A process for the production of flame-retardant down

Abstract

This application relates to the field of finishing animal feathers and discloses a method for preparing flame-retardant down. The method includes: S1, pre-sorting and removing ash from coarse down, and washing with hot water and detergent to remove surface grease; S2, soaking the down in a co-solvent, and then using a supercritical CO2 extraction device to remove refined grease from the surface; S3, adding flame retardant, antibacterial finishing agent, organosiloxane compound, pH adjuster, penetrant, and water in a certain proportion to form a flame-retardant and antibacterial finishing solution of a certain concentration, and allowing it to stand at a constant temperature; S4, draining the down treated in step S3, and adding a water-repellent finishing agent, water, and other additives. This invention, through supercritical CO2 extraction, causes the surface of the down fibers to swell and open, forming pores that facilitate the penetration of flame retardants and antibacterial agents into the fiber interior. After water-repellent finishing and heat treatment, the down fiber surface shrinks, giving the flame retardant and antibacterial agents a long-lasting flame-retardant and antibacterial effect within the down fiber.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of animal feather post-processing technology, in particular to a preparation method of flame-retardant down. BACKGROUND

[0002] Down is a kind of down feather growing on the abdomen of duck, goose and other flying birds, which is in the shape of a lotus flower. Since down is an animal protein fiber, there are millions of tiny triangular pores on the down ball fiber, which can shrink and expand with the change of air temperature, produce temperature adjustment function, absorb the heat gas flowing from the human body and isolate the invasion of cold air from the outside. From the analysis of the detection of bulkiness, the down is one grade higher than silk, cotton and other warm-keeping materials. For example, the 90 duck down with the lowest standard of 450 degrees bulkiness is also more fluffy than silk and cotton, so the economic value of down as a pure warm-keeping material is much higher than other warm-keeping materials.

[0003] At present, there is no warm-keeping material in the world that exceeds the warm-keeping performance of down. Since down is in the shape of a lotus flower, each down filament can be seen under a magnifying glass in the shape of a fish scale, with countless tiny pores storing a large amount of static air. Since the conduction coefficient of air is the lowest, it forms the good warm-keeping performance of down. In addition, down is also full of elasticity. With the down content of 50%, the test of down shows that the light fluffy degree of down is 2.5 times that of cotton and 2.2 times that of wool, so down is not only light and warm-keeping, but also has good skin touch.

[0004] Down fiber, as a protein fiber, shares a similar structural composition with other natural protein fibers, containing numerous peptide bonds. However, due to its core-sheath structure, the surface of down fibers is composed of a dense cell membrane of sterols and triphosphates, while the core layer consists of multi-strand peptide chains. Therefore, its grafting pretreatment differs from that of wool and silk. Wool fibers have a scaly surface, which must be disrupted before flame retardant treatment can be applied to graft the flame retardant into the fiber. Similarly, silk fibers require pretreatment to break down the sericin layer before flame retardant finishing of the exposed fibroin. Grafting modification of down fibers must avoid damaging the surface water-repellent layer while ensuring that small-molecule flame retardants can penetrate the fiber interior for reaction. Therefore, selecting suitable flame retardants and applying mild conditions are crucial for modification. Currently, there are no reports on flame-retardant finishing of down from abroad. Domestically, only the Qilu team at Tianjin University of Technology has conducted research on flame-retardant finishing of down. For example, treatment with 1-phosphonopropane-1,2-dicarboxylic acid increased the limiting oxygen index (LOI) of the modified down fibers from 23.8% to 28.2%. Flame-retardant finishing of down using potassium fluorotitanate alone, sodium tungstate and its compound systems, melamine / phosphate compound systems, melamine / potassium fluorozirconate compound systems, and dicyandiamide / glutaraldehyde compound systems can achieve an LIO of over 40. However, the treated down turns yellow, is prone to clumping, and has reduced loft. Therefore, maintaining the original excellent properties of down, such as whiteness, turbidity, warmth, and loft, while performing flame-retardant modification is particularly important.

[0005] Therefore, the present invention provides a method for preparing flame-retardant down to overcome the shortcomings of the prior art. Summary of the Invention

[0006] To address the shortcomings of existing technologies, the purpose of this invention is to provide a flame-retardant down feather with good loft, warmth, and flame retardancy, as well as a method for its preparation.

[0007] To achieve the above objectives, the present invention provides the following technical solution: a method for preparing flame-retardant down, comprising the following steps:

[0008] S1. Pre-sort and remove ash from the coarse down feathers, and wash the feathers with hot water and detergent to remove the coarse grease on the surface;

[0009] S2. Soak the down processed in step S1 in a co-solvent, and then use a supercritical CO2 extraction device to remove the refined oil on the surface of the washed and soaked down for further processing of the down surface and collection of refined oil, while making the down protein swell and controlling the opening of disulfide bonds.

[0010] S3. Add the down treated in step S2 into the washing device, add flame retardant, antibacterial finishing agent, organosiloxane compound, pH adjuster, penetrant and water in a certain proportion to form a flame retardant and antibacterial finishing solution of a certain concentration, and let it stand at a constant temperature.

[0011] S4. Drain the down treated in step S3, add water-repellent finishing agent, water and other auxiliaries, control the liquor ratio, and treat for 30 minutes; after draining, add fluffing agent and treat for another 10 minutes to obtain down with the mixed solution.

[0012] S5. The feathers with the mixed solution obtained in step S4 are dehydrated by a dehydrator to obtain down with a small amount of liquid.

[0013] S6. The down feathers with a small amount of liquid obtained in step S5 are dried in a high-temperature dryer to obtain finished feathers.

