Modified organic silicon resin, duplex printing textile pigment ink and preparation method thereof

Abstract

The invention provides modified organic silicon resin, duplex printing textile pigment ink and a preparation method thereof, and belongs to the technical field of digital printing of high polymer materials and textiles. The preparation method comprises the following steps: mixing a solvent, hydrogen-containing silicone oil, a modifier and a polymerization inhibitor, adding a catalyst for reaction after mixing, and removing the solvent in vacuum after the reaction is finished to obtain modified organic silicon resin; and mixing water, the aqueous solvent, the wetting agent, the resin, the modified organic silicon resin and the color paste, and filtering to obtain the duplex printing textile pigment ink. The duplex printing textile pigment ink does not need to carry out pretreatment and aftertreatment on a fabric, and the process is simple; no wastewater is generated in production, so that the production cost can be saved; and compared with traditional printing, technological processes do not need to be increased, no waste water is generated, and environment friendliness is achieved.

Description

Technical Field

[0001] The invention relates to the technical field of polymer materials and textile digital printing, and in particular to a modified organic silicon resin, a double-sided printing textile pigment ink and a preparation method thereof. Background Art

[0002] Digital textile printing has become a very popular printing technology in the textile industry because it does not require plate making, has a simple process, can respond quickly to market changes, and can achieve small batches, multiple varieties, multiple colors and personalized customization. Textile pigment inks are increasingly favored by users because they do not generate wastewater during the printing process, have simple printing processes, are non-selective to fibers, and have high light fastness. They are the development trend of textile inks.

[0003] With the rise of double-sided printing machines and their technology, double-sided printing has gradually come into people's view. However, the coating of the product after double-sided printing becomes thicker, and the feel becomes harder and worse, which poses a new challenge to textile pigment ink. With the improvement of living standards, people have higher requirements for the feel of products. Pigment ink is to fix the color by sticking the pigment to the surface of the fabric after the adhesive is cured. Therefore, the product printed by pigment ink usually feels harder than dye ink. Although the coating thickness can be reduced by adjusting the inkjet amount, it will also cause the color of the printed product to fade.

[0004] In 2014, Chinese patent CN104356277A disclosed a thickener that can improve the feel of paint printing. The patent reacts castor oil and p-toluenesulfonic acid in isopropanol and dissolves them in acrylamide. The pH value is adjusted to 5.5-6.5 with ammonia water and used as an ink additive to improve the feel of paint printing, but its acidity easily causes the resin and other components in the ink to demulsify and precipitate. Chinese patent CN100999875A discloses an acrylate emulsified thickener. The patent uses a thickener to compound modified silicone linear bodies to improve the feel of paint printing, but some industry insiders also pointed out that this method has a significant effect on fastness. Chinese patent CN104628989A discloses a water-based inkjet for cotton fabrics, which improves the feel by providing a chitosan-modified polyurethane emulsion, but its effect is greatly affected by molecular weight.

[0005] Therefore, it is very important to provide a method for improving the softness of coating ink so that it can satisfy the double-sided printing double-sided printing textile pigment ink. Summary of the invention

[0006] The purpose of the present invention is to provide a modified silicone resin, a double-sided printing textile pigment ink and a preparation method thereof, so as to solve the technical problem of poor fastness and softness of the double-sided printing textile pigment ink in the prior art.

[0007] In order to achieve the above-mentioned object of the invention, the present invention provides the following technical solutions:

[0008] The present invention provides a modified organic silicone resin, the structural formula of the modified organic silicone resin is:

[0009]

[0010] Wherein, m and n are independently 1 to 10, R1 and R2 are independently -CH3, an unsaturated polyether compound group, an unsaturated amino compound group, an unsaturated carboxyl compound group or an unsaturated carboxyl compound derivative group, and R3 is an unsaturated polyether compound group, an unsaturated amino compound group, an unsaturated carboxyl compound group or an unsaturated carboxyl compound derivative group.

[0011] Further, the unsaturated polyether compound group includes allyl polyoxyethylene ether, allyl polyoxyethylene polyoxypropylene ether or allyl glycidyl ether;

[0012] The unsaturated amino compound group includes allylamine, allylpiperazine, acrylamide or N,N-dimethylacrylamide;

[0013] The unsaturated carboxyl compound group includes acrylic acid or p-vinylbenzoic acid.

[0014] The present invention provides a method for preparing the modified organic silicone resin, comprising mixing 10 to 18 parts of a solvent, 35 to 45 parts of hydrogenated silicone oil, 30 to 50 parts of a modifier and 1 to 3 parts of a polymerization inhibitor, then adding 1 to 3 parts of a catalyst to react, and removing the solvent in vacuo after the reaction is completed to obtain the modified organic silicone resin.

