A slurry and its preparation process and application method

Through the combination of crosslinked amino silicon acrylic emulsion and reactive dye, the problem of insufficient breaking strength and pollution during dyeing of denim warp yarns is solved, the dyeing depth and finishing effect are improved, and an environmentally friendly dyeing process is realized.

CN119083202BActive Publication Date: 2025-01-14FOSHAN NANHAI YIMIAN DYEING & WEAVING CO LTD
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Patent Information

Application Number
CN202411577723.8
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-11-07
Publication Date
2025-01-14
Estimated Expiration
2044-11-07

AI Technical Summary

Technical Problem

In the existing denim warp yarn dyeing process, the yarn breaking strength and low weaving performance lead to poor warp breakage, wear and color fastness. The traditional sizing process leads to wastewater pollution and waste of resources, and self-crosslinked polyacrylate emulsion Inadequate finishing and water resistance lead to rough surface of the yarn and insufficient dyeing depth.

Method used

The combination of crosslinked amino silicon acrylic emulsion with reactive dyes and dye-promoting agents is used to prepare the slurry by copolymerization of the emulsion to form a paint film with good finishing and water resistance, reduce yarn friction, improve dyeing depth, color paste and fibers The bond strength.

Benefits of technology

It improves the yarn surface finishing effect, reduces the number of yarn hairs, improves the feel and dyeing depth of fabrics, reduces wastewater discharge and resource waste, and enhances dyeing fastness.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention discloses a slurry and a preparation process and application method thereof, and relates to the technical field of textile dyes, a slurry, including 160-180 parts of cross-linked aminosilicone acrylic emulsions, 8-12 parts of color paste dyes, 2-4 parts of accelerators, 1.8-2 parts of emulsifying dispersants and 0.08-0.1 parts of defoamers, wherein the cross-linked aminosilicone acrylic emulsion is prepared by emulsion copolymerization of acrylate monomers and aminosilicone oil modified monomers, and the aminosilicone oil modified monomers are prepared by reacting terminal amino silicone oil, terminal allyl epoxy polyether and p-vinyl aniline, the color paste dyes specifically select active dyes containing vinyl sulfone groups, and the accelerator is an alkaline accelerator. By mixing the cross-linked aminosilicone acrylic emulsion with auxiliary agents such as active dyes and alkaline accelerators to form a slurry, the slurry can not only effectively reduce the number of yarn surface hairiness, improve the yarn surface state and fabric feel, but also has good color fastness and dyeing depth.
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Description

Technical Field

[0001] The invention relates to the technical field of textile dyes, in particular to a slurry and a preparation process and an application method thereof. Background Art

[0002] With the development of textile printing and dyeing technology, more and more blended fibers (such as polyester / cotton, cotton / viscose, etc.) and new fibers have appeared, and various dyed denim warp yarns have developed rapidly, resulting in an increase in the variety and color of denim warp yarns. At present, there are many kinds of denim fabrics with rich colors available for consumers to choose from on the market.

[0003] In terms of production technology, the textile printing and dyeing process of denim usually includes warp dyeing, sizing, weaving, desizing, finishing and other processes. Among them, the warp dyeing mainly uses traditional indigo dyes to dye the denim warp yarns, and sometimes some sulfur dyes or other reducing dyes are also used. However, due to the insufficient strength and low weaving performance of the denim warp yarns, the denim blended warp yarns are prone to breakage, wear, and low color fastness in the subsequent weaving process. Therefore, in order to improve the breaking strength and wear resistance of the yarn and reduce breakage, the traditional process requires sizing of the warp yarns before weaving (the sizing rate of modified starch in the traditional process is about 8% to 10%) to meet the strength and requirements of the denim warp yarns during weaving. Since the sizing on the yarn sized by the traditional sizing process will bring difficulties to the functional finishing processing after weaving after film formation, the yarn must be desized after weaving. However, the desizing process will also bring about problems such as waste water discharge polluting the environment (pollution of all desizing sizing and part of the bleached dyes) and waste of resources and energy.

[0004] The Chinese invention patent application with publication number CN103194917A discloses a one-step dyeing and weaving desizing-free self-crosslinking acrylic emulsion slurry for denim blended warp yarn and its preparation method. The low-temperature self-crosslinking function of the slurry (the slurry after compounding the color paste) can improve the adhesion of the coloring component on various fibers of the denim blended warp yarn. The dyeing and sizing of the denim warp yarn can be achieved in just one step, which not only ensures that the denim warp yarn has certain weaving performance, but also does not require desizing after weaving, solving the problems of wastewater discharge pollution and waste of resources and energy caused by sizing and desizing processes.

[0005] However, it was found in actual applications that the finishing and water resistance of the self-crosslinking polyacrylate emulsion after crosslinking and curing were not satisfactory, so that the coating formed during the dyeing and sizing of the denim warp yarn did not provide sufficient protection for the yarn. In addition, the yarn separation rollers and yarn collection equipment would cause greater friction to the dyed yarn, which would lead to more yarn hairiness. After being woven into denim fabric, its surface was relatively rough, and the yarn dyeing rate was not high, the dyeing depth was insufficient, and the surface dyeing was lighter after being woven into denim fabric. Summary of the invention

[0006] In order to further improve the performance of dyeing slurry, improve the finishing effect of slurry on denim warp yarn, overcome surface quality problems such as excessive hairiness after dyeing and rough surface of denim after weaving, and at the same time improve the dye uptake of slurry and increase dyeing depth, the application provides a slurry and its preparation process and application method.

[0007] In the first aspect, the present application provides a slurry, which adopts the following technical solution:

[0008] A slurry comprising the following raw materials in parts by weight:

[0009] Cross-linked amino silicone acrylic emulsion: 160-180 parts;

[0010] Color paste dye: 8-12 parts;

[0011] Dyeing accelerator: 2-4 parts;

[0012] Emulsifying dispersant: 1.8-2 parts;

[0013] Defoaming agent: 0.08-0.1 parts;

[0014] Among them, the cross-linked aminosilicone acrylic emulsion is prepared by emulsion copolymerization of acrylate monomers and aminosilicone oil modified monomers, and the aminosilicone oil modified monomer uses terminal amino silicone oil as a silicon source, and is prepared by reacting terminal allyl epoxy polyether and p-vinylaniline; the reactive dye specifically uses a reactive dye containing a vinyl sulfone group, and the dyeing accelerator includes at least one of sodium sulfate, sodium carbonate, sodium phosphate or sodium hydroxide mixed with sodium chloride.

[0015] By adopting the above technical scheme, using terminal amino silicone oil as a silicon source, cooperating with terminal allyl epoxy polyether and p-vinyl aniline to obtain amino silicone oil modified monomer, and then copolymerizing with acrylate monomers to obtain cross-linked amino silicone acrylic emulsion through emulsion polymerization, and mixing with active dyes and accelerators to make slurry, compared with the prior art, the paint film formed after the slurry is cured has good finishing and water resistance, can effectively smooth the surface of the denim warp yarn, and reduce the friction effect of the yarn separation roller or yarn collection equipment on the yarn, so as to reduce the number of hairiness on the yarn surface, and improve the surface state of the yarn and the feel of the fabric. At the same time, through the cooperation of the active dye containing vinyl sulfone group and the alkaline accelerator, not only good leveling property is shown in the dyeing process, but also the directional adsorption and combination between the active dye and the fiber is promoted, and the bonding strength between the color paste dye and the fiber is improved, and the paint film formed by cross-linking and curing of the cross-linked amino silicone acrylic emulsion is conducive to further improving the color fastness and dyeing depth of the slurry.

