Nanoscale optical brightener, chemical fiber, and method of making

Abstract

The embodiment of the application discloses a kind of nanoscale fluorescent whitening agent, chemical fiber and preparation method.Nanoscale fluorescent whitening agent solution preparation method includes: fluorescent whitening agent raw powder is mixed with D5 solvent, and fluorescent whitening agent solution is obtained;In the fluorescent whitening agent solution, chemical fiber is treated with fluorescent whitening, and the mixed liquor after fluorescent whitening treatment is obtained;The mixed liquor is filtered, and the filtrate is centrifuged, and the supernatant is obtained;Wherein, the supernatant is nanoscale fluorescent whitening agent solution, not only simple preparation method, short preparation time, dispersibility and stability are good, can be easily applied to the whitening treatment of polyester fiber, while no waste water is generated in preparation process.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of textile whitening, in particular to a nanoscale fluorescent whitening agent, a chemical fiber and a preparation method. BACKGROUND

[0002] The fluorescent whitening agent OB-1 is non-toxic, has good chemical stability, good heat resistance and good light stability, and is therefore widely used in plastic products. In addition, OB-1 is also an ideal choice for polyester fiber whitening due to its washing fastness and whitening effect. However, the OB-1 molecule has high planarity, low solubility in water and poor dispersibility, so that the OB-1 molecule is easy to aggregate through van der Waals interaction force, and it is difficult to dye and whiten synthetic fibers. SUMMARY

[0003] In view of the deficiencies of the prior art, the present application provides a nanoscale fluorescent whitening agent which has good dispersibility and stability, can be easily applied to the whitening treatment of polyester fibers, and does not produce wastewater during preparation.

[0004] In a first aspect, the present application provides a preparation method of a nanoscale fluorescent whitening agent solution, which comprises:

[0005] Mixing the fluorescent whitening agent raw powder with the D5 solvent to obtain a fluorescent whitening agent solution;

[0006] Performing adsorption-desorption treatment on the chemical fiber in the fluorescent whitening agent solution to obtain a mixed solution after fluorescent whitening treatment;

[0007] Filtering the mixed solution and centrifuging the filtrate to obtain supernatant; wherein the supernatant is a nanoscale fluorescent whitening agent solution.

[0008] Further, in the preparation method of the nanoscale fluorescent whitening agent solution, the fluorescent whitening agent comprises fluorescent whitening agent OB-1.

[0009] Further, in the preparation method of the nanoscale fluorescent whitening agent solution, the mass of the fluorescent whitening agent raw powder is 0.0010% to 0.015% o.m.f.; or / and

[0010] The mass ratio of the D5 to the fluorescent whitening agent raw powder is (100000 to 1000000) to 1.

[0011] Further, in the preparation method of the nanoscale fluorescent whitening agent solution, the temperature of the adsorption-desorption treatment is 100 to 140°C, and the holding time is 0 to 40 min.

[0012] In a second aspect, the application further provides a nanoscale fluorescent whitening agent prepared by the preparation method of the nanoscale fluorescent whitening agent solution.

[0013] In a third aspect, the application further provides a method for fluorescent whitening treatment of chemical fibers, which comprises:

[0014] immersing and padding the chemical fibers in the nanoscale fluorescent whitening agent solution of the second aspect to obtain the chemical fibers after immersing and padding;

[0015] respectively pre-drying, baking, washing and drying the chemical fibers after immersing and padding to obtain the chemical fibers after fluorescent whitening treatment.

[0016] Further, in the method for fluorescent whitening treatment of chemical fibers, the liquid retention rate of the chemical fibers after immersing and padding is 70-90%.

[0017] Further, in the method for fluorescent whitening treatment of chemical fibers, the temperature of the pre-drying is 50-70℃, and the time of the pre-drying is 5-15 min; or / and

[0018] the temperature of the baking is 150-210℃, and the time of the baking is 3-8 min.

[0019] Further, in the method for fluorescent whitening treatment of chemical fibers, the chemical fibers are one or more of polyester fibers, nylon fibers and polypropylene fibers.

