Polyester filament down-like thermal insulation material and preparation method thereof

Abstract

The present application provides a polyester filament imitated down thermal insulation material, which comprises a thermal insulation layer and a heat reflection layer, and the thermal insulation layer and the heat reflection layer are arranged in parallel by one-piece air long pile structure yarn, the one-piece air long pile structure yarn comprises a core yarn and a cladding yarn, the cladding yarn forms a spherical pile knot on the core yarn, the spherical pile has a specified diameter, and the pile is continuously formed at a specified interval. The polyester filament imitated down thermal insulation material of the present application is provided as the thermal insulation layer and the heat reflection layer, and the long filament is woven into the one-piece air long pile structure yarn in various shapes and sizes, so that the thermal insulation effect is improved.

Description

Technical Field

[0001] This invention relates to the field of functional fiber materials, specifically to a polyester filament down-like thermal insulation material. Background Technology

[0002] Currently, the imitation down material on the market, collectively known as imitation down cotton, is a polyester fiber made from polyester, three-dimensional crimped hollow fiber, U-shaped hollow fiber, and ES fiber through special processing. Its fiber raw material is polyester. Imitation down cotton is lightweight, has a delicate and soft feel, good warmth retention, is not easily deformed, does not leak fibers, and has the feel of down with good warmth retention. It is widely used in down jackets, ski jackets, winter clothing, and other thermal wear.

[0003] Patent 201580011595.3 discloses an "integrated air-long down" product that reproduces the structure of waterfowl down and achieves superior warmth, breathability, and antibacterial properties, making it an ideal alternative to natural down. Due to limitations in the manufacturing equipment and process, the long down produced in this patent has relatively uniform strands and cluster sizes. To further improve the insulation effect of the integrated air-long down product while simplifying the process, the down clusters in the integrated air-long down are designed with two different diameters. By layering the integrated air-long down of different diameters, the insulation effect of the down-like material is improved. Summary of the Invention

[0004] The technical problem to be solved: The purpose of this invention is to provide a polyester filament down-like insulation material, which is set as an insulation layer and a heat-reflective layer, and uses filaments woven into an integral air-pile structure yarn of different shapes and sizes to improve the insulation effect.

[0005] Technical solution: A polyester filament down-like thermal insulation material, the thermal insulation material comprising a thermal insulation layer and a heat-reflective layer, both the thermal insulation layer and the heat-reflective layer being formed by parallel arrangement of integral air-pile structure yarns, the integral air-pile structure yarn comprising a core yarn and a covering yarn, the covering yarn forming spherical down clusters entangled on the core yarn, the spherical down clusters having a specified diameter, and the down clusters being formed continuously at specified intervals;

[0006] The core and covering fibers of the insulation layer are hollow polyester filament fibers, and the diameter of the spherical fluff clusters of the insulation layer is 0.5-1.5cm. The core and covering fibers of the heat reflective layer are modified core-sheath structure polyester filament fibers, and the diameter of the spherical fluff clusters of the heat reflective layer is 2-3.5cm.

[0007] Preferably, the method for preparing the modified core-sheath structure polyester filament fiber includes the following steps:

[0008] S1. Preparation of the core layer: Silver-coated rare earth modified silicon carbide particles are added to sodium alginate solution to obtain a modified core layer solution with a concentration of 4.5-6.5 wt%.

[0009] S2. Preparation of the skin layer: Add nanosheet zinc oxide and calcium chloride to polyester chips and melt-blend to obtain modified polyester chips. Dissolve the modified polyester chips in a mixed solvent of trifluoroacetic acid / dichloromethane to obtain a modified skin layer solution with a concentration of 15-18wt%.

[0010] S3. Wet spinning: Using a coaxial wet spinning machine, the modified core layer solution and the modified sheath layer solution are loaded into two injection pumps respectively, and the core material solution and shell material solution are pumped into a methanol coagulation bath to obtain modified core-sheath structure polyester filament fibers.

[0011] Preferably, the silver-coated rare-earth modified silicon carbide particles are prepared by the following steps:

[0012] S11. Dissolve starch in water, add concentrated sulfuric acid first, then add nano-silica, stir and dry, and pre-carbonize. The pre-carbonization temperature is 120-150℃ and the time is 6-10h.

[0013] S12. Add rare earth nitrate, starch, concentrated sulfuric acid and water to the pre-carbonized product, and pre-carbonize again at a temperature of 120-150℃ for 6-10h. Then, calcine the pre-carbonized material at a temperature of 1500-1700℃ and a heating rate of 8-10℃ / min to obtain rare earth-doped nano-silicon carbide.

[0014] S13. Rare earth-doped nano-silicon carbide is placed in hydrofluoric acid roughening solution, ultrasonically treated, and after the powder settles, it is washed and dried to obtain roughened silicon carbide.

[0015] S14. Add the roughened silicon carbide to a sensitizing solution containing Sn2+ with a concentration of 0.8-1.5wt% to obtain sensitized particles. Add the sensitized silicon carbide to a silver ammonia solution, then add an ethanol solution of glucose, and stir at a constant temperature to obtain rare earth modified silicon carbide particles coated with silver.

[0016] Preferably, in step S11, the mass ratio of starch, concentrated sulfuric acid, silicon dioxide and water is 8-10:0.6-1:6-8:40.

[0017] Preferably, in the pre-carbonized product of step S12, the mass ratio of rare earth nitrate, starch, concentrated sulfuric acid and water is 10-15:0.2-0.5:8-12:0.2-0.8:50.

[0018] Preferably, the ultrasonic treatment time in step S13 is 20-40 minutes.

[0019] Preferably, in step S14, the mass ratio of the roughened silicon carbide to the Sn2+-containing sensitizing solution is 0.5-1:100, and the concentration of the silver ammonia solution is 5-10 mmol / L.

