High-permeability phosphorus-free environment-friendly textile refining aid and preparation method thereof

CN122833862APending Publication Date: 2026-09-29YICHENG CHENGXIONG WEAVING CO LTD
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Patent Information

Application Number
CN202610989964.6
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2026-07-03
Publication Date
2026-09-29

AI Technical Summary

Technical Problem

[0008]本发明的目的在于提供一种高渗透无磷环保纺织精炼助剂及其制备方法,以解决上述背景技术中提出现有的纺织精炼助剂普遍存在渗透性不佳、含磷不环保、生物降解性差的缺陷,难以满足当下绿色纺织生产与高效精炼的使用需求的问题

Benefits of technology

[0033]与现有技术相比,本发明的有益效果是:该高渗透无磷环保纺织精炼助剂及其制备方法;

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Abstract

The application relates to the technical field of textile auxiliaries, and discloses a high-penetration phosphorus-free environment-friendly textile refining auxiliary and a preparation method thereof, which comprises alcohol ether carboxylate 1, isomeric tridecanol polyoxyethylene ether, C8-C10 alkyl glycoside, maleic anhydride-acrylic acid copolymer, tetrasodium iminodisuccinate, bio-based coconut oil fatty acid diethanolamide, foam inhibitor and deionized water. The prepared auxiliary is a phosphorus-free environment-friendly product, the wastewater is free of phosphorus pollution, water body eutrophication can be avoided, the biodegradability is good, and the ecological safety is good. A plurality of surfactants are compounded, the penetration, emulsification and cleaning capacity are prominent, various fabrics can be uniformly refined, and various impurities can be efficiently removed. The dispersing and chelating components can prevent dirt from being sticky, improve the whiteness and cleanliness of the fabrics, have good foam inhibition effect, and are suitable for continuous production. Meanwhile, the preparation process is simple and controllable, special feeding and stirring modes make the materials fully mix, the finished product system is stable, and the efficient production and green environmental protection requirements are met.
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Description

Technical Field

[0001] This invention relates to the field of textile auxiliaries technology, specifically to a high-penetration, phosphorus-free, environmentally friendly textile refining auxiliary agent and its preparation method. Background Technology

[0002] Textile scouring is the core process of pretreatment before textile printing and dyeing. It mainly removes pectin, cotton wax, ash, natural pigments and impurities such as sizing agents and machine oils added during the weaving process from the fabric itself, thereby improving the fabric's hydrophilicity and whiteness, and providing qualified fabric for subsequent dyeing and printing processes.

[0003] Currently, the mainstream traditional textile refining auxiliaries on the market have many shortcomings in terms of technology and environmental protection, and are no longer able to meet the current needs of green production and high-standard processing in the textile industry.

[0004] First, most traditional product formulations contain phosphorus-containing auxiliaries and phosphate chelating agents. These phosphorus-containing substances are directly discharged into the wastewater after textile refining, leading to serious exceedances of total phosphorus content in water bodies. When phosphorus enters natural water systems, it induces the rampant growth of algae and aquatic plants, resulting in eutrophication, water quality deterioration, oxygen depletion, and mass mortality of aquatic organisms, among other ecological problems. This contradicts the increasingly stringent national wastewater discharge standards and green and environmentally friendly production requirements. In order to reduce costs, some phosphorus-free auxiliaries use synthetic surfactants with poor or even poor biodegradability. Although this achieves phosphorus-free status, the residues of these auxiliaries and the wastewater from production still cause hidden pollution to water bodies and soil, failing to truly achieve the goal of green and environmental protection.

[0005] Secondly, traditional refining auxiliaries generally have weak penetration performance and insufficient surface-active system wetting ability. When dealing with high-density fabrics, heavy fabrics, and dense textiles with high yarn twist, the auxiliaries cannot quickly penetrate the gaps between fabric fibers and cannot complete overall wetting in a short time. This results in uneven refining of the fabric, leading to quality defects such as incomplete local impurity removal, inconsistent capillary effect, and obvious color difference, which significantly reduces the quality of the finished textile product.

[0006] In addition, the surfactants used in traditional auxiliaries are mostly recalcitrant and have low biodegradability. After the refining process, some of the auxiliaries remain inside the fabric fibers, while others flow into the natural environment with wastewater. Over time, this accumulation will cause continuous pollution to the soil and water ecosystems, not only disrupting the natural ecological balance but also hindering the textile industry from developing in a low-carbon, environmentally friendly, and sustainable direction.

