Light-absorbing heat storage down feather and preparation method thereof
By loading metal ions through the formation of chelate covalent bonds on down fibers, the problem of low adsorption rate of metal ions on the surface of down fibers is solved, achieving efficient light absorption, heat storage and warmth retention performance, while maintaining good loft.
Patent Information
- Application Number
- CN202410947272.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-07-16
- Publication Date
- 2026-01-16
- Estimated Expiration
- 2044-07-16
AI Technical Summary
In existing technologies, the surface modification of down fibers with metal ions or their oxides has low adsorption rate and poor wash fastness, resulting in limited improvement in warmth retention.
After pretreating down fibers with an aqueous solution of sodium hexametaphosphate or sodium glycerophosphate, they are impregnated with a solution of molybdenum sulfate or zirconium sulfate and subjected to oscillation treatment in an electromagnetic field to form chelate covalent bonds, thereby increasing the loading and fastness of metal ions on the down surface.
It significantly improves the light absorption and heat storage performance and infrared temperature rise performance of down, maintains excellent warmth retention performance and is washable, and the down has good loft.
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Abstract
Description
TECHNICAL FIELD
[0001] The application belongs to the technical field of down processing, and particularly relates to a light-absorbing heat-storing down and a preparation method thereof. BACKGROUND
[0002] Down fibers are natural biomass materials, have the characteristics of light texture, fluffy softness, strong warmth retention, etc., and are widely used in cold-weather clothing. Because down fibers are mainly protein macromolecules, they contain rich protein residues and active functional groups, and the development of functional down based on chemical modification / grafting has become a research hotspot in recent years.
[0003] With the development trend of lightweight clothing, how to further improve the warmth retention performance of down fibers has attracted extensive research. At present, by grafting, coating / embedding, etc., copper, zinc, zirconium and other metal ions or their oxides are modified on the down fibers, which can endow the down with light-absorbing heat-storing property and improve the warmth retention performance of the down. However, due to the hydrophobic nature of the down surface, the surface modification takes a long time, the adsorption rate of metal ions and their oxides is low, and the interaction between the metal ions and the down protein macromolecules is weak, which has problems such as poor washing fastness, etc., and therefore the application effect needs to be further improved.
[0004] Based on this, the application provides a light-absorbing heat-storing down and a preparation method thereof. SUMMARY
[0005] The purpose of the present application is to provide a light-absorbing heat-storing down and a preparation method thereof to solve the above problems.
[0006] The present application achieves the above-mentioned purpose by the following technical solutions:
[0007] As a first aspect of the present application, the present application provides a preparation method of a light-absorbing heat-storing down, comprising the following steps:
[0008] (1) performing degreasing treatment on the down raw material after cleaning and impurity removal;
[0009] (2) immersing the down raw material treated in step (1) in a pretreatment solution for oscillation treatment, and then immersing it in a molybdenum sulfate or zirconium sulfate solution for oscillation treatment;
[0010] (3) washing the down raw material treated in step (2) with clean water and then drying it;
[0011] (4) oscillating the down raw material treated in step (3) in an electromagnetic field to obtain the light-absorbing heat-storing down.
[0012] As a further optimization scheme of the present application, the step (1) is specifically that the down raw material is added into water and a degreasing agent, and the degreasing is performed at a temperature of 40-45 DEG C for 30-60 min, wherein the mass ratio of the down raw material to water is 1:30-50, and the mass ratio of the degreasing agent to water is 2-5 g:1 L.
[0013] As a further optimization scheme of the present application, in the step (2), the pretreatment liquid is a sodium hexametaphosphate aqueous solution or a sodium glycerophosphate aqueous solution with a mass concentration of 15-20 g / L, and the mass concentration of the molybdenum sulfate or zirconium sulfate solution is 2-4 g / L.
[0014] As a further optimization scheme of the present application, in the step (2), the oscillation treatment is performed at 30-60 DEG C for 2-3 h.
[0015] As a further optimization scheme of the present application, in the step (2), the bath ratio of the down raw material to the pretreatment liquid is 1:100-150, and the bath ratio of the down raw material to the molybdenum sulfate or zirconium sulfate solution is 1:100-150.
[0016] As a further optimization scheme of the present application, the drying treatment in the step (3) is specifically that the down raw material cleaned by water is sent to a hot air drying equipment for hot air drying, and the process parameters of the hot air drying equipment are that the air speed is 3-5 m / s and the drying temperature is 30-50 DEG C.
[0017] As a further optimization scheme of the present application, the step (4) is specifically that the down raw material treated by the step (3) is put into a magnetic field generator, and the down raw material is treated under the conditions that the magnetic field strength is 0.5-1.0 T and the oscillation frequency is 10-15 times / s for 5-10 min.
