Reagent for quickly decolorizing down feather and quick decolorizing method for down feather

Abstract

The invention discloses a reagent for fast decolorization of down feather and a fast decolorization process of down feather, and the reagent for fast decolorization of down feather is prepared by the following steps: successively adding n-butyl alcohol, citric acid and bis (ethyl acetoacetate) diisopropyl titanate into a reaction container, introducing protective gas, stirring, gradually heating to melt the solid, and reacting at a constant temperature; adding citric acid, reacting at 120-160 DEG C, cooling, adding an organic solvent to dissolve the product, and dropwise adding sufficient hydrochloric acid into the solution, so that the product is separated out, subjected to suction filtration and subjected to vacuum drying; obtaining the reagent for quickly decolorizing the down feather. And the down feather is treated by complexing, oxidizing and reducing ferrous ions by using the reagent for quickly decolorizing the down feather. Bleaching at a lower temperature is realized, and more than 50% of energy consumption is saved. The lower temperature is beneficial to protection of non-pigment protein, and the bulkiness of the bleached down feather is remarkably improved. The consumption of the hydrogen peroxide is obviously reduced, the damage to the down feather is reduced, and a relatively high whiteness level is ensured.

Description

Technical Field

[0001] The invention relates to a reagent for rapid decolorization of down and a rapid decolorization method of down, belonging to the technical field of decolorization of colored down. Background Art

[0002] Down is classified into white down and colored down according to color. In order to make down jackets with light-colored fabrics more beautiful, colored down is treated by bleaching and whitening. Bleaching of gray, black and other colored down can improve the appearance. Appropriate bleaching treatment can exceed the quality of white down in terms of fluffiness and whiteness. It is of great significance to increase the added value of this type of down, expand the production of down, and reduce the selling price. The annual demand is tens of millions of tons. The existing down decolorization method has two major problems: the process time is too long and the down is seriously damaged. This greatly limits the increase in production and affects the quality of bleached down. How to prepare a down rapid decolorizing agent and a down rapid decolorization method has become a problem to be solved. Summary of the invention

[0003] The invention aims to provide a reagent for rapid decolorization of down. The prepared reagent has a branched structure and can improve the adsorption of ferrous ions for oxidation by the down.

[0004] Another object of the present invention is to provide a method for rapid decolorization of down, by using a reagent for rapid decolorization of down to improve the adsorption of ferrous ions, a lower temperature can be used, energy consumption can be reduced, and damage to the down can be reduced.

[0005] To solve the above technical problems, the purpose of the present invention is achieved as follows:

[0006] The invention relates to a reagent for rapid decolorization of down, and the preparation method of the reagent for rapid decolorization of down is as follows:

[0007] Add n-butanol, citric acid and diisopropyl bis(ethyl acetoacetate) titanate into the reaction vessel one by one, pass protective gas, stir, gradually increase the temperature to melt the solid, and react at a constant temperature of 120-160° C. for 1-5 hours;

[0008] Add citric acid, maintain 120-160°C, react for 1-5 hours, add an organic solvent to dissolve the product after cooling, and drop sufficient hydrochloric acid into the solution to precipitate the product, filter it, and vacuum dry it at 30-90°C for 8-48 hours; thus, a reagent for rapid decolorization of down is obtained;

[0009] The reaction formula is as follows:

[0010]

[0011] On the basis of the above scheme and as a preferred scheme of the above scheme: the amount of n-butanol used is 13.6g, the amount of citric acid used is 11.9-76g, and the mass fraction of bis(ethyl acetoacetate) diisopropyl titanate is 0.1-0.6%.

[0012] On the basis of the above scheme and as a preferred scheme of the above scheme: the organic solvent is acetone.

[0013] The present invention also relates to a method for rapid decolorization of down, which comprises the following steps arranged in sequence:

[0014] Ferrous ion complexation: At room temperature, soak the down in an aqueous solution containing a reagent for rapid decolorization of down and JFC penetrant for a set time according to the first bath ratio; then add ferrous sulfate, sodium bisulfite and hydrosulfite, adjust the pH value of the solution to 3-5, and add warm water to the second bath ratio, stir for 5-30 minutes, and drain; then rinse the down with 10-50℃ water to remove the iron ions adsorbed on the non-pigmented proteins of the down;

[0015] Oxidation: immerse the down in an oxidation treatment solution and stir for 10-60 minutes at 10-40°C; the preparation process of the oxidation treatment solution is: first add sodium pyrophosphate and hydrogen peroxide stabilizer into water, then add a penetrant, and finally add hydrogen peroxide;

[0016] Reduction: Place the down in a reduction treatment solution, and soak it under stirring at 10-50°C for 1-3 hours. The reduction treatment solution is a mixed solution containing 1-9g / L sodium dithionite and 0.1-4g / L thiourea dioxide, and then sodium pyrophosphate is added; the amount of sodium pyrophosphate used is 2-10g / L.