[0015] Furthermore, the modifier includes one or more of allyl polyoxyethylene ether, allyl polyoxyethylene polyoxypropylene ether, allyl glycidyl ether, allyl amine, allyl piperazine and acrylic acid, the hydrogen content of the hydrogen-containing silicone oil is 0.01%-20%, the solvent includes toluene or xylene, the inhibitor includes hydroquinone, and the catalyst includes chloroplatinic acid solution.

[0016] Furthermore, the mixing is carried out during stirring, the stirring speed is 200 to 400 r / min, and the stirring temperature is 80 to 90° C.;

[0017] The reaction temperature is 120-140° C., and the reaction time is 1-5 hours.

[0018] The present invention also provides a double-sided printing textile pigment ink, which is composed of the following components in parts by weight:

[0019]

[0020] Further, the aqueous solvent includes one or more of ethanol, n-propanol, isopropanol, n-butanol, ethylene glycol, 1,3-propylene glycol, 1,4-butanediol, 1,6-hexanediol, diethylene glycol, triethylene glycol, polyethylene glycol 200, polyethylene glycol 400, polyethylene glycol 600, diethylene glycol, glycerol, pentaerythritol, 2-pyrrolidone and N-methylpyrrolidone;

[0021] The resin includes one or more of Mitsui polyurethane resin 6110, Shenyang Chemical Research Institute polyurethane resin 101, Shenyang Chemical Research Institute polyurethane resin 110, Hefei Ruipin polyurethane resin 831, Hefei Ruipin polyurethane resin 801, Guangzhou Guanzhi polyurethane resin 8120 and Hefei Huayue New Material 8001B-2.

[0022] Further, the closed curing agent includes one or more of Shanghai Bolino BL-8119 closed curing agent, Shanghai Bolino BL-935 closed curing agent, Guangzhou Zengmao Chemical ZS-835 closed curing agent, ZS-1890D closed curing agent, Anhui Yuanchen YC-2820 closed curing agent, Guangzhou Haoyi WH-1993 closed curing agent and Guangzhou Haoyi WH-3192 closed curing agent;

[0023] The color paste includes a nano pigment color paste with good dispersion stability and a particle size D50 of 100-130nm;

[0024] The wetting agent includes an organic silicon wetting agent, and the organic silicon wetting agent includes one or more of Hydropalat WE 3323, Hydropalat WE 3322, Hydropalat WE 110, Hydropalat WE 120, BYK DISPERBYK 2012, BYK DISPERBYK 180, BYK DISPERBYK 2010, BYK DISPERBYK 2055, BYK DISPERBYK 190, BYK DISPERBYK 192, BYK DISPERBYK 182 and BYK DISPERBYK 102.

[0025] The invention also provides a method for preparing the double-sided printing textile pigment ink, which comprises mixing water, aqueous solvent, wetting agent, resin, modified organic silicon resin and color paste, filtering and obtaining the double-sided printing textile pigment ink.

[0026] Furthermore, the mixing is carried out during stirring, the stirring speed is 250 to 350 r / min, and the stirring time is 0.5 to 2 h.

[0027] Beneficial effects of the present invention:

[0028] The invention obtains a modified silicone resin by subjecting hydrogenated silicone oil to a silylation reaction with a hydrophilic group, thereby imparting hydrophilicity to the hydrogenated silicone oil, and applying the modified silicone resin in an ink formulation, thereby utilizing the flexibility of the modified silicone resin to toughen the ink coating, thereby improving the softness and hand feel of the final product while taking other properties into consideration, and being suitable for double-sided printing; the invention does not require pre- and post-treatment of the fabric, and has a simple process; the invention does not generate wastewater during production, and can save production costs; and while improving the softness and hand feel, the invention does not generate sedimentation; compared with traditional printing, there is no need to increase the process flow, no wastewater is generated, and the invention is environmentally friendly. DETAILED DESCRIPTION

[0029] The present invention provides a modified organic silicone resin, the structural formula of the modified organic silicone resin is:

[0030]

[0031] Wherein, m and n are independently 1 to 10, R1 and R2 are independently -CH3, an unsaturated polyether compound group, an unsaturated amino compound group, an unsaturated carboxyl compound group or an unsaturated carboxyl compound derivative group, and R3 is an unsaturated polyether compound group, an unsaturated amino compound group, an unsaturated carboxyl compound group or an unsaturated carboxyl compound derivative group.

[0032] Preferably, m and n are independently 2 to 9, R1 and R2 are independently -CH3, an unsaturated polyether compound group, an unsaturated carboxyl compound group or an unsaturated carboxyl compound derivative group, and R3 is an unsaturated polyether compound group, an unsaturated carboxyl compound group or an unsaturated carboxyl compound derivative group.