[0018] As a second aspect of the present application, the present application further provides a light-absorbing heat-storing down, which is prepared by any of the above preparation methods.
[0019] The present application has the following beneficial effects:
[0020] In the present application, the down raw material is first treated by a pretreatment liquid and then immersed in a molybdenum sulfate or zirconium sulfate solution, and the sodium hexametaphosphate or sodium glycerophosphate used in the pretreatment liquid enables the metal ions to be bonded to the surface of the down in a chelate covalent bond manner, so that the load amount and the load firmness of the metal ions on the surface of the down are greatly improved, the down is endowed with strong light-absorbing heat-storing performance, the down can maintain excellent infrared temperature rise and heat preservation performance after being washed for many times, and the down has good loftiness and excellent comprehensive performance. DETAILED DESCRIPTION
[0021] Further detailed description of the present application is made below, it is necessary to point out here that the following detailed embodiments are only used to further illustrate the present application, and cannot be understood as limiting the scope of protection of the present application, and the skilled in the art can make some non-essential improvements and adjustments to the present application according to the above application content.
[0022] The specific method is not specified in the following examples, and can be carried out according to the conventional method. The materials, reagents, etc. used, if not specially specified, can be obtained through commercial channels.
[0023] Example 1
[0024] The present embodiment provides a preparation method of light-absorbing heat-storing down feather, comprising the following steps:
[0025] (1) The down feather raw material is added to water and a degreasing agent, and degreased at a temperature of 40℃ for 60min, wherein the mass ratio of the down feather raw material to water is 1:30, the dosage ratio of the degreasing agent to water is 5g:1L, and the degreasing agent is dodecyl betaine (BS-12);
[0026] (2) A sodium hexametaphosphate aqueous solution with a mass concentration of 15g / L and a molybdenum sulfate solution with a mass concentration of 2g / L are prepared, and the calculated amount of the down feather raw material treated in step (1) is immersed in 5000ml of the sodium hexametaphosphate aqueous solution with a mass concentration of 15g / L according to a bath ratio (g:ml) of 1:100, and oscillated and treated at 60℃ for 2h, and then the pretreated down feather is immersed in 5000ml of the molybdenum sulfate solution with a mass concentration of 2g / L according to a bath ratio (g:ml) of 1:100, and oscillated and treated at 60℃ for 2h;
[0027] (3) The down feather raw material treated in step (2) is washed with water, and then sent to a hot air drying equipment for hot air drying, and the process parameters of the hot air drying equipment are as follows: air speed is 3m / s, and drying temperature is 50℃;
[0028] (4) The down feather raw material treated in step (3) is put into a magnetic field generator, and treated under the condition of a magnetic field strength of 0.5T and an oscillation frequency of 15 times / s for 5min, so that the light-absorbing heat-storing down feather is obtained.
[0029] Example 2
[0030] The present embodiment provides a preparation method of light-absorbing heat-storing down feather, comprising the following steps:
[0031] (1) The down feather raw material is added to water and a degreasing agent, and degreased at a temperature of 45℃ for 30min, wherein the mass ratio of the down feather raw material to water is 1:50, the dosage ratio of the degreasing agent to water is 2g:1L, and the degreasing agent is dodecyl betaine (BS-12);
[0032] (2) A sodium hexametaphosphate solution with a mass concentration of 20 g / L and a molybdenum sulfate solution with a mass concentration of 4 g / L are prepared, and the calculated amount of the down raw material treated in step (1) is immersed in 5000 ml of the sodium hexametaphosphate solution with a mass concentration of 20 g / L at a bath ratio (g: ml) of 1: 100, and oscillation treatment is performed at 30°C for 3 h, and then the pretreated down is immersed in the molybdenum sulfate solution with a mass concentration of 4 g / L at a bath ratio (g: ml) of 1: 100, and oscillation treatment is performed at 30°C for 3 h;
[0033] (3) The down raw material treated in step (2) is washed with water and then sent to a hot air drying device for hot air drying, and the process parameters of the hot air drying device are that the air speed is 5 m / s and the drying temperature is 30°C;
[0034] (4) The down raw material treated in step (3) is put into a magnetic field generator, and the magnetic field strength is 1.0T and the oscillation frequency is 10 times / s, and the treatment is performed for 10 min, and the light-absorbing heat-storing down is obtained.
