 C, and more preferably 25 C.
[0059] The preparation method provided by the present disclosure has simple process with mild and easy-to-control conditions, and broad application prospects.
[0060] The present disclosure provides a water-based low-temperature heat transfer printing adhesive, prepared from raw materials comprising the following components: 20-30 parts by weight of an ethylene acrylic acid resin, 3-10 parts by weight of an alkaline neutralizing agent, 0.3-0.5 part by weight of a leveling agent, 1-5 parts by weight of a wax emulsion, 1-3 parts by weight of a plasticizer, 0.01-0.05 part by weight of a defoamer, and 65-80 parts by weight of water, wherein the plasticizer is one or more selected from glycerin, dioctyl adipate and dioctyl sebacate. Compared with the prior art, the water-based low-temperature heat transfer printing adhesive provided by the present disclosure is prepared from specific contents of components and achieves a better overall interaction, and the product has better levelling property, water resistance, scratch resistance, and excellent completeness of the transfer printing image-text at low temperature, and it is a pure water-based material, eco-friendly, and pollution-free. The experimental results have shown that the water-based low-temperature heat transfer printing adhesive provided in the present application has good levelling property, the formed coating does not whiten and swell after being washed in water at a temperature of 45 C-60 C for 1 h; the coating appearance remains intact after being scratched; the coating can be stretched for 2-2.6 times without breaking; the transfer printing image-text at low Date Recue/Date Received 2021-09-15 temperature of 110 C-125 C is intact, and it shows a good printing performanc, can make ink not fall off and show bright color.
[0061] In addition, the preparation method provided by the present disclosure has simple process with mild and easy-to-control conditions, and broad application prospects.
[0062] In order to further describe the present disclosure, examples will be given below for detailed description. The raw materials used in the present disclosure are all commercially available.
[0063] Example 1 [0064] (1) The weight ratio and specific types of the raw materials were limited below:
100651 an ethylene acrylic acid resin 20 parts, [0066] an alkaline neutralizing agent 3 parts, [0067] a leveling agent 0.5 part, [0068] a wax emulsion 5 parts, [0069] a plasticizer 1 parts, [0070] a defoamer 0.01 part, and [0071] soft water 80 parts, [0072] wherein the ethylene acrylic acid resin had a melt index of 300, and a melting point of 77 C;
[0073] the alkaline neutralizing agent was ammonia liqour;
[0074] the leveling agent was Glide 410;
[0075] the wax emulsion was oxidized polyethylene wax;
[0076] the plasticizer was glycerin; and [0077] the defoamer was a polyether modified organosilicon-based defoamer.
[0078] (2) The preparation method included steps as follows:
[0079] To a reaction kettle, 70 wt% of the total amount of soft water was added, and stirring Date Recue/Date Received 2021-09-15 was started and controlled at a rotation rate of 100 r/min, 80 wt% of the alkaline neutralizing agent and all of the plasticizer were added and stirred for 5 min, then all of the ethylene acrylic acid resin was added, to perform reaction for 1 h with temperature controlled at 90 C;
after that, the remaining 20 wt% of the alkaline neutralizing agent was added slowly dropwise at a rate of 5 g/s, to perform the reaction for 0.5 h with the emulsion temperature controlled at 95 C; after that, the remaining 30 wt% of the soft water was added at a rate of 50 g/s, to perform the reaction for 2 h with the emulsion temperature controlled at 95 C;
finally, after cooling to 25 C, all the defoamer and leveling agent were added and well mixed, and finally all of the wax emulsion was added, to obtain the water-based low-temperature heat transfer printing adhesive. The obtained water-based low-temperature heat transfer printing adhesive had a solid content of 21.5 wt%.
[0080] The water-based low-temperature heat transfer printing adhesive provided by Example 1 of the present disclosure was coated on a PET release film. The emulsion exhibited good levelling properties, and formed a coating after being dried, with a dry adhesive content of 50 g/m2. The test showed that the coating did not whiten and swell after being washed in water at a temperature of 45 C for 1 h; the coating appearance remained intact after being scratched; the coating can be stretched for 2 times without breaking (using a stretching machine to test the peel strength, the coating would not break when its length was stretched to 2 times); the transfer printing image-text at low temperature of 125 C was intact, and it showed a good printing performanc, can make ink not fall off, and showed bright color.
[0081] Example 2 [0082] (1) The weight ratio and specific types of the raw materials were limited below:
[0083] an ethylene acrylic acid resin 25 parts, [0084] an alkaline neutralizing agent 8 parts, [0085] a leveling agent 0.3 part, [0086] a wax emulsion 3 parts, [0087] a plasticizer 2 parts, [0088] a defoamer 0.02 part, and Date Recue/Date Received 2021-09-15 [0089] soft water 75 parts, [0090] wherein the ethylene acrylic acid resin had a melt index of 300, and a melting point of 77 C;
[0091] the alkaline neutralizing agent was a mixture of ammonia liqour and triethylamine at a weight ratio of 1: 1;
[0092] the leveling agent was Wet KL 245;
[0093] the wax emulsion was polyethylene wax;
[0094] the plasticizer was dioctyl adipate; and [0095] the defoamer was a polyether modified organosilicon-based defoamer.
[0096] (2) The preparation method included steps as follows:
[0097] To a reaction kettle, 80 wt% of the total amount of soft water was added, stirring was started and controlled at a rotation rate of 300 r/min, 70 wt% of the alkaline neutralizing agent and all of the plasticizer were added and stirred for 5 min, then all of the ethylene acrylic acid resin was added, to perform reaction for 1 h with temperature controlled at 95 C;
after that, the remaining 30 wt% of the alkaline neutralizing agent was added slowly dropwise at a rate of 5 g/s, to perform the reaction for 0.5 h with the emulsion temperature controlled at 95 C; after that, the remaining 20 wt% of the soft water was added at a rate of 50 g/s, to perform the reaction for 2 h with the emulsion temperature controlled at 99 C;
finally, after cooling to 25 C, all the defoamer and leveling agent were added and well mixed, and finally all of the wax emulsion was added, to obtain the water-based low-temperature heat transfer printing adhesive. The obtained water-based low-temperature heat transfer printing adhesive had a solid content of 26.3 wt%.
[0098] The water-based low-temperature heat transfer printing adhesive provided by Example 2 of the present disclosure was coated on a PET release film. The emulsion exhibited good levelling properties, and formed a coating after being dried, with a dry adhesive content of 80 g/m2. The test showed that the coating did not whiten and swell after being washed in water at a temperature of 50 C for 1 h; the coating appearance remained intact after being scratched; the coating can be stretched for 2 times without breaking (using a stretching Date Recue/Date Received 2021-09-15 machine to test the peel strength, the coating would not break when its length was stretched to 2 times); the transfer printing image-text at low temperature of 125 C was intact, and it showed a good printing performanc, can make ink not fall off, and showed bright color.
[0099] Example 3 [0100] (1) The weight ratio and specific types of the raw materials were limited below:
[0101] an ethylene acrylic acid resin 28 parts, [0102] an alkaline neutralizing agent 10 parts, [0103] a leveling agent 0.4 part, [0104] a wax emulsion 5 parts, [0105] a plasticizer 1 parts, [0106] a defoamer 0.01 part, and [0107] soft water 72 parts, [0108] wherein the ethylene acrylic acid resin had a melt index of 1300, and a melting point of 77 C;
[0109] the alkaline neutralizing agent was a mixture of ammonia liqour and triethylamine at a weight ratio of 1: 1;
[0110] the leveling agent is Wet KL 245;
[0111] the wax emulsion was oxidized polyethylene wax;
[0112] the plasticizer was glycerin; and .. [0113] the defoamer was a polyether modified organosilicon-based defoamer.
[0114] (2) The preparation method included steps as follows:
[0115] To a reaction kettle, 90 wt% of the total amount of soft water was added, stirring was started and controlled at a rotation rate of 100 r/min, 80 wt% of the alkaline neutralizing agent and all of the plasticizer were added and stirred for 5 min, then all of the ethylene acrylic acid resin was added, to perform reaction for 1 h with temperature controlled at 90 C;
after that, the remaining 20 wt% of the alkaline neutralizing agent was added slowly dropwise Date Recue/Date Received 2021-09-15 at a rate of 5 g/s, to perform the reaction for 0.5 h with the emulsion temperature controlled at 95 C; after that, the remaining 10 wt% of the soft water was added at a rate of 50 g/s, to perform the reaction for 2 h with the emulsion temperature controlled at 95 C;
finally, after cooling to 25 C all the defoamer and leveling agent were added and well mixed, and finally all of the wax emulsion was added, to obtain the water-based low-temperature heat transfer printing adhesive. The obtained water-based low-temperature heat transfer printing adhesive had a solid content of 30.0 wt%.
[0116] The water-based low-temperature heat transfer printing adhesive provided by Example 3 of the present disclosure was coated on a release paper. The emulsion exhibited good levelling properties, and formed a coating after being dried, with a dry adhesive content of 60 g/m2. The test showed that the coating did not whiten and swell after being washed in water at a temperature of 60 C for 1 h; the coating appearance remained intact after being scratched; the coating can be stretched for 2.6 times without breaking (using a stretching machine to test the peel strength, the coating would not break when its length was stretched to 2.6 times); the transfer printing image-text at low temperature of 110 C was intact, and it showed a good printing performance, can make ink not fall off, and showed bright color.
[0117] Example 4 [0118] (1) The weight ratio and specific types of the raw materials were limited below:
[0119] an ethylene acrylic acid resin 26 parts, [0120] an alkaline neutralizing agent 9 parts, [0121] a leveling agent 0.4 part, [0122] a wax emulsion 3 parts, [0123] a plasticizer 2 parts, [0124] an defoamer 0.02 part, and [0125] soft water 74 parts, [0126] wherein the ethylene acrylic acid resin had a melt index of 1300, and a melting point of 77 C;