[0014] Preferably, in step S2, the co-solvent is one of ethanol, diethyl ether, petroleum ether, carbon tetrachloride, and n-hexane.

[0015] Preferably, the flame retardant is a guanidine flame retardant or a boron-based flame retardant. The guanidine flame retardant is one or a mixture of several of guanidine hydrochloride, guanidine nitrate, guanidine dihydrogen phosphate, diguanidine hydrogen phosphate, guanidine polyphosphate, biguanidine phosphate, guanidine aminosulfonate, amidourea phosphate guanidine salt, ammonium aminosulfonate, thiourea, thiourea monohydrochloride, and aminophosphate ester. The boron-based flame retardant is one or a mixture of several of boric acid, sodium borate, ammonium borate, and potassium borate.

[0016] Preferably, the antibacterial finishing agent is an organosilicon quaternary ammonium salt, an organonitrogen compound, a nitrofuran, a biguanide, or a chlorobenzamide, and the organosiloxane compound is one or a mixture of several of the following: trimethoxysiloxane, methyltrimethoxysiloxane, tetramethoxysiloxane, vinyltrimethoxysiloxane, vinyltriisopropoxysiloxane, triethoxysiloxane, phenyltrimethoxysiloxane, and phenyltriethoxysiloxane.

[0017] Preferably, the acid-base regulator is a polyacid, specifically one or a mixture of several of oxalic acid, hydroxysuccinic acid, dihydroxysuccinic acid, citric acid, phosphoric acid, butanetetracarboxylic acid, and polymaleic acid; the penetrant is nonionic and anionic, specifically one or a mixture of several of JFC, JFC-1, JFC-2, JFC-E nonionic penetrant or rapid penetrant T, alkali-resistant penetrant OEP-70, and alkali-resistant penetrant AEP anionic penetrant.

[0018] Preferably, the water-repellent finishing agent is a fluorocarbon-based water-repellent agent, an organosilicon-based water-repellent finishing agent, a paraffin-based water-repellent finishing agent, or a non-fluorinated water-repellent finishing agent, and the fluffing agent is a down-specific fluffing agent. The concentration of the water-repellent finishing agent is 20-100 g / L, and the concentration of the fluffing agent is 20-100 g / L.

[0019] Preferably, in step S3, the ratio of the flame retardant, antibacterial finishing agent, and down is 50:1-5:1; the mass ratio of the flame retardant to down is 5%-50%; the mass ratio of the antibacterial finishing agent to down is 0.5-5%; the mass ratio of the pH adjuster to down is 1%-5%; the mass ratio of the penetrant to down is 1-10%; and the constant temperature static treatment temperature is 30-90℃, and the treatment time is 30-150 minutes.

[0020] Preferably, in step S5, after the feathers containing the mixed solution are dehydrated by a dehydrator, the liquid content of the down is 50%-200%.

[0021] Preferably, in step S4, the drying temperature in the dryer is 110-150℃, and the drying time is 5-30 minutes.

[0022] This invention provides a method for preparing flame-retardant down. It has the following beneficial effects:

[0023] 1. This invention utilizes supercritical CO2 extraction to open up the surface of down fibers, creating pores that facilitate the penetration of flame retardants and antibacterial agents into the fiber interior. After water-repellent finishing and heat treatment, the down fiber surface shrinks, allowing the flame retardants and antibacterial agents to have long-lasting flame-retardant and antibacterial effects within the down fibers. Simultaneously, the supercritical CO2 extraction process reduces internal factors that promote bacterial growth, the antibacterial agents inhibit bacterial growth, and the water-repellent finishing prevents external moisture from entering, eliminating the moisture-absorbing odor of the treated down.

[0024] 2. This invention uses supercritical CO2 extraction to extract oil from down fibers, which is then further purified to obtain down oil. This down oil can be used alone and has skin-care, soothing, and moisturizing effects, and can also be added to other cosmetics as a functional ingredient.

[0025] 3. Through water-repellent finishing and fluffing treatment, the down's fluffiness is maintained, and external moisture is blocked from entering, without reducing the down's warmth retention. Attached Figure Description

[0026] Figure 1 This is a flowchart of the present invention. Detailed Implementation

[0027] The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. 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 skilled in the art without creative effort are within the scope of protection of the present invention.

[0028] Please see the appendix Figure 1 This invention provides a method for preparing flame-retardant down, comprising the following steps:

[0029] S1: Pre-treatment of coarse down, including pre-sorting and de-ashing operations, aims to remove impurities and surface grease from the down. This improves the purity and quality of the down and prepares it for subsequent processing steps.

[0030] S2: Through soaking and supercritical CO2 extraction, refined oils on the surface of the down are removed, and the down proteins swell and disulfide bonds are opened under controlled conditions. This step aims to further purify the down and improve its flame-retardant properties. The swelling of the down proteins and the opening of disulfide bonds increase the softness and plasticity of the fibers, aiding in subsequent finishing processes. The refined oils collected through supercritical CO2 extraction can be used as an additive in cosmetics, forming a lanolin-like substance. Further purification allows for its use alone with skin-care, soothing, and moisturizing effects, or it can be added to other cosmetics as a functional ingredient.

[0031] S3: The down treated in S2 is mixed with flame retardant, antibacterial finishing agent, organosiloxane compound, pH adjuster, penetrant, and water to form a flame retardant and antibacterial finishing solution of a certain concentration, and then allowed to stand at a constant temperature. The purpose of this step is to allow the down to fully absorb the flame retardant and antibacterial agent and distribute them evenly in the finishing solution, thereby improving the flame retardant properties and antibacterial effect of the down.