[0007] In view of this, and in response to the above problems, we conducted in-depth research and proposed a high-penetration, phosphorus-free, environmentally friendly textile refining agent and its preparation method. Summary of the Invention

[0008] The purpose of this invention is to provide a high-penetration, phosphorus-free, environmentally friendly textile refining agent and its preparation method, in order to solve the problems mentioned in the background art, such as poor permeability, phosphorus content and environmental unfriendliness, and poor biodegradability of existing textile refining auxiliaries, which make it difficult to meet the current needs of green textile production and efficient refining.

[0009] To achieve the above objectives, the present invention provides the following technical solution: a high-penetration, phosphorus-free, environmentally friendly textile refining auxiliary agent, comprising the following components by mass percentage: Alcohol ether carboxylates: 18%–26%; Isomeric tridecyl alcohol polyoxyethylene ether 7%–12%; C8-C10 alkyl glycosides 9%–16%; 3%–5% maleic anhydride-acrylic acid copolymer; Tetrasodium iminodisuccinate 4%–7%; Bio-based coconut oil fatty acid diethanolamide 1.5%–3%; Defoamer 1%–2%; The remainder is deionized water.

[0010] Using the above technical solution, the formula is phosphorus-free, green, environmentally friendly and pollution-free; the surfactant compound works synergistically, with excellent penetration, emulsification, impurity removal and cleaning capabilities, while having good compatibility and system stability, which can meet the refining and processing needs of various fabrics.

[0011] As a preferred embodiment of the present invention, the alcohol ether carboxylate is sodium fatty alcohol polyoxyethylene ether carboxylate, with a surface tension ≤32mN / m and a solid content ≥98%.

[0012] The above technical solution can effectively reduce the surface tension of the system, improve the wetting, penetration and emulsification ability of the auxiliaries on the fabric fibers, and reduce ineffective components due to the high solid content, thereby enhancing the cleaning and impurity removal effect.

[0013] As a preferred embodiment of the present invention, the EO addition number of the isomeric tridecyl alcohol polyoxyethylene ether is 5 to 7, and the penetration power is ≤8s.

[0014] The above technical solution facilitates the imbuing of auxiliaries with ultra-fast penetration properties, enabling them to quickly penetrate the fiber gaps of high-density, thick fabrics, ensuring uniform refining throughout the fabric, and avoiding problems such as incomplete impurity removal and uneven capillary effect.

[0015] As a preferred embodiment of the present invention, the degree of polymerization of the C8-C10 alkyl glycoside is 1.2 to 1.4.

[0016] Using the above technical solution, the component has excellent biodegradability, and the production wastewater has extremely low harm to the ecological environment, which meets the requirements of environmentally friendly production. At the same time, it can further enhance the emulsification and dispersing properties of the additives.

[0017] As a preferred embodiment of the present invention, the maleic anhydride-acrylic acid copolymer has a number-average molecular weight of 2000-4000 and a solid content of 40%.

[0018] The above technical solution facilitates excellent dispersion, chelation and anti-redeposition effects, can firmly wrap the stripped impurities, prevent dirt from re-adhering to the fabric surface, and improve the whiteness and cleanliness of the refined product.

[0019] A method for preparing a high-penetration, phosphorus-free, environmentally friendly textile refining auxiliary agent includes the following steps:

[0020] Step 1: Preparation of base solution: At room temperature, add 50% to 60% of the formula amount of deionized water to the reaction vessel and heat and stir.

[0021] Step 2, surfactant compounding: Add isotridecyl alcohol polyoxyethylene ether and C8-C10 alkyl glycoside to the reaction vessel at the same time, and stir continuously at a constant temperature until the system is completely transparent without layering or gel clumping.

[0022] Step 3, Addition of functional components: Slowly add alcohol ether carboxylate, and continue stirring at a constant temperature after the addition is complete. Then add maleic anhydride-acrylic acid copolymer, tetrasodium iminodisuccinate and bio-based coconut oil fatty acid diethanolamide in sequence, and heat and stir.

[0023] Step 4, Post-processing and molding: After cooling, add defoaming agent, add remaining deionized water, continue stirring, let stand, adjust pH, and filter to obtain high-permeability phosphorus-free environmentally friendly textile refining auxiliary product.

[0024] The above technical solution has a simple and controllable process flow. The components are added in steps and react in a gradient, which can ensure that the raw materials are fully integrated and avoid stratification and clumping. The resulting additive system is uniform and has stable performance.

[0025] As a preferred technical solution of the present invention, in step one, the stirring speed is set to 250-300 r / min, the temperature is raised to 40-45℃, and the temperature is kept constant for 5 min.

[0026] The above technical solution facilitates the matching of appropriate temperature and rotation speed, which can not only ensure that the deionized water is heated evenly, but also create a good environment for the subsequent dissolution and mixing of raw materials, thereby improving the material compatibility efficiency.