[0020] In a fourth aspect, the application further provides a chemical fiber after nanoscale fluorescent whitening agent treatment, which is prepared by the method for fluorescent whitening treatment of chemical fibers of the third aspect.

[0021] The nanoscale fluorescent whitening agent, the chemical fibers and the preparation method provided by the application are prepared by mixing the fluorescent whitening agent raw powder with the D5 solvent to obtain a fluorescent whitening agent solution, then performing adsorption-desorption treatment on the chemical fibers in the fluorescent whitening agent solution to obtain a mixed solution after fluorescent whitening treatment, and finally filtering the mixed solution, centrifugally separating the filtrate, and obtaining the nanoscale fluorescent whitening agent solution as the supernatant. The nanoscale fluorescent whitening agent solution has the advantages of simple preparation method, short preparation time, good dispersibility and stability, and can be easily applied to the whitening treatment of polyester fibers, and no wastewater is generated in the preparation process. DETAILED DESCRIPTION

[0022] With reference to the accompanying drawings, the specific embodiments of the present application will be described in detail below. Obviously, the described embodiments are only a part of the embodiments of the present application, but not all the embodiments. Based on the embodiments of the present application, all the other embodiments obtained by those skilled in the art without creative work shall fall within the scope of the present application.

[0023] It should be understood that the terms "comprise" and "include" as used in the specification and the appended claims indicate the presence of the described features, integers, steps, operations, elements, and / or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and / or groups thereof.

[0024] It should also be understood that the terms used in the present application specification are only for the purpose of describing specific embodiments and are not intended to limit the present application. As used in the present application specification and the appended claims, the singular forms "a", "an" and "the" are intended to include the plural forms unless the context clearly indicates otherwise.

[0025] It should be further understood that the term "and / or" as used in the present application specification and the appended claims means any combination of one or more of the associated listed items and all possible combinations thereof, and includes these combinations.

[0026] Chinese patent CN106758132 A develops a fluorescent whitening slurry and is used for polyester whitening finishing. However, the preparation process of the fluorescent whitening slurry is long, and a large amount of chemical additives are needed. At the same time, the dyeing of polyester fiber is generally at 130℃, because at this temperature, the macromolecular chain of polyester becomes soft, the pore in the molecular chain increases, and the monomolecular form of disperse dye can penetrate into the polyester fiber.

[0027] In view of the above defects, the present application provides a preparation method of a nanoscale fluorescent whitening agent solution, which comprises:

[0028] Mixing the fluorescent whitening agent raw powder with the D5 solvent to obtain a fluorescent whitening agent solution;

[0029] Performing fluorescent whitening treatment on the chemical fiber in the fluorescent whitening agent solution to obtain a mixed solution after fluorescent whitening treatment;

[0030] Filtering the mixed solution, and centrifugally separating the filtrate to obtain an upper clear liquid; wherein the upper clear liquid is a nanoscale fluorescent whitening agent solution.

[0031] The process of disperse dye polyester dyeing exists adsorption and desorption process, that is, the form of disperse dye desorbed should be single molecule state, but it can be aggregated with disperse dye again to form larger size disperse dye particles in the dye bath. That is, the nanoscale fluorescent whitening agent prepared by the application is the desorbed fluorescent whitening agent.

[0032] At present, the OB-1 raw powder can only be dissolved in decamethylcyclopentasiloxane (D5) in a small amount. If D5 is directly used as a solvent to dissolve the OB-1 raw powder and to perform fluorescent whitening treatment on chemical fibers, OB-1 raw powder must be added in excess, which makes the whitening effect poor, and the residual liquid after the whitening treatment cannot be fully utilized, thereby increasing the production cost.

[0033] In the application, a proper amount of OB-1 raw powder and polyester fiber are added to D5 for treatment at high temperature, so that the desorbed OB-1 molecules can be uniformly dispersed in D5, and then the larger OB-1 particles are removed, thereby preparing a nanoscale fluorescent whitening agent OB-1 organic solution which can be applied to the dyeing and whitening finishing of polyester fibers. The preparation method is simple, the preparation time is short, the dispersity and stability are good, and the prepared nanoscale fluorescent whitening agent can be easily applied to the whitening treatment of polyester fibers, and no wastewater is generated in the preparation process.

