Anti-wicking component as well as preparation method and application thereof
By using monomers such as bis-trimethylolpropane tetraacrylate and anti-wicking components of ammonium persulfate catalysts, combining anti-static and antibacterial agents, the emulsion-type oil agent is formed, and the anti-core resistance of polyester fibers in high temperature environments is solved. The problem of poor absorption effect achieves fluorine-free and multifunctional waterproofing and heat resistance, avoiding defects and environmental pollution during spinning.
Patent Information
- Application Number
- CN202411248974.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-06
- Publication Date
- 2024-12-13
AI Technical Summary
The existing polyester fiber waterproofing agents show poor anti-wicking effect, great impact on spinning conditions, and poor heat resistance in high temperature and high stretching environments. Fluorine-containing substances are harmful to the environment and health and do not contain them on the market. There are fewer fluorine-type waterproofing agents.
Anti-wicking components composed of bis-trimethylolpropane tetraacrylate, methyl methacrylate or hydroxyethyl acrylate, ammonium persulfate catalyst, Tween-20 and other emulsifiers, are prepared by specific preparation Methods The emulsion type oil agent is formed, combining antistatic and antibacterial agents to form a versatile oil agent, and applied to the fiber surface to achieve anti-wicking, antistatic and antibacterial effects.
It achieves fluorine-free, good anti-wicking effect, spinning and heat resistance, and can maintain the waterproof performance of the fiber surface under high temperature environment, avoids the phenomenon of broken heads and wool silk, and reduces the risk of corrosion and deterioration of functional oil agents .
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Abstract
Description
Technical Field
[0001] The present application relates to an anti-wicking component and a preparation method and application thereof, belonging to the technical field of treatment preparations for fiber modification. Background Art
[0002] Polyester fiber multifilaments are usually composed of multiple monofilaments, such as the typical specification 1000D / 192f, which is composed of 192 monofilaments. When the fabric is immersed in liquid, the gaps between the monofilaments will cause the water absorption rate to increase due to the wicking effect. In outdoor scenes such as light box advertising cloth and swimming pool base cloth, the wicking effect and fabric water absorption will significantly affect the use effect.
[0003] At present, the waterproof function of polyester fiber is mostly achieved by coating the fiber surface with anti-wicking oil agent. Due to the characteristics of high electronegativity and low surface energy, fluorine-containing oil agents have excellent waterproof and oil-proof properties, from the earliest C8 waterproof agent to C6 waterproof agent. However, fluorine-containing substances are prone to bioaccumulation, which poses a huge challenge to human health and the ecological environment.
[0004] However, there are few types of fluorine-free water repellents on the market. In addition, for the harsh environment of polyester industrial yarn spinning process, such as temperature up to 250°C, stretching ratio up to 6 times, high hydrophobicity, etc., the commercially available oils generally show the following disadvantages:
[0005] 1. The anti-wicking effect is not good and cannot achieve the effect of 0 wicking (≤10mm);
[0006] 2. It has a great impact on the spinning conditions and is prone to cause breakage, hairline hair, roller entanglement, etc.
[0007] 3. Poor heat resistance, easy to scale in high temperature environment, affecting the dry heat shrinkage rate and uniformity of the product.
[0008] Based on this, this application is filed. Summary of the invention
[0009] In view of this, the present application first provides an anti-wicking component, which not only has a good anti-wicking effect, but also has good compatibility with other modified preparations, thereby realizing the multifunctionality of the oil agent.
[0010] Specifically, the present application is implemented through the following scheme:
[0011] The anti-wicking component comprises the following components:
[0012] First monomer: di-trimethylolpropane tetraacrylate, methyl methacrylate (MMA) or hydroxyethyl acrylate (2-hydroxyethyl acrylate, HEA), 20-40%;
[0013] Second monomer: methyl methacrylate or butyl acrylate, 4-10%;
[0014] Catalyst: ammonium persulfate or potassium persulfate, 0.4-0.8%;
[0015] Emulsifier: any one of Tween-20, fatty alcohol polyoxyethylene ether, sorbitan fatty acid ester, lauryl alcohol polyoxyethylene ether, 1-5%;
[0016] The balance is water.
[0017] The anti-wicking component constructed above has the following core advantages:
[0018] 1. It does not contain fluorine and is an environmentally friendly, emulsion-type anti-wicking component;
[0019] 2. Good spinnability, adding oil-aid spreading and antistatic components to the components to protect the fibers during the spinning process;
[0020] 3. Good heat resistance, resistant to high temperature of 236-265℃.