[0035] Example 3
[0036] The embodiment provides a preparation method of light-absorbing heat-storing down, which comprises the following steps:
[0037] (1) The down raw material is added into water and a degreasing agent, and degreasing is performed at a temperature of 40°C for 60 min, wherein the mass ratio of the down raw material to water is 1:45, and the amount ratio of the degreasing agent to water is 3.5g:1L, and the degreasing agent is dodecyl betaine (BS-12);
[0038] (2) A sodium glycerophosphate solution with a mass concentration of 18 g / L and a zirconium sulfate solution with a mass concentration of 3 g / L are prepared, and the calculated amount of the down raw material treated in step (1) is immersed in 5000 ml of the sodium glycerophosphate solution with a mass concentration of 18 g / L at a bath ratio (g: ml) of 1: 150, and oscillation treatment is performed at 45°C for 2 h, and then the pretreated down is immersed in 5000 ml of the zirconium sulfate solution with a mass concentration of 3 g / L at a bath ratio (g: ml) of 1: 150, and oscillation treatment is performed at 45°C for 2 h;
[0039] (3) The down raw material treated in step (2) is washed with water and then sent to a hot air drying device for hot air drying, and the process parameters of the hot air drying device are that the air speed is 4 m / s and the drying temperature is 40°C;
[0040] (4) The down raw material treated in step (3) is put into a magnetic field generator, and the magnetic field strength is 0.8T and the oscillation frequency is 12 times / s, and the treatment is performed for 7 min, and the light-absorbing heat-storing down is obtained.
[0041] Verification test
[0042] 1. To explore the effect of pretreatment liquid on the performance of down, the following comparative examples were set up:
[0043] Comparative Example 1
[0044] The difference between this comparative example and Example 1 is in step (2): a glycerol sodium phosphate aqueous solution with a mass concentration of 15 g / L and a molybdenum sulfate solution with a mass concentration of 2 g / L were prepared, and the calculated amount of down raw material treated in step (1) was immersed in 5000 ml of the glycerol sodium phosphate aqueous solution with a mass concentration of 15 g / L according to a bath ratio (g: ml) of 1:100, and treated by oscillation at 60°C for 2 h, and then the pretreated down was immersed in 5000 ml of the molybdenum sulfate solution with a mass concentration of 2 g / L according to a bath ratio (g: ml) of 1:100, and treated by oscillation at 60°C for 2 h.
[0045] Comparative Example 2
[0046] The difference between this comparative example and Example 1 is in step (2): a phosphoric acid solution with a mass concentration of 15 g / L and a molybdenum sulfate solution with a mass concentration of 2 g / L were prepared, and the calculated amount of down raw material treated in step (1) was immersed in 5000 ml of the glycerol sodium phosphate aqueous solution with a mass concentration of 15 g / L according to a bath ratio (g: ml) of 1:100, and treated by oscillation at 60°C for 2 h, and then the pretreated down was immersed in 5000 ml of the molybdenum sulfate solution with a mass concentration of 2 g / L according to a bath ratio (g: ml) of 1:100, and treated by oscillation at 60°C for 2 h.
[0047] Comparative Example 3
[0048] The difference between this comparative example and Example 1 is in step (2): cyclodextrin with a mass concentration of 15 g / L and citric acid with a mass concentration of 3.75 g / L were taken, and the concentration ratio of sodium hypophosphite to citric acid was 4:5, and the dry down raw material was immersed in the solution according to a bath ratio of 1:150, and placed in a water bath kettle for heating and stirring, and modified down was obtained after reaction for 4 h, and then the pretreated down was immersed in 5000 ml of a molybdenum sulfate solution with a mass concentration of 2 g / L according to a bath ratio (g: ml) of 1:100, and treated by oscillation at 60°C for 2 h.
[0049] Comparative Example 4
[0050] The difference between this comparative example and Example 1 is in step (2): the down raw material was immersed in 5000 ml of a molybdenum sulfate solution with a mass concentration of 2 g / L according to a bath ratio (g: ml) of 1:100, and treated by oscillation at 60°C for 2 h.
[0051] The down obtained by preparing examples 1-3 and comparative examples 1-4 was subjected to infrared temperature rise performance test and heat retention performance test, and the down subjected to defatting treatment in step (1) was taken as a control group, and the specific process was as follows:
[0052] (1) Infrared temperature rise performance test: according to GB / T 30127-2013 “Textiles Far Infrared Performance and Evaluation”, the infrared temperature rise instrument was used to test the temperature rise change of the down under the same initial temperature condition. The specific test operation was as follows: 0.5 g of down was taken from each group and laid flat in the test circular groove (radius 3 cm, depth 3 cm), the sample surface was flattened, and the down surface received infrared light source radiation, wherein the infrared radiation source wavelength was 5-14 μm, the radiation power was 150 W, and the temperature of the sample was recorded at intervals of 30 s. Each sample was tested 5 times, and the average value was taken.