[0034] In the application, the fluorescent whitening agent is preferably fluorescent whitening agent OB-1.

[0035] In some embodiments, the mass of the fluorescent whitening agent raw powder is 0.0010% to 0.015% o.m.f., and preferably 0.01% o.m.f.

[0036] In some embodiments, the mass ratio of the D5 to the fluorescent whitening agent raw powder is (100000 to 1000000) to 1, and preferably 500000 to 1.

[0037] In some embodiments, the adsorption-desorption treatment temperature is 100 to 140°C, and the holding time is 0 to 40 min. Preferably, the adsorption-desorption treatment temperature is 130°C, and the holding time is 30 min.

[0038] In some embodiments, the centrifugal separation speed is 5000 to 15000 rpm / min, and the centrifugal separation time is 2 to 8 min. Preferably, the centrifugal separation speed is 10000 rpm / min, and the centrifugal separation time is 5 min.

[0039] In some embodiments, the application further provides a nanoscale fluorescent whitening agent prepared by the above-mentioned preparation method of the nanoscale fluorescent whitening agent solution. In some embodiments, the application further provides a nanoscale fluorescent whitening agent prepared by the above-mentioned preparation method of the nanoscale fluorescent whitening agent solution.

[0040] In some embodiments, the present application also provides a method for fluorescent whitening treatment of chemical fibers, comprising:

[0041] immersing and padding the chemical fibers in the nanoscale fluorescent whitening agent solution described above to obtain the immersed and padded chemical fibers;

[0042] respectively pre-drying, baking, washing, and drying the immersed and padded chemical fibers to obtain the fluorescent whitening treated chemical fibers.

[0043] In some embodiments, the liquid retention rate of the immersed and padded chemical fibers is 70-90%. Preferably, the liquid retention rate is 80%.

[0044] In some embodiments, the pre-drying temperature is 50-70°C, and the pre-drying time is 5-15 min. Preferably, the pre-drying temperature is 60°C, and the pre-drying time is 10 min.

[0045] In some embodiments, the baking temperature is 150-210°C, and the baking time is 3-8 min. Preferably, the baking temperature is 180°C, and the baking time is 5 min.

[0046] In some embodiments, the chemical fibers are one or more of polyester fibers, nylon fibers, and polypropylene fibers. Preferably, the chemical fibers are polyester fibers.

[0047] In some embodiments, the present application also provides a chemical fiber treated by a nanoscale fluorescent whitening agent, which is prepared by the method for fluorescent whitening treatment of chemical fibers described above.

[0048] The technical solutions of the present application are illustrated in detail below.

[0049] Example 1

[0050] 10 g of polyester yarn, 10 g of nylon yarn, and 10 g of polypropylene yarn were respectively mixed with 0.0010 g (0.01% o.m.f) of OB-1 raw powder and 500 g of D5 to prepare three treatment samples, which were heated to 130°C and kept for 30 minutes, and then cooled to room temperature. The treatment samples of the polyester yarn, the nylon yarn, and the polypropylene yarn were respectively filtered to collect the filtrate. The filtrate was centrifuged at a speed of 10000 rpm for 5 minutes, and the supernatant was collected to complete the preparation of the D5 whitening solution of the nanoscale fluorescent whitening agent OB-1. The particle size is shown in Table 1.