[0032] S4: After S3 treatment, the down is drained and water-repellent finishing agent, water, and other auxiliaries are added, with the treatment time controlled at 30 minutes. Subsequently, a lofting agent is added and treated for another 10 minutes to obtain down with a mixed solution. The purpose of this step is to further improve the flame retardant and antibacterial properties of the down, increase its loft and softness, and enhance the comfort and insulation performance of down products.

[0033] S5: After the S4 treatment, the down containing the mixed solution is dehydrated in a dehydrator to obtain down with a small amount of liquid. The dehydration process removes excess moisture, making the down drier and preparing it for subsequent drying.

[0034] S6: After the S5 treatment, the down feathers containing a small amount of liquid are dried in a high-temperature dryer to obtain the final finished down feathers. High-temperature drying can completely remove residual moisture and restore the down feathers to their ideal fluffy state, while also improving flame retardant effect and antibacterial properties.

[0035] In step S2, the co-solvent is one of ethanol, diethyl ether, petroleum ether, carbon tetrachloride, and n-hexane. These co-solvents have good solubility and extraction properties, which can effectively remove refined oils from the surface of down and promote the swelling of down proteins and the opening of disulfide bonds.

[0036] The flame retardant is a guanidine flame retardant or a boron-based flame retardant. The guanidine flame retardant is one or a mixture of several of the following: guanidine hydrochloride, guanidine nitrate, guanidine dihydrogen phosphate, diguanidine hydrogen phosphate, guanidine polyphosphate, biguanidine phosphate, guanidine aminosulfonate, amidourea phosphate guanidine salt, ammonium aminosulfonate, thiourea, thiourea monohydrochloride, and aminophosphate ester. The boron-based flame retardant is one or a mixture of several of the following: boric acid, sodium borate, ammonium borate, and potassium borate.

[0037] Guanidine flame retardants include guanidine hydrochloride, guanidine nitrate, guanidine dihydrogen phosphate, diguanidine hydrogen phosphate, guanidine polyphosphate, biguanidine phosphate, guanidine aminosulfonate, amidourea phosphate guanidine salt, ammonium aminosulfonate, aminothiourea, aminothiourea monohydrochloride, and aminophosphate esters. These guanidine flame retardants can inhibit the spread of flames by releasing reaction products such as nitrogen, water vapor, and inert gases.

[0038] Boron-based flame retardants include boric acid, sodium borate, ammonium borate, and potassium borate. These boron-based flame retardants have excellent flame-retardant properties and can undergo chemical reactions at high temperatures to form a protective layer, reducing the burning rate of materials and the spread of flames.

[0039] The use of these flame retardants can bring the following beneficial effects:

[0040] Flame retardant properties: Both guanidine flame retardants and boron-based flame retardants possess excellent flame retardant properties, effectively inhibiting flame spread and the burning rate of materials. This contributes to improving product safety and reliability.

[0041] Thermal stability: Flame retardants can improve the thermal stability of materials, reducing material decomposition and gas release at high temperatures. This is especially important for products that need to be used in high-temperature environments.

[0042] Toxicity Control: Guanidine flame retardants and boron-based flame retardants are relatively environmentally friendly, with their reaction products exhibiting low toxicity to humans and the environment. This helps reduce the potential harm of the products to human health and the environment.

[0043] The antibacterial finishing agent is an organosilicon quaternary ammonium salt, an organonitrogen compound, a nitrofuran, a biguanide, or a chlorobenzamide. The organosiloxane compound is one or a mixture of several of the following: trimethoxysiloxane, methyltrimethoxysiloxane, tetramethoxysiloxane, vinyltrimethoxysiloxane, vinyltriisopropoxysiloxane, triethoxysiloxane, phenyltrimethoxysiloxane, and phenyltriethoxysiloxane.

[0044] Organosilicon quaternary ammonium salts are commonly used antibacterial finishing agents with good antibacterial properties. They achieve their antibacterial effect by reacting with microorganisms on the fabric surface, disrupting cell membrane structures, and inhibiting the growth and reproduction of microorganisms.

[0045] Organic nitrogen compounds are also common antibacterial finishing agents. Their molecular structure contains nitrogen atoms, giving them strong antibacterial activity. They can interact with the cell walls or cell membranes of microorganisms, disrupting their structure and function, thus exerting an antibacterial effect.

[0046] Nitrofurans are a class of compounds with broad-spectrum antibacterial activity, capable of inhibiting the growth and reproduction of various bacteria and fungi. They exert their antibacterial effect by interfering with the metabolic processes of microorganisms and disrupting their cell structure.

[0047] Biguanides are a class of antibacterial agents with strong antibacterial properties. They achieve their antibacterial effect by interacting with intracellular components of microorganisms, disrupting their metabolic processes, and inhibiting their growth and reproduction.

[0048] Chlorfenimazoles are also a commonly used class of antibacterial finishing agents with broad-spectrum antibacterial activity. They can react with the DNA or RNA of microorganisms, blocking the transmission and replication of genetic information, thereby inhibiting the growth and reproduction of microorganisms.

[0049] In addition, organosiloxane compounds, such as trimethoxysiloxane, methyltrimethoxysiloxane, and tetramethoxysiloxane, are also commonly used in antibacterial finishing agents. They have good hydrophilicity and wettability, and can form a protective layer on the fiber surface, preventing the attachment and growth of microorganisms.

[0050] The use of these antibacterial finishing agents can bring the following beneficial effects:

[0051] Antibacterial properties: These antibacterial finishing agents can effectively inhibit the growth and reproduction of microorganisms, reduce the number of bacteria, fungi and other microorganisms on fabrics, and thus have an antibacterial effect.