[0033] More preferably, m and n are independently 3 to 8, R1 and R2 are independently -CH3, an unsaturated polyether compound group or an unsaturated carboxyl compound derivative group, and R3 is an unsaturated polyether compound group or an unsaturated carboxyl compound derivative group.

[0034] In the present invention, the unsaturated polyether compound group includes allyl polyoxyethylene ether, allyl polyoxyethylene polyoxypropylene ether or allyl glycidyl ether, preferably allyl polyoxyethylene ether or allyl polyoxyethylene polyoxypropylene ether, and more preferably allyl polyoxyethylene ether;

[0035] The unsaturated amino compound group includes allylamine, allylpiperazine, acrylamide or N,N-dimethylacrylamide, preferably allylamine, acrylamide or N,N-dimethylacrylamide, and more preferably allylamine or N,N-dimethylacrylamide;

[0036] The unsaturated carboxyl compound group includes acrylic acid or p-vinylbenzoic acid, preferably acrylic acid.

[0037] The present invention provides a method for preparing the modified organic silicone resin, comprising mixing 10 to 18 parts of a solvent, 35 to 45 parts of hydrogenated silicone oil, 30 to 50 parts of a modifier and 1 to 3 parts of a polymerization inhibitor, then adding 1 to 3 parts of a catalyst to react, and removing the solvent in vacuo after the reaction is completed to obtain the modified organic silicone resin.

[0038] In the present invention, the modifier is preferably present in an amount of 32 to 47 parts by weight, and more preferably 35 to 45 parts by weight.

[0039] In the present invention, the modifier includes one or more of allyl polyoxyethylene ether, allyl polyoxyethylene polyoxypropylene ether, allyl glycidyl ether, allyl amine, allyl piperazine and acrylic acid, preferably one or more of allyl polyoxyethylene ether, allyl polyoxyethylene polyoxypropylene ether, allyl glycidyl ether, allyl piperazine and acrylic acid, and further preferably one or more of allyl polyoxyethylene ether, allyl polyoxyethylene polyoxypropylene ether, allyl glycidyl ether and acrylic acid.

[0040] In the present invention, the hydrogen-containing silicone oil is preferably 36 to 44 parts by weight, and more preferably 37 to 42 parts by weight.

[0041] In the present invention, the hydrogen content of the hydrogen-containing silicone oil is 0.01%-20%, preferably 2%-19%, and more preferably 5%-18%.

[0042] In the present invention, the solvent is preferably present in an amount of 11 to 17 parts by weight, and more preferably 12 to 16 parts by weight.

[0043] In the present invention, the solvent comprises toluene or xylene, preferably toluene.

[0044] In the present invention, the polymerization inhibitor is preferably present in an amount of 1.5 to 2.5 parts by weight, more preferably 2 parts by weight.

[0045] In the present invention, the polymerization inhibitor is preferably hydroquinone.

[0046] In the present invention, the catalyst is preferably present in an amount of 1.5 to 2.5 parts by weight, more preferably 2 parts by weight.

[0047] In the present invention, the catalyst is preferably a chloroplatinic acid solution.

[0048] In the present invention, the mixing is carried out under stirring, the stirring speed is 200-400 r / min, preferably 250-350 r / min, more preferably 300 r / min; the stirring temperature is 80-90° C., preferably 82-88° C., more preferably 84-86° C.;

[0049] The reaction temperature is 120-140° C., preferably 122-138° C., and more preferably 125-135° C.; the reaction time is 1-5 h, preferably 2-4 h, and more preferably 3 h.

[0050] The present invention also provides a double-sided printing textile pigment ink, which is composed of the following components in parts by weight:

[0051]

[0052] In the present invention, the amount of the water-soluble solvent is preferably 12 to 18 parts by weight, and more preferably 14 to 16 parts by weight.