[0027] As a preferred technical solution of the present invention, in step two, isotridecyl alcohol polyoxyethylene ether and C8-C10 alkyl glycoside are added simultaneously in batches. The amount of isotridecyl alcohol polyoxyethylene ether and C8-C10 alkyl glycoside added in a single batch is 1 / 3 of their respective total addition amount. After each batch of simultaneous addition is completed, the next batch of addition is carried out after an interval of 5 to 8 minutes. After all three batches of addition are completed, the mixture is stirred for 10 to 15 minutes.

[0028] The above technical solution facilitates batch intermittent feeding, preventing material agglomeration and gelation caused by excessive feeding at one time, and allows the two surfactants to fully dissolve, ensuring a clear and stable mixed system.

[0029] As a preferred embodiment of the present invention, in step three, after the alcohol ether carboxylate is added dropwise at a uniform rate of 8-12 min, the mixture is stirred for 15-20 min; the maleic anhydride-acrylic acid copolymer is added in two equal portions, with an interval of 3 min between each addition; after all the maleic anhydride-acrylic acid copolymer has been added for 5 min, the tetrasodium iminodisuccinate is added in two equal portions, with an interval of 3 min between each addition; after all the tetrasodium iminodisuccinate has been added for 5 min, the bio-based coconut oil fatty acid diethanolamide is added in two equal portions, with an interval of 3 min between each addition; after all the materials have been added for 8 min, the temperature is raised to 50-55°C, the rotation speed is increased to 400-450 r / min, the mixture is stirred for 10-15 min, and then kept at this temperature for 30 min.

[0030] The above technical solution facilitates uniform dripping, batch feeding combined with gradient heating to accelerate the reaction, and allows each functional component to react and compound in sequence, maximizing synergistic effects and comprehensively improving the overall performance of the additive in terms of penetration, chelation, and solubilization.

[0031] As a preferred technical solution of the present invention, in step four, the temperature is lowered to 30-35°C and an antifoaming agent is added; after the remaining deionized water is added, the mixture is stirred for 20-25 minutes and then allowed to stand for 1 hour. The pH is adjusted to 7.0-8.0 using glacial acetic acid and then filtered through a 200-mesh filter.

[0032] The above technical solution allows for the addition of defoaming agents at low temperatures to avoid their failure at high temperatures, and the neutral to weakly alkaline pH is suitable for textile refining conditions. Static filtration can remove trace impurities, ensuring the appearance and stability of the finished product, while effectively controlling the amount of foam and adapting to continuous production.

[0033] Compared with the prior art, the beneficial effects of the present invention are: the high-penetration phosphorus-free environmentally friendly textile refining auxiliary agent and its preparation method; 1. No phosphorus-containing raw materials or phosphate chelating agents are added throughout the entire process. It is a phosphorus-free and environmentally friendly product. The wastewater generated during the production and use process will not cause the phosphorus content of the water body to exceed the standard. It can effectively avoid the problem of eutrophication of water bodies, which is in line with the national wastewater discharge standards and the green and low-carbon development trend of the textile industry, and the ecological safety is greatly improved. 2. Utilizing a multi-high-performance surfactant compound system, this product employs a synergistic effect of low-surface-tension fatty alcohol polyoxyethylene ether sodium carboxylate, high-penetration isomeric tridecyl alcohol polyoxyethylene ether, and highly biodegradable C8-C10 alkyl glycosides. This significantly enhances the overall wetting and penetration capabilities of the auxiliaries, enabling them to quickly penetrate the fiber gaps of high-density, thick, and high-twist fabrics, achieving uniform refining of the fabric as a whole. This completely solves quality problems such as uneven impurity removal, inconsistent capillary effect, and color difference in finished products caused by insufficient penetration of traditional auxiliaries. Furthermore, it strengthens emulsification and cleaning capabilities, effectively removing various impurities such as pectin, cotton wax, sizing agents, and machine oil from the fabric. Simultaneously, the residual auxiliaries can rapidly degrade in the natural environment, preventing long-term pollution of soil and water bodies. 3. Maleic anhydride-acrylic acid copolymer has good dispersing and anti-redeposition properties. Combined with the chelating properties of tetrasodium iminodisuccinate, it can firmly wrap the stripped dirt and impurities, effectively preventing dirt from sticking back to the fabric surface, and further improving the whiteness and cleanliness of the fabric after refining. Combined with the compatibility optimization system of bio-based coconut oil fatty acid diethanolamide, and supplemented with defoaming agents to precisely control the amount of foam, it can be perfectly adapted to the continuous refining production conditions of textiles. 4. In terms of preparation process, the process is simple and the parameters are controllable. The method of step feeding, uniform dripping, intermittent feeding, gradient heating and segmented stirring is adopted to effectively avoid problems such as raw material agglomeration, gelation and stratification, and ensure that the components are fully integrated and react synergistically. The resulting auxiliary system is uniform and stable in performance. Its comprehensive performance is far superior to traditional products, and it can meet the dual needs of efficient refining and green environmental protection in the textile industry at the same time. Attached Figure Description