[0021] Therefore, the anti-wicking component provided in the present application can be used before entering the hot roller. After being coated on the fiber surface, it forms a film on the fiber surface after being cured at a high temperature of up to 250°C by the hot roller, thus giving the fiber durable anti-wicking properties.
[0022] Further, as a preference:
[0023] The addition amount of the first monomer is 25-30%, the addition amount of the second monomer is 4-6%, the addition amount of the catalyst is 0.4-0.5%, and the addition amount of the emulsifier is 2-3%.
[0024] The added mass ratio of the first monomer to the second monomer is preferably controlled at 5 to 7:1, and preferably 6:1.
[0025] The second object of the applicant is to provide a method for preparing the anti-wicking component, the process is as follows:
[0026] Step 1, weigh the emulsifier and catalyst respectively, add them into deionized water, and stir and heat at 70-85° C. for 15-30 minutes;
[0027] Step 2: After the first monomer and the second monomer are uniformly mixed, they are slowly added dropwise to the reaction system of step 1 using a constant pressure dropping funnel, and the reaction is continued for 1 to 3 hours;
[0028] Step 3: After cooling to room temperature to complete the reaction, filtering is performed and the pH is adjusted to 7-8 to obtain the anti-wicking component.
[0029] More preferably,
[0030] In step 1, the stirring speed is 200-400 r / min.
[0031] In step three,
[0032] The filter mesh size is 200 to 300 meshes.
[0033] The pH is preferably adjusted using aqueous ammonia.
[0034] The above preparation process realizes the emulsification of each component, ensuring that the finished anti-wicking component presents a uniform emulsion and has stable performance.
[0035] The third object of the applicant is to provide the application of the above anti-wicking component, mixing the anti-wicking component with a smoothing agent, an emulsifier, an antistatic agent, an antibacterial agent and water to form a functional oil, and the composition of each component is as follows:
[0036] Anti-wicking component: 25-40%,
[0037] Smoothing agent: 12-25%,
[0038] Emulsifier: 10-18%,
[0039] Antistatic agent: 2-8%,
[0040] Antimicrobial agent: 1-5%,
[0041] Water: 20-40%.
[0042] The anti-wicking component of the present application is combined with an antistatic agent and an antibacterial agent to form a multifunctional product having anti-wicking, antistatic and antibacterial properties; combined with a smoothing agent and an emulsifier, the oil is given excellent viscosity and uniformity, ensuring uniform oiling and achieving a better and longer-lasting anti-wicking effect.
[0043] More preferably,
[0044] The lubricant is polyethylene glycol laurate or polyethylene glycol sorbitan oleate.
[0045] The emulsifier is POE polyol alkyl ester ether.
[0046] The antistatic agent is any one of alkyl sulfonate, alkyl phosphate, sodium docusate, and quaternary ammonium salt, which can increase the cohesive performance of the yarn bundle and cooperate with the anti-wicking component to ensure strong cohesion between the single-filament yarn bundles and avoid hardening caused by film formation of the anti-wicking component.
[0047] The antibacterial agent is methyl parahydroxybenzoate or butyl parahydroxybenzoate, which, in combination with the anti-wicking component, gives the functional oil agent good stability, thereby preventing the functional oil agent from being corrupted and deteriorated during storage and use.
[0048] The preparation method of the functional oil is as follows: add water to the anti-wicking component and heat it to 30-45°C, add a smoothing agent and an emulsifier under stirring, then add an antistatic agent and an antibacterial agent, stir until a transparent homogeneous state, and cool to room temperature to obtain the functional oil. DETAILED DESCRIPTION
[0049] In order to make the technical problems, technical solutions and beneficial effects to be solved by this application clearer, the technical solutions of this application will be further described in detail below in combination with the specific cases in the embodiments of this application. It should be understood that the specific embodiments described herein are only used to explain this application and are not used to limit the technical solutions of this application. Based on the embodiments in this application, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of this application.
[0050] Example 1
[0051] 1. Preparation of anti-wicking components:
[0052] Weigh 4.5g of Tween-20 (mass percentage is about 3.2%) and 0.75g of ammonium persulfate (about 0.5%) respectively, place them in a 250mL three-necked flask, add 90.0g of deionized water (about 65.7%) and stir, set the speed to 250r / min, heat at 80°C for 30min, then place 36.0g of methyl methacrylate (about 26.2%) and 6.0g of butyl acrylate (about 4.4%) in a beaker and mix, and slowly add them dropwise to the reaction system through a constant pressure dropping funnel, continue the reaction at 80°C for 2.5h, cool to room temperature to complete the reaction, filter with a 200-mesh filter, and adjust the pH value to 7 with ammonia water, which is the anti-wicking component.