[0053] In the present invention, the aqueous solvent includes one or more of ethanol, n-propanol, isopropanol, n-butanol, ethylene glycol, 1,3-propylene glycol, 1,4-butanediol, 1,6-hexanediol, diethylene glycol, triethylene glycol, polyethylene glycol 200, polyethylene glycol 400, polyethylene glycol 600, diethylene glycol, glycerol, pentaerythritol, 2-pyrrolidone and N-methylpyrrolidone, preferably ethanol, n-propanol, isopropanol, n-butanol, ethylene glycol, 1,3-propylene glycol, 1,4-butanediol, 1,6-hexanediol, diethylene glycol, triethylene glycol, polyethylene glycol 200, polyethylene glycol 400, polyethylene glycol 600, diethylene glycol, glycerol, pentaerythritol, 2-pyrrolidone and N-methylpyrrolidone. The invention can be selected from the group consisting of 4-butanediol, diethylene glycol, triethylene glycol, polyethylene glycol 200, polyethylene glycol 400, diethylene glycol, propylene glycol, pentaerythritol, 2-pyrrolidone and N-methylpyrrolidone, and more preferably selected from the group consisting of ethanol, n-propanol, isopropanol, n-butanol, ethylene glycol, 1,3-propylene glycol, diethylene glycol, triethylene glycol, polyethylene glycol 200, diethylene glycol, propylene glycol, pentaerythritol, 2-pyrrolidone and N-methylpyrrolidone.

[0054] In the present invention, the amount of the resin is preferably 18 to 22 parts by weight, and more preferably 20 parts by weight.

[0055] In the present invention, the resin includes one or more of Mitsui polyurethane resin 6110, Shenyang Chemical Research Institute polyurethane resin 101, Shenyang Chemical Research Institute polyurethane resin 110, Hefei Ruipin polyurethane resin 831, Hefei Ruipin polyurethane resin 801, Guangzhou Guanzhi polyurethane resin 8120 and Hefei Huayue new material 8001B-2, preferably one or more of Mitsui polyurethane resin 6110, Shenyang Chemical Research Institute polyurethane resin 101, Shenyang Chemical Research Institute polyurethane resin 110, Hefei Ruipin polyurethane resin 801, Guangzhou Guanzhi polyurethane resin 8120 and Hefei Huayue new material 8001B-2, further preferably one or more of Mitsui polyurethane resin 6110, Shenyang Chemical Research Institute polyurethane resin 101, Shenyang Chemical Research Institute polyurethane resin 110, Guangzhou Guanzhi polyurethane resin 8120 and Hefei Huayue new material 8001B-2.

[0056] In the present invention, the amount of the blocked curing agent is preferably 12 to 18 parts by weight, and more preferably 14 to 16 parts by weight.

[0057] In the present invention, the blocked curing agent includes one or more of Shanghai Bolino BL-8119 blocked curing agent, Shanghai Bolino BL-935 blocked curing agent, Guangzhou Zengmao Chemical ZS-835 blocked curing agent, ZS-1890D blocked curing agent, Anhui Yuanchen YC-2820 blocked curing agent, Guangzhou Haoyi WH-1993 blocked curing agent and Guangzhou Haoyi WH-3192 blocked curing agent, preferably Shanghai Bolino BL-8119 blocked curing agent, Shanghai Bolino BL-935 blocked curing agent, Guangzhou Zengmao Chemical ZS-835 blocked curing agent, Guangzhou Zengmao Chemical ZS-1890D blocked curing agent, Anhui Yuanchen YC-2820 blocked curing agent, Guangzhou Haoyi WH-1993 blocked curing agent and Guangzhou Haoyi WH-3192 blocked curing agent. Agent, Guangzhou Zengmao Chemical ZS-835 closed curing agent, Anhui Yuanchen YC-2820 closed curing agent, Guangzhou Haoyi WH-1993 closed curing agent and Guangzhou Haoyi WH-3192 closed curing agent one or more, further preferably Shanghai Bolino BL-8119 closed curing agent, Shanghai Bolino BL-935 closed curing agent, Guangzhou Zengmao Chemical ZS-835 closed curing agent, Guangzhou Haoyi WH-1993 closed curing agent and Guangzhou Haoyi WH-3192 closed curing agent one or more.

[0058] In the present invention, the amount of the color paste is preferably 32 to 38 parts by weight, and more preferably 34 to 36 parts by weight.

[0059] In the present invention, the color paste includes a nano pigment color paste with good dispersion stability, and the particle size D50 is 100-130nm, preferably 105-125nm, and more preferably 110-120nm.

[0060] In the present invention, the amount of the modified silicone resin is preferably 6 to 9 parts by weight, and more preferably 7 to 8 parts by weight.

[0061] In the present invention, the amount of the wetting agent is preferably 12 to 18 parts by weight, and more preferably 14 to 16 parts by weight.