[0034] Figure 1 This is a flowchart of the present invention. Detailed Implementation

[0035] The technical solutions of 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 of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0036] Example 1

[0037] Please see Figure 1 The technical solution of this invention is: a high-penetration, phosphorus-free, environmentally friendly textile refining auxiliary agent, comprising the following components by mass percentage: 18% alcohol ether carboxylates; 7% isomeric tridecyl alcohol polyoxyethylene ether; 9% C8-C10 alkyl glycosides; 3% maleic anhydride-acrylic acid copolymer; Tetrasodium iminodisuccinate 4%; Bio-based coconut oil fatty acid diethanolamide 3%; 1% defoamer; The remainder is deionized water.

[0038] The alcohol ether carboxylate is sodium fatty alcohol polyoxyethylene ether carboxylate, with a surface tension ≤32mN / m and a solid content ≥98%.

[0039] The EO addition number of isomeric tridecyl alcohol polyoxyethylene ether is 5, and the penetration power is ≤8s.

[0040] The degree of polymerization of the C8-C10 alkyl glycosides is 1.2.

[0041] The maleic anhydride-acrylic acid copolymer has a number average molecular weight of 2000 and a solid content of 40%.

[0042] A method for preparing a high-penetration, phosphorus-free, environmentally friendly textile refining auxiliary agent includes the following steps:

[0043] Step 1, Preparation of base solution: At room temperature, add 50% of the formula amount of deionized water to the reaction vessel and heat and stir.

[0044] Step 2, surfactant compounding: Add isotridecyl alcohol polyoxyethylene ether and C8-C10 alkyl glycoside to the reaction vessel at the same time, and stir continuously at a constant temperature until the system is completely transparent without layering or gel clumping.

[0045] Step 3, Addition of functional components: Slowly add alcohol ether carboxylate, and continue stirring at a constant temperature after the addition is complete. Then add maleic anhydride-acrylic acid copolymer, tetrasodium iminodisuccinate and bio-based coconut oil fatty acid diethanolamide in sequence, and heat and stir.

[0046] Step 4, Post-processing and molding: After cooling, add defoaming agent, add remaining deionized water, continue stirring, let stand, adjust pH, and filter to obtain high-permeability phosphorus-free environmentally friendly textile refining auxiliary product.

[0047] In step one, the stirring speed is set to 250 r / min, the temperature is raised to 45℃, and the temperature is kept constant for 5 minutes.

[0048] In step two, isotridecyl alcohol polyoxyethylene ether and C8-C10 alkyl glycoside are added simultaneously in batches. The amount of isotridecyl alcohol polyoxyethylene ether and C8-C10 alkyl glycoside added in a single batch is 1 / 3 of their total addition amount. After each batch of simultaneous addition is completed, the next batch of addition is carried out after a 5-minute interval. After all three batches of addition are completed, the mixture is stirred for 10 minutes.

[0049] In step three, after the alcohol ether carboxylate is added dropwise at a uniform rate for 8 minutes, the mixture is stirred for 15 minutes. The maleic anhydride-acrylic acid copolymer is added in two equal portions, with an interval of 3 minutes between each addition. After all the maleic anhydride-acrylic acid copolymer has been added for 5 minutes, tetrasodium iminodisuccinate is added in two equal portions, with an interval of 3 minutes between each addition. After all the tetrasodium iminodisuccinate has been added for 5 minutes, bio-based coconut oil fatty acid diethanolamide is added in two equal portions, with an interval of 3 minutes between each addition. After all the materials have been added for 8 minutes, the temperature is raised to 50°C, the rotation speed is increased to 400 r / min, and the mixture is stirred for 15 minutes and then kept at this temperature for 30 minutes.

[0050] In step four, the temperature is lowered to 30°C and an antifoaming agent is added; after adding the remaining deionized water, the mixture is stirred for 20 minutes and then allowed to stand for 1 hour. The pH is then adjusted to 7.0 using glacial acetic acid and filtered through a 200-mesh filter.

