An insulating wool and a method for producing the same

Abstract

The application discloses a heat preservation down and a preparation method thereof, and belongs to the down technical field, and the preparation method comprises the following steps: taking natural down, washing and deodorizing the natural down by water, and drying the natural down, then mixing the natural down with expanded fibers according to a mass ratio of 20:1 to obtain mixed down; placing the mixed down in a compression groove, and compressing the mixed down by a gas cylinder to obtain compressed down; pressing a modified polyurethane adhesive on a surface of the compressed down through an OPP transfer film, naturally drying the modified polyurethane adhesive until the surface of the modified polyurethane adhesive is dry, drying the modified polyurethane adhesive at 50 DEG C until the weight of the modified polyurethane adhesive is constant, immersing the modified polyurethane adhesive in a zirconium sulfate solution with a concentration of 0.3-0.4 g / L, oscillating the modified polyurethane adhesive at 30 DEG C for 2-2.5 h, fully rinsing the modified polyurethane adhesive by distilled water, centrifugally dehydrating the modified polyurethane adhesive, and finally drying the modified polyurethane adhesive at 40 DEG C until the weight of the modified polyurethane adhesive is constant, so that the heat preservation down is obtained.

Description

Technical Field

[0001] This invention belongs to the field of fleece technology, specifically relating to a thermal fleece and its preparation method. Background Technology

[0002] Down, with its lightweight and high loft, is the best-performing natural fiber for warmth and is widely used in the processing of winter clothing and bedding. With the growing trend towards lightweight and convenient clothing and increasing market demand, how to further improve the functionality and warmth retention of down fibers has attracted considerable attention from scholars.

[0003] Based on the far-infrared effect of metal ions and their oxides, the thermal insulation performance of down can be improved by modifying down fibers with metal ions such as copper, zinc, and zirconium or their oxides through grafting, coating / embedding. However, because the surface of down is composed of a bilayer of sterols and triphosphates, which has hydrophobic properties, grafting is time-consuming, has a low grafting rate, and has a limited metal ion loading capacity. At the same time, the interaction between metal ions and down protein macromolecules is weak, resulting in problems such as low wash fastness. The use of coating agents such as cyclodextrin also affects the loft of down. All of these factors hinder the large-scale production of metal ion-modified down. Summary of the Invention

[0004] The purpose of this invention is to provide a thermal insulation down and its preparation method to solve the following technical problems: Existing methods for modifying down fibers with metal ions such as copper, zinc, zirconium or their oxides through grafting, coating / embedding to improve the thermal insulation performance of down have problems such as long grafting time, low grafting rate, limited metal ion loading, low wash fastness or reduced down loft.

[0005] The objective of this invention can be achieved through the following technical solutions:

[0006] A method for preparing thermal insulation fleece includes the following preparation steps:

[0007] Step 1: Take natural down, wash and deodorize it with water, dry it, and then mix it with expanded fibers at a mass ratio of 20:1 to obtain mixed down;

[0008] Step 2: Place the mixed fleece in the compression tank and compress it using a cylinder to obtain compressed fleece;

[0009] Step 3: Imprint the modified polyurethane adhesive onto the surface of the compressed fleece using an OPP transfer film, allow it to dry naturally until the film surface is dry, dry it to constant weight at 50°C, immerse it in a zirconium sulfate solution with a concentration of 0.3-0.4 g / L, shake it at 30°C for 2-2.5 h, rinse it thoroughly with distilled water, centrifuge it to remove water, and finally dry it to constant weight at 40°C to obtain a thermal insulation fleece.

[0010] As a further aspect of the present invention, the expanded fiber is made of polyester fiber.

[0011] As a further aspect of the present invention, the expanded fiber is provided with pores, the average pore diameter of which is 0.01-0.05 mm.

[0012] As a further aspect of the present invention, the density of the compressed fleece is 52-57 g / m³. 3 .

[0013] As a further aspect of the present invention, the modified polyurethane adhesive is prepared by the following steps:

[0014] Step 1: Under a nitrogen atmosphere, add polytetrahydrofuran ether diol, isoflurane diisocyanate and dibutyltin dilaurate catalyst to the reaction vessel, react at 50°C for 30-40 min, then raise the temperature to 70°C and continue the reaction for 1.5-2 h to obtain polyurethane prepolymer;

[0015] Step 2: Add acetone, 1,4-butanediol, and the hydrophilic chain extender 2,3-dimethylolpropionic acid to the polyurethane prepolymer. After heating to 80°C and reacting for 2-2.5 hours, add phytic acid and continue the reaction for 2.5-3 hours. Cool down to 35°C, add triethylamine to neutralize for 30-40 minutes, add deionized water and stir to emulsify for 30-40 minutes. Remove the solvent acetone by vacuum distillation to obtain the modified polyurethane adhesive.