[0051] Table 1. Particle size of OB-1 under treatment of different fibers

[0052] Fiber D0.9 (nm) D0.5 (nm) Polyester yarn 83 25 Polyamide yarn 368 126 Polypropylene yarn 467 289

[0053] Three pieces of 10 g bleached polyester cloth were immersed in the D5 whitening solution of the fluorescent whitening agent OB-1 treated with polyester yarn, nylon yarn and polypropylene yarn respectively, and the excess whitening solution was rolled off. The weight of the three pieces of bleached polyester cloth was 18 g, and an additional piece of polyester cloth without whitening treatment was taken as a control sample. Then the four pieces of polyester cloth were pre-dried at 60 °C for 10 min, and then baked at 180 °C for 5 min, and then soaped, dried and detected for whiteness. After the bleached polyester cloth was whitened by the D5 whitening solution of the fluorescent whitening agent OB-1 treated with polyester yarn, nylon yarn and polypropylene yarn, the whiteness was detected by the spectrophotometer CS-650A of Hangzhou Caipu Technology Co., Ltd. using the built-in standard WI (CIE), and the whiteness was 135, 108 and 105 respectively, while the whiteness of the bleached polyester cloth without whitening treatment was 86.

[0054] Example 2

[0055] 10 g of polyester yarn, 0.0001 g (0.0010% o.m.f), 0.005 g (0.005% o.m.f), 0.0010 g (0.01% o.m.f) and 0.0015 g (0.015% o.m.f) of OB-1 raw powder and 500 g of D5 were mixed to prepare four treatment samples, which were heated to 130 °C and kept for 30 min, and then cooled to room temperature. The treatment samples of 0.0001 g, 0.005 g, 0.0010 g and 0.0015 g of OB-1 raw powder were filtered respectively, and the filtrate was collected. Then the filtrate was centrifuged at 10,000 rpm for 5 min, and the supernatant was taken to complete the preparation of the D5 whitening solution of the nanoscale fluorescent whitening agent OB-1. The particle size is shown in Table 2.

[0056] Table 2. Particle size of OB-1 under different OB-1 raw powder mass treatments

[0057] OB-1 raw powder (g) Fiber weight (%, o.m.f) D0.9 (nm) D0.5 (nm) 0.0001 0.001 85 27 0.0005 0.005 85 26 0.0010 0.010 83 25 0.0015 0.015 84 26

[0058] Four pieces of 10 g bleached polyester cloth were immersed in 0.0001 g, 0.005 g, 0.0010 g and 0.0015 g of OB-1 raw powder treated fluorescent whitening agent OB-1 D5 whitening solution respectively, and the excess whitening solution was rolled off. The weight of the four pieces of bleached polyester cloth was 18 g each. An additional piece of polyester cloth without whitening treatment was taken as a control sample. Then, the samples were pre-dried at 60 °C for 10 min, and then baked at 180 °C for 5 min. Then, the samples were soaped, dried and the whiteness was detected. After the bleached polyester cloth was whitened by 0.0001 g, 0.005 g, 0.0010 g and 0.0015 g of OB-1 raw powder treated fluorescent whitening agent OB-1 D5 whitening solution, the whiteness was detected by a spectrophotometer CS-650A from Hangzhou Caipu Technology Co., Ltd. using the built-in standard WI (CIE), and the whiteness was 104, 123, 135 and 130 respectively. The whiteness of the bleached polyester cloth without whitening treatment was 86.

[0059] Example 3

[0060] 10 g of polyester yarn, 0.0010 g (0.01% o.m.f) of OB-1 raw powder and 100 g (D5 to OB-1 mass ratio of 100000:1), 300 g (D5 to OB-1 mass ratio of 300000:1), 500 g (D5 to OB-1 mass ratio of 500000:1), 1000 g (D5 to OB-1 mass ratio of 1000000:1) of D5 were mixed to prepare four treatment samples, which were heated to 130 °C and maintained for 30 min, and then cooled to room temperature. The treatment samples of 100 g, 300 g, 500 g and 1000 g of D5 were filtered respectively, and the filtrate was collected. Then, the filtrate was centrifuged at 10000 rpm for 5 min, and the supernatant was taken to complete the preparation of the nanoscale fluorescent whitening agent OB-1 D5 whitening solution. The particle size is shown in Table 3.