[0052] Long-lasting effect: Some antibacterial finishing agents have a long-lasting effect and can maintain good antibacterial properties even after multiple washes and uses, thus extending the service life of fabrics.

[0053] Health and Hygiene: By using antimicrobial finishing agents, the number of bacteria and fungi on the surface of fabrics can be reduced, which helps to improve the hygiene performance of the product and reduce potential impacts on human health.

[0054] The acid-base regulator is a polybasic acid, specifically one or a mixture of several of the following: oxalic acid, hydroxysuccinic acid, dihydroxysuccinic acid, citric acid, phosphoric acid, butanetetracarboxylic acid, and polymaleic acid; the penetrant is nonionic or anionic, specifically one or a mixture of several of the following: JFC, JFC-1, JFC-2, JFC-E nonionic penetrant or rapid penetrant T, alkali-resistant penetrant OEP-70, and alkali-resistant penetrant AEP anionic penetrant.

[0055] Polybasic acids are a class of commonly used acid-base regulators that can adjust the pH of a solution to maintain it within an appropriate acid-base range. Specifically, oxalic acid, hydroxysuccinic acid, and dihydroxysuccinic acid can release hydrogen ions in solution, thus acting as an acid regulator; citric acid, phosphoric acid, and butanetetracarboxylic acid can release hydroxide ions or phosphate ions in solution, thus acting as an alkaline regulator; and polymaleic acid can adjust the pH value in solution through an acid-base balance reaction.

[0056] Regarding penetrants, nonionic and anionic penetrants can be selected, such as JFC, JFC-1, JFC-2, and JFC-E nonionic penetrants, or fast penetrant T, alkali-resistant penetrant OEP-70, and alkali-resistant penetrant AEP anionic penetrants, etc.

[0057] Nonionic penetrants have good penetration properties, improving the dispersion and penetration of dyes and auxiliaries in fabrics and enhancing the overall dyeing effect. Anionic penetrants, on the other hand, have good alkali resistance, remaining stable under high alkaline conditions, and exhibiting excellent penetration properties for fiber dyeing and finishing.

[0058] The use of these pH adjusters and penetrants can bring the following beneficial effects:

[0059] pH adjustment: Polybasic acids can effectively adjust the pH value of the solution to adapt to different process requirements and improve the effect of dyeing, finishing and other processes.

[0060] Penetration performance: Nonionic and anionic penetrants can improve the penetration performance of dyes and auxiliaries in fabrics, and improve the uniformity of dyeing and color fastness.

[0061] Stability: Some penetrants have good stability and can maintain good performance under different process conditions, thus improving the stability and consistency of the product.

[0062] By selecting polybasic acids as pH adjusters and combining them with nonionic and anionic penetrants, the pH value of the solution can be effectively adjusted and the penetration performance of dyes can be improved, thereby enhancing the dyeing effect and product stability.

[0063] The water-repellent finishing agent is a fluorocarbon-based water-repellent agent, an organosilicon-based water-repellent finishing agent, a paraffin-based water-repellent finishing agent, or a non-fluorinated water-repellent finishing agent. The fluffing agent is a special fluffing agent for down products. The concentration of the water-repellent finishing agent is 20-100g / L, and the concentration of the fluffing agent is 20-100g / L.

[0064] Fluorocarbon water-repellent agents are a commonly used class of water-repellent finishing agents with excellent water-repellent properties. They can form a durable hydrophobic film on the fiber surface, preventing water penetration and improving the waterproof performance of the fabric.

[0065] Organosilicon water-repellent finishing agents are also common water-repellent agents. They can form tiny particles on the fiber surface, increase the surface tension of the fabric, and cause water to form droplets and slide off, thus achieving a water-repellent effect.

[0066] Paraffin-based water-repellent finishing agents achieve their water-repellent effect primarily by forming a thin film on the fiber surface. This film has a certain degree of air permeability, preventing moisture penetration while maintaining a certain level of moisture permeability.

[0067] Non-fluorinated water-repellent finishing agents are water-repellent agents that do not contain fluorinated carbon compounds, and their water-repellent effect is mainly based on other chemical principles. These water-repellent agents usually have good environmental friendliness and sustainability.

[0068] Regarding lofting agents, down-specific lofting agents can be used to treat down products, helping to restore the loft and elasticity of the down. They can improve the porosity between down fibers, enhancing the fabric's insulation and comfort.

[0069] In terms of application, the concentration of water-repellent finishing agents is generally 20-100 g / L, and the concentration of leavening agents is also 20-100 g / L. The specific concentration can be adjusted according to different product requirements and processes.

[0070] By selecting fluorocarbon water-repellent agents, silicone water-repellent finishing agents, paraffin water-repellent finishing agents, or non-fluorinated water-repellent finishing agents as water-repellent finishing agents, and down-specific fluffing agents as fluffing agents, waterproofing and fluffing treatments of fabrics can be achieved.

[0071] In step S3, the ratio of flame retardant, antibacterial finishing agent, and down is 50:1-5:1; the mass ratio of flame retardant to down is 5%-50%; the mass ratio of antibacterial finishing agent to down is 0.5-5%; the mass ratio of pH adjuster to down is 1%-5%; the mass ratio of penetrant to down is 1-10%; the constant temperature treatment temperature is 30-90℃, and the treatment time is 30-150 minutes.

[0072] In step S5, after the feathers containing the mixed solution are dehydrated by a dehydrator, the liquid content of the down is 50%-200%.

[0073] Liquid content refers to the ratio of the weight of residual liquid in down to the dry weight of the down itself. During the dehydration process in a centrifuge, methods such as rotation or squeezing are used to remove as much liquid as possible from the down to minimize the impact of residual liquid on the down.