[0062] In the present invention, the wetting agent is preferably a silicone wetting agent, and the silicone wetting agent includes one or more of Hydropalat WE 3323, Hydropalat WE 3322, Hydropalat WE 110, Hydropalat WE 120, BYKDISPERBYK 2012, BYK DISPERBYK 180, BYK DISPERBYK 2010, BYK DISPERBYK 2055, BYKDISPERBYK 190, BYK DISPERBYK 192, BYK DISPERBYK 182 and BYK DISPERBYK 102, preferably Hydropalat WE 3323, Hydropalat WE 110, Hydropalat WE 120, BYKDISPERBYK 2012, BYK DISPERBYK 180, BYK DISPERBYK 2010, BYK DISPERBYK 2055, BYKDISPERBYK 190, BYK DISPERBYK 192, BYK DISPERBYK 182 and BYK DISPERBYK 102. BYK DISPERBYK 180, BYK DISPERBYK 2055, BYK DISPERBYK 190, BYK DISPERBYK 192, BYK DISPERBYK 182 and BYK DISPERBYK 102, and more preferably one or more of Hydropalat WE 3323, Hydropalat WE 110, Hydropalat WE 120, BYK DISPERBYK 2012, BYK DISPERBYK 180, BYK DISPERBYK 190, BYK DISPERBYK 192, BYK DISPERBYK 182 and BYK DISPERBYK 102.

[0063] In the present invention, the amount of water used is preferably 3 to 25 parts by weight, and more preferably 4.5 to 20 parts by weight.

[0064] The invention also provides a method for preparing the double-sided printing textile pigment ink, which comprises mixing water, aqueous solvent, wetting agent, resin, modified organic silicon resin and color paste, filtering and obtaining the double-sided printing textile pigment ink.

[0065] In the present invention, the mixing is carried out under stirring, the stirring speed is 250-350 r / min, preferably 260-320 r / min, more preferably 280-300 r / min; the stirring time is 0.5-2 h, preferably 0.8-1.5 h, more preferably 1 h.

[0066] The technical solutions provided by the present invention are described in detail below in conjunction with the embodiments, but they should not be construed as limiting the protection scope of the present invention.

[0067] Example 1

[0068] 16 g of toluene, 40 g of hydrogen-containing silicone oil, 40 g of allyl polyoxyethylene ether, and 2 g of hydroquinone were mixed, the mixture was stirred, and the temperature was raised to 85° C., and then 2 g of chloroplatinic acid solution was added, and the mixture was reacted at 130° C. for 3 h. After the reaction was completed, the solvent was removed in vacuo to obtain an allyl polyoxyethylene ether silicone resin;

[0069] 17.5 g of water, 15 g of propylene glycol, 20 g of Mitsui 6110 resin, 10 g of BL-8119 blocked curing agent, 5 g of allyl polyoxyethylene ether silicone resin, 32 g of color paste and 0.5 g of Hydropalat WE 3323 wetting agent were mixed and stirred at a speed of 300 r / min for 1 h. After the stirring, the mixture was filtered with a 0.45 μm PP filter membrane to obtain a double-sided printing textile pigment ink.

[0070] Example 2

[0071] 12g of xylene, 37g of hydrogen-containing silicone oil, 47g of allyl polyoxyethylene polyoxypropylene ether, and 2g of hydroquinone are mixed, the mixture is stirred, and the temperature is raised to 85°C, and then 2g of chloroplatinic acid solution is added, and the mixture is reacted at 130°C for 3h. After the reaction is completed, the solvent is removed in vacuo to obtain an allyl polyoxyethylene polyoxypropylene ether silicone resin;

[0072] 16 g of water, 16.7 g of diethylene glycol, 2 g of N-methylpyrrolidone, 18 g of Shenyang Chemical Research Institute 101 resin, 11 g of BL-935 blocked curing agent, 6 g of allyl polyoxyethylene polyoxypropylene ether silicone resin, 30 g of color paste and 0.3 g of Hydropalat WE 110 wetting agent were mixed and stirred at a speed of 300 r / min for 1 h. After the stirring, the mixture was filtered with a 0.45 μm PP filter membrane to obtain a double-sided printing textile pigment ink.

[0073] Example 3

[0074] 6 g of toluene, 10 g of xylene, 35 g of hydrogenated silicone oil, 45 g of allyl glycidyl ether, and 2 g of hydroquinone were mixed, the mixture was stirred, and the temperature was raised to 85° C., and then 2 g of chloroplatinic acid solution was added, and the mixture was reacted at 130° C. for 3 h. After the reaction was completed, the solvent was removed in vacuo to obtain an allyl glycidyl ether silicone resin;

[0075] 21g of water, 15g of polyethylene glycol 200, 5g of N-methylpyrrolidone, 15g of Shenyang Chemical Research Institute 110 resin, 12g of ZS-835 blocked curing agent, 6.5g of allyl glycidyl ether silicone resin, 25g of color paste, and 0.5g of BYKDISPERBYK2012 wetting agent were mixed and stirred at a speed of 300r / min for 1h. After the stirring, the mixture was filtered with a 0.45μmPP filter membrane to obtain a double-sided printing textile pigment ink.