[0016] Optionally, the cross-linked aminosilicone acrylic emulsion comprises the following raw materials in parts by weight:

[0017] Butyl acrylate: 15-20 parts;

[0018] 2-Ethylhexyl methacrylate: 5-10 parts;

[0019] Hydroxymethacrylate: 10-20 parts;

[0020] Amino silicone oil modified monomer: 20-25 parts;

[0021] Cross-linking monomer: 2-3.2 parts;

[0022] Sodium dodecyl sulfate: 2.5-4.5 parts;

[0023] Ammonium persulfate: 0.3-0.6 parts;

[0024] γ-aminopropyltriethoxysilane: 2-3 parts;

[0025] Soft water: 80-100 parts;

[0026] The hydroxy methacrylate can be selected from hydroxyethyl methacrylate and hydroxypropyl methacrylate, and the cross-linking monomer is specifically a mixture of diacetone acrylamide and adipic acid dihydrazide in a weight ratio of 1: (0.06-0.12);

[0027] The amino silicone oil modified monomer comprises the following raw materials in parts by weight:

[0028] Terminal allyl epoxy polyether: 15-20 parts;

[0029] Amino-terminated silicone oil: 4-8 parts;

[0030] p-vinylaniline: 2.5-5 parts;

[0031] Triethylamine: 0.02-0.05 parts;

[0032] The average molecular weight of the terminal allyl epoxy polyether is in the range of 450-1000, and the terminal amino silicone oil is bis(3-aminopropyl)-terminated dimethylsiloxane with an amine value of 0.4-0.6 mmol / g.

[0033] By adopting the above technical scheme, butyl acrylate, 2-ethylhexyl methacrylate and hydroxymethyl acrylate are used as acrylate monomers, aminosilicone oil modified monomers and cross-linking monomers are used to prepare aminosilicone acrylic emulsion, and finally γ-aminopropyltriethoxysilane is used as a curing agent, so that a cross-linked aminosilicone acrylic emulsion that can self-crosslink under specific conditions can be configured. After the sizing and dyeing of the slurry is completed, a soft and smooth paint film can be formed on the surface of the yarn through the cross-linking and curing of the cross-linked aminosilicone acrylic emulsion, which is beneficial for smooth finishing of the yarn surface and reducing the hairiness of the yarn surface, and is also beneficial for fully protecting the colored yarn and improving the color fastness of the slurry. Secondly, when the aminosilicone oil modified monomer is selected from terminal allyl epoxy polyether with an average molecular weight in the range of 450-1000 and bis(3-aminopropyl)-terminated dimethylsiloxane with an amino value of 0.4-0.6mmol / g, the cross-linked aminosilicone acrylic emulsion formed has good softness and smoothness of the paint film after curing, and can also reduce the possibility of yellowing of the yarn after coloring, which is conducive to further improving the finishing effect of the slurry.

[0034] Optionally, the preparation method of the aminosilicone oil modified monomer comprises the following steps:

[0035] First, preliminarily mix the terminal allyl epoxy polyether and the terminal amino silicone oil, then increase the temperature to 65-72°C and start stirring for 150-200 minutes, then add p-vinylaniline and triethylamine, increase the temperature to 75-80°C again and continue stirring and reacting for 60-90 minutes to obtain the amino silicone oil modified monomer.

[0036] By adopting the above technical scheme, the epoxy group in the terminal allyl epoxy polyether is first reacted with the amino group in the terminal amino silicone oil to undergo an epoxy ring-opening reaction, and then reacted with p-vinylaniline and triethylamine, which is beneficial for preparing an amino silicone oil-modified monomer that is not easily hydrolyzed and oxidized, and further beneficial for improving the stability of the cross-linked amino silicone acrylic emulsion.

[0037] Optionally, the preparation method of the cross-linked amino silicone acrylic emulsion comprises the following steps:

[0038] A1. 40% by weight of soft water, 40% by weight of sodium lauryl sulfate and 20% by weight of ammonium persulfate are stirred and mixed to obtain a pre-emulsified base liquid; 10% by weight of soft water and the remaining ammonium persulfate are stirred and mixed to obtain an initiating solution; amino silicone oil modified monomer, butyl acrylate, 2-ethylhexyl methacrylate, hydroxymethyl acrylate, crosslinking monomer and the remaining sodium lauryl sulfate and soft water are stirred and mixed to obtain a mixed monomer liquid;

[0039] A2. Add 10% by weight of the mixed monomer liquid to the pre-emulsified base liquid at one time, heat to 78-82°C and stir continuously. When the emulsion starts to turn slightly blue, slowly add the remaining mixed monomer liquid to the pre-emulsified base liquid, and add the initiator solution once every 0.5h. Control the amount added each time so that the mixed monomer liquid and the initiator solution can be added within 2.5-3h. Stir continuously during the reaction and keep the temperature constant. After the addition is completed, raise the temperature to 83-85°C and keep warm for 1h.

[0040] A3. After the heat preservation is completed, the temperature is naturally lowered to 37-40°C, γ-aminopropyltriethoxysilane is added, stirred for 3-5 minutes, and then the pH value is adjusted to between 7 and 9 with ammonia water to obtain a cross-linked aminosilicone acrylic emulsion.

[0041] By adopting the above technical scheme, the aminosilicone oil modified monomer is grafted onto the acrylic ester emulsion by emulsion copolymerization to form a cross-linked aminosilicone acrylic emulsion, which is not only beneficial to improve the stability of the cross-linked aminosilicone acrylic emulsion, so that it has good film-forming properties and is not prone to hydrolysis or demulsification, but also enables the acrylic ester emulsion to have the excellent characteristics of terminal amino silicone oil, which is beneficial to improve the finishing and water resistance of the slurry, and is beneficial to improve the finishing and coloring effects of the slurry.

[0042] Optionally, the reactive dye is specifically a B-type reactive dye, and the dyeing accelerator is specifically selected from sodium chloride, sodium carbonate and sodium hydroxide mixed in a weight ratio of 10: (0.8-1): 0.2.

[0043] By adopting the above technical solution, the alkaline environment created by the dyeing accelerator has excellent dyeing and fixing effects on B-type reactive dyes, which is beneficial to further improve the color fastness and dyeing depth of the slurry.

[0044] Optionally, the emulsifying dispersant is a mixture of sodium lignin sulfonate and triethanolamine in a weight ratio of 1: (0.15-0.25).

[0045] By adopting the above technical scheme, sodium lignin sulfonate and triethanolamine can produce a synergistic effect, which can not only make the color paste dye fully dispersed in the cross-linked amino silicone acrylic emulsion, reduce the agglomeration of the color paste dye, which is beneficial to improve the levelness of the slurry, but also further improve the water resistance of the slurry, which is beneficial to improve the color fastness of the yarn under wet friction.