[0053] (2) Heat retention performance test: flat plate type heat retention instrument was used for test. The specific operation was as follows: 10 g of down was taken from each group and put into a 30 cm x 30 cm pure cotton cloth sample bag, sealed and laid flat in the specified area for test, the test temperature was 25℃, and the relative humidity was 65%. Each sample was tested 5 times, and the average value was taken.
[0054] The results are shown in Table 1.
[0055] Table 1. Result statistics table
[0056]
[0057] As can be seen from Table 1, compared with the control group, examples 1-3 use molybdenum metal ions or zirconium metal ions to modify the down, which can impart the down with light absorption and heat storage properties due to the far infrared effect of metal ions and their oxides, and can improve the heat retention performance of the down, so that the down has excellent infrared temperature rise performance, and the temperature rise after 30 s of infrared radiation is as high as 2.7℃.
[0058] In addition, comparative example 4 uses a pretreatment liquid to treat the down before modifying the down with molybdenum metal ions, and the data results show that the infrared temperature rise and warmth retention rate of the down of comparative example 4 are not as good as those of examples 1 and comparative examples 1-3, which shows that using a pretreatment liquid to treat the down before modifying the down with metal ions has a positive effect on improving the infrared temperature rise and warmth retention rate of the down.
[0059] The types of pretreatment liquids used in examples 1 and comparative examples 1-2 are different, the pretreatment liquid of example 1 is a sodium hexametaphosphate aqueous solution, the pretreatment liquid of comparative example 1 is a glycerol sodium phosphate aqueous solution, and the pretreatment liquid of comparative example 2 is a phosphoric acid solution. In addition, comparative example 3 is different from example 1 in that the pretreatment liquid is modified by a cyclodextrin inclusion method, and the results show that the effects of examples 1-2 on improving the infrared temperature rise and warmth retention rate of the down are not as good as that of example 1, and comparative example 3 is equivalent to example 1.
[0060] Since the heat retention performance of down is positively correlated with the loading amount of metal ions on the down fibers, based on the differences between Comparative Examples 1-4 and Example 1, the Mo 6+ loading amount on the surface of down washed 0 and 10 times was further tested.
[0061] The specific test method is as follows: the mass concentration of Mo 6+ in the molybdenum sulfate solution before and after treatment is tested by inductively coupled plasma atomic emission spectrometry (ICP-AES). Six Mo (SO4)3standard solution solutions with different gradients (5, 20, 40, 60, 80, and 100 mg / L) are prepared, and the ion intensity is tested at a wavelength of 470 nm, which corresponds to the characteristic absorption of Mo 6+ . Then, the standard curve is constructed according to the tested ion intensity, and the equation is y = 2132x + 43805 (in the equation, y is the intensity, 10 5 (count·s -1 ); x is the mass concentration, mg / L).
[0062] The loading amount of Mo 6+ on the surface of down fibers is calculated according to the following formula: η = (ΔC × V) / m; in the formula: η is the loading amount of Mo 6+ , mg / g; ΔC is the mass concentration difference of Mo 6+ in the molybdenum sulfate solution before and after treatment, mg / L; V is the volume of Mo 6+ solution to be adsorbed, mL; m is the mass of down, g.
[0063] The method for washing down is as follows: 1 g of down is immersed in 500 mL of distilled water, and washed at 40°C with shaking every 15 min. The mass concentration of Mo 6+ in the water after washing is determined.
[0064] The results are shown in Table 2.
[0065] Table 2. Result statistics table
[0066]
[0067] As can be seen from Table 2, the Mo 6+ loading amount on the surface of down in Example 1 is the highest, while the unmodified down in Comparative Example 4 is hydrophobic, lacks active functional groups, and has few Mo 6+ binding sites, mainly relying on physical adsorption, and the ability of down to adsorb Mo 6+ on the surface is not as good as that of Example 1.
[0068] After the down jacket in Example 1 is treated by immersion in a sodium hexametaphosphate aqueous solution, the down surface adsorbs Mo 6+The ability of the down surface to adsorb Mo 6+ The Mo 6+ load of the down surface was significantly enhanced. In addition, the Mo 6+ load of the down surface was tested after 10 washes, and it was found that the Mo 6+ load of the down surface of Example 1 was significantly higher than that of Comparative Examples 1-3. 6+ The Mo
[0069] 2. To further explore the influence of the preparation process on the loft of the down, the following comparative examples were further set up:
[0070] Comparative Example 5
[0071] The difference between this comparative example and Example 1 is that step (4) is not performed.