[0020] Preferably, in step S14, the mass ratio of sensitized silicon carbide, glucose, and silver ammonia solution is 0.5-1:1-3:100.

[0021] The preparation method of the above-mentioned polyester filament down-like thermal insulation material includes the following steps:

[0022] Hollow polyester fibers and modified core-sheath structure polyester filament fibers are interwoven into an integrated air-fiber yarn.

[0023] The insulation layer is made of an integral air-fiber long-pile structure yarn woven from hollow polyester fibers.

[0024] Modified core-sheath structure polyester filament fibers are interwoven into an integrated air-fiber structure yarn and laid out as a heat-reflective layer.

[0025] The insulation layer and the heat reflective layer are stacked one on top of the other to obtain a polyester filament down-like insulation material.

[0026] Beneficial effects: The polyester filament down-like thermal insulation material of the present invention has the following advantages:

[0027] In this invention, the polyester filament down-like thermal insulation material is composed of two layers: the side closer to the human body is the thermal insulation layer, and the side farther away from the human body is the heat-reflective layer. The thermal insulation layer plays the role of heat storage and insulation, while the heat-reflective layer plays the role of reducing heat loss and improving the thermal insulation performance of the material.

[0028] In this invention, the piles of the insulation layer and the heat reflective layer are designed differently. The pile diameter of the insulation layer is smaller than that of the heat reflective layer. The insulation layer uses smaller piles because the insulation layer with the same thickness has more piles and better insulation effect. The heat reflective layer uses larger piles because the heat reflective layer has less piles with the same thickness, but better reflection effect, which is conducive to heating and improving insulation effect.

[0029] In this invention, the insulation layer is made of modified core-sheath structure polyester filament fiber. The core layer contains rare earth modified silicon carbide particles coated with silver, and the sheath layer contains zinc oxide particles. The synergistic effect of the two has a better heat reflection effect. In order to improve the heat reflection effect, the silicon carbide in the core layer is modified with rare earth and coated with silver, which further improves the heat reflection effect. Detailed Implementation

[0030] The present invention will be further described below with reference to embodiments. These embodiments are illustrative of the present invention, but the present invention is not limited to these embodiments:

[0031] Example 1

[0032] A polyester filament down-like thermal insulation material, the thermal insulation material comprising a thermal insulation layer and a heat-reflective layer, both the thermal insulation layer and the heat-reflective layer being formed by parallel arrangement of integral air-pile structure yarns, the integral air-pile structure yarn comprising a core yarn and a covering yarn, the covering yarn forming spherical down clusters entangled on the core yarn, the spherical down clusters having a specified diameter, and the down clusters being formed continuously at specified intervals;

[0033] The core and covering fibers of the insulation layer are hollow polyester filament fibers, and the diameter distribution of the spherical fluff clusters selected in the insulation layer is 0.5-1.5cm. The core and covering fibers of the heat reflective layer are modified core-sheath structure polyester filament fibers, and the diameter distribution of the spherical fluff clusters selected in the heat reflective layer is 2-3.5cm.

[0034] The method for preparing the modified core-sheath structure polyester filament fiber includes the following steps:

[0035] S1. Preparation of the core layer: Silver-coated rare earth modified silicon carbide particles were added to sodium alginate solution to obtain a modified core layer solution with a concentration of 4.5 wt%.

[0036] S2. Preparation of the skin layer: Nanosheet zinc oxide and calcium chloride are added to polyester chips in a mass ratio of 5:0.5:100. The mixture is melt-blended to obtain modified polyester chips. The modified polyester chips are dissolved in a mixed solvent of trifluoroacetic acid and dichloromethane to obtain a modified skin layer solution with a concentration of 15wt%.

[0037] S3. Wet spinning: Using a coaxial wet spinning machine, the modified core layer solution and the modified sheath layer solution are loaded into two injection pumps respectively, and the core material solution and shell material solution are pumped into a methanol coagulation bath to obtain modified core-sheath structure polyester filament fibers.

[0038] The silver-coated rare-earth modified silicon carbide particles are prepared through the following steps:

[0039] S11. Dissolve starch in water, add concentrated sulfuric acid first and then nano-silica. The mass ratio of starch, concentrated sulfuric acid, silica and water is 10:0.6:6:40. After stirring, dry and pre-carbonize at 120℃ for 10 hours.

[0040] S12. Rare earth nitrate, starch, concentrated sulfuric acid and water are added to the pre-carbonized product. The mass ratio of rare earth nitrate, starch, concentrated sulfuric acid and water is 10:0.2:8:0.8:50. Pre-carbonization is carried out again at 120℃ for 10 hours. The pre-carbonized material is then calcined at 1500℃ at a heating rate of 8℃ / min to obtain rare earth-doped nano-silicon carbide.

[0041] S13. Rare earth-doped nano-silicon carbide is placed in hydrofluoric acid roughening solution, ultrasonically treated for 20 min, and after the powder settles, it is washed and dried to obtain roughened silicon carbide.

[0042] S14. Add the roughened silicon carbide to a Sn-containing concentration of 0.8 wt%. 2+ In the sensitizing solution, roughened silicon carbide and Sn-containing... 2+ The mass ratio of the sensitizing solution was 1:100 to obtain sensitized particles. The sensitized silicon carbide was added to a silver ammonia solution with a concentration of 5 mmol / L, and then an ethanol solution of glucose was added. The mass ratio of the sensitized silicon carbide, glucose and silver ammonia solution was 1:3:100. The mixture was stirred at a constant temperature to obtain rare earth modified silicon carbide particles coated with silver.