[0046] Optionally, the defoaming agent is a mixture of any one or more of SAG 672 or SAG 622.

[0047] In the second aspect, the present application provides a slurry preparation process, which adopts the following technical solution:

[0048] A slurry preparation process comprises the following steps:

[0049] First, the cross-linked aminosilicone acrylic emulsion, emulsifying dispersant and defoaming agent are mixed in proportion, heated to 60-63° C. and stirred for not less than 60 minutes, and then a preliminary slurry is obtained after cooling, and the slurry is sealed and stored separately from light with the color paste dye and the dyeing accelerator; before the denim warp yarn needs to be pad-dyed, the preliminary slurry is stirred and mixed with the color paste dye and the dyeing accelerator in sequence to obtain a slurry.

[0050] By adopting the above technical solution, it is beneficial to obtain a slurry with uniform mixing and good performance. In addition, the mixed prepared slurry is stored separately from the color paste dye and the dyeing accelerator, and then mixed in sequence as needed before use, which can effectively prevent the high alkaline environment provided by the dyeing accelerator from gradually hydrolyzing the cross-linked aminosilicone acrylic emulsion or the color paste dye during storage, or causing the cross-linked aminosilicone acrylic emulsion to self-crosslink, thereby helping to increase the storage time of the slurry and extend the effectiveness of the slurry.

[0051] In a third aspect, the present application provides a method for applying a slurry, which adopts the following technical solution:

[0052] A slurry application method comprises the following steps:

[0053] B1. Dilute and mix the slurry with soft water in a weight ratio of 1:2, then add the diluted slurry into the slurry tank of the slurry-dyeing machine, send the washed and dried denim warp yarn into the slurry-dyeing machine, and perform slurry-dyeing through a 2-dipping 2-rolling dyeing process, wherein in the first dipping and rolling, the slurry is a mixture of the preparatory slurry and the color paste dye, and in the second dipping and rolling, the slurry is a mixture of the preparatory slurry, the color paste dye and the dyeing accelerator, so that the denim warp yarn can be fully coated and colored by the slurry, and then heated and dried to obtain the preliminarily colored denim warp yarn;

[0054] B2. Dilute and mix the prepared slurry without adding color paste dye and accelerator with soft water in a weight ratio of 1:1, then add the diluted prepared slurry into the slurry tank, and perform color fixing and protection treatment on the denim warp yarn that has been initially colored through a dyeing process of 1 dipping and 1 padding, so that the denim warp yarn can be fully covered by the prepared slurry. After heating and drying, let it stand at room temperature for at least 12 hours, and then you can get the denim warp yarn that has been dyed and fixed by slurry.

[0055] Among them, in the "2 dips and 2 rolls" dyeing process of step B1 and the "1 dip and 1 roll" dyeing process of step B2, dipping refers to the process of completely immersing the denim warp yarn in the slurry. This process allows the denim warp yarn to fully absorb the slurry in the slurry tank and lays the foundation for subsequent processing. Rolling refers to quickly passing the denim warp yarn soaked in the slurry through two sets of rollers for squeezing. This process allows the denim warp yarn to remove excess slurry and allow the slurry to fully adhere to the denim warp yarn.

[0056] By adopting the above technical scheme, in the first impregnation process, a slurry with color paste dye added is used. At this time, the color paste dye has good diffusivity and can be evenly adsorbed on the yarn surface under the action of the emulsion and fully diffused inside the yarn, which is beneficial to improving the dyeing rate and levelness of the slurry; in the second impregnation, since the air in the yarn is fully discharged when passing through the roller for the first time and a negative pressure is formed inside the yarn, the slurry can be fully absorbed in the second impregnation, and the slurry used in the second impregnation is added with a dyeing accelerator, which can fully penetrate into the fiber with the slurry to dye the color paste. The material and the fiber fully react and combine, and the cross-linked aminosilicone acrylic emulsion undergoes self-cross-linking under the roller and high-temperature drying to form a paint film, so that the color paste dye can fully adhere to the yarn; and the third dipping and rolling can coat a layer of transparent cross-linked aminosilicone acrylic emulsion without color paste dye on the surface of the yarn, which can not only re-arrange the yarn, but also protect the underlying colored paint film, and can effectively reduce the friction damage of the yarn separation roller and the yarn collection equipment to the colored paint film, which is beneficial to improve the color fastness of the slurry, and also improve the yarn strength, which is beneficial to further improve the weaving efficiency.

[0057] Optionally, in the 2-immersion 2-rolling paddle dyeing treatment in step B1, the slurry temperature needs to be controlled not higher than 30°C, the roller temperatures of the first group of rollers and the second group of rollers are set to 50-55°C, and the drying temperature is set to 105-110°C; in the 1-immersion 1-rolling color fixing protection treatment in step B2, the temperature of the prepared slurry needs to be controlled not higher than 50°C, the roller temperatures of the rollers are set to 65-70°C, and the drying temperature is set to 105-110°C.

[0058] By adopting the above technical scheme, a lower temperature is used in the first two padding processes, which is beneficial to improving the dyeing effect of the slurry on the denim warp yarn, so that the color paste dye can be fully dispersed on the fiber and combined with the fiber. In the third padding process, increasing the padding temperature is beneficial to preheating and promoting the curing of the slurry, so that the cross-linked amino silicone acrylic emulsion can evenly and quickly form a protective paint film, which is beneficial to improving the slurry finishing effect.

[0059] In summary, the technical solution of this application has at least one of the following beneficial effects:

[0060] 1. By using terminal amino silicone oil as a silicon source, terminal allyl epoxy polyether and p-vinylaniline are reacted to obtain amino silicone oil modified monomers, and then cross-linked amino silicone acrylic emulsion is obtained by emulsion polymerization and copolymerization with acrylate monomers. The emulsion is mixed with auxiliary agents such as reactive dyes and dyeing accelerators to form a slurry. The slurry can effectively smooth the surface of the denim warp yarn and reduce the friction effect of the yarn separation roller or yarn collection equipment on the yarn, which is beneficial to reduce the amount of hairiness on the yarn surface and improve the surface state of the yarn and the feel of the fabric.

[0061] 2. Through the cooperation of active dyes containing vinyl sulfone groups and alkaline dyeing accelerators, not only good level dyeing is exhibited during the dyeing process, but also the directional adsorption and combination between the active dyes and the fibers are promoted, thereby improving the bonding strength between the color paste dye and the fibers. Combined with the paint film formed by cross-linking and curing of the cross-linked aminosilicone acrylic emulsion, it is beneficial to further improve the color fastness and dyeing depth of the slurry. DETAILED DESCRIPTION

[0062] The present application is further described in detail below in combination with preparation examples, embodiments and comparative examples.

[0063] Preparation Example

[0064] [Preparation Example 1-1]

[0065] An amino silicone oil modified monomer is prepared by the following preparation steps:

[0066] First, 20 kg of terminal allyl epoxy polyether and 8 kg of terminal amino silicone oil were preliminarily mixed, and then the temperature was raised to 70 ° C and stirring began for 150 minutes. Then, 3 kg of p-vinylaniline and 0.03 kg of triethylamine were added at the same time, and the temperature was raised to 80 ° C again and the stirring reaction was continued for 60 minutes to obtain an amino silicone oil modified monomer.