Date Recue/Date Received 2021-09-15 [0127] the alkaline neutralizing agent was NaOH;
[0128] the leveling agent was Glide 496;
[0129] the wax emulsion was oxidized polyethylene wax;
[0130] the plasticizer was dioctyl sebacate; and [0131] the defoamer was a polyether modified organosilicon-based defoamer.
[0132] (2) The preparation method included steps as follows:
[0133] To a reaction kettle, 80 wt% of the total amount of soft water was added, stirring was started and controlled at a rotation rate of 500 r/min, 80 wt% of the alkaline neutralizing agent and all of the plasticizer were added and stirred for 5 min, then all of the ethylene acrylic acid resin was added, to perform reaction for 2 h with temperature controlled at 98 C;
after that, the remaining 20 wt% of the alkaline neutralizing agent was added slowly dropwise at a rate of 5 g/s, to perform the reaction for 0.5 h with the emulsion temperature controlled at 95 C; after that, the remaining 20 wt% of the soft water was added at a rate of 50 g/s, to perform the reaction for 1 h with the emulsion temperature controlled at 100 C; finally, after cooling to 25 C all the defoamer and leveling agent were added and well mixed, and finally all of the wax emulsion was added, to obtain the water-based low-temperature heat transfer printing adhesive. The obtained water-based low-temperature heat transfer printing adhesive had a solid content of 27.5 wt%.
[0134] The water-based low-temperature heat transfer printing adhesive provided by Example 4 of the present disclosure was coated on a PET release film. The emulsion exhibited good levelling properties, and formed a coating after being dried, with a dry adhesive content of 50 g/m2. The test showed that the coating did not whiten and swell after being washed in water at a temperature of 50 C for 1 h; the coating appearance remained intact after being scratched; the coating can be stretched for 2 times without breaking (using a stretching machine to test the peel strength, the coating would not break when its length was stretched to 2 times); the transfer printing image-text at low temperature of 120 C was intact, and it showed a good printing performance, can make ink not fall off, and showed bright color.