[0051] Example 2

[0052] Please see Figure 1 The technical solution of this invention is: a high-penetration, phosphorus-free, environmentally friendly textile refining auxiliary agent, comprising the following components by mass percentage:

[0053] 20% alcohol ether carboxylates;

[0054] 10% isomeric tridecyl alcohol polyoxyethylene ether;

[0055] C8-C10 alkyl glycosides 12%;

[0056] 4% maleic anhydride-acrylic acid copolymer;

[0057] Tetrasodium iminodisuccinate 5%;

[0058] Bio-based coconut oil fatty acid diethanolamide 2%;

[0059] 1% defoamer;

[0060] The remainder is deionized water.

[0061] The alcohol ether carboxylate is sodium fatty alcohol polyoxyethylene ether carboxylate, with a surface tension ≤32mN / m and a solid content ≥98%.

[0062] The EO addition number of isomeric tridecyl alcohol polyoxyethylene ether is 5, and the penetration power is ≤8s.

[0063] The degree of polymerization of the C8-C10 alkyl glycosides is 1.3.

[0064] The maleic anhydride-acrylic acid copolymer has a number-average molecular weight of 3000 and a solid content of 40%.

[0065] A method for preparing a high-penetration, phosphorus-free, environmentally friendly textile refining auxiliary agent includes the following steps:

[0066] Step 1, Preparation of base solution: At room temperature, add 55% of the formula amount of deionized water to the reaction vessel and heat and stir.

[0067] Step 2, surfactant compounding: Add isotridecyl alcohol polyoxyethylene ether and C8-C10 alkyl glycoside to the reaction vessel at the same time, and stir continuously at a constant temperature until the system is completely transparent without layering or gel clumping.

[0068] Step 3, Addition of functional components: Slowly add alcohol ether carboxylate, and continue stirring at a constant temperature after the addition is complete. Then add maleic anhydride-acrylic acid copolymer, tetrasodium iminodisuccinate and bio-based coconut oil fatty acid diethanolamide in sequence, and heat and stir.

[0069] Step 4, Post-processing and molding: After cooling, add defoaming agent, add remaining deionized water, continue stirring, let stand, adjust pH, and filter to obtain high-permeability phosphorus-free environmentally friendly textile refining auxiliary product.

[0070] In step one, the stirring speed is set to 270 r / min, the temperature is raised to 42℃, and the temperature is kept constant for 5 minutes.

[0071] In step two, isotridecyl alcohol polyoxyethylene ether and C8-C10 alkyl glycoside are added simultaneously in batches. The amount of isotridecyl alcohol polyoxyethylene ether and C8-C10 alkyl glycoside added in a single batch is 1 / 3 of their total addition amount. After each batch of simultaneous addition is completed, the next batch of addition is carried out after a 6-minute interval. After all three batches of addition are completed, the mixture is stirred for 12 minutes.

[0072] In step three, after the alcohol ether carboxylate is added dropwise at a uniform rate for 10 minutes, the mixture is stirred for 17 minutes. The maleic anhydride-acrylic acid copolymer is added in two equal portions, with a 3-minute interval between each addition. Five minutes after all the maleic anhydride-acrylic acid copolymer has been added, tetrasodium iminodisuccinate is added in two equal portions, with a 3-minute interval between each addition. Five minutes after all the tetrasodium iminodisuccinate has been added, bio-based coconut oil fatty acid diethanolamide is added in two equal portions, with a 3-minute interval between each addition. Eight minutes after all the materials have been added, the temperature is raised to 52°C, the rotation speed is increased to 420 r / min, and the mixture is stirred for 13 minutes and then kept at this temperature for 30 minutes.

[0073] In step four, the temperature is lowered to 32°C and an antifoaming agent is added; after adding the remaining deionized water, the mixture is stirred for 22 minutes and then allowed to stand for 1 hour. The pH is then adjusted to 7.5 using glacial acetic acid and filtered through a 200-mesh filter.

[0074] Example 3

[0075] Please see Figure 1 The technical solution of this invention is: a high-penetration, phosphorus-free, environmentally friendly textile refining auxiliary agent, comprising the following components by mass percentage:

[0076] Alcohol ether carboxylates 26%;

[0077] 12% isomeric tridecyl alcohol polyoxyethylene ether;

[0078] C8-C10 alkyl glycosides 16%;

[0079] 5% maleic anhydride-acrylic acid copolymer;

[0080] Tetrasodium iminodisuccinate 7%;

[0081] Bio-based coconut oil fatty acid diethanolamide 1.5%;

[0082] 2% defoamer;

[0083] The remainder is deionized water.

[0084] The alcohol ether carboxylate is sodium fatty alcohol polyoxyethylene ether carboxylate, with a surface tension ≤32mN / m and a solid content ≥98%.