[0074] The liquid content range can be adjusted according to specific process requirements and product performance. A lower liquid content allows down to dry faster and improves production efficiency, but may affect certain performance indicators. A higher liquid content can maintain the softness and elasticity of down, but may require a longer drying time.

[0075] Therefore, the specific liquid carryover rate should be determined based on product requirements, process flow, and equipment capabilities. In practice, experiments and optimizations can be conducted to find the most suitable liquid carryover rate range for the product.

[0076] In step S4, the drying temperature in the dryer is 110-150℃, and the drying time is 5-30 minutes.

[0077] Example 1:

[0078] This invention provides a method for preparing flame-retardant down, comprising the following steps:

[0079] S1. First, pre-sort and remove ash from the coarse down feathers, and wash the down feathers 10 times with hot water and detergent to remove the coarse grease on the surface.

[0080] S2. Soak the cleaned down in ethanol (99%, time 30 min), and then transfer it into a supercritical CO2 extraction instrument for extraction. The extraction pressure is 25 MPa, the extraction temperature is 50℃, and the extraction time is 60 min. The yield of down oil is 18%.

[0081] S3. Mix 10% boric acid, 5% trimethoxysiloxane, 5% organosilicon quaternary ammonium salt antibacterial finishing agent, 10% ethanol, 3% penetrant JFC-1 and water to form a finishing solution. Add oxalic acid to adjust the pH to 3 and heat to 30°C. Then add the down feathers that have undergone supercritical CO2 extraction of oil in step S2 to the above solution. The ratio of finishing solution to down feathers is 40:1, and the treatment time is 120 min.

[0082] S4. Drain the down treated in step S3. After draining, add silicone water-repellent finishing agent (concentration 60g / L) and water, with a bath ratio of 20:1 and a temperature of 50℃ for 30 minutes. After draining, add down fluffing agent (40g / L) and water, with a bath ratio of 20:1 and a temperature of 30℃ for 10 minutes.

[0083] S5. Pour the mixed solution into a high-speed centrifugal dehydrator and dehydrate for 15 minutes to obtain wet down with 100% liquid content.

[0084] S6. The obtained wet down is put into a 130℃ hot air dryer for 19 minutes, and then it enters the cooling and feather separation process to obtain down with good flame retardant, antibacterial and water repellent effects.

[0085] Taking 80% flame-retardant down as an example, its performance is as follows:

[0086]

[0087] Example 2:

[0088] This invention provides a method for preparing flame-retardant down, comprising the following steps:

[0089] S1. First, pre-sort and remove ash from the coarse down feathers, and wash the down feathers 10 times with hot water and detergent to remove the coarse grease on the surface.

[0090] S2. The cleaned down was extracted using a supercritical CO2 extraction instrument at an extraction pressure of 35 MPa, an extraction temperature of 50°C, and an extraction time of 80 min. The yield of down oil was 17%.

[0091] S3. Add the down treated in step S2 to the washing device, add 20% by weight (down) of guanidine polyphosphate, 2% by weight (down) of nitrofuran antibacterial agent, 2% by weight (down) of citric acid, 3% by weight (down) of penetrant JFC-1, and an appropriate amount of water, mix and stir evenly to form a flame retardant and antibacterial finishing solution of a certain concentration; the bath ratio of the flame retardant and antibacterial finishing solution to the down is 30:1, heat to 60℃, and stir for 100 minutes;

[0092] S4. Drain the down treated in step S3. After draining, add C8 water-repellent finishing agent (concentration 40g / L) and water, with a bath ratio of 20:1 and a temperature of 50℃ for 30 minutes. After draining, add down fluffing agent (40g / L) and water, with a bath ratio of 20:1 and a temperature of 30℃ for 10 minutes.

[0093] S5. Pour the mixed solution into a high-speed centrifugal dehydrator and dehydrate for 10 minutes to obtain wet down with 120% liquid content.

[0094] S6. The obtained wet down is put into a 120℃ hot air dryer for 24 minutes, and then it enters the cooling and feather separation process to obtain down with good flame retardant, antibacterial and water repellent effects.

[0095] Taking 80% flame-retardant down as an example, its performance is as follows:

[0096]

[0097] Example 3:

[0098] This invention provides a method for preparing flame-retardant down, comprising the following steps:

[0099] S1. First, pre-sort and remove ash from the coarse down feathers, and wash the down feathers 10 times with hot water and detergent to remove the coarse grease on the surface.

[0100] S2. The cleaned down was extracted using a supercritical CO2 extraction instrument at an extraction pressure of 30 MPa, an extraction temperature of 60°C, and an extraction time of 100 min. The yield of down oil was 16%.

[0101] S3. Add the down treated in step S2 to the washing device, add 25% by weight (down) of dihydroguanidine phosphate, 3% by weight (down) of chlorfenapyrazole antibacterial agent, 3% by weight (down) of phosphoric acid, 5% by weight (down) of penetrant JFC-2, and an appropriate amount of water, mix and stir evenly to form a flame retardant and antibacterial finishing solution of a certain concentration; the bath ratio of the flame retardant and antibacterial finishing solution to the down is 20:1, heat to 70℃, and stir for 90 minutes;

[0102] S4. Drain the down treated in step S3. After draining, add silicone water-repellent finishing agent (concentration 60g / L) and water, with a bath ratio of 20:1 and a temperature of 50℃ for 30 minutes. After draining, add down fluffing agent (40g / L) and water, with a bath ratio of 20:1 and a temperature of 30℃ for 10 minutes.