[0043] Example 2

[0044] A polyester filament down-like thermal insulation material, the thermal insulation material comprising a thermal insulation layer and a heat-reflective layer, both the thermal insulation layer and the heat-reflective layer being formed by parallel arrangement of integral air-pile structure yarns, the integral air-pile structure yarn comprising a core yarn and a covering yarn, the covering yarn forming spherical down clusters entangled on the core yarn, the spherical down clusters having a specified diameter, and the down clusters being formed continuously at specified intervals;

[0045] The core and covering fibers of the insulation layer are hollow polyester filament fibers, and the diameter distribution of the spherical fluff clusters selected in the insulation layer is 0.5-1.5cm. The core and covering fibers of the heat reflective layer are modified core-sheath structure polyester filament fibers, and the diameter distribution of the spherical fluff clusters selected in the heat reflective layer is 2-3.5cm.

[0046] The method for preparing the modified core-sheath structure polyester filament fiber includes the following steps:

[0047] S1. Preparation of the core layer: Silver-coated rare earth modified silicon carbide particles were added to sodium alginate solution to obtain a modified core layer solution with a concentration of 6.5 wt%.

[0048] S2. Preparation of the skin layer: Nanosheet zinc oxide and calcium chloride are added to polyester chips in a mass ratio of 3:0.5:100. The mixture is melt-blended to obtain modified polyester chips. The modified polyester chips are dissolved in a mixed solvent of trifluoroacetic acid and dichloromethane to obtain a modified skin layer solution with a concentration of 18wt%.

[0049] S3. Wet spinning: Using a coaxial wet spinning machine, the modified core layer solution and the modified sheath layer solution are loaded into two injection pumps respectively, and the core material solution and shell material solution are pumped into a methanol coagulation bath to obtain modified core-sheath structure polyester filament fibers.

[0050] The silver-coated rare-earth modified silicon carbide particles are prepared through the following steps:

[0051] S11. Dissolve starch in water, add concentrated sulfuric acid first and then nano-silica. The mass ratio of starch, concentrated sulfuric acid, silica and water is 10:1:8:40. After stirring, dry and pre-carbonize at 150℃ for 60 hours.

[0052] S12. Rare earth nitrate, starch, concentrated sulfuric acid and water are added to the pre-carbonized product. The mass ratio of rare earth nitrate, starch, concentrated sulfuric acid and water is 15:0.5:12:0.2:50. Pre-carbonize again at 150℃ for 6 hours. The pre-carbonized material is then calcined at 1700℃ at a heating rate of 10℃ / min to obtain rare earth-doped nano-silicon carbide.

[0053] S13. Rare earth-doped nano-silicon carbide is placed in hydrofluoric acid roughening solution, ultrasonically treated for 40 min, and after the powder settles, it is washed and dried to obtain roughened silicon carbide.

[0054] S14. Add the roughened silicon carbide to a Sn-containing concentration of 1.5 wt%. 2+ In the sensitizing solution, roughened silicon carbide and Sn-containing... 2+ The mass ratio of the sensitizing solution was 0.5:100 to obtain sensitized particles. The sensitized silicon carbide was added to a 10 mmol / L silver ammonia solution, and then an ethanol solution of glucose was added. The mass ratio of the sensitized silicon carbide, glucose and silver ammonia solution was 0.5:1:100. The mixture was stirred at a constant temperature to obtain rare earth modified silicon carbide particles coated with silver.

[0055] Example 3

[0056] A polyester filament down-like thermal insulation material, the thermal insulation material comprising a thermal insulation layer and a heat-reflective layer, both the thermal insulation layer and the heat-reflective layer being formed by parallel arrangement of integral air-pile structure yarns, the integral air-pile structure yarn comprising a core yarn and a covering yarn, the covering yarn forming spherical down clusters entangled on the core yarn, the spherical down clusters having a specified diameter, and the down clusters being formed continuously at specified intervals;

[0057] The core and covering fibers of the insulation layer are hollow polyester filament fibers, and the diameter distribution of the spherical fluff clusters selected in the insulation layer is 0.8-1.4cm. The core and covering fibers of the heat reflective layer are modified core-sheath structure polyester filament fibers, and the diameter distribution of the spherical fluff clusters selected in the heat reflective layer is 2.5-3.2cm.

[0058] The method for preparing the modified core-sheath structure polyester filament fiber includes the following steps:

[0059] S1. Preparation of the core layer: Silver-coated rare earth modified silicon carbide particles were added to sodium alginate solution to obtain a modified core layer solution with a concentration of 5wt%.

[0060] S2. Preparation of the skin layer: Nanosheet zinc oxide and calcium chloride are added to polyester chips in a mass ratio of 3:0.5:100. The mixture is melt-blended to obtain modified polyester chips. The modified polyester chips are dissolved in a mixed solvent of trifluoroacetic acid and dichloromethane to obtain a modified skin layer solution with a concentration of 17wt%.

[0061] S3. Wet spinning: Using a coaxial wet spinning machine, the modified core layer solution and the modified sheath layer solution are loaded into two injection pumps respectively, and the core material solution and shell material solution are pumped into a methanol coagulation bath to obtain modified core-sheath structure polyester filament fibers.

[0062] The silver-coated rare-earth modified silicon carbide particles are prepared through the following steps:

[0063] S11. Dissolve starch in water, add concentrated sulfuric acid first and then nano-silica. The mass ratio of starch, concentrated sulfuric acid, silica and water is 8.5:0.6:6.5:40. After stirring, dry and pre-carbonize at 135℃ for 8 hours.

[0064] S12. Rare earth nitrate, starch, concentrated sulfuric acid and water are added to the pre-carbonized product. The mass ratio of rare earth nitrate, starch, concentrated sulfuric acid and water is 12:0.3:9:0.4:50. Pre-carbonize again at 135℃ for 10 hours. The pre-carbonized material is then calcined at 1600℃ at a heating rate of 10℃ / min to obtain rare earth-doped nano-silicon carbide.