[0085] The EO addition number of isomeric tridecyl alcohol polyoxyethylene ether is 7, and the penetration power is ≤8s.

[0086] The degree of polymerization of the C8-C10 alkyl glycosides is 1.4.

[0087] The maleic anhydride-acrylic acid copolymer has a number-average molecular weight of 4000 and a solid content of 40%.

[0088] A method for preparing a high-penetration, phosphorus-free, environmentally friendly textile refining auxiliary agent includes the following steps:

[0089] Step 1, Preparation of base solution: At room temperature, add 60% of the formula amount of deionized water to the reaction vessel and heat and stir.

[0090] Step 2, surfactant compounding: Add isotridecyl alcohol polyoxyethylene ether and C8-C10 alkyl glycoside to the reaction vessel at the same time, and stir continuously at a constant temperature until the system is completely transparent without layering or gel clumping.

[0091] Step 3, Addition of functional components: Slowly add alcohol ether carboxylate, and continue stirring at a constant temperature after the addition is complete. Then add maleic anhydride-acrylic acid copolymer, tetrasodium iminodisuccinate and bio-based coconut oil fatty acid diethanolamide in sequence, and heat and stir.

[0092] Step 4, Post-processing and molding: After cooling, add defoaming agent, add remaining deionized water, continue stirring, let stand, adjust pH, and filter to obtain high-permeability phosphorus-free environmentally friendly textile refining auxiliary product.

[0093] In step one, the stirring speed is set to 300 r / min, the temperature is raised to 45℃, and the temperature is kept constant for 5 minutes.

[0094] In step two, isotridecyl alcohol polyoxyethylene ether and C8-C10 alkyl glycoside are added simultaneously in batches. The amount of isotridecyl alcohol polyoxyethylene ether and C8-C10 alkyl glycoside added in a single batch is 1 / 3 of their total addition amount. After each batch of simultaneous addition is completed, the next batch of addition is carried out after an 8-minute interval. After all three batches of addition are completed, the mixture is stirred for 15 minutes.

[0095] In step three, after the alcohol ether carboxylate is added dropwise at a uniform rate for 12 minutes, the mixture is stirred for 20 minutes. The maleic anhydride-acrylic acid copolymer is added in two equal portions, with a 3-minute interval between each addition. Five minutes after all the maleic anhydride-acrylic acid copolymer has been added, tetrasodium iminodisuccinate is added in two equal portions, with a 3-minute interval between each addition. Five minutes after all the tetrasodium iminodisuccinate has been added, bio-based coconut oil fatty acid diethanolamide is added in two equal portions, with a 3-minute interval between each addition. Eight minutes after all the materials have been added, the temperature is raised to 55°C, the rotation speed is increased to 450 r / min, and the mixture is stirred for 10 minutes and then kept at this temperature for 30 minutes.

[0096] In step four, during the post-treatment molding process, the temperature is lowered to 35℃ and an antifoaming agent is added; after adding the remaining deionized water, the mixture is stirred for 25 minutes and then allowed to stand for 1 hour. The pH is then adjusted to 8.0 using glacial acetic acid and filtered through a 200-mesh filter.

[0097] Comparative Example 1

[0098] Commercially available traditional phosphorus-containing textile refining auxiliaries (mainstream industrial grade)

[0099] The product comprises the following components by weight percentage: sodium dodecylbenzenesulfonate 15%; fatty alcohol polyoxyethylene ether 10%; sodium tripolyphosphate 8%; sodium dihydrogen phosphate 2%; sodium polyacrylate 3%; coconut oil diethanolamide 2%; defoamer 1%; and the balance being deionized water.

[0100] Preparation method: Using the common preparation process of traditional refining auxiliaries in the textile industry, deionized water is added to the reaction vessel at room temperature, and all the above components are added in sequence. The mixture is stirred at 300 r / min for 30 min until completely dissolved. The pH is adjusted to 7.5 using glacial acetic acid, and the mixture is filtered through a 200-mesh filter to obtain the finished product.

[0101] Comparative Example 2

[0102] This method is completely consistent with the preparation method of Example 2, except that isomeric tridecyl alcohol polyoxyethylene ether is not added, while the other process parameters, feeding sequence and reaction conditions remain unchanged.

[0103] Comparative Example 3

[0104] This method is completely consistent with the preparation method of Example 2, except that maleic anhydride-acrylic acid copolymer and tetrasodium iminodisuccinate are not added. All other process parameters, feeding sequence and reaction conditions remain unchanged.