[0053] 2. Anti-wicking components are used in the preparation of functional oils:
[0054] Add 30g of deionized water to a four-necked flask, take 30g of the above anti-wicking component, heat to 40°C, stir for 20min, then slowly add 20g of polyethylene glycol sorbitan oleate, 14g of POE polyol alkyl ester ether (laureth-8), then add 5g of sodium dodecyl sulfate, 1g of butyl paraben (paraben), stir for 2h until a transparent homogeneous state, cool to room temperature and discharge to obtain a functional oil.
[0055] 3. Oiling of functional oil:
[0056] 10 kg of crude oil type GXM-100 oil from Matsumoto Oil Co., Ltd. was taken as the base oil, kept in an oil drum at 50°C, deionized water and a functional oil with an effective concentration (i.e., solid content) of 30% were added, and a mixed oil (oil density 1.02 g / cm2) was prepared in a manner that the mass ratio of the base oil to the functional oil was 1:1. 3 ), control the oil wheel speed, apply oil with double row oil nozzles, apply oil before entering the hot roller (1+2 rollers), and spin G1005SP (specification 1110dtex / 192f, fineness 1115dtex, theoretical yarn output 289.9g / min).
[0057] The spinning parameters are as follows:
[0058] 1+2 roller: 496m / min;
[0059] 3+4 rollers: 516m / min, 90℃;
[0060] 5+6 rollers: 1950m / min, 120℃;
[0061] 7+8 rollers: 2920 m / min, 236°C;
[0062] 9+10 rollers: 2737m / min, 230℃;
[0063] Winding speed: 2600m / min,
[0064] Oil pump specification: 0.3cm 3 / r.
[0065] A 1000D fluorine-free anti-wicking sample was trial-produced on the A17-4 spinning position. The introduction of antistatic agent in the functional oil effectively increased the cohesiveness of the yarn bundle. The number of breakages improved with the increase of the amount of anti-wicking oil added. The antibacterial agent gave the functional oil emulsion good resistance to corruption and deterioration during storage and use. The configured emulsion must be used up within 24 hours. No agglomeration, mildew, etc. occurred during storage and use.
[0066] When the oil wheel speed is controlled at 8-40rpm, the oil agent attached to the fiber is 0.4-2.0% of the total fiber mass. Taking the theoretical oil rate of 0.2%, 0.4%, 1.0%, and 1.7% as an example, there are four gradients, each of which corresponds to one silk cake (oiling with two rows of oil nozzles). The wicking height is tested in the material inspection room. The test results are shown in Table 1.
[0067] Table 1: Comparison of wicking performance of finished products with different oiling rates
[0068]
[0069]
[0070] It can be seen from Table 1 that when using the imported finished anti-wicking oil agent (taking Japan Daikin TG-5574 as an example), the average wicking height is 11.82mm when the oiling rate is 0.4%, and the wicking height range is 1 to 45, which is a big difference. When using the functional oil agent in this case, when the oiling rate is 0.4%, the average wicking height is 5.33mm, and the wicking height range is 2 to 10, and the extreme difference is significantly reduced compared with the imported finished anti-wicking oil agent; when the oiling rate is 1.0%, the average wicking height is 4.75mm, and the wicking height range is 0 to 9, and the uniformity is improved to meet customer requirements; when the oiling rate is around 2.0%, such as 1.7% in Table 1, the average wicking height is 6.58, and the data range is 0 to 13. This is mainly because the fiber surface is difficult to bear too high an oiling rate, and excessive oiling causes the oil nozzle to splash strongly, and the oil agent that actually remains on the fiber surface is less and uneven. Therefore, 1.0% oil loading rate is the best oil loading rate for the oil agent applied for in this case, which can take into account both the requirements of wicking height and economy.
[0071] Example 2
[0072] The configuration of this embodiment is the same as that of embodiment 1, except that the effect of the amount of the second monomer added on the oiling performance is shown in Table 2.
[0073] Table 2: Effect of the amount of the second monomer added on oiling performance
[0074]
[0075] In the present application, when the first monomer is used alone without adding the second monomer, a long-chain acrylic polymer cannot be formed, and therefore, it has basically no anti-wicking effect (see sequence number 9 in Table 2); with the addition of the second monomer, the second monomer and the first monomer undergo a polymerization reaction to achieve a synergistic anti-wicking effect. As can be seen from Table 2, its effect on performance is mainly manifested in the effect on strength and elongation at break: with the increase in the amount of addition, the fiber strength increases and the elongation decreases. There is basically no effect on dry heat shrinkage.
