Textile hyperchromic emulsion and preparation method thereof

Abstract

The invention relates to the technical field of spinning, in particular to a color enhancing emulsion for spinning and a preparation method thereof. The invention relates to a color enhancing emulsion for spinning. The color enhancing emulsion comprises 1-2 parts of chitosan-reactive red composite nanoparticles, 10-50 parts of acrylate monomers, 0.1-1 part of an initiator, 3-20 parts of an emulsifier and 40-85 parts of deionized water, the preparation method comprises the following steps: weighing the raw materials; the preparation method comprises the following steps: stirring and dispersing chitosan-reactive red composite nanoparticles into deionized water; stirring is kept, an emulsifier is added, and stirring is stopped after uniform stirring; adding an acrylate monomer, adding an initiator after ultrasonic emulsification, heating to 65 DEG C, and stirring at a low speed for 6 hours; standing and cooling to 25 DEG C to obtain a hyperchromic emulsion; pigment does not need to be added when the hyperchromic emulsion is prepared, and the situation that the color difference of the emulsion is large due to pigment adsorption is avoided; in addition, the chitosan-reactive red composite nanoparticles also have the technical effect similar to that of nanocellulose for preventing the textile emulsion from adhering to the roller.

Description

Technical Field

[0001] The invention relates to the field of textile technology, in particular to a color-enhancing emulsion for textiles and a preparation method thereof. Background Art

[0002] During the textile finishing process, functional emulsion additives, also known as textile emulsions, are used to enhance certain textile properties. For example, emulsions used to enhance textile color are called textile color-enhancing emulsions. Generally, textile emulsions contain polyacrylate binders, which can easily cause the emulsion to adhere to rollers during the finishing process. Current approaches to address this issue involve adding a certain amount of nanocellulose to the emulsion. For example, a Chinese patent application titled "A Polyacrylate Textile Emulsion for Anti-Stick Rollers, Its Preparation and Application" (Granted Publication No. 115073670B) describes the emulsion as being obtained by heating a polyacrylate pre-emulsion to allow an initiator to initiate a polymerization reaction of acrylic ester monomers. The pre-emulsion comprises, by weight, 0.05-1 part nanocellulose, 10-50 parts acrylic ester monomers, 0.05-1 part initiator, 3-20 parts emulsifier, and 40-85 parts deionized water. By introducing nanocellulose into traditional polyacrylate emulsions, the industry's pain point problem of this type of textile emulsion additives sticking to textile rollers during the actual processing and finishing process in the factory is effectively solved.

[0003] The existing technology has defects: since nanocellulose is highly adsorbent to water-soluble pigments, when a color-enhancing emulsion needs to be prepared, part of the pigment is adsorbed by the nanocellulose during the emulsion preparation process, resulting in a large color difference in the emulsion. Summary of the Invention

[0004] In view of the deficiencies of the prior art, one of the objects of the present invention is to provide a color-enhancing emulsion for textiles; a second object of the present invention is to provide a method for preparing the color-enhancing emulsion for textiles.

[0005] One of the objectives of the present invention is achieved through the following technical solutions:

[0006] A color-enhancing emulsion for textiles is prepared from the following raw materials in parts by weight:

[0007] 1-2 parts of chitosan-reactive red composite nanoparticles, 10-50 parts of acrylate monomers, 0.1-1 parts of initiator, 3-20 parts of emulsifier and 40-85 parts of deionized water.

[0008] Furthermore, the acrylic acid ester monomer is a mixture of heptadecafluorodecyl methacrylate, octadecyl acrylate and methyl methacrylate in a weight ratio of 11:26:13.

[0009] Furthermore, the initiator is azobisisobutylamidine hydrochloride.

[0010] Furthermore, the emulsifier is a mixture of C12 fatty alcohol polyoxyethylene ether-3 nonionic surfactant and cetyltrimethylammonium chloride cationic surfactant in a weight ratio of 53:22.

[0011] The second object of the present invention is achieved through the following technical solutions:

[0012] A method for preparing a color-enhancing emulsion for textiles comprises the following steps:

[0013] Step 1, preparing chitosan-reactive red composite nanoparticles;

[0014] Step 2: weigh the raw materials according to the formula;

[0015] Step 3, stirring and dispersing chitosan-reactive red composite nanoparticles in deionized water;

[0016] Step 4: Keep stirring and add emulsifier, and stop stirring after stirring evenly;

[0017] Step 5: Add acrylate monomer, add initiator after ultrasonic emulsification, heat to 65°C, and stir at low speed for 6 hours;

[0018] Step 6: Let the mixture stand and cool to 25° C. to obtain a color-enhancing emulsion.