[0065] S13. Rare earth-doped nano-silicon carbide is placed in hydrofluoric acid roughening solution, ultrasonically treated for 30 min, and after the powder settles, it is washed and dried to obtain roughened silicon carbide.

[0066] S14. Add the roughened silicon carbide to a Sn-containing concentration of 1.2 wt%. 2+ In the sensitizing solution, roughened silicon carbide and Sn-containing... 2+ The mass ratio of the sensitizing solution was 0.8:100 to obtain sensitized particles. The sensitized silicon carbide was added to a silver ammonia solution with a concentration of 9 mmol / L, and then an ethanol solution of glucose was added. The mass ratio of the sensitized silicon carbide, glucose and silver ammonia solution was 0.8:1.5:100. The mixture was stirred at a constant temperature to obtain rare earth modified silicon carbide particles coated with silver.

[0067] Example 4

[0068] A polyester filament down-like thermal insulation material, the thermal insulation material comprising a thermal insulation layer and a heat-reflective layer, both the thermal insulation layer and the heat-reflective layer being formed by parallel arrangement of integral air-pile structure yarns, the integral air-pile structure yarn comprising a core yarn and a covering yarn, the covering yarn forming spherical down clusters entangled on the core yarn, the spherical down clusters having a specified diameter, and the down clusters being formed continuously at specified intervals;

[0069] The core and covering fibers of the insulation layer are hollow polyester filament fibers, and the diameter distribution of the spherical fluff clusters selected in the insulation layer is 0.8-1.4cm. The core and covering fibers of the heat reflective layer are modified core-sheath structure polyester filament fibers, and the diameter distribution of the spherical fluff clusters selected in the heat reflective layer is 2.5-3.2cm.

[0070] The method for preparing the modified core-sheath structure polyester filament fiber includes the following steps:

[0071] S1. Preparation of the core layer: Silver-coated rare earth modified silicon carbide particles were added to sodium alginate solution to obtain a modified core layer solution with a concentration of 6wt%.

[0072] S2. Preparation of the skin layer: Nano-sheet zinc oxide and calcium chloride are added to polyester chips in a mass ratio of 5:0.5:100. The mixture is melt-blended to obtain modified polyester chips. The modified polyester chips are dissolved in a mixed solvent of trifluoroacetic acid and dichloromethane to obtain a modified skin layer solution with a concentration of 15.5 wt%.

[0073] S3. Wet spinning: Using a coaxial wet spinning machine, the modified core layer solution and the modified sheath layer solution are loaded into two injection pumps respectively, and the core material solution and shell material solution are pumped into a methanol coagulation bath to obtain modified core-sheath structure polyester filament fibers.

[0074] The silver-coated rare-earth modified silicon carbide particles are prepared through the following steps:

[0075] S11. Dissolve starch in water, add concentrated sulfuric acid first, then add nano-silica. The mass ratio of starch, concentrated sulfuric acid, silica and water is 9.5:0.8:7.5:40. After stirring, dry and pre-carbonize at 150℃ for 9 hours.

[0076] S12. Rare earth nitrate, starch, concentrated sulfuric acid and water are added to the pre-carbonized product. The mass ratio of rare earth nitrate, starch, concentrated sulfuric acid and water is 14:0.4:11:0.6:50. Pre-carbonization is carried out again at a temperature of 150℃ for 8 hours. The pre-carbonized material is then calcined at a temperature of 1650℃ and a heating rate of 8℃ / min to obtain rare earth-doped nano-silicon carbide.

[0077] S13. Rare earth-doped nano-silicon carbide is placed in hydrofluoric acid roughening solution, ultrasonically treated for 40 min, and after the powder settles, it is washed and dried to obtain roughened silicon carbide.

[0078] S14. Add the roughened silicon carbide to a Sn-containing concentration of 1.2 wt%. 2+ In the sensitizing solution, roughened silicon carbide and Sn-containing... 2+ The mass ratio of the sensitizing solution was 0.5:100 to obtain sensitized particles. The sensitized silicon carbide was added to a silver ammonia solution with a concentration of 6 mmol / L, and then an ethanol solution of glucose was added. The mass ratio of the sensitized silicon carbide, glucose and silver ammonia solution was 0.6:2.5:100. The mixture was stirred at a constant temperature to obtain rare earth modified silicon carbide particles coated with silver.

[0079] Example 5

[0080] A polyester filament down-like thermal insulation material, the thermal insulation material comprising a thermal insulation layer and a heat-reflective layer, both the thermal insulation layer and the heat-reflective layer being formed by parallel arrangement of integral air-pile structure yarns, the integral air-pile structure yarn comprising a core yarn and a covering yarn, the covering yarn forming spherical down clusters entangled on the core yarn, the spherical down clusters having a specified diameter, and the down clusters being formed continuously at specified intervals;

[0081] The core and covering fibers of the insulation layer are hollow polyester filament fibers, and the diameter distribution of the spherical fluff clusters selected in the insulation layer is 0.8-1.4cm. The core and covering fibers of the heat reflective layer are modified core-sheath structure polyester filament fibers, and the diameter distribution of the spherical fluff clusters selected in the heat reflective layer is 2.5-3.2cm.

[0082] The method for preparing the modified core-sheath structure polyester filament fiber includes the following steps:

[0083] S1. Preparation of the core layer: Silver-coated rare earth modified silicon carbide particles were added to sodium alginate solution to obtain a modified core layer solution with a concentration of 5.5 wt%.

[0084] S2. Preparation of the skin layer: Nanosheet zinc oxide and calcium chloride are added to polyester chips in a mass ratio of 4:0.5:100. The mixture is melt-blended to obtain modified polyester chips. The modified polyester chips are dissolved in a mixed solvent of trifluoroacetic acid and dichloromethane to obtain a modified skin layer solution with a concentration of 16wt%.