[0017] On the basis of the above scheme and as a preferred scheme of the above scheme: the concentration of the reagent for rapid decolorization of down is 0.1-3g / L, and the concentration of the JFC penetrant is 0.5-2g / L.

[0018] On the basis of the above scheme and as a preferred scheme of the above scheme: the first bath ratio is 1:10, the second bath ratio is 1:15-50; and the setting time is 10 minutes.

[0019] On the basis of the above scheme and as a preferred scheme of the above scheme: the dosage of ferrous sulfate is 1-30 g / L; the dosage of sodium bisulfite is 1-2 g / L; and hydrochloric acid is used to adjust the pH value of the solution.

[0020] Compared with conventional processes, it has the following advantages:

[0021] (1) A lower temperature is achieved, bleaching can be done at 10-50°C, saving more than 50% of energy consumption.

[0022] (2) Lower temperatures are beneficial to the protection of non-pigmented proteins and significantly improve the fluffiness of bleached down.

[0023] (3) The applicability of the process is greatly improved, allowing the use of relatively simple treatment equipment without heating and constant temperature functions, and allowing the use of a one-step water heating method, such as adding 50°C hot water at one time. Conventional processes require a continuous constant temperature of 50°C.

[0024] (4) It significantly reduces the consumption of hydrogen peroxide, reduces the damage to down, and ensures a higher level of whiteness.

[0025] The above beneficial effects are all due to the fact that the ferrous ions are fully adsorbed onto the colored protein particles by complexation, which can significantly improve the oxidation efficiency of hydrogen peroxide and reduce the amount of hydrogen peroxide used, oxidation time and oxidation temperature. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] Figure 1 This is a comparison table of the test results of the ferrous ion adsorption efficiency of the reagent for rapid decolorization of down prepared in Example 1;

[0027] Figure 2 This is a liquid chromatogram of the reagent for rapid decolorization of down prepared in Example 1. DETAILED DESCRIPTION

[0028] The present invention is further described below in conjunction with specific embodiments.

[0029] Embodiment 1

[0030] The down rapid decolorization reagent involved in this embodiment is a hyperbranched molecule. The preparation method of the down rapid decolorization reagent is as follows:

[0031] S1. Add n-butanol, citric acid and diisopropyl bis(ethyl acetoacetate) titanate into a reaction vessel one by one, pass protective gas, stir, gradually increase the temperature to melt the solid, and react at a constant temperature of 120-160° C. for 1-5 hours.

[0032] Furthermore, the protective gas used in S1 is nitrogen, and the stirring is magnetic stirring.

[0033] Further, in S1, the amount of n-butanol is 13.6 g, the amount of citric acid is 11.9-76 g, and the mass fraction of diisopropyl bis(ethyl acetoacetate) titanate is 0.1-0.6%. Specifically in this embodiment, the amount of citric acid is 15 g, and the mass fraction of diisopropyl bis(ethyl acetoacetate) titanate is 0.3%.

[0034] S2, adding citric acid, maintaining 120-160°C, reacting for 1-5 hours, adding an organic solvent to dissolve the product after cooling, and dropping sufficient hydrochloric acid into the solution to precipitate the product, filtering it, and vacuum drying it at 30-90°C for 8-48 hours; thus, a reagent for rapid decolorization of down is obtained.

[0035] Specifically in this embodiment, after adding citric acid, the temperature was maintained at about 140° C. and the reaction was carried out for 3 hours; after filtration, vacuum drying was carried out at 60° C. for 24 hours.

[0036] Furthermore, the amount of citric acid added in S2 is 0.1 mol. The organic solvent used is acetone.