[0067] The terminal allyl epoxy polyether is KL-11 produced by Cologne Chemicals, and its average molecular weight is about 400; the terminal amino silicone oil is bis(3-aminopropyl)-terminated dimethylsiloxane having an amino value of 0.6.

[0068] [Preparation Example 1-2]

[0069] An amino silicone oil modified monomer is prepared by the following preparation steps:

[0070] First, 20 kg of terminal allyl epoxy polyether and 6 kg of terminal amino silicone oil were preliminarily mixed, and then the temperature was raised to 65 ° C and stirring was started for 200 minutes. Then, 5 kg of p-vinylaniline and 0.05 kg of triethylamine were added at the same time, and the temperature was raised to 75 ° C again and the stirring reaction was continued for 90 minutes to obtain an amino silicone oil modified monomer.

[0071] The terminal allyl epoxy polyether is specifically selected from KL-11 of Cologne Chemicals, which has an average molecular weight of about 400; the terminal amino silicone oil is specifically selected from bis(3-aminopropyl)-terminated dimethylsiloxane with an amino value of 1.

[0072] [Preparation Example 1-3]

[0073] An amino silicone oil modified monomer is prepared by the following preparation steps:

[0074] First, 15 kg of terminal allyl epoxy polyether and 4 kg of terminal amino silicone oil were preliminarily mixed, and then the temperature was raised to 70 ° C and stirring was started for 200 minutes. Then, 2.5 kg of p-vinylaniline and 0.02 kg of triethylamine were added at the same time, and the temperature was raised to 75 ° C again and the stirring reaction was continued for 90 minutes to obtain an amino silicone oil modified monomer.

[0075] The terminal allyl epoxy polyether is KL-986 produced by Cologne Chemicals, and its average molecular weight is about 1000; the terminal amino silicone oil is bis(3-aminopropyl)-terminated dimethylsiloxane having an amino value of 0.4.

[0076] [Preparation Example 1-4]

[0077] An amino silicone oil modified monomer, which is different from [Preparation Example 1-1] in that the molecular weight of the terminal allyl epoxy polyether is different.

[0078] In this preparation example, the terminal allyl epoxy polyether is specifically selected from KL-986 of Cologne Chemicals, and its average molecular weight is about 1000.

[0079] [Preparation Example 1-5]

[0080] An amino silicone oil modified monomer, which differs from [Preparation Example 1-4] in that the amino value of the terminal amino silicone oil is different.

[0081] In this preparation example, the amino-terminated silicone oil is specifically selected from bis(3-aminopropyl)-terminated dimethylsiloxane having an amino value of 0.4.

[0082] [Preparation Example 1-6]

[0083] An amino silicone oil modified monomer, which differs from [Preparation Example 1-4] in that the amino value of the terminal amino silicone oil is different.

[0084] In this preparation example, the amino-terminated silicone oil is specifically selected from bis(3-aminopropyl)-terminated dimethylsiloxane having an amino value of 1.

[0085] [Preparation Example 2-1]

[0086] A cross-linked amino silicone acrylic emulsion, comprising the following raw materials:

[0087] 20kg butyl acrylate, 5kg 2-ethylhexyl methacrylate, 15kg hydroxyethyl methacrylate, 25kg amino silicone oil modified monomer, 2.2kg cross-linking monomer, 3kg sodium dodecyl sulfonate, 0.4kg ammonium persulfate, 2.5kg γ-aminopropyltriethoxysilane and 100kg soft water.

[0088] Among them, the amino silicone oil modified monomer is specifically selected from an amino silicone oil modified monomer prepared in [Preparation Example 1-1], and the cross-linking monomer is specifically a mixture of diacetone acrylamide and adipic acid dihydrazide in a weight ratio of 1:0.1, that is, the cross-linking monomer includes 2kg of diacetone acrylamide and 0.2kg of adipic acid dihydrazide.

[0089] A method for preparing a cross-linked aminosilicone acrylic emulsion comprises the following steps:

[0090] A1. First, 40% by weight of soft water, 40% by weight of sodium lauryl sulfate and 20% by weight of ammonium persulfate are stirred and mixed to obtain a pre-emulsified base liquid; 10% by weight of soft water and the remaining weight of ammonium persulfate are stirred and mixed to obtain an initiating solution; amino silicone oil modified monomer, butyl acrylate, 2-ethylhexyl methacrylate, hydroxyethyl methacrylate, crosslinking monomer and the remaining weight of sodium lauryl sulfate and soft water are stirred and mixed to obtain a mixed monomer liquid;

[0091] A2. Add 10% by weight of the mixed monomer liquid to the pre-emulsified base liquid at one time, heat to 78°C and continue stirring. When the emulsion begins to turn slightly blue, slowly add the remaining mixed monomer liquid to the pre-emulsified base liquid, and add the initiator solution once every 0.5h. Control the amount added each time so that the mixed monomer liquid and the initiator solution can be added within 3h. Stir continuously during the reaction and keep the temperature constant. After the addition is completed, raise the temperature to 83°C and keep warm for 1h.

[0092] A3. After the heat preservation is completed, the temperature is naturally lowered to about 40°C, γ-aminopropyltriethoxysilane is added, and it is stirred for 3 minutes to mix, and then the pH value is adjusted to between 7 and 9 with ammonia water to obtain a cross-linked aminosilicone acrylic emulsion.

[0093] [Preparation Example 2-2]

[0094] A cross-linked amino silicone acrylic emulsion, comprising the following raw materials:

[0095] 15kg butyl acrylate, 10kg 2-ethylhexyl methacrylate, 20kg hydroxypropyl methacrylate, 25kg amino silicone oil modified monomer, 3.2kg cross-linking monomer, 4.5kg sodium dodecyl sulfonate, 0.6kg ammonium persulfate, 3kg γ-aminopropyltriethoxysilane and 80kg soft water.

[0096] Among them, the amino silicone oil modified monomer is specifically selected from an amino silicone oil modified monomer prepared in [Preparation Example 1-2], and the cross-linking monomer is specifically a mixture of diacetone acrylamide and adipic acid dihydrazide in a weight ratio of 1:0.06, that is, the cross-linking monomer includes 3.02kg of diacetone acrylamide and 0.18kg of adipic acid dihydrazide.

[0097] A method for preparing a cross-linked aminosilicone acrylic emulsion comprises the following steps:

[0098] A1. First, 40% by weight of soft water, 40% by weight of sodium lauryl sulfate and 20% by weight of ammonium persulfate are stirred and mixed to obtain a pre-emulsified base liquid; 10% by weight of soft water and the remaining weight of ammonium persulfate are stirred and mixed to obtain an initiating solution; amino silicone oil modified monomer, butyl acrylate, 2-ethylhexyl methacrylate, hydroxyethyl methacrylate, crosslinking monomer and the remaining weight of sodium lauryl sulfate and soft water are stirred and mixed to obtain a mixed monomer liquid;

[0099] A2. Add 10% by weight of the mixed monomer liquid to the pre-emulsified base liquid at one time, heat to 82°C and continue stirring. When the emulsion begins to turn slightly blue, slowly add the remaining mixed monomer liquid to the pre-emulsified base liquid, and add the initiator solution once every 0.5h. Control the amount added each time so that the mixed monomer liquid and the initiator solution can be added within 2h. Stir continuously during the reaction and keep the temperature constant. After the addition is completed, raise the temperature to 85°C and keep warm for 1h.