[0019] Furthermore, the preparation of chitosan-reactive red composite nanoparticles in step 1 comprises the following steps:

[0020] S1: dissolving chitosan in 1% (V / V) acetic acid solution to a concentration of 0.3% (W / V), stirring until transparent, and then filtering out insoluble matter to obtain a chitosan solution;

[0021] S2: Dissolve Reactive Red 195 in deionized water to a concentration of 5% (W / V), and stir to obtain a Reactive Red solution;

[0022] S3: dissolving sodium tripolyphosphate in deionized water to a concentration of 1% (W / V), and stirring to obtain a sodium tripolyphosphate solution;

[0023] S4: mixing the chitosan solution and the reactive red solution in a weight ratio of 6:1 and stirring uniformly to obtain a mixed solution;

[0024] S5: Add sodium tripolyphosphate solution dropwise to the mixed solution while stirring, the amount of which is 1 / 5 of the weight of the chitosan solution, and continue stirring for 1 hour after the addition is completed to obtain a mother solution;

[0025] S6: centrifuging the mother liquor at 10,000 rpm to obtain a precipitate, washing the precipitate with deionized water and then freeze-drying it into a powder, which is chitosan-reactive red composite nanoparticles.

[0026] Furthermore, the chitosan has a deacetylation degree of ≥80%. As is known, the deacetylation degree of chitosan directly affects properties such as solubility and viscosity. In order to obtain particles with better mechanical properties, chitosan with a high deacetylation degree should be used.

[0027] Furthermore, the chitosan solution has a pH of 4.5-5.5, and the sodium tripolyphosphate solution has a pH of 8-9. Electrostatic interaction between chitosan (positively charged, pH < 6.5) and an anionic crosslinker (sodium tripolyphosphate, TPP) is utilized to form nanoparticles, which simultaneously encapsulate the pigment (Reactive Red 195).

[0028] Furthermore, the stirring and dispersing speed in step 3 is 300 rpm. Mechanical stirring at medium and low speeds is very conducive to the dispersion of nano-sized particles in water.

[0029] Furthermore, the low-speed stirring speed in step 5 is 200 rpm. Stirring at a relatively low speed is beneficial to the polymerization reaction of the monomers.

[0030] The present invention has the following beneficial effects: chitosan-reactive red composite nanoparticles are used to replace nanocellulose; since the chitosan-reactive red composite nanoparticles are themselves pigments, no pigment needs to be added when preparing a color-enhancing emulsion; even if the chitosan-reactive red composite nanoparticles also have adsorptive properties, the adsorption of pigments will not result in a large color difference in the emulsion; and the chitosan-reactive red composite nanoparticles also have a technical effect similar to nanocellulose of preventing textile emulsion from adhering to rollers. DETAILED DESCRIPTION

[0031] The following is further explained in conjunction with specific implementation methods:

[0032] Instructions for use:

[0033] Chitosan used in the following examples and comparative examples was purchased from Shandong Pingju Biotechnology Co., Ltd. with a deacetylation degree of 80%; sodium tripolyphosphate was purchased from Wujiang Aokang Chemical Co., Ltd. with a purity of ≥95%; and Reactive Red 195 was purchased from Shanghai Jizhi Biochemical Technology Co., Ltd. with a purity of ≥99%. All other materials were purchased from conventional sources. The acrylate monomer was a mixture of heptadecafluorodecyl methacrylate, octadecyl acrylate, and methyl methacrylate in a weight ratio of 11:26:13. The initiator was azobisisobutylamidine hydrochloride. The emulsifier was a mixture of a C12 fatty alcohol polyoxyethylene ether-3 nonionic surfactant and a hexadecyltrimethylammonium chloride cationic surfactant in a weight ratio of 53:22.

[0034] Example 1

[0035] Preparation of chitosan-reactive red composite nanoparticles:

[0036] Chitosan was dissolved in 1% (V / V) acetic acid solution to a concentration of 0.3% (W / V), stirred until transparent, and then insoluble matter was filtered out to obtain a chitosan solution. The pH value was 4.8.

[0037] Dissolve Reactive Red 195 in deionized water to a concentration of 5% (W / V) and stir to obtain a Reactive Red solution;

[0038] Sodium tripolyphosphate was dissolved in deionized water to a concentration of 1% (W / V), and the mixture was stirred to obtain a sodium tripolyphosphate solution, the pH of which was 8.6.

[0039] The chitosan solution and the reactive red solution were mixed in a weight ratio of 6:1 and stirred to obtain a mixed solution;

[0040] Sodium tripolyphosphate solution was added dropwise to the mixed solution while stirring, with the amount of addition being 1 / 5 of the weight of the chitosan solution. After the addition was completed, stirring was continued for 1 hour to obtain a mother solution.