[0105] Comparative Example 4

[0106] Commercially available phosphate-free textile refining auxiliaries (commercially available environmentally friendly versions of the same type)

[0107] The product comprises the following components by weight percentage: sodium fatty alcohol polyoxyethylene ether carboxylate 20%; dodecyl glycoside 10%; sodium citrate 5%; sodium polyacrylate 3%; coconut oil diethanolamide 2%; defoamer 1%; and the balance being deionized water.

[0108] Preparation method: Using the common preparation process of commercially available phosphorus-free refining additives, deionized water is added to the reaction vessel at room temperature, and all the above components are added in sequence. The mixture is stirred at 300 r / min for 30 min until completely dissolved. The pH is adjusted to 7.8 using glacial acetic acid, and the mixture is filtered through a 200-mesh filter to obtain the finished product.

[0109] Detection

[0110] High-density pure cotton poplin fabric was selected. The additives used in the above examples and comparative examples were 2 g / L, the liquor ratio was 1:20, the scouring temperature was 95℃, the holding time was 60 min, and the fabric was washed three times with hot water and once with cold water. After drying, the fabric was tested, and the results are shown in the table below. Total phosphorus content (mg / L) 0 0 0 128.6 0 0 0 Biodegradation rate (%) 96.2 96.8 97.1 82.5 95.8 95.6 93.2 Canvas infiltration and settling time (s) 6.2 5.8 5.5 15.6 22.3 6.5 12.8 30-minute capillary effect (cm) 14.2 15.6 16.3 8.5 6.2 13.8 10.5 CIE Whiteness of Fabrics 56.3 87.5 88.2 82.1 85.2 80.3 84.6 Dewaxing rate (%) 98.6 99.2 99.5 95.3 97.2 96.8 96.5 Pectin removal rate (%) 99.1 99.5 99.7 96.8 98.3 97.5 98.0 Ash residue (%) 0.09 0.07 0.06 0.21 0.12 0.18 0.15 Foam height (mm) after standing for 5 minutes 26 25 22 45 32 30 38

[0111] By comparing the above test data, we can see that:

[0112] 1. The total phosphorus content of all embodiments of the present invention is 0, which completely solves the core problem of excessive total phosphorus in wastewater and eutrophication caused by traditional phosphorus-containing additives (Comparative Example 1); the biodegradation rate is ≥96%, which is much higher than the 82.5% of traditional additives and also better than ordinary phosphorus-free additives on the market. The additive residues can be rapidly degraded in the natural environment, which fully meets the national green and environmentally friendly production requirements.

[0113] 2. In the embodiments of the present invention, the canvas settling time is only 5.5 to 6.2 seconds, which is 1 / 3 of that of traditional phosphorus-containing auxiliaries and 1 / 2 of that of ordinary phosphorus-free auxiliaries, and far lower than that of Comparative Example 2, which lacks the core penetrating component; the capillary effect reaches a maximum of 16.3 cm in 30 minutes, which is 1.9 times that of traditional auxiliaries. This fully verifies that the present invention achieves ultra-fast penetration through the synergistic compounding of multiple surfactants, which can quickly penetrate the gaps between high-density fabric fibers and completely solve the quality problems such as uneven impurity removal, inconsistent capillary effect, and color difference caused by insufficient penetration of traditional auxiliaries.

[0114] 3. The dewaxing rate of the embodiments of the present invention is ≥98.6% and the pectin removal rate is ≥99.1%, both significantly higher than all comparative examples; the CIE whiteness of the refined fabric reaches as high as 88.2, and the ash residue is only 0.06%, which is far superior to traditional auxiliaries and ordinary phosphorus-free products. In particular, comparative example 3, which lacks a chelation system, has a whiteness of only 80.3 and an ash residue of 0.18%, which fully verifies the anti-redeposition, whitening and cleaning effect of the phosphorus-free chelation dispersion system of the present invention, and can greatly improve the adaptability of the fabric for subsequent dyeing and printing.

[0115] 4. In the embodiment of the present invention, the foam height after 5 minutes is only 22-26mm, which is much lower than the 45mm of traditional auxiliaries and the 38mm of ordinary phosphorus-free auxiliaries. It has excellent foam suppression effect and can effectively avoid problems such as fabric oil floating, color spots and production interruption caused by excessive foam during the refining process. It is perfectly adapted to the working conditions of continuous and automated refining production in the textile industry and greatly improves production efficiency and product qualification rate.