[0100] A3. After the heat preservation is completed, the temperature is naturally lowered to about 37°C, γ-aminopropyltriethoxysilane is added, and it is stirred for 5 minutes to mix, and then the pH value is adjusted to between 7 and 9 with ammonia water to obtain a cross-linked aminosilicone acrylic emulsion.

[0101] [Preparation Example 2-3]

[0102] A cross-linked amino silicone acrylic emulsion, which differs from [Preparation Example 2-1] in that the added raw materials and the added amounts are different. In this preparation example, the following raw materials are included:

[0103] 15kg butyl acrylate, 5kg 2-ethylhexyl methacrylate, 10kg hydroxyethyl methacrylate, 20kg amino silicone oil modified monomer, 2kg cross-linking monomer, 2.5kg sodium dodecyl sulfonate, 0.3kg ammonium persulfate, 2kg γ-aminopropyltriethoxysilane and 80kg soft water.

[0104] Among them, the amino silicone oil modified monomer is specifically selected from an amino silicone oil modified monomer prepared in [Preparation Example 1-3], and the cross-linking monomer is specifically a mixture of diacetone acrylamide and adipic acid dihydrazide in a weight ratio of 1:0.12, that is, the cross-linking monomer includes 1.79 kg of diacetone acrylamide and 0.21 kg of adipic acid dihydrazide.

[0105] [Preparation Example 2-4]

[0106] A cross-linked aminosilicone acrylic emulsion, which differs from [Preparation Example 2-1] in that the aminosilicone oil-modified monomer is different.

[0107] In this preparation example, the aminosilicone oil-modified monomer is specifically selected from an aminosilicone oil-modified monomer prepared in [Preparation Example 1-4].

[0108] [Preparation Example 2-5]

[0109] A cross-linked aminosilicone acrylic emulsion, which differs from [Preparation Example 2-1] in that the aminosilicone oil-modified monomer is different.

[0110] In this preparation example, the aminosilicone oil-modified monomer is specifically selected from an aminosilicone oil-modified monomer prepared in [Preparation Example 1-5].

[0111] [Preparation Example 2-6]

[0112] A cross-linked aminosilicone acrylic emulsion, which differs from [Preparation Example 2-1] in that the aminosilicone oil-modified monomer is different.

[0113] In this preparation example, the aminosilicone oil-modified monomer is specifically selected from an aminosilicone oil-modified monomer prepared in [Preparation Example 1-6].

[0114] [Preparation Example 3-1]

[0115] A polyacrylate emulsion, which differs from [Preparation Example 2-1] in that no amino silicone oil modified monomer is added, and the amino silicone oil modified monomer is replaced with butyl acrylate, 2-ethylhexyl methacrylate and hydroxyethyl methacrylate according to the mixing ratio. Specifically, the following raw materials are included:

[0116] 32.5 kg butyl acrylate, 8.125 kg 2-ethylhexyl methacrylate, 24.375 kg hydroxyethyl methacrylate, 2.2 kg crosslinking monomer, 3 kg sodium dodecyl sulfonate, 0.4 kg ammonium persulfate, 2.5 kg γ-aminopropyltriethoxysilane and 100 kg soft water.

[0117] The cross-linking monomer is specifically diacetone acrylamide and adipic acid dihydrazide mixed in a weight ratio of 1:0.1, that is, the cross-linking monomer includes 2kg of diacetone acrylamide and 0.2kg of adipic acid dihydrazide.

[0118] Example

[0119] [Example 1]

[0120] A slurry comprising the following raw materials:

[0121] 165kg cross-linked amino silicone acrylic emulsion, 10kg color paste dye, 2.5kg dye accelerator, 1.8kg emulsion dispersant and 0.1kg defoaming agent.

[0122] Among them, the cross-linked aminosilicone acrylic emulsion is specifically selected from a cross-linked aminosilicone acrylic emulsion prepared in [Preparation Example 2-1]; the color paste dye is selected from type B reactive dye, specifically navy blue B-BF; the dyeing accelerator is a mixture of sodium chloride and sodium carbonate in a weight ratio of 10:1, that is, the dyeing accelerator includes 2.273kg of sodium chloride and 0.227kg of sodium carbonate; the emulsifying dispersant is a mixture of sodium lignin sulfonate and triethanolamine in a weight ratio of 1:0.25, that is, the emulsifying dispersant includes 1.44kg of sodium lignin sulfonate and 0.36kg of triethanolamine; the defoaming agent is specifically selected from SAG 672.

[0123] A slurry preparation process comprises the following steps:

[0124] First, the cross-linked aminosilicone acrylic emulsion, the emulsifying dispersant and the defoaming agent are mixed in proportion, heated to 60°C and stirred for 60 minutes, and then cooled to obtain a preliminary slurry, which is sealed and stored separately from light with the color paste dye and the dyeing accelerator; before the denim warp yarn needs to be pad-dyed, the preliminary slurry is stirred and mixed with the color paste dye and the dyeing accelerator in sequence as required to obtain a slurry.

[0125] A slurry application method comprises the following steps:

[0126] B1. Dilute and mix the slurry with soft water in a weight ratio of 1:2, then add the diluted slurry into the slurry tank of the slurry-dyeing machine, send the washed and dried denim warp yarn into the slurry-dyeing machine, and perform slurry-dyeing through the "2-immersion 2-rolling" dyeing process, wherein the "2-immersion 2-rolling" process means that the denim warp yarn needs to be immersed and rolled for the second time after one immersion and one rolling. During the first immersion and rolling, the slurry is a mixture of the preparatory slurry and the color paste dye, and the slurry temperature is controlled at 20°C. During the second immersion and rolling, the slurry is a mixture of the preparatory slurry, the color paste dye and the dyeing accelerator, and the slurry temperature is controlled at 30°C. The roller temperatures of the first group of rollers and the second group of rollers are both set to 50°C, so that the denim warp yarn can be fully coated and colored by the slurry. Finally, the oven is heated to 105°C and dried for 5 minutes to obtain the preliminarily colored denim warp yarn; yi

[0127] B2. Dilute and mix the prepared slurry without adding color paste dye and accelerator with soft water in a weight ratio of 1:1, then add the diluted prepared slurry into the slurry tank, and fix the denim warp yarn after preliminary coloring through the "1 dip 1 roll" dyeing process again, wherein "1 dip 1 roll" means that the denim warp yarn is only dipped and rolled once, the temperature of the prepared slurry is controlled at 50℃, the temperature of the roll is set to 65℃, and then it is heated and dried in a 105℃ oven for 5 minutes, and then left to stand at room temperature for at least 12 hours, and then the denim warp yarn that has been dyed and fixed by slurry can be obtained.