[0041] The mother liquor was centrifuged at 10,000 rpm to obtain a precipitate, which was washed with deionized water and freeze-dried into a powder, resulting in chitosan-reactive red composite nanoparticles. Dynamic light scattering (DLS) analysis revealed that the chitosan-reactive red composite nanoparticles prepared in Example 1 had a Z-average particle size of 180-220 nm and a PDI <0.3.

[0042] Preparation of color-enhancing emulsion for textiles:

[0043] Weigh 1 part of chitosan-reactive red composite nanoparticles, 10 parts of acrylate monomer, 0.1 part of initiator, 3 parts of emulsifier and 40 parts of deionized water according to weight;

[0044] Chitosan-reactive red composite nanoparticles were dispersed in deionized water at a stirring speed of 300 rpm;

[0045] Keep stirring and add emulsifier, and stop stirring after stirring evenly;

[0046] Add acrylate monomers, add initiator after ultrasonic emulsification, raise the temperature to 65°C, and stir at a low speed of 200 rpm for 6 hours;

[0047] The mixture was allowed to stand and cooled to 25°C to obtain a color-enhanced emulsion.

[0048] Padding finishing:

[0049] First, a padding finishing solution is prepared according to which each liter of padding finishing solution contains 60g of color enhancing emulsion, and then the polyester woven fabric is subjected to a padding and padding finishing. The drying temperature of the polyester woven fabric after finishing is pre-treated at 100℃ for 10s and then treated at 200℃ for 50s to obtain the fabric.

[0050] Example 2

[0051] The only difference from Example 1 is that 2 parts of chitosan-reactive red composite nanoparticles, 50 parts of acrylate monomers, 1 part of initiator, 20 parts of emulsifier and 85 parts of deionized water are weighed in parts by weight.

[0052] Example 3

[0053] The only difference from Example 1 is that 1.5 parts of chitosan-reactive red composite nanoparticles, 25 parts of acrylate monomers, 0.7 parts of initiator, 15 parts of emulsifier and 60 parts of deionized water are weighed in parts by weight.

[0054] Comparative Example 1

[0055] The only difference from Example 1 is that the step of preparing chitosan-reactive red composite nanoparticles is removed, and the chitosan-reactive red composite nanoparticles are replaced with a mixed powder of equal weight of nanocellulose (cellulose nanocrystals with a length of about 200 nm and a diameter of about 100 nm) and reactive red in a weight ratio of 1:1.

[0056] Comparative Example 2

[0057] Preparation of mixed powder:

[0058] Chitosan, Reactive Red 195 and sodium tripolyphosphate were uniformly mixed in a weight ratio of 30:5:6 to obtain a mixed powder.

[0059] Preparation of color-enhancing emulsion for textiles:

[0060] Weigh 1 part of mixed powder, 10 parts of acrylic acid ester monomer, 0.1 part of initiator, 3 parts of emulsifier and 40 parts of deionized water according to weight;

[0061] The mixed powder was dispersed in deionized water at a stirring speed of 300 rpm;

[0062] Keep stirring and add emulsifier, and stop stirring after stirring evenly;

[0063] Add acrylate monomers, add initiator after ultrasonic emulsification, raise the temperature to 65°C, and stir at a low speed of 200 rpm for 6 hours;

[0064] The mixture was allowed to stand and cooled to 25°C to obtain a color-enhanced emulsion.

[0065] Padding finishing:

[0066] First, a padding finishing solution is prepared according to which each liter of padding finishing solution contains 60g of color enhancing emulsion, and then the polyester woven fabric is subjected to a padding and padding finishing. The drying temperature of the polyester woven fabric after finishing is pre-treated at 100℃ for 10s and then treated at 200℃ for 50s to obtain the fabric.

[0067] Color difference experiment

[0068] 1. Experimental purpose: to verify that the color difference of the color-enhancing emulsion obtained by the present invention is small.

[0069] 2. Experimental method: The fabrics obtained in Examples 1-3 and Comparative Examples 1-2 were tested for color difference using a colorimeter, and the test was repeated three times to obtain the average value.

[0070] 3. Experimental results, see Table 1.

[0071] Table 1 Color difference mean

[0072]

[0073]

[0074] When the color difference value is greater than 3.0, it is clearly discernible to the human eye. The color difference values ​​of the fabrics obtained by the present invention are all less than 3.0, and even less than 1.7, meeting the coloring requirements of most textiles. However, the color difference of Comparative Example 1 is visible to the naked eye, even exceeding 3.0, and is considered unqualified according to most textile standards.