[0085] S3. Wet spinning: Using a coaxial wet spinning machine, the modified core layer solution and the modified sheath layer solution are loaded into two injection pumps respectively, and the core material solution and shell material solution are pumped into a methanol coagulation bath to obtain modified core-sheath structure polyester filament fibers.

[0086] The silver-coated rare-earth modified silicon carbide particles are prepared through the following steps:

[0087] S11. Dissolve starch in water, add concentrated sulfuric acid first, then add nano-silica. The mass ratio of starch, concentrated sulfuric acid, silica and water is 9:0.7:7:40. After stirring, dry and pre-carbonize at 145℃ for 8.5h.

[0088] S12. Rare earth nitrate, starch, concentrated sulfuric acid and water are added to the pre-carbonized product. The mass ratio of rare earth nitrate, starch, concentrated sulfuric acid and water is 13:0.35:10:0.5:50. Pre-carbonization is carried out again at a temperature of 145℃ for 9 hours. The pre-carbonized material is then calcined at a temperature of 1600℃ and a heating rate of 8℃ / min to obtain rare earth-doped nano-silicon carbide.

[0089] S13. Rare earth-doped nano-silicon carbide is placed in hydrofluoric acid roughening solution, ultrasonically treated for 30 min, and after the powder settles, it is washed and dried to obtain roughened silicon carbide.

[0090] S14. Add the roughened silicon carbide to a Sn-containing concentration of 1.1 wt%. 2+ In the sensitizing solution, roughened silicon carbide and Sn-containing... 2+ The mass ratio of the sensitizing solution was 0.7:100 to obtain sensitized particles. The sensitized silicon carbide was added to a silver ammonia solution with a concentration of 8 mmol / L, and then an ethanol solution of glucose was added. The mass ratio of the sensitized silicon carbide, glucose and silver ammonia solution was 0.7:2:100. The mixture was stirred at a constant temperature to obtain rare earth modified silicon carbide particles coated with silver.

[0091] Comparative Example 1

[0092] A polyester filament down-like insulation material, the insulation material comprising a double insulation layer, both of which are composed of parallel arrangement of integral air-pile structure yarns, the integral air-pile structure yarn comprising a core yarn and a covering yarn, the covering yarn forming spherical down clusters entangled on the core yarn, the spherical down clusters having a specified diameter, and the down clusters being continuously formed at specified intervals;

[0093] The core and covering fibers of the insulation layer are made of hollow polyester filament fibers, and the diameter of the spherical fluff clusters selected for the insulation layer is 2.5-3.2 cm.

[0094] Comparative Example 2

[0095] A polyester filament down-like insulation material, the insulation material comprising a double insulation layer, both of which are composed of parallel arrangement of integral air-pile structure yarns, the integral air-pile structure yarn comprising a core yarn and a covering yarn, the covering yarn forming spherical down clusters entangled on the core yarn, the spherical down clusters having a specified diameter, and the down clusters being continuously formed at specified intervals;

[0096] The core and covering fibers of the insulation layer are modified core-sheath structure polyester filament fibers, and the diameter distribution of the spherical fluff clusters selected for the heat reflective layer is 2.5-3cm.

[0097] The method for preparing the modified core-sheath structure polyester filament fiber includes the following steps:

[0098] S1. Preparation of the core layer: Silver-coated rare earth modified silicon carbide particles were added to sodium alginate solution to obtain a modified core layer solution with a concentration of 6wt%.

[0099] S2. Preparation of the skin layer: Nano-sheet zinc oxide and calcium chloride are added to polyester chips in a mass ratio of 5:0.5:100. The mixture is melt-blended to obtain modified polyester chips. The modified polyester chips are dissolved in a mixed solvent of trifluoroacetic acid and dichloromethane to obtain a modified skin layer solution with a concentration of 15.5 wt%.

[0100] S3. Wet spinning: Using a coaxial wet spinning machine, the modified core layer solution and the modified sheath layer solution are loaded into two injection pumps respectively, and the core material solution and shell material solution are pumped into a methanol coagulation bath to obtain modified core-sheath structure polyester filament fibers.

[0101] The silver-coated rare-earth modified silicon carbide particles are prepared through the following steps:

[0102] S11. Dissolve starch in water, add concentrated sulfuric acid first, then add nano-silica. The mass ratio of starch, concentrated sulfuric acid, silica and water is 9.5:0.8:7.5:40. After stirring, dry and pre-carbonize at 150℃ for 9 hours.

[0103] S12. Rare earth nitrate, starch, concentrated sulfuric acid and water are added to the pre-carbonized product. The mass ratio of rare earth nitrate, starch, concentrated sulfuric acid and water is 14:0.4:11:0.6:50. Pre-carbonization is carried out again at a temperature of 150℃ for 8 hours. The pre-carbonized material is then calcined at a temperature of 1650℃ and a heating rate of 8℃ / min to obtain rare earth-doped nano-silicon carbide.

[0104] S13. Rare earth-doped nano-silicon carbide is placed in hydrofluoric acid roughening solution, ultrasonically treated for 40 min, and after the powder settles, it is washed and dried to obtain roughened silicon carbide.

[0105] S14. Add the roughened silicon carbide to a Sn-containing concentration of 1.1 wt%. 2+ In the sensitizing solution, roughened silicon carbide and Sn-containing... 2+ The mass ratio of the sensitizing solution was 0.5:100 to obtain sensitized particles. The sensitized silicon carbide was added to a silver ammonia solution with a concentration of 6 mmol / L, and then an ethanol solution of glucose was added. The mass ratio of the sensitized silicon carbide, glucose and silver ammonia solution was 0.6:2.5:100. The mixture was stirred at a constant temperature to obtain rare earth modified silicon carbide particles coated with silver.