[0128] Among them, in the "2 dips and 2 rolls" dyeing process of step B1 and the "1 dip and 1 roll" dyeing process of step B2, dipping refers to the process of completely immersing the denim warp yarn in the slurry. This process allows the denim warp yarn to fully absorb the slurry in the slurry tank and lays the foundation for subsequent processing. Rolling refers to quickly passing the denim warp yarn soaked in the slurry through two sets of rollers for squeezing. This process allows the denim warp yarn to remove excess slurry and allow the slurry to fully adhere to the denim warp yarn.

[0129] [Example 2]

[0130] A slurry comprising the following raw materials:

[0131] 180kg cross-linked amino silicone emulsion, 12kg color paste dye, 4kg dye accelerator, 2kg emulsion dispersant and 0.1kg defoaming agent.

[0132] Among them, the cross-linked aminosilicone acrylic emulsion is specifically selected from a cross-linked aminosilicone acrylic emulsion prepared in [Preparation Example 2-2]; the color paste dye is selected from type B reactive dye, specifically navy blue B-BF; the dyeing accelerator is a mixture of sodium chloride, sodium sulfate and sodium hydroxide in a weight ratio of 10:2:0.5, that is, the dyeing accelerator includes 3.2kg of sodium chloride, 0.64kg of sodium sulfate and 0.16kg of sodium hydroxide; the emulsifying dispersant is a mixture of sodium lignin sulfonate and triethanolamine in a weight ratio of 1:0.15, that is, the emulsifying dispersant includes 1.739kg of sodium lignin sulfonate and 0.261kg of triethanolamine; the defoaming agent is specifically selected from SAG 622.

[0133] A slurry preparation process comprises the following steps:

[0134] First, the cross-linked aminosilicone acrylic emulsion, the emulsifying dispersant and the defoaming agent are mixed in proportion, heated to 63° C. and stirred for 60 minutes, and then cooled to obtain a preliminary slurry, which is sealed and stored separately from light with the color paste dye and the dyeing accelerator; before the denim warp yarn needs to be pad-dyed, the preliminary slurry is stirred and mixed with the color paste dye and the dyeing accelerator in sequence as required to obtain a slurry.

[0135] A slurry application method comprises the following steps:

[0136] B1. The prepared slurry is diluted and mixed with soft water in a weight ratio of 1:2, and then the diluted slurry is added to the slurry tank of the slurry-dyeing machine. The washed and dried denim warp yarn is sent to the slurry-dyeing machine and slurried and dyed through the "2-immersion 2-rolling" dyeing process. In the first immersion and rolling, the slurry is a mixture of the pre-slurry and the color paste dye, and the slurry temperature is controlled at 20°C. In the second immersion and rolling, the slurry is a mixture of the pre-slurry, the color paste dye and the accelerator, and the slurry temperature is controlled at 30°C. The roller temperatures of the first group of rollers and the second group of rollers are both set to 55°C, so that the denim warp yarn can be fully covered and colored by the slurry. Finally, the oven is heated to 110°C and dried for 3 minutes to obtain the denim warp yarn with preliminary coloring.

[0137] B2. Dilute and mix the prepared slurry without adding color paste dye and accelerator with soft water in a weight ratio of 1:1, then add the diluted prepared slurry into the slurry tank, and fix the denim warp yarn after preliminary coloring through the "1 dip 1 roll" dyeing process again, wherein "1 dip 1 roll" means that the denim warp yarn is only dipped and rolled once, the temperature of the prepared slurry is controlled at 50℃, the temperature of the roll is set to 70℃, and then it is heated and dried in a 110℃ oven for 3 minutes, and then left to stand at room temperature for at least 12 hours, and then the denim warp yarn that has been dyed and fixed by slurry can be obtained.

[0138] Among them, in the "2 dips and 2 rolls" dyeing process of step B1 and the "1 dip and 1 roll" dyeing process of step B2, dipping refers to the process of completely immersing the denim warp yarn in the slurry. This process allows the denim warp yarn to fully absorb the slurry in the slurry tank and lays the foundation for subsequent processing. Rolling refers to quickly passing the denim warp yarn soaked in the slurry through two sets of rollers for squeezing. This process allows the denim warp yarn to remove excess slurry and allow the slurry to fully adhere to the denim warp yarn.

[0139] [Example 3]

[0140] A slurry, which differs from [Example 1] in that the added raw materials and the added amounts are different. In this example, the slurry includes the following raw materials:

[0141] 160kg cross-linked amino silicone acrylic emulsion, 8kg color paste dye, 2kg dye accelerator, 1.5kg emulsion dispersant and 0.08kg defoaming agent.

[0142] Among them, the cross-linked aminosilicone acrylic emulsion is specifically selected from a cross-linked aminosilicone acrylic emulsion prepared in [Preparation Example 2-3]; the color paste dye is selected from type B reactive dye, specifically navy blue B-BF; the dyeing accelerator is a mixture of sodium chloride and sodium phosphate in a weight ratio of 10:1, that is, the dyeing accelerator includes 1.818kg of sodium chloride and 0.182kg of sodium phosphate; the emulsifying dispersant is a mixture of sodium lignin sulfonate and triethanolamine in a weight ratio of 1:0.2, that is, the emulsifying dispersant includes 1.25kg of sodium lignin sulfonate and 0.25kg of triethanolamine; the defoaming agent is specifically selected from SAG 672.

[0143] [Example 4]

[0144] A slurry, which is different from [Example 1] in that the cross-linked amino silicone acrylic emulsion is different.

[0145] In this embodiment, the cross-linked amino silicone acrylic emulsion is specifically selected from a cross-linked amino silicone acrylic emulsion prepared in [Preparation Example 2-4].

[0146] [Example 5]

[0147] A slurry, which is different from [Example 4] in that the cross-linked amino silicone acrylic emulsion is different.

[0148] In this embodiment, the cross-linked amino silicone acrylic emulsion is specifically selected from a cross-linked amino silicone acrylic emulsion prepared in [Preparation Example 2-5].

[0149] [Example 6]

[0150] A slurry, which is different from [Example 4] in that the cross-linked amino silicone acrylic emulsion is different.

[0151] In this embodiment, the cross-linked amino silicone acrylic emulsion is specifically selected from a cross-linked amino silicone acrylic emulsion prepared in [Preparation Example 2-6].

[0152] [Example 7]

[0153] A slurry, which is different from [Example 4] in that the dyeing accelerator is different.

[0154] In this embodiment, the dyeing accelerator is a mixture of sodium chloride, sodium carbonate and sodium hydroxide in a weight ratio of 1:0.8:0.2, that is, the dyeing accelerator includes 2.273 kg of sodium chloride, 0.182 kg of sodium carbonate and 0.045 kg of sodium hydroxide.

[0155] [Example 8]

[0156] A slurry, which differs from [Example 7] in that the dyeing accelerator is different.

[0157] In this embodiment, an equal amount of sodium carbonate in the dyeing accelerator is replaced by sodium sulfate.

[0158] [Example 9]

[0159] A slurry, which differs from [Example 7] in that the dyeing accelerator is different.

[0160] In this embodiment, an equal amount of sodium carbonate in the dyeing accelerator is replaced by sodium phosphate. Comparative Example

[0161] [Comparative Example 1]

[0162] A slurry, which differs from [Example 1] in that no cross-linked amino silicone acrylic emulsion is added.