[0016] As a further embodiment of the present invention, the mass ratio of polytetrahydrofuran ether diol, isoflurane diisocyanate, and catalyst dibutyltin dilaurate in step 1 is 20-30g:10-15g:1.5-2.2g.

[0017] As a further embodiment of the present invention, the mass ratio of polyurethane prepolymer, acetone, 1,4-butanediol, 2,3-dimethylolpropionic acid, phytic acid, triethylamine, and deionized water in step 2 is 100-110:40-45:2-2.2:5-5.5:2-5:8.5-9.5:25.

[0018] A type of thermal insulation fleece is prepared by the above-described preparation method.

[0019] The beneficial effects of this invention are:

[0020] This invention firstly obtains compressed down by blending natural down with expanded fibers and compressing them to a certain density. On the one hand, the expanded fibers provide structural support for the down, ensuring its fluffiness and warmth. On the other hand, the expanded fibers have pores that help to lock still air inside. Still air has a low thermal conductivity, which further improves the warmth retention.

[0021] This invention produces a thermal insulation fleece by transferring a modified polyurethane adhesive onto the surface of compressed fleece and then immersing it in a zirconium sulfate solution to chelate and adsorb zirconium ions. This further improves the thermal insulation performance and provides good wash fastness. The main principle is as follows:

[0022] First, a polyurethane prepolymer is synthesized using polytetrahydrofuran ether diol and isoflurane diisocyanate under a catalyst. Then, phytic acid is grafted onto the polyurethane molecular chain by reacting the hydroxyl groups (-OH) of phytic acid with the isocyanate groups (-NCO) of the polyurethane system to obtain a modified polyurethane adhesive. On one hand, after the modified polyurethane adhesive is transferred to the surface of compressed fleece, the phytic acid undergoes an ester crosslinking reaction with the hydroxyl groups on the surface of the natural fleece, thus firmly bonding the polyurethane adhesive to the surface of the compressed fleece. Compared with directly impregnating the compressed fleece with phytic acid, this invention only acts on the surface of the compressed fleece, without damaging the three-dimensional structure and morphology of the internal fleece clusters and filaments, ensuring the fluffiness and heat insulation performance of the compressed fleece. On the other hand, after the modified polyurethane adhesive is imprinted onto the surface of the compressed fleece, it is impregnated with zirconium sulfate solution. Phytic acid, down protein fibers, and zirconium ions co-chelate to form a ternary complex. The zirconium ions are bonded to the surface of the compressed fleece by chelate covalent bonds, exhibiting strong wash fastness. At the same time, the zirconium ions have an infrared temperature-raising function, absorbing ambient infrared rays, further improving the heat insulation performance. Detailed Implementation

[0023] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0024] Example 1

[0025] Modified polyurethane adhesives are prepared by the following steps:

[0026] Step 1: Under a nitrogen atmosphere, add 20g of polytetrahydrofuran ether diol, 10g of isoflurane diisocyanate and 1.5g of catalyst dibutyltin dilaurate to the reaction vessel, react at 50℃ for 30min, and then raise the temperature to 70℃ and continue the reaction for 1.5h to obtain polyurethane prepolymer.

[0027] Step 2: Add 40g acetone, 2g 1,4-butanediol, and 5g hydrophilic chain extender 2,3-dimethylolpropionic acid to 100g polyurethane prepolymer. After heating to 80℃ and reacting for 2h, add 2g phytic acid and continue the reaction for 2.5h. Cool down to 35℃, add 8.5g triethylamine to neutralize for 30min, add 25g deionized water and stir to emulsify for 30min. Remove the solvent acetone by vacuum distillation to obtain the modified polyurethane adhesive.

[0028] Example 2

[0029] Modified polyurethane adhesives are prepared by the following steps:

[0030] Step 1: Under a nitrogen atmosphere, add 30g of polytetrahydrofuran ether diol, 15g of isoflurane diisocyanate and 2.2g of catalyst dibutyltin dilaurate to the reaction vessel, react at 50℃ for 40min, and then raise the temperature to 70℃ and continue the reaction for 2h to obtain polyurethane prepolymer.

[0031] Step 2: Add 45g acetone, 2.2g 1,4-butanediol, and 5.5g hydrophilic chain extender 2,3-dimethylolpropionic acid to 110g polyurethane prepolymer. After heating to 80℃ and reacting for 2.5h, add 5g phytic acid and continue reacting for 3h. Cool down to 35℃, add 9.5g triethylamine to neutralize for 40min, add 25g deionized water and stir to emulsify for 40min. Remove the solvent acetone by vacuum distillation to obtain modified polyurethane adhesive.