[0037] The reaction formula is as follows:

[0038]

[0039] The ferrous ion adsorption efficiency of the prepared down rapid decolorization reagent was tested and compared: two cups of solution with a ferrous ion concentration of 8g / L were prepared, one of which contained 1g / L of the down rapid decolorization reagent. At 25°C, 100g of down was soaked in the two solutions according to the bath ratio of 1:15 (i.e. 1kg of down, 15L of water), and then taken out after soaking for a specific time, rinsed with clean water, and then dried at 120°C for 1h, and then taken out and rehumidified in a constant temperature and humidity chamber for 24 hours. The data obtained can be seen in Figure 1 .exist Figure 1 The addition of hyperbranched molecules shown in the figure refers to the addition of the down rapid decolorization reagent prepared in this example, which can effectively improve the adsorption efficiency of ferrous ions.

[0040] Embodiment 2

[0041] The present embodiment relates to a method for rapid decolorization of down, which comprises the following steps arranged in sequence: ferrous ion complexation, oxidation and reduction.

[0042] Ferrous ion complexation means that at room temperature, the down is immersed in an aqueous solution containing a reagent for rapid decolorization of down and JFC penetrant for a set time according to the first bath ratio; then ferrous sulfate, sodium bisulfite and insurance powder are added, the pH value of the solution is adjusted to 3-5 with hydrochloric acid, and warm water is added to the second bath ratio, stirred for 5-30 minutes, and the liquid is drained; then the down is rinsed with 10-50℃ water to remove the iron ions adsorbed on the non-pigmented proteins of the down.

[0043] Further, the concentration of ferrous sulfate is 1-30 g / L, the concentration of sodium bisulfite is 1-2 g / L, and the concentration of hydrosulfite is 1-2 g / L. In this embodiment, 15 g / L, 1.5 g / L and 1.5 g / L are selected in sequence.

[0044] Further, the concentration of the down rapid decolorization reagent is 0.1-3 g / L, and the concentration of the JFC penetrant is 0.5-2 g / L. In this embodiment, 1.5 g / L and 1.3 g / L are selected respectively.

[0045] In the ferrous ion complexation step, the first bath ratio is 1:10, the second bath ratio is 1:15-50, and the setting time is 10 minutes. Specifically, in this embodiment, the second bath ratio is selected to be 1:15. After replenishing to the second bath ratio, stir for 25 minutes, and then rinse the down with 35°C water.

[0046] Oxidation refers to immersing the down complexed with ferrous ions into an oxidation treatment solution with a bath ratio of 1:15-50, and then stirring for 10-60 minutes at 10-40°C; the preparation process of the oxidation treatment solution is: first add sodium pyrophosphate and hydrogen peroxide stabilizer into water, then add a penetrant, and finally add hydrogen peroxide. The bath ratio in this step is 1:15.

[0047] In the process of preparing the oxidation treatment solution, the order of adding reagents must be followed: sodium pyrophosphate and hydrogen peroxide stabilizer, water; penetrant, hydrogen peroxide. After the oxidation treatment solution is prepared, add the down sewn with ferrous ions.

[0048] The conventional down processing process involves immersing the down in an oxidation treatment solution at a process temperature of 50-70°C for 3-12 hours.

[0049] The oxidation step has the following advantages over conventional treatment processes:

[0050] A lower temperature is achieved, bleaching can be done at 10-50℃, saving more than 50% of energy consumption. Lower temperature is conducive to the protection of non-pigmented proteins and significantly improves the fluffiness of bleached down.

[0051] The applicability of the process has been greatly improved, allowing the use of simpler processing equipment without heating and constant temperature functions, and allowing the use of a one-step water heating method. For example, adding 50°C hot water at one time will also oxidize the down during the cooling process of the hot water. The conventional process requires a continuous constant temperature of 50°C.

[0052] It significantly reduces the consumption of hydrogen peroxide, reduces the damage to down, and ensures a higher level of whiteness.

[0053] The above advantages are all due to the previous step of complexation, which allows the ferrous ions to be fully adsorbed onto the colored protein particles of the down, which can significantly improve the oxidation efficiency of hydrogen peroxide and reduce the amount of hydrogen peroxide used, oxidation time and oxidation temperature.

[0054] Reduction refers to placing the oxidized down in a reduction treatment solution, stirring and soaking it at 10-50°C for 1-3 hours, wherein the reduction treatment solution is first prepared with a mixed solution containing 1-9g / L sodium dithionite and 0.1-4g / L thiourea dioxide, and then sodium pyrophosphate is added; the amount of sodium pyrophosphate used is 2-10g / L.