[0163] In this comparative example, the cross-linked aminosilicone acrylic emulsion was replaced by an equal amount of a polyacrylate emulsion prepared in [Preparation Example 3-1].

[0164] [Comparative Example 2]

[0165] A slurry, which differs from [Example 1] in that no cross-linked amino silicone acrylic emulsion is added.

[0166] In this comparative example, the cross-linked aminosilicone acrylic emulsion was replaced by an equal amount of a polyacrylate emulsion prepared in [Preparation Example 3-1]. At the same time, when the cross-linking monomer was added during the preparation process, an additional 5 kg of bis(3-aminopropyl)-terminated dimethylsiloxane with an amino value of 0.6 was added.

[0167] [Comparative Example 3]

[0168] A slurry, which is different from [Example 1] in that no dyeing accelerator is added, and the color paste dye does not use reactive dyes.

[0169] In this comparative example, the color paste dye is replaced by direct dye in equal amounts, specifically direct blended navy blue DR is selected, and the CI number is direct blue 297.

[0170] Performance test data

[0171] 1. Subjective test: The denim warp yarns were sized and dyed with the sizing agents of the embodiments and comparative examples respectively, and then woven into denim fabrics. The appearance and hand feel of the denim fabrics after sizing and dyeing with the sizing agents of the embodiments and comparative examples were compared by visual inspection, touch, etc. Among them, the subjective judgment standard for the hand feel of denim fabrics is: soft < softer < harder < hard.

[0172] 2. Hairiness test: Refer to "FZ / T 01086-2020 Textile Yarn Hairiness Determination Method Projection Counting Method" to test the average hairiness of the yarn before and after sizing, and calculate the hairiness reduction rate (%) of the yarn before and after sizing and dyeing. The hairiness setting length is 2mm, the yarn length is 10m, and the hairiness reduction rate calculation formula is as follows:

[0173] Hairiness reduction rate = [(N 1 -N 2 ) / N 1 ]*100%

[0174] Where N 1 N is the average hairiness of the original yarn (roots / m), 2 It is the average value of the hairiness of sized yarn (roots / m).

[0175] 3. Color fastness test: refer to GB / T 3920-2008 Textiles Color fastness test - Color fastness to rubbing to test the sizing yarn, and record the color fastness grade of each embodiment and comparative example sizing after sizing and dyeing.

[0176] 4. Color depth (K / S value): The denim warp yarns sizing and dyeing with the sizing agents of the embodiments and comparative examples were woven into denim fabrics, and then the dyed denim fabrics were folded twice (four layers), and the K / S value of the dyed fabrics was measured at λmax using a Datacolor SF60OX computer colorimeter. Each sample was measured four times and the average value was taken. The higher the K / S value, the higher the dyeing depth.

[0177] Table 1 Partial performance test of yarn

[0178]

[0179] Combining Example 1 with Comparative Examples 1-3 and the data in Table 1, it can be seen that Example 1 uses terminal amino silicone oil as a silicon source, cooperates with terminal allyl epoxy polyether and p-vinylaniline to react to obtain an amino silicone oil modified monomer, and then copolymerizes with an acrylate monomer through emulsion polymerization to obtain a cross-linked amino silicone acrylic emulsion. Compared with the polyacrylate emulsion of Comparative Example 1, after being mixed with a color paste dye to form a slurry and sizing and dyeing the denim warp yarn, it can not only greatly reduce the yarn surface hairiness, improve the yarn surface state and feel, but also has higher color fastness and dyeing depth.

[0180] Secondly, it can be seen from the comparison of Example 1 and Comparative Examples 1-2 that in Comparative Example 2, the amino-terminated silicone oil and the polyacrylate emulsion are directly mixed to configure the emulsion. Although the prepared slurry has a certain improvement on the yarn surface compared to the slurry in Comparative Example 1, the effect is not great, and the effect on its color fastness is not great, and even the color fastness grade is reduced under wet friction, and the color depth is reduced by a small amount. This may be because the compatibility of the amino-terminated silicone oil and the polyacrylate emulsion is not high, the stability is poor, and the color paste dye and the accelerator will cause the slurry to be in a high alkaline environment, and the amino-terminated silicone oil directly mixed may be hydrolyzed and even cause the emulsion to break, thereby losing the finishing effect on the yarn. In Example 1, the amino-terminated silicone oil is first synthesized into monomers by combining the amino-terminated silicone oil with the terminal allyl epoxy polyether and p-vinylaniline, and then the amino-terminated silicone oil can be connected to the polyacrylate main chain in a grafting manner by a chemical copolymerization method. The prepared silicone acrylic emulsion has good stability and alkali resistance, and is not prone to hydrolysis or demulsification.

[0181] Comparative Example 1 and Comparative Example 3 show that when the color paste dye in the slurry uses a reactive dye containing a vinyl sulfone group and is combined with an alkaline dyeing accelerator, the slurry exhibits good color fastness and dyeing depth during the dyeing process compared to traditional direct dyes. This may be because the vinyl sulfone group in the reactive dye has high diffusivity during the first padding process, can be fully dispersed in the fiber, and has a good dyeing rate and leveling effect, and during the second padding, the alkaline dyeing accelerator in the slurry promotes the activation of the vinyl sulfone group, so that the color paste dye can fully react and combine with the hydroxyl group on the yarn fiber, thereby improving the bonding strength between the color paste dye and the fiber, which is beneficial to improving the color fastness and dyeing depth of the slurry.

[0182] Combining Example 1 with Example 4 and the data in Table 1, it can be seen that as the average molecular weight of the terminal allyl epoxy polyether of the amino silicone oil modified monomer increases, the slurry finally prepared has a better finishing effect on the yarn, not only the yarn softness is further improved, but also the hairiness reduction rate is improved, that is, the hairiness on the yarn surface is less. This may be because as the average molecular weight of the terminal allyl epoxy polyether increases, that is, the longer the branched chain segment of the cross-linked amino silicone emulsion after grafting, it is beneficial to improve the flexibility and plasticity of the formed paint film, thereby improving the finishing effect of the slurry on the yarn surface.

[0183] Combining Examples 4-6 and the data in Table 1, it can be seen that as the ammonia value of the amino-terminated silicone oil increases, the finishing effect of the slurry on the fiber gradually increases, and the hairiness reduction rate increases, but when the ammonia value reaches 1, the surface of the dyed yarn is slightly yellowed. This may be because as the ammonia value of the amino-terminated silicone oil increases, the amino content in the slurry is higher. Although the amino functional group can promote the combination of the slurry and the fiber, in an alkaline environment containing a dye accelerator, the amino group in the slurry is easily oxidized during padding and forms a chromophore, resulting in slightly yellowing of the yarn.

[0184] Combining Example 4 with Examples 7-9 and the data in Table 1, it can be seen that when the dyeing accelerator is sodium chloride, sodium carbonate and sodium hydroxide mixed in a weight ratio of 1:0.8:0.2, the alkaline environment prepared has the best dyeing and fixing effect on B-type reactive dyes. However, the finishing effect is greatly reduced after replacing sodium carbonate with sodium phosphate. This may be because the alkaline environment formed by the equal replacement of sodium phosphate is too high, which in turn affects the finishing effect of the cross-linked aminosilicone acrylic emulsion.