[0061] Table 3. Particle size of OB-1 under different D5 mass treatment

[0062] D5 (g) D5 to OB-1 mass ratio D0.9 (nm) D0.5 (nm) 100 100000:1 90 30 300 300000:1 88 28 500 500000:1 83 25 1000 1000000:1 85 27

[0063] Four pieces of 10g bleached polyester cloth were immersed in 100g, 300g, 500g and 1000g of D5 whitening solution of fluorescent whitening agent OB-1 treated by D5, and the excess whitening solution was removed. The weight of the four pieces of bleached polyester cloth was 18g, and an additional piece of polyester cloth without whitening treatment was taken as a control sample. Then, pre-drying was performed at 60°C for 10min, and baking was performed at 180°C for 5min. Then, soaping, drying and detection of whiteness were performed. The whiteness of the bleached polyester cloth treated by 100g, 300g, 500g and 1000g of D5 whitening solution of fluorescent whitening agent OB-1 treated by D5 was detected by spectrophotometer CS-650A of Hangzhou Caipu Technology Co., Ltd., and the whiteness was 112, 125, 135 and 131, respectively. The whiteness of the bleached polyester cloth without whitening treatment was 86.

[0064] Example 4

[0065] 10g of polyester yarn, 0.0010g (0.01%o.m.f) of OB-1 raw powder and 500g of D5 were mixed to prepare three mixed treatment samples, which were heated to 100°C, 130°C and 140°C, respectively, and kept at the temperature for 30min, and then cooled to room temperature. The 100°C, 130°C and 140°C treatment samples were filtered, respectively, and the filtrate was collected. The filtrate was centrifuged at 10000rpm for 5min, and the supernatant was taken to prepare the D5 whitening solution of nanoscale fluorescent whitening agent OB-1. The particle size is shown in Table 4.

[0066] Table 4. Particle size of OB-1 treated at different temperatures

[0067] Temperature (°C) D0.9 (nm) D0.5 (nm) 100 205 65 130 83 25 140 83 26

[0068] Three pieces of 10g bleached polyester cloth were immersed in D5 whitening solution of fluorescent whitening agent OB-1 treated by D5 at 100°C, 130°C and 140°C, respectively, and the excess whitening solution was removed. The weight of the three pieces of bleached polyester cloth was 18g, and an additional piece of polyester cloth without whitening treatment was taken as a control sample. Then, pre-drying was performed at 60°C for 10min, and baking was performed at 180°C for 5min. Then, soaping, drying and detection of whiteness were performed. The whiteness of the bleached polyester cloth treated by D5 whitening solution of fluorescent whitening agent OB-1 treated by D5 at 100°C, 130°C and 140°C was detected by spectrophotometer CS-650A of Hangzhou Caipu Technology Co., Ltd., and the whiteness was 110, 135 and 133, respectively. The whiteness of the bleached polyester cloth without whitening treatment was 86.

[0069] Example 5

[0070] Mix 10 g of polyester yarn, 0.0010 g (0.01% o.m.f) of OB-1 raw powder and 500 g of D5, prepare 5 mixed treatment samples in parallel, respectively heated to 130°C, and kept for 0 min, 10 min, 20 min, 30 min and 40 min, respectively, and then cooled to room temperature; filter the samples treated for 0 min, 10 min, 20 min, 30 min and 40 min, respectively, and collect the filtrate; then centrifuge the filtrate at a speed of 10000 rpm for 5 minutes, take the supernatant, and complete the preparation of the D5 whitening solution of the nanoscale fluorescent whitening agent OB-1. The particle size is shown in Table 5.

[0071] Table 5. Particle size of OB-1 under different holding time treatments

[0072] Soaking time (min) D0.9 (nm) D0.5 (nm) 0 164 73 10 96 47 20 88 32 30 83 25 40 84 27

[0073] Dip 5 pieces of 10 g of bleached polyester cloth into the D5 whitening solution of the fluorescent whitening agent OB-1 treated for 0 min, 10 min, 20 min, 30 min and 40 min respectively, wring out the excess whitening solution, and finally the weight of the 5 pieces of bleached polyester cloth is 18 g, and additionally take one piece of polyester cloth without whitening treatment as a control sample; then pre-dry at 60°C for 10 min, and then bake at 180°C for 5 min, and then soapy wash, dry and detect the whiteness. After the bleached polyester cloth is whitened by the D5 whitening solution of the fluorescent whitening agent OB-1 treated for 0 min, 10 min, 20 min, 30 min and 40 min, use the spectrophotometer CS-650A of Hangzhou Caipu Technology Co., Ltd., and select the built-in standard WI(CIE) to detect the whiteness, and the whiteness is 103, 111, 126, 135 and 132 respectively, while the whiteness of the bleached polyester cloth without whitening treatment is 86.