[0075] Roller sticking and stability tests

[0076] 1. Experimental purpose: to verify that the color-enhancing emulsion obtained by the present invention has the effect of anti-roller sticking, and to observe the stability of the color-enhancing emulsion.

[0077] 2. Experimental Method: The padding finishing solutions obtained in Examples 1-3 and Comparative Example 2 were subjected to a roller sticking test. Roll sticking was determined by observing the surface of the textile rollers during the dyeing and finishing process and after 6000 meters of fabric had been run to see if there was any adhesion (roll sticking). Stability was determined by observing the color-enhancing emulsions for delamination or precipitation after 12 months of sealed storage at room temperature.

[0078] 3. Experimental results, see Table 2.

[0079] Table 2 Sticking roller observation table

[0080] Padding finishing liquid Example 1 Example 2 Example 3 Comparative Example 2 Roller sticking none none none Sticky roller Stability none none none none

[0081] As can be seen from Table 2, the color enhancement emulsion obtained by the present invention has an anti-roller sticking effect, and the product has a stability comparable to similar products.

[0082] The above embodiments and descriptions are only for explaining the principles and best embodiments of the present invention. Without departing from the spirit and scope of the present invention, the present invention may be subject to various changes and improvements, which shall fall within the scope of the invention to be protected.

Claims

1. A color-enhancing emulsion for textiles, characterized in that: The invention is prepared from the following raw materials in parts by weight: 1-2 parts of chitosan-reactive red composite nanoparticles, 10-50 parts of acrylate monomers, 0.1-1 parts of initiator, 3-20 parts of emulsifier and 40-85 parts of deionized water.

2. The textile color enhancing emulsion according to claim 1, characterized in that: The acrylic acid ester monomer is prepared by mixing heptadecafluorodecyl methacrylate, octadecyl acrylate and methyl methacrylate in a weight ratio of 11:26:

13.

3. The textile color-enhancing emulsion according to claim 1, characterized in that: The initiator is azobisisobutylamidine hydrochloride.

4. The textile color-enhancing emulsion according to claim 1, characterized in that: The emulsifier is a mixture of a C12 fatty alcohol polyoxyethylene ether-3 nonionic surfactant and a cetyltrimethylammonium chloride cationic surfactant in a weight ratio of 53:

22.

5. A method for preparing the textile color-enhancing emulsion according to claim 1, characterized in that: The following steps are involved: Step 1, preparing chitosan-reactive red composite nanoparticles; Step 2: weigh the raw materials according to the formula; Step 3, stirring and dispersing chitosan-reactive red composite nanoparticles in deionized water; Step 4: Keep stirring and add emulsifier, and stop stirring after stirring evenly; Step 5: Add acrylate monomer, add initiator after ultrasonic emulsification, heat to 65°C, and stir at low speed for 6 hours; Step 6: Let the mixture stand and cool to 25° C. to obtain a color-enhancing emulsion.

6. The method for preparing the textile color-enhancing emulsion according to claim 5, characterized in that: The preparation of chitosan-reactive red composite nanoparticles in step 1 comprises the following steps: S1: dissolving chitosan in 1% (V / V) acetic acid solution to a concentration of 0.3% (W / V), stirring until transparent, and then filtering out insoluble matter to obtain a chitosan solution; S2: Dissolve Reactive Red 195 in deionized water to a concentration of 5% (W / V), and stir to obtain a Reactive Red solution; S3: dissolving sodium tripolyphosphate in deionized water to a concentration of 1% (W / V), and stirring to obtain a sodium tripolyphosphate solution; S4: mixing the chitosan solution and the reactive red solution in a weight ratio of 6:1 and stirring uniformly to obtain a mixed solution; S5: Add sodium tripolyphosphate solution dropwise to the mixed solution while stirring, the amount of which is 1 / 5 of the weight of the chitosan solution, and continue stirring for 1 hour after the addition is completed to obtain a mother solution; S6: centrifuging the mother liquor at 10,000 rpm to obtain a precipitate, washing the precipitate with deionized water and then freeze-drying it into a powder, which is chitosan-reactive red composite nanoparticles.

7. The method for preparing the textile color-enhancing emulsion according to claim 6, wherein: The deacetylation degree of the chitosan is ≥80%.

8. The method for preparing the textile color-enhancing emulsion according to claim 6, wherein: The chitosan solution has a pH of 4.5-5.5, and the sodium tripolyphosphate solution has a pH of 8-9.

9. The method for preparing the textile color-enhancing emulsion according to claim 5, characterized in that: The stirring and dispersing speed in the step 3 is 300 rpm.

10. The method for preparing the color-enhancing emulsion for textile use according to claim 5, characterized in that: The low-speed stirring speed in the step 5 is 200 rpm.

Images