[0103] S5. Pour the mixed solution into a high-speed centrifugal dehydrator and dehydrate for 15 minutes to obtain wet down with 100% liquid content.

[0104] S6. The obtained wet down is put into a 130℃ hot air dryer for 19 minutes, and then it enters the cooling and feather separation process to obtain down with good flame retardant, antibacterial and water repellent effects.

[0105] Taking 90% flame-retardant down as an example, its performance is as follows:

[0106]

[0107] Example 4:

[0108] This invention provides a method for preparing flame-retardant down, comprising the following steps:

[0109] S1. First, pre-sort and remove ash from the coarse down feathers, and wash the down feathers 10 times with hot water and detergent to remove the coarse grease on the surface.

[0110] S2. The cleaned down was extracted using a supercritical CO2 extraction instrument at an extraction pressure of 40 MPa, an extraction temperature of 60°C, and an extraction time of 100 min. The yield of down oil was 20%.

[0111] S3. Add the down treated in step S2 to the washing device, add 30% by weight (down) of biguanide phosphate, 4% by weight (down) of chlorfenapyrazole antibacterial agent, 2% by weight (down) of butanetetracarboxylic acid, 6% by weight (down) of penetrant JFC-2, and an appropriate amount of water, mix and stir evenly to form a flame retardant and antibacterial finishing solution of a certain concentration; the bath ratio of the flame retardant and antibacterial finishing solution to the down is 15:1, heat to 80℃, and stir for 70 minutes;

[0112] S4. Drain the down treated in step S3. After draining, add a paraffin-based water-repellent finishing agent (concentration 50g / L) and water at a bath ratio of 20:1 and a temperature of 50℃ for 30 minutes. After draining, add a down fluffing agent (40g / L) and water at a bath ratio of 20:1 and a temperature of 30℃ for 10 minutes.

[0113] S5. Pour the mixed solution into a high-speed centrifugal dehydrator and dehydrate for 20 minutes to obtain wet down with 85% liquid content.

[0114] S6. The obtained wet down is put into a 140℃ hot air dryer for 13 minutes, and then it enters the cooling and feather separation process to obtain down with good flame retardant, antibacterial and water repellent effects.

[0115] Taking 80% flame-retardant down as an example, its performance is as follows:

[0116]

[0117] Example 5:

[0118] This invention provides a method for preparing flame-retardant down, comprising the following steps:

[0119] S1. First, pre-sort and remove ash from the coarse down feathers, and wash the down feathers 10 times with hot water and detergent to remove the coarse grease on the surface.

[0120] S2. The cleaned down was extracted using a supercritical CO2 extraction instrument at an extraction pressure of 40 MPa, an extraction temperature of 65°C, and an extraction time of 120 min. The yield of down oil was 22%.

[0121] S3. Add the down treated in step S2 to the washing device, add 30% by weight (down) of guanidine aminosulfonate, 5% by weight (down) of chlorfenapyrazole antibacterial agent, 2% by weight (down) of polymaleic acid, 8% by weight (down) of penetrant JFC-1, and an appropriate amount of water, mix and stir evenly to form a flame retardant and antibacterial finishing solution of a certain concentration; the bath ratio of the flame retardant and antibacterial finishing solution to the down is 10:1, heat to 90℃, and stir for 40 minutes;

[0122] S4. Drain the down treated in step S3. After draining, add silicone water-repellent finishing agent (concentration 60g / L) and water, with a bath ratio of 20:1 and a temperature of 50℃ for 30 minutes. After draining, add down fluffing agent (40g / L) and water, with a bath ratio of 20:1 and a temperature of 30℃ for 10 minutes.

[0123] S5. Pour the mixed solution into a high-speed centrifugal dehydrator and dehydrate for 30 minutes to obtain wet down with 60% liquid content.

[0124] S6. The obtained wet down is put into a 150℃ hot air dryer for 7 minutes, and then cooled and separated to obtain down with good flame retardant, antibacterial and water-repellent effects.

[0125] Taking 80% flame-retardant down as an example, its performance is as follows:

[0126]

[0127] Example 6:

[0128] This invention provides a method for preparing flame-retardant down, comprising the following steps:

[0129] S1. First, pre-sort and remove ash from the coarse down feathers, and wash the down feathers 10 times with hot water and detergent to remove the coarse grease on the surface.

[0130] S2. Soak the cleaned down in ethanol (99%, time 30 min), and then transfer it into a supercritical CO2 extraction instrument for extraction. The extraction pressure is 25 MPa, the extraction temperature is 50℃, and the extraction time is 60 min. The yield of down oil is 18%.

[0131] S3. Mix 10% boric acid, 5% trimethoxysiloxane, 5% organosilicon quaternary ammonium salt antibacterial finishing agent, 10% ethanol, 3% penetrant JFC-1 and water to form a finishing solution. Add oxalic acid to adjust the pH to 3 and heat to 30°C. Then add the down feathers that have undergone supercritical CO2 extraction of oil in step S2 to the above solution. The ratio of finishing solution to down feathers is 40:1, and the treatment time is 120 min.

[0132] S4. Drain the down treated in step S3. After draining, add silicone water-repellent finishing agent (concentration 60g / L) and water, with a bath ratio of 20:1 and a temperature of 50℃ for 30 minutes. After draining, add down fluffing agent (40g / L) and water, with a bath ratio of 20:1 and a temperature of 30℃ for 10 minutes.

[0133] S5. Pour the mixed solution into a high-speed centrifugal dehydrator and dehydrate for 15 minutes to obtain wet down with 100% liquid content.