[0074] As can be seen from the above examples, the nanoscale fluorescent whitening agent, the chemical fiber and the preparation method provided by the application, by mixing the fluorescent whitening agent raw powder with the D5 solvent to obtain a fluorescent whitening agent solution, then performing fluorescent whitening treatment on the chemical fiber in the fluorescent whitening agent solution to obtain a mixed liquid after fluorescent whitening treatment, and finally filtering the mixed liquid and centrifuging the filtrate to obtain the nanoscale fluorescent whitening agent solution as the supernatant, the preparation method is simple, the preparation time is short, the dispersibility and stability are good, and it can be easily applied to the whitening treatment of polyester fibers, and no wastewater is generated during the preparation process.

[0075] The above merely provides the specific implementation of the present application, but the protection scope of the present application is not limited to this. Any person skilled in the art can easily think of various equivalent modifications or replacements within the technical range disclosed by the present application, and these modifications or replacements should be covered in the protection scope of the present application. Therefore, the protection scope of the present application should be subject to the protection scope of the claims.

Claims

1. A method of preparing a nanoscale optical brightener solution, characterized by, The application relates to a preparation method of a nano fluorescent brightener solution. The fluorescent brightener raw powder is mixed with decamethylcyclopentasiloxane D5 solvent to obtain a fluorescent brightener solution; wherein the mass ratio of the decamethylcyclopentasiloxane D5 to the fluorescent brightener raw powder is (100000-1000000):1, and the fluorescent brightener comprises fluorescent brightener OB-1. Chemical fibers are subjected to adsorption-desorption treatment in the fluorescent brightener solution to obtain a treated mixed solution. The mixed solution is filtered, and the filtrate is subjected to centrifugal separation to obtain supernatant; wherein the supernatant is a nano fluorescent brightener solution.

2. The method for preparing the nanoscale fluorescent whitening agent solution according to claim 1, characterized in that, The mass of the fluorescent brightener raw powder is 0.0010%-0.015% o.m.f.

3. The method for preparing the nanoscale fluorescent whitening agent solution according to claim 1, characterized in that, The temperature of the adsorption-desorption treatment is 100-140 DEG C, and the holding time is 0-40 min.

4. A nanoscale optical brightener characterized by, The nano fluorescent brightener solution is prepared by the preparation method of any one of claims 1-3.

5. A method for fluorescent whitening of chemical fibers, characterized in that The application relates to a fluorescent brightening treatment method of chemical fibers. The chemical fibers are subjected to immersion and pad treatment in the nano fluorescent brightener solution of claim 4 to obtain chemical fibers after immersion and pad treatment. The chemical fibers after immersion and pad treatment are subjected to pre-drying, baking, washing and drying treatment respectively to obtain chemical fibers after fluorescent brightening treatment.

6. The method for the fluorescent whitening treatment of chemical fibers according to claim 5, characterized in that, The liquid retention rate of the chemical fibers after immersion and pad treatment is 70-90%.

7. The method for the fluorescent whitening treatment of chemical fibers according to claim 5, characterized in that, The temperature of the pre-drying is 50-70 DEG C, and the pre-drying time is 5-15 min; or / and The temperature of the baking is 150-210 DEG C, and the baking time is 3-8 min.

8. The method for the fluorescent whitening treatment of chemical fibers according to claim 5, characterized in that, The chemical fibers are one or more of polyester fibers, polyamide fibers and polypropylene fibers.

9. A chemical fiber treated with a nanoscale optical brightener, characterized by, The chemical fibers are prepared by the fluorescent brightening treatment method of any one of claims 5-8.