[0106] Comparative Example 3

[0107] A polyester filament down-like thermal insulation material, the thermal insulation material comprising a thermal insulation layer and a heat-reflective layer, both the thermal insulation layer and the heat-reflective layer being formed by parallel arrangement of integral air-pile structure yarns, the integral air-pile structure yarn comprising a core yarn and a covering yarn, the covering yarn forming spherical down clusters entangled on the core yarn, the spherical down clusters having a specified diameter, and the down clusters being formed continuously at specified intervals;

[0108] The core and covering fibers of the insulation layer are hollow polyester filament fibers, and the diameter of the spherical fluff clusters selected for the insulation layer is 2.5-3.5cm. The core and covering fibers of the heat reflective layer are modified core-sheath structure polyester filament fibers, and the diameter of the spherical fluff clusters selected for the heat reflective layer is 2.5-3.5cm.

[0109] The method for preparing the modified core-sheath structure polyester filament fiber includes the following steps:

[0110] S1. Preparation of the core layer: Silver-coated rare earth modified silicon carbide particles were added to sodium alginate solution to obtain a modified core layer solution with a concentration of 6.5 wt%.

[0111] S2. Preparation of the skin layer: Nanosheet zinc oxide and calcium chloride are added to polyester chips in a mass ratio of 3:0.5:100. The mixture is melt-blended to obtain modified polyester chips. The modified polyester chips are dissolved in a mixed solvent of trifluoroacetic acid and dichloromethane to obtain a modified skin layer solution with a concentration of 18wt%.

[0112] S3. Wet spinning: Using a coaxial wet spinning machine, the modified core layer solution and the modified sheath layer solution are loaded into two injection pumps respectively, and the core material solution and shell material solution are pumped into a methanol coagulation bath to obtain modified core-sheath structure polyester filament fibers.

[0113] The silver-coated rare-earth modified silicon carbide particles are prepared through the following steps:

[0114] S11. Dissolve starch in water, add concentrated sulfuric acid first and then nano-silica. The mass ratio of starch, concentrated sulfuric acid, silica and water is 10:1:8:40. After stirring, dry and pre-carbonize at 150℃ for 60 hours.

[0115] S12. Rare earth nitrate, starch, concentrated sulfuric acid and water are added to the pre-carbonized product. The mass ratio of rare earth nitrate, starch, concentrated sulfuric acid and water is 15:0.5:12:0.2:50. Pre-carbonize again at 150℃ for 6 hours. The pre-carbonized material is then calcined at 1700℃ at a heating rate of 10℃ / min to obtain rare earth-doped nano-silicon carbide.

[0116] S13. Rare earth-doped nano-silicon carbide is placed in hydrofluoric acid roughening solution, ultrasonically treated for 40 min, and after the powder settles, it is washed and dried to obtain roughened silicon carbide.

[0117] S14. Add the roughened silicon carbide to a Sn-containing concentration of 1.5 wt%. 2+ In the sensitizing solution, roughened silicon carbide and Sn-containing... 2+ The mass ratio of the sensitizing solution was 0.5:100 to obtain sensitized particles. The sensitized silicon carbide was added to a 10 mmol / L silver ammonia solution, and then an ethanol solution of glucose was added. The mass ratio of the sensitized silicon carbide, glucose and silver ammonia solution was 0.5:1:100. The mixture was stirred at a constant temperature to obtain rare earth modified silicon carbide particles coated with silver.

[0118] Comparative Example 4

[0119] A polyester filament down-like thermal insulation material, the thermal insulation material comprising a thermal insulation layer and a heat-reflective layer, both the thermal insulation layer and the heat-reflective layer being formed by parallel arrangement of integral air-pile structure yarns, the integral air-pile structure yarn comprising a core yarn and a covering yarn, the covering yarn forming spherical down clusters entangled on the core yarn, the spherical down clusters having a specified diameter, and the down clusters being formed continuously at specified intervals;

[0120] The core and covering fibers of the insulation layer are hollow polyester filament fibers, and the diameter distribution of the spherical fluff clusters selected in the insulation layer is 0.8-1.4cm. The core and covering fibers of the heat reflective layer are modified core-sheath structure polyester filament fibers, and the diameter distribution of the spherical fluff clusters selected in the heat reflective layer is 2.5-3.2cm.

[0121] The method for preparing the modified core-sheath structure polyester filament fiber includes the following steps:

[0122] S1. Preparation of the core layer: Rare earth modified silicon carbide particles were added to sodium alginate solution to obtain a modified core layer solution with a concentration of 5.5 wt%.

[0123] S2. Preparation of the skin layer: Nanosheet zinc oxide and calcium chloride are added to polyester chips in a mass ratio of 4:0.5:100. The mixture is melt-blended to obtain modified polyester chips. The modified polyester chips are dissolved in a mixed solvent of trifluoroacetic acid and dichloromethane to obtain a modified skin layer solution with a concentration of 16wt%.

[0124] S3. Wet spinning: Using a coaxial wet spinning machine, the modified core layer solution and the modified sheath layer solution are loaded into two injection pumps respectively, and the core material solution and shell material solution are pumped into a methanol coagulation bath to obtain modified core-sheath structure polyester filament fibers.

[0125] The rare earth-modified silicon carbide particles are prepared through the following steps:

[0126] S11. Dissolve starch in water, add concentrated sulfuric acid first, then add nano-silica. The mass ratio of starch, concentrated sulfuric acid, silica and water is 9:0.7:7:40. After stirring, dry and pre-carbonize at 145℃ for 8.5h.