[0116] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A high-penetration, phosphorus-free, environmentally friendly textile refining auxiliary agent, characterized in that, The following components are included by mass percentage: Alcohol ether carboxylates: 18%–26%; Isomeric tridecyl alcohol polyoxyethylene ether 7%–12%; C8-C10 alkyl glycosides 9%–16%; 3%–5% maleic anhydride-acrylic acid copolymer; Tetrasodium iminodisuccinate 4%–7%; Bio-based coconut oil fatty acid diethanolamide 1.5%–3%; Defoamer 1%–2%; The remainder is deionized water.

2. The high-penetration, phosphorus-free, environmentally friendly textile refining auxiliary agent according to claim 1, characterized in that, The alcohol ether carboxylate is sodium fatty alcohol polyoxyethylene ether carboxylate, with a surface tension ≤32mN / m and a solid content ≥98%.

3. The high-permeability, phosphorus-free, environmentally friendly textile refining auxiliary agent and its preparation method according to claim 1, characterized in that, The isomeric tridecyl alcohol polyoxyethylene ether has an EO addition number of 5 to 7 and a penetration power of ≤8s.

4. The high-penetration, phosphorus-free, environmentally friendly textile refining auxiliary agent according to claim 1, characterized in that, The degree of polymerization of the C8-C10 alkyl glycoside is 1.2 to 1.

4.

5. The high-penetration, phosphorus-free, environmentally friendly textile refining auxiliary agent according to claim 1, characterized in that, The maleic anhydride-acrylic acid copolymer has a number-average molecular weight of 2000-4000 and a solid content of 40%.

6. A method for preparing a high-permeability, phosphorus-free, environmentally friendly textile refining auxiliary agent according to any one of claims 1-5, characterized in that, Includes the following steps: Step 1: Preparation of base solution: At room temperature, add 50% to 60% of the formula amount of deionized water to the reaction vessel and heat and stir. Step 2, surfactant compounding: Add isotridecyl alcohol polyoxyethylene ether and C8-C10 alkyl glycoside to the reaction vessel at the same time, and stir continuously at a constant temperature until the system is completely transparent without layering or gel clumping. Step 3, Addition of functional components: Slowly add alcohol ether carboxylate, and continue stirring at a constant temperature after the addition is complete. Then add maleic anhydride-acrylic acid copolymer, tetrasodium iminodisuccinate and bio-based coconut oil fatty acid diethanolamide in sequence, and heat and stir. Step 4, Post-processing and molding: After cooling, add defoaming agent, add remaining deionized water, continue stirring, let stand, adjust pH, and filter to obtain high-permeability phosphorus-free environmentally friendly textile refining auxiliary product.

7. The preparation method of a high-permeability, phosphorus-free, environmentally friendly textile refining auxiliary agent according to claim 6, characterized in that, In step one, the stirring speed is set to 250-300 r / min, the temperature is raised to 40-45℃, and the temperature is kept constant for 5 minutes.

8. The method for preparing a high-penetration, phosphorus-free, environmentally friendly textile refining auxiliary agent according to claim 6, characterized in that, In step two, isotridecyl alcohol polyoxyethylene ether and C8-C10 alkyl glycoside are added simultaneously in batches. The amount of isotridecyl alcohol polyoxyethylene ether and C8-C10 alkyl glycoside added in a single batch is 1 / 3 of their respective total addition amount. After each batch of simultaneous addition is completed, the next batch of addition is carried out after an interval of 5 to 8 minutes. After all three batches of addition are completed, the mixture is stirred for 10 to 15 minutes.

9. The method for preparing a high-permeability, phosphorus-free, environmentally friendly textile refining auxiliary agent according to claim 6, characterized in that, In step three, after the alcohol ether carboxylate is added dropwise at a uniform rate of 8-12 min, the mixture is stirred for 15-20 min. The maleic anhydride-acrylic acid copolymer is added in two equal portions, with a 3-min interval between each addition. Five minutes after all the maleic anhydride-acrylic acid copolymer has been added, tetrasodium iminodisuccinate is added in two equal portions, with a 3-min interval between each addition. Five minutes after all the tetrasodium iminodisuccinate has been added, bio-based coconut oil fatty acid diethanolamide is added in two equal portions, with a 3-min interval between each addition. Eight minutes after all the materials have been added, the temperature is raised to 50-55°C, the rotation speed is increased to 400-450 r / min, and the mixture is stirred for 10-15 min, followed by a 30-min holding period.

10. The high-permeability, phosphorus-free, environmentally friendly textile refining auxiliary agent and its preparation method according to claim 6, characterized in that, In step four, the temperature is lowered to 30-35°C and an antifoaming agent is added; after adding the remaining deionized water, stirring is continued for 20-25 minutes, and the mixture is allowed to stand for 1 hour. The pH is then adjusted to 7.0-8.0 using glacial acetic acid and filtered through a 200-mesh filter.