[0055] Specifically in this embodiment, the reduction treatment solution is first prepared as a mixed solution containing 5g / L sodium dithionite and 2g / L thiourea dioxide under stirring and immersion at 30°C for 2 hours, and then sodium pyrophosphate is added; the amount of sodium pyrophosphate used is 6g / L.

[0056] The quality of the treated down is tested, including:

[0057] Process comparison, temperature and energy consumption comparison (taking the typical case of processing 1 ton of down as an example, the water temperature starts from 0℃ and heats up) Q=C*M*ΔT.

[0058] Down whiteness measurement method: Put the down in a plastic bag of a certain size, exhaust the air in the bag as much as possible, and seal the bag to ensure that the down layer is not transparent during the test. Randomly select 6 different areas of each sample for testing and take the average value.

[0059] The down fluffiness measurement method is based on FZ / T 80001-2002 “Test method for washed feathers and down”.

[0060] The test results are shown in Table 1.

[0061] Table 1 Comparison between conventional technology and this embodiment

[0062]

[0063] It can be seen from the above table that the down treated in this embodiment has higher whiteness and fluffiness, and can shorten the processing time and significantly reduce energy consumption.

[0064] The preferred specific embodiments of the present invention are described in detail above. It should be understood that a person skilled in the art can make many modifications and changes based on the concept of the present invention without creative work. Therefore, any technical solution that can be obtained by a person skilled in the art through logical analysis, reasoning or limited experiments based on the concept of the present invention on the basis of the prior art should be within the scope of protection determined by the claims.

Claims

1. A reagent for rapid decolorization of down, characterized in that: The preparation method of the reagent for rapid decolorization of down is as follows: Add n-butanol, citric acid and diisopropyl bis(ethyl acetoacetate) titanate into the reaction vessel one by one, pass protective gas, stir, gradually increase the temperature to melt the solid, and react at a constant temperature of 120-160° C. for 1-5 hours; Add citric acid, maintain 120-160°C, react for 1-5 hours, add an organic solvent to dissolve the product after cooling, and drop sufficient hydrochloric acid into the solution to precipitate the product, filter it, and vacuum dry it at 30-90°C for 8-48 hours; thus, a reagent for rapid decolorization of down is obtained; The reaction formula is as follows:

2. A reagent for rapid decolorization of down according to claim 1, characterized in that: The dosage of n-butanol is 13.6 g, the dosage of citric acid is 11.9-76 g, and the mass fraction of diisopropyl bis(ethyl acetoacetate) titanate is 0.1-0.6%.

3. A reagent for rapid decolorization of down according to claim 1, characterized in that: The organic solvent is acetone.

4. A method for rapid decolorization of down, characterized in that: The method comprises the following steps arranged in sequence: Ferrous ion complexation: At room temperature, soak the down in an aqueous solution containing a reagent for rapid decolorization of down and JFC penetrant for a set time according to the first bath ratio; then add ferrous sulfate, sodium bisulfite and hydrosulfite, adjust the pH value of the solution to 3-5, and add warm water to the second bath ratio, stir for 5-30 minutes, and drain; then rinse the down with 10-50℃ water to remove the iron ions adsorbed on the non-pigmented proteins of the down; Oxidation: immerse the down in an oxidation treatment solution and stir for 10-60 minutes at 10-40°C; the preparation process of the oxidation treatment solution is: first add sodium pyrophosphate and hydrogen peroxide stabilizer into water, then add a penetrant, and finally add hydrogen peroxide; Reduction: Place the down in a reduction treatment solution, and soak it under stirring at 10-50°C for 1-3 hours. The reduction treatment solution is a mixed solution containing 1-9g / L sodium dithionite and 0.1-4g / L thiourea dioxide, and then sodium pyrophosphate is added; the amount of sodium pyrophosphate used is 2-10g / L.

5. A method for rapid decolorization of down according to claim 4, characterized in that: The concentration of the reagent for rapid decolorization of down is 0.1-3 g / L, and the concentration of the JFC penetrant is 0.5-2 g / L.

6. A method for rapid decolorization of down according to claim 4, characterized in that: The first bath ratio is 1:10, the second bath ratio is 1:15-50; and the setting time is 10 minutes.

7. A method for rapid decolorization of down according to claim 4, characterized in that: The dosage of the ferrous sulfate is 1-30 g / L; the dosage of the sodium bisulfite is 1-2 g / L; and hydrochloric acid is used to adjust the pH value of the solution.

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