[0127] S12. Rare earth nitrates, starch, concentrated sulfuric acid, and water are added to the pre-carbonized product. The mass ratio of rare earth nitrates, starch, concentrated sulfuric acid, and water is 13:0.35:10:0.5:50. Pre-carbonization is carried out again at a temperature of 145℃ for 9 hours. The pre-carbonized material is then calcined at a temperature of 1600℃ and a heating rate of 8℃ / min to obtain rare earth-doped nano-silicon carbide.

[0128] Comparative Example 5

[0129] A polyester filament down-like thermal insulation material, the thermal insulation material comprising a thermal insulation layer and a heat-reflective layer, both the thermal insulation layer and the heat-reflective layer being formed by parallel arrangement of integral air-pile structure yarns, the integral air-pile structure yarn comprising a core yarn and a covering yarn, the covering yarn forming spherical down clusters entangled on the core yarn, the spherical down clusters having a specified diameter, and the down clusters being formed continuously at specified intervals;

[0130] The core and covering fibers of the insulation layer are hollow polyester filament fibers, and the diameter distribution of the spherical fluff clusters selected in the insulation layer is 0.8-1.5cm. The core and covering fibers of the heat reflective layer are modified core-sheath structure polyester filament fibers, and the diameter distribution of the spherical fluff clusters selected in the heat reflective layer is 2.5-3.2cm.

[0131] The method for preparing the modified core-sheath structure polyester filament fiber includes the following steps:

[0132] S1. Preparation of the core layer: Add silver-coated silicon carbide particles to sodium alginate solution to obtain a modified core layer solution with a concentration of 6wt%;

[0133] S2. Preparation of the skin layer: Nano-sheet zinc oxide and calcium chloride are added to polyester chips in a mass ratio of 5:0.5:100. The mixture is melt-blended to obtain modified polyester chips. The modified polyester chips are dissolved in a mixed solvent of trifluoroacetic acid and dichloromethane to obtain a modified skin layer solution with a concentration of 15.5 wt%.

[0134] S3. Wet spinning: Using a coaxial wet spinning machine, the modified core layer solution and the modified sheath layer solution are loaded into two injection pumps respectively, and the core material solution and shell material solution are pumped into a methanol coagulation bath to obtain modified core-sheath structure polyester filament fibers.

[0135] The silver-coated silicon carbide particles are prepared through the following steps:

[0136] S11. Dissolve starch in water, add concentrated sulfuric acid first, then add nano-silica. The mass ratio of starch, concentrated sulfuric acid, silica and water is 9.5:0.8:7.5:40. After stirring, dry and pre-carbonize at 150℃ for 9 hours.

[0137] S12. Add starch, concentrated sulfuric acid and water, and rare earth nitrate to the pre-carbonized product. The mass ratio of starch, concentrated sulfuric acid and water is 14:0.4:11:0.6:50. Pre-carbonize again at 150℃ for 8 hours. Then calcine the pre-carbonized material at 1650℃ with a heating rate of 8℃ / min to obtain nano-silicon carbide.

[0138] S13. Place the nano-silicon carbide in hydrofluoric acid roughening solution, sonicate for 40 min, and after the powder settles, wash and dry to obtain roughened silicon carbide.

[0139] S14. Add the roughened silicon carbide to a Sn-containing solution with a concentration of 1 wt%. 2+ In the sensitizing solution, roughened silicon carbide and Sn-containing... 2+ The mass ratio of the sensitizing solution was 0.5:100 to obtain sensitized particles. The sensitized silicon carbide was added to a silver ammonia solution with a concentration of 6 mmol / L, and then an ethanol solution of glucose was added. The mass ratio of the sensitized silicon carbide, glucose and silver ammonia solution was 0.6:2.5:100. The mixture was stirred at a constant temperature to obtain silver-coated silicon carbide particles.

[0140] Examples 1-5 and Comparative Examples 3-5 were prepared using the same method, namely:

[0141] Hollow polyester fibers and modified core-sheath structure polyester filament fibers are interwoven into an integrated air-fiber yarn.

[0142] The insulation layer is made of an integral air-fiber long-pile structure yarn woven from hollow polyester fibers.

[0143] Modified core-sheath structure polyester filament fibers are interwoven into an integrated air-fiber structure yarn and laid out as a heat-reflective layer.

[0144] The insulation layer and the heat reflective layer are stacked one on top of the other to obtain a polyester filament down-like insulation material.

[0145] Comparative Examples 1-2 were prepared by the following method:

[0146] Hollow polyester fibers or modified core-sheath structure polyester filament fibers are interwoven into an integrated air-fiber yarn.

[0147] The insulation layer is made of an integral air-fiber long-pile structure yarn woven from hollow polyester fibers or modified core-sheath structure polyester filament fibers.

[0148] Two layers of insulation are stacked one on top of the other to obtain a polyester filament down-like insulation material.

[0149] Performance testing:

[0150] The thermal insulation performance of Examples 1-5 and Comparative Examples 1-5 was tested and compared using a flatbed thermal insulation tester. The specific operation was as follows: The polyester filament down-like thermal insulation material prepared in Examples 1-5 and Comparative Examples 1-5 was filled into the inner lining fabric of a 30cm×30cm down jacket, with a unit filling amount of 100g / m². 2After sealing, the samples were laid flat in the specified area for testing. The test temperature was (25±5)℃ and the relative humidity was (65±5)%. Each sample was tested 3 times and the average value was taken.

[0151] Table 1

[0152] Thermal insulation rate / % Cro value Example 1 80.9 2.80 Example 2 81.2 2.89 Example 3 80.5 2.76 Example 4 80.8 2.78 Example 5 81.1 2.85 Comparative Example 1 74.5 2.36 Comparative Example 2 76.6 2.60 Comparative Example 3 78.2 2.68 Comparative Example 4 77.6 2.59 Comparative Example 5 78.0 2.65

[0153] According to GB / T 30127-2013, the infrared heating performance of Comparative Examples 1-5 and Comparative Examples 1-5 was evaluated, and the specific procedures were as follows: The polyester filament down-like insulation material prepared in Examples 1-5 and Comparative Examples 1-5 was filled into the inner lining fabric of a 30cm×30cm down jacket, with a unit filling amount of 100g / m². 2 The sample was cut to a diameter of 60 mm and then tested.