[0076] Example 4

[0077] 15 g of toluene, 40 g of hydrogenated silicone oil, 35 g of allylamine, and 2 g of hydroquinone were mixed, the mixture was stirred, and the temperature was raised to 85° C., and then 2 g of chloroplatinic acid solution was added, and the mixture was reacted at 130° C. for 3 h. After the reaction was completed, the solvent was removed in vacuo to obtain an allylamine silicone resin;

[0078] 13.5 g of water, 15 g of 1,3-propylene glycol, 5 g of 2-pyrrolidone, 15 g of Hefei Ruipin 831 polyurethane resin, 14 g of ZS-1890D blocked curing agent, 7 g of allylamine silicone resin, 26 g of color paste, and 0.5 g of DISPERBYK 180 wetting agent were mixed and stirred at a speed of 300 r / min for 1 h. After the stirring, the mixture was filtered with a 0.45 μm PP filter membrane to obtain a double-sided printing textile pigment ink.

[0079] Example 5

[0080] 15 g of xylene, 42 g of hydrogenated silicone oil, 32 g of allyl piperazine, and 2 g of hydroquinone were mixed, the mixture was stirred, and the temperature was raised to 85° C., and then 2 g of chloroplatinic acid solution was added, and the mixture was reacted at 130° C. for 3 h. After the reaction was completed, the solvent was removed in vacuo to obtain an allyl piperazine silicone resin;

[0081] 14 g of water, 14 g of 1,6-hexanediol, 6 g of 2-pyrrolidone, 20 g of Hefei Ruipin 801 polyurethane resin, 13 g of YC-2820 blocked curing agent, 7.5 g of allyl piperazine silicone resin, 27 g of color paste, and 0.5 g of BYKDISPERBYK 192 wetting agent were mixed and stirred at a speed of 300 r / min for 1 h. After the stirring, the mixture was filtered with a 0.45 μm PP filter membrane to obtain a double-sided printing textile pigment ink.

[0082] Example 6

[0083] 15 g of toluene, 2 g of xylene, 45 g of hydrogenated silicone oil, 37 g of acrylic acid, and 2 g of hydroquinone were mixed, the mixture was stirred, and the temperature was raised to 85° C., and then 2 g of chloroplatinic acid solution was added, and the mixture was reacted at 130° C. for 3 h. After the reaction was completed, the solvent was removed in vacuo to obtain an acrylic silicone resin;

[0084] 4.5 g of water, 15 g of diethylene glycol, 5 g of 2-pyrrolidone, 21 g of Guangzhou Guanzhi 8120 polyurethane resin, 15 g of WH-1993 blocked curing agent, 8 g of acrylic silicone resin, 28 g of color paste, and 0.5 g of BYKDISPERBYK 102 wetting agent were mixed and stirred at a speed of 300 r / min for 1 h. After the stirring, the mixture was filtered with a 0.45 μm PP filter membrane to obtain a double-sided printing textile pigment ink.

[0085] Comparative Example 1

[0086] 22.5 g of water, 15 g of propylene glycol, 20 g of Mitsui 6110 resin, 10 g of BL-8119 blocked curing agent, 32 g of color paste and 0.5 g of Hydropalat WE 3323 wetting agent were mixed and stirred at a speed of 300 r / min for 1 h. After the stirring, the mixture was filtered with a 0.45 μm PP filter membrane to obtain a double-sided printing textile pigment ink.

[0087] Comparative Example 2

[0088] 22g of water, 16.7g of diethylene glycol, 2g of N-methylpyrrolidone, 18g of Shenyang Chemical Research Institute 101 resin, 11g of BL-935 blocked curing agent, 30g of color paste and 0.3g of Hydropalat WE 110 wetting agent were mixed and stirred at a speed of 300r / min for 1h. After the stirring, the mixture was filtered with a 0.45μmPP filter membrane to obtain a double-sided printing textile pigment ink.

[0089] Comparative Example 3

[0090] 26.5 g of water, 16 g of polyethylene glycol 200, 5 g of N-methylpyrrolidone, 15 g of Shenyang Chemical Research Institute 110 resin, 12 g of ZS-835 blocked curing agent, 25 g of color paste and 0.5 g of BYK DISPERBYK 2012 wetting agent were mixed and stirred at a speed of 300 r / min for 1 h. After the stirring, the mixture was filtered with a 0.45 μm PP filter membrane to obtain a double-sided printing textile pigment ink.