Date Recue/Date Received 2021-09-15 [0135] Example 5 [0136] (1) The weight ratio and specific types of the raw materials were limited below:
[0137] an ethylene acrylic acid resin 25 parts, [0138] an alkaline neutralizing agent 8 parts, [0139] a leveling agent 0.3 part, [0140] a wax emulsion 2 parts, [0141] a plasticizer 2 parts, [0142] a defoamer 0.05 part, and [0143] soft water 75 parts, [0144] wherein the ethylene acrylic acid resin had a melt index of 300, and a melting point of 77 C;
[0145] the alkaline neutralizing agent is was a mixture of triethanolamine and KOH at a weight ratio of 5: 1;
[0146] the leveling agent was Glide 410;
[0147] the wax emulsion was oxidized polyethylene wax;
[0148] the plasticizer was dioctyl adipate; and [0149] the defoamer was a polyether modified organosilicon-based defoamer.
[0150] (2) The preparation method included steps as follows:
[0151] To a reaction kettle, 70 wt% of the total amount of soft water was added, and stirring was started and controlled at a rotation rate of 300 r/min, 80 wt% of the alkaline neutralizing agent and all of the plasticizer were added and stirred for 5 min, then all of the ethylene acrylic acid resin was added, to perform reaction for 2 h with temperature controlled at 92 C;
after that, the remaining 20 wt% of the alkaline neutralizing agent was added slowly dropwise at a rate of 5 g/s, to perform the reaction for 1 h with the emulsion temperature controlled at 98 C; after that, the remaining 30 wt% of the soft water was added at a rate of 50 g/s, to perform the reaction for 2 h with the emulsion temperature controlled at 95 C;
finally, after Date Recue/Date Received 2021-09-15 cooling to 25 C all the defoamer and leveling agent were added and well mixed, and finally all of the wax emulsion was added, to obtain the water-based low-temperature heat transfer printing adhesive. The obtained water-based low-temperature heat transfer printing adhesive had a solid content of 25.5 wt%.
[0152] The water-based low-temperature heat transfer printing adhesive provided by Example 5 of the present disclosure was coated on a release paper. The emulsion exhibited good levelling properties, and formed a coating after being dried, with a dry adhesive content of 70 g/m2. The test showed that the coating did not whiten and swell after being washed in water at a temperature of 60 C for 1 h; the coating appearance remained intact after being .. scratched; the coating can be stretched for 2.2 times without breaking (using a stretching machine to test the peel strength, the coating would not break when its length was stretched to 2.2 times); the transfer printing image-text at low temperature of 110 C was intact, and it showed a good printing performance, can make ink not fall off, and showed bright color.
[0153] The above description is only the preferred embodiments of the present disclosure. It .. should be noted that for those skilled in the art, various improvements and modifications may be made without departing from the principle of the present disclosure, and these improvements and modifications should fall within the scope of protection of the present disclosure.