[0154] Table 2

[0155] Temperature rise difference / ℃ Example 1 3.5 Example 2 3.4 Example 3 3.5 Example 4 3.4 Example 5 3.6 Comparative Example 1 2.9 Comparative Example 2 3.4 Comparative Example 3 3.1 Comparative Example 4 2.9 Comparative Example 5 3.0

[0156] Obviously, the above embodiments are merely illustrative examples for clear explanation and are not intended to limit the implementation. Those skilled in the art will recognize that other variations or modifications can be made based on the above description. It is neither necessary nor possible to exhaustively list all possible implementations here. However, obvious variations or modifications derived therefrom are still within the scope of protection of this invention.

Claims

1. A polyester filament down-like thermal insulation material, characterized by: The thermal insulation material comprises a thermal insulation layer and a heat reflection layer, both of which are arranged in parallel by integral air long pile structure yarns, the integral air long pile structure yarns comprise core filaments and coating filaments, the coating filaments form spherical pile tufts intertwined on the core filaments, the spherical pile tufts have a specified diameter, and the pile tufts are continuously formed at a specified interval; The core filaments and the coating filaments of the thermal insulation layer are hollow polyester filament fibers, the diameter of the spherical pile tufts of the thermal insulation layer is 0.5-1.5 cm, the core filaments and the coating filaments of the heat reflection layer are modified sheath-core structure polyester filament fibers, and the diameter of the spherical pile tufts of the heat reflection layer is 2-3.5 cm; The preparation method of the modified sheath-core structure polyester filament fiber comprises the following steps: S1. Preparation of the core layer: silver-coated rare earth modified silicon carbide particles are added to a sodium alginate solution to obtain a modified core layer solution with a concentration of 4.5-6.5 wt%; S2. Preparation of the sheath layer: nanosheet-shaped zinc oxide and calcium chloride are added to polyester chips, and then melt-blended to obtain modified polyester chips, which are dissolved in a mixed solvent of trifluoroacetic acid / dichloromethane to obtain a modified sheath layer solution with a concentration of 15-18 wt%; S3. Wet spinning: a coaxial wet spinning machine is used, the modified core layer solution and the modified sheath layer solution are respectively loaded into two injection pumps, the core material solution and the shell material solution are pumped into a methanol coagulation bath to obtain a modified sheath-core structure polyester filament fiber.

2. The polyester filament down-like thermal insulation material according to claim 1, characterized in that, The silver-coated rare earth modified silicon carbide particles are prepared by the following steps: S11. Starch is dissolved in water, concentrated sulfuric acid is added first, then nanosilica is added, and after stirring, it is dried, pre-carbonized, the pre-carbonization temperature is 120-150℃, and the time is 6-10h; S12. The pre-carbonized product is added with rare earth nitrate, starch, concentrated sulfuric acid and water, pre-carbonized again, the pre-carbonization temperature is 120-150℃, and the time is 6-10h, the pre-carbonized material is calcined, the calcination temperature is 1500-1700℃, and the heating rate is 8-10℃ / min, to obtain rare earth doped nanosilicon carbide; S13. The rare earth doped nanosilicon carbide is placed in a hydrofluoric acid roughening solution, ultrasonic treatment is performed, after the powder is settled, it is washed and dried to obtain roughened silicon carbide; S14. The roughened silicon carbide is added to a sensitizing solution containing Sn at a concentration of 0.8-1.5 wt% to obtain sensitized particles. The sensitized silicon carbide is added to an agueous silver ammine solution, and then an ethanolic solution of glucose is added. The mixture is stirred at a constant temperature to obtain silver-coated rare earth modified silicon carbide particles. 2+ S14. The roughened silicon carbide is added to a sensitizing solution containing Sn at a concentration of 0.8-1.5 wt% to obtain sensitized particles. The sensitized silicon carbide is added to an agueous silver ammine solution, and then an ethanolic solution of glucose is added. The mixture is stirred at a constant temperature to obtain silver-coated rare earth modified silicon carbide particles.

3. The polyester filament down-like thermal insulation material according to claim 2, characterized in that: The mass ratio of starch, concentrated sulfuric acid, silicon dioxide and water in step S11 is 8-10:0.6-1:6-8:

40.

4. The polyester filament down-like thermal insulation material according to claim 2, characterized in that: The ultrasonic treatment time in step S13 is 20-40min.

5. The polyester filament down-like thermal insulation material according to claim 2, characterized in that: The silicon carbide and Sn-containing solution of the roughening treatment in the step S14 2+ The mass ratio of the sensitizing solution is 0.5-1:100, and the concentration of the silver ammine solution is 5-10 mmol / L.

6. The polyester filament down-like thermal insulation material according to claim 2, wherein: The mass ratio of sensitized silicon carbide, glucose and silver ammine solution in step S14 is 0.5-1:1-3:

100.

7. The method for preparing the polyester filament down-like thermal insulation material according to claim 1, characterized in that, The steps comprise: Hollow polyester filament fibers and modified sheath-core structure polyester filament fibers are interwoven into integral air long pile structure yarns; The hollow polyester filament fibers are interwoven into integral air long pile structure yarns, which are laid as the thermal insulation layer; The modified sheath-core structure polyester filament fibers are interwoven into integral air long pile structure yarns, which are laid as the heat reflection layer; The thermal insulation layer and the heat reflection layer are stacked and laid to obtain a polyester filament down-like thermal insulation material.