[0032] Example 3

[0033] A method for preparing thermal insulation fleece includes the following preparation steps:

[0034] Step 1: Take natural down, wash and deodorize it with water, dry it, and then mix it with expanded fiber (the expanded fiber is made of polyester fiber, and the expanded fiber has holes distributed on it, with an average hole diameter of 0.01mm) at a mass ratio of 20:1 to obtain mixed down;

[0035] Step 2: Place the mixed fleece in a compression tank and compress it using a cylinder until the density reaches 52 g / m³. 3 , to obtain compressed fleece;

[0036] Step 3: The modified polyurethane adhesive obtained in Example 1 is imprinted onto the surface of the compressed fleece using an OPP transfer film. It is then allowed to dry naturally until the film surface is dry. After drying to constant weight at 50°C, it is immersed in a 0.3 g / L zirconium sulfate solution and shaken at 30°C for 2 hours. After thorough rinsing with distilled water, centrifugation is performed to remove water. Finally, it is dried to constant weight at 40°C to obtain a thermal insulation fleece.

[0037] Example 4

[0038] A method for preparing thermal insulation fleece includes the following preparation steps:

[0039] Step 1: Take natural down, wash and deodorize it with water, dry it, and then mix it with expanded fiber (expanded fiber is made of polyester fiber, and the expanded fiber has holes distributed on it, with an average hole diameter of 0.05mm) at a mass ratio of 20:1 to obtain mixed down;

[0040] Step 2: Place the mixed fleece in a compression tank and compress it using a cylinder until the density reaches 57 g / m³. 3 , to obtain compressed fleece;

[0041] Step 3: The modified polyurethane adhesive obtained in Example 2 is imprinted onto the surface of the compressed fleece using an OPP transfer film. It is then allowed to dry naturally until the film surface is dry. After drying to constant weight at 50°C, it is immersed in a 0.4 g / L zirconium sulfate solution and shaken at 30°C for 2.5 h. After thorough rinsing with distilled water, centrifugation is performed to remove water. Finally, it is dried to constant weight at 40°C to obtain a thermal insulation fleece.

[0042] Comparative Example 1

[0043] A method for preparing thermal insulation fleece includes the following preparation steps:

[0044] Step 1: After washing, deodorizing, and drying natural down, place it in a compression tank and compress the blended down using a cylinder until the density reaches 52g / m³. 3 , to obtain compressed fleece;

[0045] Step 2: The modified polyurethane adhesive obtained in Example 1 is imprinted onto the surface of the compressed fleece using an OPP transfer film. It is then allowed to dry naturally until the film surface is dry. After drying to constant weight at 50°C, it is immersed in a 0.3 g / L zirconium sulfate solution and shaken at 30°C for 2 hours. After thorough rinsing with distilled water, centrifugation is performed to remove water. Finally, it is dried to constant weight at 40°C to obtain a thermal insulation fleece.

[0046] Comparative Example 2

[0047] A method for preparing thermal insulation fleece includes the following preparation steps:

[0048] Step 1: Take natural down, wash and deodorize it with water, dry it, and then mix it with expanded fiber (the expanded fiber is made of polyester fiber, and the expanded fiber has holes distributed on it, with an average hole diameter of 0.01mm) at a mass ratio of 20:1 to obtain mixed down;

[0049] Step 2: Place the mixed fleece in a compression tank and compress it using a cylinder until the density reaches 52 g / m³. 3 , to obtain compressed fleece;

[0050] Step 3: Immerse the compressed fleece in a 25% phytic acid solution and shake at 60°C for 2 hours. After rinsing thoroughly with distilled water, immerse it in a 0.3g / L zirconium sulfate solution and shake at 30°C for 2 hours. After rinsing thoroughly with distilled water, centrifuge to remove water, and finally dry at 40°C to constant weight to obtain a thermal insulation fleece.

[0051] Performance testing:

[0052] (1) The thermal insulation performance of the thermal insulation fleece prepared in Examples 3-4 and Comparative Examples 1-2 was tested: 10g of the thermal insulation fleece to be tested was put into a 30cm×30cm pure cotton cloth sample bag, sealed, and laid flat in the specified area for testing. The thermal insulation rate and Clo value were tested using a flat plate thermal insulation instrument. The test temperature was (25±5)℃ and the relative humidity was (65±5)%. Each thermal insulation fleece was tested 3 times and the average value was taken. The test results are shown in Table 1:

[0053] Table 1

[0054] Test Items Example 3 Example 4 Comparative Example 1 Comparative Example 2 Warmth retention rate / % 84.6 93.1 80.6 73.8 Cro value 3.023 3.303 2.880 2.251

[0055] As can be seen from Table 1, the thermal insulation fleece prepared in Examples 3-4 has higher thermal insulation performance than the thermal insulation fleece prepared in Comparative Examples 1-2, with a thermal insulation rate of up to 93.1%.