Date Recue/Date Received 2021-09-15

Claims

1. A water-based low-temperature heat transfer printing adhesive, prepared from raw materials comprising the following components:
20-30 parts by weight of an ethylene acrylic acid resin, 3-10 parts by weigh of an alkaline neutralizing agent, 0.3-0.5 part by weight of a leveling agent, 1-5 parts by weigh of a wax emulsion, 1-3 parts by weight of a plasticizer, 0.01-0.05 part by weight of a defoamer, and 65-80 parts by weight of water, wherein the plasticizer is one or more selected from glycerin, dioctyl adipate and dioctyl seb ac ate.

2. The water-based low-temperature heat transfer printing adhesive according to claim 1, wherein the ethylene acrylic acid resin has a melt index of 300-1300, and a melting point of 75 C-78 C.

3. The water-based low-temperature heat transfer printing adhesive according to claim 1, wherein the alkaline neutralizing agent is one or more selected from ammonia liqour, KOH, NaOH and triethylamine.

4. The water-based low-temperature heat transfer printing adhesive according to claim 1, wherein the leveling agent is one or more selected from Glide 410, Wet KL 245 and Glide 496.

5. The water-based low-temperature heat transfer printing adhesive according to claim 1, wherein the wax emulsion is one or more selected from palm wax, polyethylene wax, oxidized polyethylene wax and micronized wax.

6. A preparation method of the water-based low-temperature heat transfer printing adhesive according to any one of claims 1-5, comprising the following steps:
a) under stirring conditions, mixing a first amount of water, a second amount of an alkaline neutralizing agent and a plasticizer, and then adding an ethylene acrylic acid resin to perform a Date recue/Date received 2023-03-10 first reaction; then adding the remaining alkaline neutralizing agent dropwise at a rate of 4 g/s-6 g/s to perform a second reaction; after that, adding the remaining water at a rate of 45 g/s-55 g/s to perform a third reaction; after cooling, adding and well mixing a defoamer and a leveling agent, and finally adding a wax emulsion, to obtain a water-based low-temperature heat transfer printing adhesive.

7. The preparation method according to claim 6, wherein in step a), the stirring is carried out at a rotation rate of 100 r/min-500 r/min; the first amount of water, the second amount of the alkaline neutralizing agent and the plasticizer are mixed for a duration of 1 min-10 min.

8. The preparation method according to claim 6, wherein in step a) the first amount of water accounts for 70-90 wt% of the total amount of water; the second amount of the alkaline neutralizing agent accounts for 70-80 wt% of the total amount of the alkaline neutralizing agent.

9. The preparation method according to claim 6, wherein in step a) the first reaction is carried out at a temperature of 90 C-100 C for a duration of 1 h-2 h;
the second reaction is carried out at a temperature of 90 C-100 C for a duration of 0.5 h-1 h; and the third reaction is carried out at a temperature of 90 C-100 C for a duration of 1 h-2 h.

10. The preparation method according to claim 6, wherein in step a), a temperature of the cooling is 20 C-30 C.

Date recue/Date received 2023-03-10