[0134] S6. The obtained wet down is put into a 130℃ hot air dryer for 19 minutes, and then it enters the cooling and feather separation process to obtain down with good flame retardant, antibacterial and water repellent effects.

[0135] Taking 80% flame-retardant down as an example, its performance is as follows:

[0136]

[0137] Example 7:

[0138] This invention provides a method for preparing flame-retardant down, comprising the following steps:

[0139] S1. First, pre-sort and remove ash from the coarse down feathers, and wash the down feathers 10 times with hot water and detergent to remove the coarse grease on the surface.

[0140] S2. Soak the cleaned down in ethanol (99%, time 30 min), and then transfer it into a supercritical CO2 extraction instrument for extraction. The extraction pressure is 30 MPa, the extraction temperature is 55℃, and the extraction time is 80 min. The yield of down oil is 20%.

[0141] S3. Mix 15% boric acid, 10% vinyltrimethoxysiloxane, 10% nitrofuran antibacterial finishing agent, 15% ethanol, 5% penetrant JFC-1, and water to form a finishing solution. Add hydroxysuccinic acid to adjust the pH to 3 and heat to 40℃. Then, add the down feathers that have undergone supercritical CO2 extraction of oil in step S2 to the above solution. The ratio of finishing solution to down feathers is 30:1, and the treatment time is 100 min. After draining, add C8 water-repellent finishing agent (concentration 40 g / L) and water. The bath ratio is 20:1, the temperature is 50℃, and the treatment time is 30 min.

[0142] S4. Drain the down treated in step S3. After draining, add down fluffing agent (40g / L) and water at a bath ratio of 20:1 and a temperature of 30℃ for 10 minutes.

[0143] S5. Pour the mixed solution into a high-speed centrifugal dehydrator and dehydrate for 10 minutes to obtain wet down with 120% liquid content.

[0144] S6. The obtained wet down is put into a 120℃ hot air dryer for 24 minutes, and then cooled and separated to obtain down with good flame retardant, antibacterial and water-repellent effects.

[0145] Taking 80% flame-retardant down as an example, its performance is as follows:

[0146]

[0147] Example 8:

[0148] This invention provides a method for preparing flame-retardant down, comprising the following steps:

[0149] S1. First, pre-sort and remove ash from the coarse down feathers, and wash the down feathers 10 times with hot water and detergent to remove the coarse grease on the surface.

[0150] S2. Soak the cleaned down in ethanol (99%, time 30 min), and then transfer it into a supercritical CO2 extraction instrument for extraction. The extraction pressure is 35 MPa, the extraction temperature is 60℃, and the extraction time is 100 min. The yield of down oil is 24%.

[0151] S3. Mix 20% sodium borate, 15% vinyltrimethoxysiloxane, 15% organosilicon quaternary ammonium salt antibacterial finishing agent, 15% ethanol, 7% penetrant JFC-2 and water to form a finishing solution. Add citric acid to adjust the pH to 4 and heat to 50°C. Then add the down feathers that have undergone supercritical CO2 extraction of oil in step S2 to the above solution. The ratio of finishing solution to down feathers is 20:1, and the treatment time is 90 min.

[0152] S4. Drain the down treated in step S3. After draining, add silicone water-repellent finishing agent (concentration 60g / L) and water, with a bath ratio of 20:1 and a temperature of 50℃ for 30 minutes. After draining, add down fluffing agent (40g / L) and water, with a bath ratio of 20:1 and a temperature of 30℃ for 10 minutes.

[0153] S5. Pour the mixed solution into a high-speed centrifugal dehydrator and dehydrate for 15 minutes to obtain wet down with 100% liquid content.

[0154] S6. The obtained wet down is put into a 130℃ hot air dryer for 19 minutes, and then it enters the cooling and feather separation process to obtain down with good flame retardant, antibacterial and water repellent effects.

[0155] Taking 90% flame-retardant down as an example, its performance is as follows:

[0156]

[0157]

[0158] Example 9:

[0159] This invention provides a method for preparing flame-retardant down, comprising the following steps:

[0160] S1. First, pre-sort and remove ash from the coarse down feathers, and wash the down feathers 10 times with hot water and detergent to remove the coarse grease on the surface.

[0161] S2. Soak the cleaned down in ethanol (99%, time 30 min), and then transfer it into a supercritical CO2 extraction instrument for extraction. The extraction pressure is 40 MPa, the extraction temperature is 60℃, and the extraction time is 120 min. The yield of down oil is 28%.

[0162] S3. Mix 30% ammonium borate, 15% phenyltrimethoxysiloxane, 15% chlorobenzamide antibacterial finishing agent, 20% ethanol, 7% penetrant JFC-2 and water to form a finishing solution. Add phosphoric acid to adjust the pH to 4 and heat to 60°C. Then add the down feathers that have undergone supercritical CO2 extraction of oil in step S2 to the above solution. The ratio of finishing solution to down feathers is 10:1, and the treatment time is 80 min.

[0163] S4. Drain the down treated in step S3. After draining, add a paraffin-based water-repellent finishing agent (concentration 50g / L) and water at a bath ratio of 20:1 and a temperature of 50℃ for 30 minutes. After draining, add a down fluffing agent (40g / L) and water at a bath ratio of 20:1 and a temperature of 30℃ for 10 minutes.

[0164] S5. Pour the mixed solution into a high-speed centrifugal dehydrator and dehydrate for 20 minutes to obtain wet down with 85% liquid content.

[0165] S6. The obtained wet down is put into a 140℃ hot air dryer for 13 minutes, and then it enters the cooling and feather separation process to obtain down with good flame retardant, antibacterial and water repellent effects.