[0091] Comparative Example 4

[0092] 20.5 g of water, 16 g of 1,3-propylene glycol, 5 g of 2-pyrrolidone, 15 g of Hefei Ruipin 831 polyurethane resin, 14 g of ZS-1890D blocked curing agent, 26 g of color paste and 0.5 g of DISPERBYK 180 wetting agent were mixed and stirred at a speed of 300 r / min for 1 h. After the stirring, the mixture was filtered with a 0.45 μm PP filter membrane to obtain a double-sided printing textile pigment ink.

[0093] Comparative Example 5

[0094] 18.5 g of water, 14 g of 1,6-hexanediol, 7 g of 2-pyrrolidone, 20 g of Hefei Ruipin 801 polyurethane resin, 13 g of YC-2820 blocked curing agent, 27 g of color paste and 0.5 g of BYKDISPERBYK 192 wetting agent were mixed and stirred at a speed of 300 r / min for 1 h. After the stirring, the mixture was filtered with a 0.45 μm PP filter membrane to obtain a double-sided printing textile pigment ink.

[0095] Comparative Example 6

[0096] 12.5 g of water, 17 g of diethylene glycol, 6 g of 2-pyrrolidone, 21 g of Guangzhou Guanzhi 8120 polyurethane resin, 15 g of WH-1993 blocked curing agent, 28 g of color paste and 0.5 g of BYKDISPERBYK 102 wetting agent were mixed and stirred at a speed of 300 r / min for 1 h. After the stirring, the mixture was filtered with a 0.45 μm PP filter membrane to obtain a double-sided printing textile pigment ink.

[0097] The double-sided printing textile pigment ink prepared in Examples 1 to 6 and Comparative Examples 1 to 6 was added to an ink cartridge, and digital printing was performed under the conditions of an ambient temperature of 25° C. and a humidity of 50%. The digital textile pigment ink was printed on the fabric using a double-sided synchronous digital printing printer equipped with a Kyocera KJ4B-0300 printhead, and the printed fabric product was placed in a color fixing machine for high-temperature color fixing at a temperature of 160° C. for 2 minutes to obtain a final product for testing. The test method for color fastness to rubbing is: test and evaluate according to GB / T3920-2008; the test method for color fastness to soaping is: test and evaluate according to GB / T3921-2008, the test temperature is 60℃, and the test time is 30min; the test method for softness is: using the hand touch method, in an environment with a temperature of 25℃ and a humidity of 50%, 5 testers touch the sample and give the test rating results according to the soft, softer, medium, harder, and hard feel. The test ratings from hard to soft are 5, 4, 3, 2, and 1, and one and a half levels are added in every two levels, namely 4-5, 3-4, 2-3, and 1-2. The test results are valid when three or more people agree on the test results, otherwise retest; the test method for particle size D50 is: take a small amount of ink, dilute it to 300-500cps with distilled water, place it in a cuvette for testing, and test five sets of data in parallel at 25℃ to get the average value; the test method for filterability is: take 100mL of color paste, filter it with 0.45μm glass fiber membrane at 25℃ and 0.8MPa, and record the filtration time to measure the filtration performance of the ink sample; the test method for thermal storage stability is: take 500mL of ink and seal it in a sample bottle, place it in a 60℃ environment for 7 days, take it out and test various physical and chemical indicators, and the indicator change is within 10% to be qualified. The test results are shown in Table 1.

[0098] Table 1 Performance results of coatings prepared using double-sided printing textile pigment inks of Examples 1 to 6 and Comparative Examples 1 to 6

[0099]

[0100]

[0101] As can be seen from the above embodiments, the present invention provides a modified silicone resin, a double-sided printing textile pigment ink and a preparation method thereof, wherein a solvent, a hydrogenated silicone oil, a modifier and a polymerization inhibitor are mixed, a catalyst is added after mixing to react, and the solvent is removed in vacuo after the reaction is completed to obtain a modified silicone resin; then water, an aqueous solvent, a wetting agent, a resin, a modified silicone resin and a color paste are mixed, filtered, and a double-sided printing textile pigment ink is obtained. The modified silicone resin prepared by the present invention is obtained by a silylation reaction between a hydrogenated silicone oil and a modifier containing an unsaturated hydrophilic group, and the hydrophilic group gives the silicone resin good dispersion stability in water, so that the silicone resin has good particle size, filterability and thermal storage stability in the ink, and the silicon-oxygen bond conformation in the silicone resin has flexibility, which can have a toughening effect on the ink coating, and improve the feel of the printed product while taking into account other properties. The double-sided printing textile pigment ink prepared by the present invention does not require pre- and post-treatment of fabrics, and the process is simple; no waste water is generated during production, and production costs can be saved; the present invention has a soft hand feel, is suitable for a double-sided printing process, and does not produce sedimentation while improving the softness and hand feel; compared with traditional printing, there is no need to increase the process flow, no waste water is generated, and is environmentally friendly.