[0072] Comparative Example 6
[0073] The difference between this comparative example and Comparative Example 4 is that step (4) is not performed.
[0074] The down samples prepared in Example 1 and Comparative Examples 1-5, and the control group were subjected to loft determination. Specifically, 20 g of sample was taken from each group, dried at 70°C, and after 45 min, the sample was shaken by hand into a pretreatment box to fully fluff the sample. The sample was allowed to stand for 24 h under the conditions of a temperature of 20°C and a relative humidity of 65%. 18 g of sample was accurately weighed in the pretreatment box, gently moved to a national standard loft meter, and stirred evenly with a glass rod. The sample was lightly pressed by an aluminum pressure plate, and the pressure plate was allowed to fall naturally. After the aluminum plate stopped falling, it was allowed to stand for 1 min, and the scale on both sides of the loft meter was recorded. The test was repeated 5 times, and the average value was taken.
[0075] The results are shown in Table 3.
[0076] Table 3. Test results of down performance
[0077]
[0078]
[0079] As can be seen from Table 3, the loft of the down treated by the processing method disclosed in Example 1 is better than that of the down obtained by treating by other comparative examples.
[0080] Comparing the data of Comparative Example 5 with Example 1, it can be seen that the down of Comparative Example 5 is not subjected to the magnetization treatment of step (4), and the loft of the down is not as good as that of Example 1, because the straightening of the down fiber molecules under the action of the electromagnetic field can promote the compression resistance of the down fibers, and thus the loft of the down is improved to a certain extent. In addition, the loft of Comparative Example 5 is not as good as that of the control group, which shows that the treatment of step (2) has an impact on the loft, and the addition of step (4) can make up for the loss of the loft of the down caused by the treatment of step (2), and is helpful to the recovery and improvement of the loft of the down. In addition, compared with Example 1, the loft of the down treated by the cyclodextrin inclusion of Comparative Example 3 is not as good as that of Example 1.
[0081] The above examples only express several embodiments of the present application, and the description is more specific and detailed, but it cannot be understood as a limitation on the scope of the patent of the present application. It should be pointed out that for ordinary skilled persons in the art, several modifications and improvements can be made without departing from the concept of the present application, and these all belong to the protection scope of the present application.
Claims
1. A method for preparing a light-absorbing heat-storing down feather, characterized by comprising the steps of: The method comprises the following steps: (1) defatting treatment of the cleaned and impurity-removed down raw material; (2) oscillation treatment of the down raw material treated in step (1) in a pretreatment liquid and then in a molybdenum sulfate or zirconium sulfate solution, the pretreatment liquid being a 15-20 g / L sodium hexametaphosphate aqueous solution, and the mass concentration of the molybdenum sulfate or zirconium sulfate solution being 2-4 g / L; (3) water cleaning and drying of the down raw material treated in step (2); (4) oscillation treatment of the down raw material treated in step (3) in an electromagnetic field to obtain the light-absorbing heat-storing down; The step (4) is specifically that the down raw material treated in step (3) is put into a magnetic field generator, the magnetic field strength is 0.5-1.0 T, the oscillation frequency is 10-15 times / s, and the treatment time is 5-10 min.
2. The method for preparing the light-absorbing heat-storing down feather according to claim 1, characterized in that: The step (1) is specifically that the down raw material is added into water and a defatting agent, the defatting time is 30-60 min at a temperature of 40-45 °C, the mass ratio of the down raw material to water is 1:30-50, and the amount ratio of the defatting agent to water is 2-5 g:1 L.
3. The method for preparing a light-absorbing and heat-storing down according to claim 1, characterized in that: In the step (2), the oscillation treatment is performed at 30-60 °C for 2-3 h.
4. The method for preparing a light-absorbing heat-storing down according to claim 1, characterized in that: In the step (2), the bath ratio of the down raw material to the pretreatment liquid is 1:100-150, and the bath ratio of the down raw material to the molybdenum sulfate or zirconium sulfate solution is 1:100-150.
5. The method for preparing a light-absorbing and heat-storing down according to claim 1, characterized in that: The drying treatment in the step (3) is specifically that the water-cleaned down raw material is sent to a hot air drying equipment for hot air drying, the air speed of the hot air drying equipment is 3-5 m / s, and the drying temperature is 30-50 °C.
6. A light-absorbing heat-accumulating down feather, characterized by: The light-absorbing heat-storing down is prepared by the method of any one of claims 1-5.
Citation Information
Patent Citations
Self-heating functional material as well as preparation method and application thereof
CN112941919A