[0185] This specific implementation manner is merely an explanation of the present application and is not a limitation of the present application. After reading this specification, those skilled in the art may make non-creative modifications to the specific implementation manner as needed, but such modifications are protected by the patent law as long as they are within the scope of the claims of the present application.

Claims

1. A slurry, characterized in that: It includes the following raw materials in parts by weight: Cross-linked amino silicone acrylic emulsion: 160-180 parts; Color paste dye: 8-12 parts; Dyeing accelerator: 2-4 parts; Emulsifying dispersant: 1.8-2 parts; Defoaming agent: 0.08-0.1 parts; The color paste dye is specifically selected from active dyes containing vinyl sulfone groups, and the dyeing accelerator includes at least one of sodium sulfate, sodium carbonate, sodium phosphate or sodium hydroxide mixed with sodium chloride; The cross-linked amino silicone acrylic emulsion comprises the following raw materials in parts by weight: Butyl acrylate: 15-20 parts; 2-Ethylhexyl methacrylate: 5-10 parts; Hydroxymethacrylate: 10-20 parts; Amino silicone oil modified monomer: 20-25 parts; Cross-linking monomer: 2-3.2 parts; Sodium dodecyl sulfate: 2.5-4.5 parts; Ammonium persulfate: 0.3-0.6 parts; γ-aminopropyltriethoxysilane: 2-3 parts; Soft water: 80-100 parts; The hydroxy methacrylate is selected from hydroxyethyl methacrylate and hydroxypropyl methacrylate, and the cross-linking monomer is specifically diacetone acrylamide and adipic acid dihydrazide mixed in a weight ratio of 1: (0.06-0.12); The amino silicone oil modified monomer comprises the following raw materials in parts by weight: Terminal allyl epoxy polyether: 15-20 parts; Amino-terminated silicone oil: 4-8 parts; p-vinylaniline: 2.5-5 parts; Triethylamine: 0.02-0.05 parts; The average molecular weight of the terminal allyl epoxy polyether is in the range of 450-1000, and the terminal amino silicone oil is bis(3-aminopropyl)-terminated dimethylsiloxane with an amine value of 0.4-0.6 mmol / g; The preparation method of the amino silicone oil modified monomer comprises the following steps: First, preliminarily mix the terminal allyl epoxy polyether and the terminal amino silicone oil, then raise the temperature to 65-72°C and start stirring for 150-200 minutes, then add p-vinylaniline and triethylamine, raise the temperature to 75-80°C again and continue stirring and reacting for 60-90 minutes to obtain an amino silicone oil modified monomer; The preparation method of the cross-linked amino silicone acrylic emulsion comprises the following steps: A1. 40% by weight of soft water, 40% by weight of sodium lauryl sulfate and 20% by weight of ammonium persulfate are stirred and mixed to obtain a pre-emulsified base liquid; 10% by weight of soft water and the remaining ammonium persulfate are stirred and mixed to obtain an initiating solution; amino silicone oil modified monomer, butyl acrylate, 2-ethylhexyl methacrylate, hydroxymethyl acrylate, crosslinking monomer and the remaining sodium lauryl sulfate and soft water are stirred and mixed to obtain a mixed monomer liquid; A2. Add 10% by weight of the mixed monomer liquid to the pre-emulsified base liquid at one time, heat to 78-82°C and stir continuously. When the emulsion starts to turn slightly blue, slowly add the remaining mixed monomer liquid to the pre-emulsified base liquid, and add the initiator solution once every 0.5h. Control the amount added each time so that the mixed monomer liquid and the initiator solution can be added within 2.5-3h. Stir continuously during the reaction and keep the temperature constant. After the addition is completed, raise the temperature to 83-85°C and keep warm for 1h. A3. After the heat preservation is completed, the temperature is naturally lowered to 37-40°C, γ-aminopropyltriethoxysilane is added, stirred for 3-5 minutes, and then the pH value is adjusted to between 7 and 9 with ammonia water to obtain a cross-linked aminosilicone acrylic emulsion.

2. A slurry according to claim 1, characterized in that: The reactive dye is specifically a B-type reactive dye, and the dyeing accelerator is specifically selected from sodium chloride, sodium carbonate and sodium hydroxide, which are mixed and compounded in a weight ratio of 10: (0.8-1): 0.

2.

3. A slurry according to claim 1, characterized in that: The emulsifying dispersant is a mixture of sodium lignin sulfonate and triethanolamine in a weight ratio of 1: (0.15-0.25).

4. A slurry according to claim 1, characterized in that: The defoaming agent is specifically selected from any one or more of SAG 672 or SAG 622.

5. A slurry preparation process, used for preparing the slurry according to any one of claims 1 to 4, characterized in that: The following steps are involved: First, the cross-linked aminosilicone acrylic emulsion, emulsifying dispersant and defoaming agent are mixed in proportion, heated to 60-63° C. and stirred for not less than 60 minutes, and then a preliminary slurry is obtained after cooling, and the slurry is sealed and stored separately from light with the color paste dye and the dyeing accelerator; before the denim warp yarn needs to be pad-dyed, the preliminary slurry is stirred and mixed with the color paste dye and the dyeing accelerator in sequence to obtain a slurry.

6. A method for applying a slurry, applicable to the slurry prepared by the preparation process according to claim 5, characterized in that: The following steps are involved: B1. Dilute and mix the slurry with soft water in a weight ratio of 1:2, then add the diluted slurry into the slurry tank of the slurry-dyeing machine, send the washed and dried denim warp yarn into the slurry-dyeing machine, and perform slurry-dyeing through a 2-dipping 2-rolling dyeing process, wherein in the first dipping and rolling, the slurry is a mixture of the preparatory slurry and the color paste dye, and in the second dipping and rolling, the slurry is a mixture of the preparatory slurry, the color paste dye and the dyeing accelerator, so that the denim warp yarn can be fully coated and colored by the slurry, and then heated and dried to obtain the preliminarily colored denim warp yarn; B2. Dilute and mix the prepared slurry without adding color paste dye and accelerator with soft water in a weight ratio of 1:1, then add the diluted prepared slurry into the slurry tank, and perform color fixing and protection treatment on the denim warp yarn that has been initially colored through a dyeing process of 1 dipping and 1 padding, so that the denim warp yarn can be fully covered by the prepared slurry. After heating and drying, let it stand at room temperature for at least 12 hours, and then you can get the denim warp yarn that has been dyed and fixed by slurry.

7. The method for applying a slurry according to claim 6, characterized in that: In the 2-dip 2-roll paddle dyeing treatment in step B1, the slurry temperature needs to be controlled not higher than 30°C, the roller temperatures of the first set of rollers and the second set of rollers are set to 50-55°C, and the drying temperature is set to 105-110°C; in the 1-dip 1-roll color fixing protection treatment in step B2, the temperature of the preparatory slurry needs to be controlled not higher than 50°C, the roller temperatures of the rollers are set to 65-70°C, and the drying temperature is set to 105-110°C.

Citation Information

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