[0102] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principle of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims

1. A modified silicone resin, characterized in that: The structural formula of the modified silicone resin is: Wherein, m and n are independently 1 to 10, R1 and R2 are independently -CH3, an unsaturated polyether compound group, an unsaturated amino compound group, an unsaturated carboxyl compound group or an unsaturated carboxyl compound derivative group, and R3 is an unsaturated polyether compound group, an unsaturated amino compound group, an unsaturated carboxyl compound group or an unsaturated carboxyl compound derivative group.

2. The modified silicone resin according to claim 1, characterized in that The unsaturated polyether compound group includes allyl polyoxyethylene ether, allyl polyoxyethylene polyoxypropylene ether or allyl glycidyl ether; The unsaturated amino compound group includes allylamine, allylpiperazine, acrylamide or N,N-dimethylacrylamide; The unsaturated carboxyl compound group includes acrylic acid or p-vinylbenzoic acid.

3. A method for preparing the modified silicone resin according to claim 1 or 2, characterized in that: 10 to 18 parts of solvent, 35 to 45 parts of hydrogenated silicone oil, 30 to 50 parts of modifier and 1 to 3 parts of polymerization inhibitor are mixed, and then 1 to 3 parts of catalyst are added to react. After the reaction is completed, the solvent is removed in vacuo to obtain a modified silicone resin.

4. The method for preparing the modified silicone resin according to claim 3, characterized in that: The modifier comprises one or more of allyl polyoxyethylene ether, allyl polyoxyethylene polyoxypropylene ether, allyl glycidyl ether, allyl amine, allyl piperazine and acrylic acid; the hydrogen content of the hydrogen-containing silicone oil is 0.01%-20%; the solvent comprises toluene or xylene; the inhibitor comprises hydroquinone; and the catalyst comprises chloroplatinic acid solution.

5. The method for preparing the modified silicone resin according to claim 3 or 4, characterized in that: The mixing is carried out during stirring, the stirring speed is 200-400 r / min, and the stirring temperature is 80-90° C.; The reaction temperature is 120-140° C., and the reaction time is 1-5 hours.

6. A double-sided printing textile pigment ink, characterized in that: It is composed of the following components in parts by weight:

7. The double-sided printing textile pigment ink according to claim 6, characterized in that: The aqueous solvent includes one or more of ethanol, n-propanol, isopropanol, n-butanol, ethylene glycol, 1,3-propylene glycol, 1,4-butanediol, 1,6-hexanediol, diethylene glycol, triethylene glycol, polyethylene glycol 200, polyethylene glycol 400, polyethylene glycol 600, diethylene glycol, glycerol, pentaerythritol, 2-pyrrolidone and N-methylpyrrolidone; The resin includes one or more of Mitsui polyurethane resin 6110, Shenyang Chemical Research Institute polyurethane resin 101, Shenyang Chemical Research Institute polyurethane resin 110, Hefei Ruipin polyurethane resin 831, Hefei Ruipin polyurethane resin 801, Guangzhou Guanzhi polyurethane resin 8120 and Hefei Huayue New Material 8001B-2.

8. The double-sided printing textile pigment ink according to claim 6 or 7, characterized in that: The closed curing agent includes one or more of Shanghai Bolino BL-8119 closed curing agent, Shanghai Bolino BL-935 closed curing agent, Guangzhou Zengmao Chemical ZS-835 closed curing agent, ZS-1890D closed curing agent, Anhui Yuanchen YC-2820 closed curing agent, Guangzhou Haoyi WH-1993 closed curing agent and Guangzhou Haoyi WH-3192 closed curing agent; The color paste includes a nano pigment color paste with good dispersion stability and a particle size D50 of 100-130nm; The wetting agent includes an organic silicon wetting agent, and the organic silicon wetting agent includes one or more of Hydropalat WE 3323, Hydropalat WE 3322, Hydropalat WE 110, Hydropalat WE 120, BYK DISPERBYK 2012, BYK DISPERBYK 180, BYK DISPERBYK 2010, BYK DISPERBYK 2055, BYK DISPERBYK 190, BYK DISPERBYK 192, BYK DISPERBYK 182 and BYK DISPERBYK 102.

9. A method for preparing a double-sided printing textile pigment ink according to any one of claims 6 to 8, characterized in that: Water, aqueous solvent, wetting agent, resin, modified silicone resin and color paste are mixed and filtered to obtain double-sided printing textile pigment ink.

10. The method for preparing double-sided printing textile pigment ink according to claim 9, characterized in that: The mixing is carried out during stirring, the stirring speed is 250-350 r / min, and the stirring time is 0.5-2 h.

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