[0056] (2) Wash fastness test of the thermal insulation fleece prepared in Examples 3-4: The thermal insulation fleece to be tested was subjected to multiple wash treatments (1g of thermal insulation fleece to be tested was immersed in 500mL of distilled water, and washed by shaking at 40℃, with each wash lasting 15min). The zirconium ion concentration (Zr) in the water was tested after each wash. 4+ The mass concentration of ) and the test results are shown in Table 2:

[0057] Table 2

[0058]

[0059]

[0060] As can be seen from Table 2, the chelated zirconium ions in the thermal insulation fleece prepared in Examples 3-4 have strong fastness and can withstand a certain number of washes.

[0061] (3) The loft of the thermal insulation down prepared in Examples 3-4 and Comparative Examples 1-2 was tested: The loft of the thermal insulation down was tested according to GB / T 10288—201 "Test Methods for Down and Feathers". The test results are shown in Table 3.

[0062] Table 3

[0063] Test Items Example 3 Example 4 Comparative Example 1 Comparative Example 2 Loftiness / cm 18.6 18.4 18.5 13.8

[0064] As can be seen from Table 3, the thermal insulation fleece prepared in Examples 3-4 has a higher loft than the thermal insulation fleece prepared in Comparative Example 2.

[0065] It should be noted that, in this document, relational terms such as "first" and "second" are used only to distinguish one entity or operation from another, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Furthermore, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such process, method, article, or apparatus.

[0066] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A method for preparing thermal insulation fleece, characterized in that, The preparation steps include the following: Step 1: Take natural down, wash and deodorize it with water, dry it, and then mix it with expanded fibers at a mass ratio of 20:1 to obtain mixed down; Step 2: Place the mixed fleece in the compression tank and compress it using a cylinder to obtain compressed fleece; Step 3: Imprint the modified polyurethane adhesive onto the surface of the compressed fleece using an OPP transfer film, allow it to dry naturally until the film surface is dry, dry it to constant weight at 50°C, immerse it in a zirconium sulfate solution with a concentration of 0.3-0.4 g / L, shake it at 30°C for 2-2.5 h, rinse it thoroughly with distilled water, centrifuge it to remove water, and finally dry it to constant weight at 40°C to obtain a thermal insulation fleece. The expanded fiber has pores distributed on it, and the average pore diameter is 0.01-0.05 mm; The modified polyurethane adhesive is prepared by the following steps: Step 1: Under a nitrogen atmosphere, add polytetrahydrofuran ether diol, isoflurane diisocyanate and dibutyltin dilaurate to the reaction vessel, react at 50°C for 30-40 min, then raise the temperature to 70°C and continue the reaction for 1.5-2 h to obtain polyurethane prepolymer; Step 2: Add acetone, 1,4-butanediol, and 2,3-dimethylolpropionic acid to the polyurethane prepolymer. After heating to 80°C and performing a chain extension reaction for 2-2.5 hours, add phytic acid and continue the reaction for 2.5-3 hours. Cool down to 35°C, add triethylamine to neutralize for 30-40 minutes, add deionized water and stir to emulsify for 30-40 minutes. Remove acetone by vacuum distillation to obtain the modified polyurethane adhesive.

2. The method for preparing thermal insulation fleece according to claim 1, characterized in that, The expanded fiber is made of polyester fiber.

3. The method for preparing thermal insulation fleece according to claim 1, characterized in that, The density of the compressed fleece is 52-57 g / m³. 3 .

4. The method for preparing thermal insulation fleece according to claim 1, characterized in that, The mass ratio of polytetrahydrofuran ether diol, isoflurane diisocyanate, and dibutyltin dilaurate in step 1 is 20-30g:10-15g:1.5-2.2g.

5. The method for preparing thermal insulation fleece according to claim 1, characterized in that, The mass ratio of the polyurethane prepolymer, acetone, 1,4-butanediol, 2,3-dimethylolpropionic acid, phytic acid, triethylamine, and deionized water in step 2 is 100-110:40-45:2-2.2:5-5.5:2-5:8.5-9.5:

25.

6. A type of thermal insulation fleece, characterized in that, It is prepared by the preparation method described in any one of claims 1-5.

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