[0166] Taking 80% flame-retardant down as an example, its performance is as follows:

[0167]

[0168]

[0169] Example 10:

[0170] This invention provides a method for preparing flame-retardant down, comprising the following steps:

[0171] S1. First, pre-sort and remove ash from the coarse down feathers, and wash the down feathers 10 times with hot water and detergent to remove the coarse grease on the surface.

[0172] S2. Soak the cleaned down in ethanol (99%, time 30 min), and then transfer it into a supercritical CO2 extraction instrument for extraction. The extraction pressure is 40 MPa, the extraction temperature is 60℃, and the extraction time is 150 min. The yield of down oil is 30%.

[0173] S3. Mix 40% potassium borate, 20% phenyltriethoxysiloxane, 20% chlorobenzamide antibacterial finishing agent, 20% ethanol, 9% penetrant JFC-1, and water to form a finishing solution. Add butanetetracarboxylic acid to adjust the pH to 2 and heat to 60℃. Then add the down feathers that have undergone supercritical CO2 extraction in step S2 to the above solution. The ratio of finishing solution to down feathers is 5:1, and the treatment time is 60 min. After draining, add organosilicon water-repellent finishing agent (concentration 60 g / L) and water. The bath ratio is 20:1, the temperature is 50℃, and the treatment time is 30 min.

[0174] S4. Drain the down treated in step S3. After draining, add down fluffing agent (40g / L) and water at a bath ratio of 20:1 and a temperature of 30℃ for 10 minutes.

[0175] S5. Pour the mixed solution into a high-speed centrifugal dehydrator and dehydrate for 30 minutes to obtain wet down with 60% liquid content.

[0176] S6. The obtained wet down is put into a 150℃ hot air dryer for 7 minutes, and then cooled and separated to obtain down with good flame retardant, antibacterial and water-repellent effects.

[0177] Taking 80% flame-retardant down as an example, its performance is as follows:

[0178]

[0179]

[0180] 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 flame-retardant down, characterized in that, Includes the following steps: S1. Pre-sort and remove ash from the coarse down feathers, and wash the feathers with hot water and detergent to remove the coarse grease on the surface; S2. Soak the down processed in step S1 in a co-solvent, and then use a supercritical CO2 extraction device to remove the refined oil on the surface of the washed and soaked down for further processing of the down surface and collection of refined oil, while making the down protein swell and controlling the opening of disulfide bonds. S3. Add the down treated in step S2 to a washing device, and add flame retardant, antibacterial finishing agent, organosiloxane compound, pH adjuster, penetrant, and water in a certain proportion to form a flame retardant and antibacterial finishing solution of a certain concentration. Let it stand at a constant temperature. In this step, the ratio of the flame retardant, antibacterial finishing agent, and down is 50:1-5:1; the flame retardant accounts for 5%-50% of the down mass; the antibacterial finishing agent accounts for 0.5-5% of the down mass; the pH adjuster accounts for 1%-5% of the down mass; the penetrant accounts for 1-10% of the down mass; the constant temperature standing treatment temperature is 30-90℃, and the treatment time is 30-150 minutes. S4. Drain the down treated in step S3, add water-repellent finishing agent, water and other auxiliaries, control the liquor ratio, and treat for 30 minutes; after draining, add fluffing agent and treat for another 10 minutes to obtain down with the mixed solution. S5. The feathers with mixed solution obtained in step S4 are dehydrated by a dehydrator to obtain down with a small amount of liquid. In this step, the liquid content of the down after the feathers with mixed solution are dehydrated by the dehydrator is 50%-200%. S6. The down with a small amount of liquid obtained in step S5 is dried in a high-temperature dryer to obtain finished feathers. In this step, the drying temperature in the dryer is 110-150℃ and the drying time is 5-30 minutes.

2. The method for preparing flame-retardant down according to claim 1, characterized in that, In step S2, the co-solvent is one of ethanol, diethyl ether, petroleum ether, carbon tetrachloride, and n-hexane.

3. The method for preparing flame-retardant down according to claim 1, characterized in that, The flame retardant is a guanidine flame retardant or a boron-based flame retardant. The guanidine flame retardant is one or a mixture of several of guanidine hydrochloride, guanidine nitrate, guanidine dihydrogen phosphate, diguanidine hydrogen phosphate, guanidine polyphosphate, biguanidine phosphate, guanidine aminosulfonate, and guanidine amidourea phosphate. The boron-based flame retardant is one or a mixture of several of boric acid, sodium borate, ammonium borate, and potassium borate.

4. The method for preparing flame-retardant down according to claim 1, characterized in that, The antibacterial finishing agent is an organosilicon quaternary ammonium salt, an organonitrogen compound, a nitrofuran, a biguanide, or a chlorobenzamide, and the organosiloxane compound is one or a mixture of several of the following: trimethoxysiloxane, methyltrimethoxysiloxane, tetramethoxysiloxane, vinyltrimethoxysiloxane, vinyltriisopropoxysiloxane, triethoxysiloxane, phenyltrimethoxysiloxane, and phenyltriethoxysiloxane.

5. The method for preparing flame-retardant down according to claim 1, characterized in that, The acid-base regulator is a polyacid, specifically one or a mixture of several of citric acid, phosphoric acid, butanetetracarboxylic acid, and polymaleic acid.

6. The method for preparing flame-retardant down according to claim 1, characterized in that, The water-repellent finishing agent is a fluorocarbon-based water-repellent agent or a non-fluorinated water-repellent finishing agent, and the fluffing agent is a special fluffing agent for down products. The concentration of the water-repellent finishing agent is 20-100g / L, and the concentration of the fluffing agent is 20-100g / L.

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