[0076] Therefore, the addition amount of the second monomer relative to the first monomer is appropriately controlled at 1:5-7, and its addition amount in the anti-wicking component is appropriately controlled at 4-10%. At this time, the wicking height is basically controlled within 10 mm, and it is best when the second monomer addition amount is around 4-6%. At this time, the wicking height is basically maintained below 5 mm; especially when the second monomer: first monomer = 1:6 (mass ratio) and the mass percentage of the second monomer added in the anti-wicking component is 6%, the anti-wicking effect is best, and the wicking height is about 4.4 mm.
[0077] Example 3
[0078] The configuration of this embodiment is the same as that of embodiment 1, except that the amount of catalyst added is as shown in Table 3.
[0079] Table 3: Effect of catalyst dosage on product performance (oil content 1.0%)
[0080]
[0081] Catalysts catalyze the polymerization reaction of monomers. The use of inorganic catalysts can ensure the catalytic effect while also helping to control costs. However, excessive addition of inorganic catalysts will have an adverse effect on spinning conditions, especially inorganic salts, which act like "blades" on the fiber surface, making it easy to produce lint or broken ends and also prone to coking on the surface of the hot roller.
[0082] From the data in Table 3, it can be seen that as the amount of catalyst added increases, the amount of fuzzy yarns, the number of broken ends, and the extreme difference in dry heat shrinkage tend to increase. Therefore, the amount of catalyst added in the anti-wicking component is appropriately controlled at 0.1-0.8%, the wicking height can be controlled to be around 10 mm, and the spinning condition is good; especially when the amount of catalyst added is controlled at around 0.4% (0.4-0.6%), the wicking height is basically maintained within 10 mm, the amount of fuzzy yarns and the number of broken ends during the spinning process are small, and there is basically no coking on the surface of the hot roller (maximum temperature 236°C).
[0083] When the catalyst is replaced by potassium persulfate, its addition amount shows the same trend as above. Relatively speaking, under the same conditions, when ammonium persulfate is used as the catalyst, the coking situation on the hot roller surface is slightly better than when potassium persulfate is used as the catalyst.
[0084] Example 4
[0085] The configuration of this embodiment is the same as that of embodiment 1, except that the amount of emulsifier used is as shown in Table 4.
[0086] Table 4: Effect of emulsifier dosage on oiling performance
[0087] Serial number Emulsifier Breaking strength, cN / dtex Wicking height, mm 1 1% 6.98 13.2 2 2% 7.01 8.6 3 3% 7.03 3.9 4 4% 7.01 7.1 5 5% 6.99 8.3 .
[0088] In this application, the emulsifier not only ensures the stability of the emulsion, so that it does not stratify during long-term storage; it also gives it good permeability, so that the oil solution can quickly form a film and spread on the fiber surface. However, if the emulsifier is added in too much amount (such as more than 5%), it will make it difficult for the oil to remain on the fiber surface, resulting in more waste. Therefore, the amount of emulsifier added in the anti-wicking component is appropriately controlled at 1-5%.
[0089] Example 5
[0090] The configuration of this embodiment is the same as that of embodiment 1, except that the compositions of the first monomer and the second monomer are as shown in Table 5.
[0091] Table 5: Effect of different monomers on oiling effect
[0092]
[0093] The several monomers selected in this case can all achieve a wicking height of around 10 mm. Among them, when the first monomer is di-trimethylolpropane tetraacrylate, methyl methacrylate (MMA) or hydroxyethyl acrylate (HEA), and the second monomer is methyl methacrylate or butyl acrylate, the oiling effects of the oils obtained by different combinations are different: because the longer methylene chain hydrophobic segments in butyl acrylate react with the hydroxyl groups on the fiber to form chemical bonds, it can improve the waterproof performance of the fiber. Therefore, when butyl acrylate is used as the second monomer, the wicking height is slightly lower than that of methyl methacrylate.
[0094] Example 6
[0095] The configuration of this embodiment is the same as that of embodiment 1, except that the preparation process of the anti-wicking component is different, specifically: raw materials of the anti-wicking components having the same composition as that of embodiment 1 are respectively taken, and the raw materials are directly mixed to form the anti-wicking components.
[0096] Table 6: Effect of different anti-wicking components preparation process
[0097]
[0098] Compared with the compounding method of Example 1, when the oil agent obtained by the direct mixing method (sequence number 2 in Table 6) is used for spinning, under the same oil content, the spinning condition deteriorates, the number of end hairs and the number of breakages are significantly increased, and the finished polyester industrial yarn has basically no wicking effect; it can be seen that the anti-wicking component provided by the present application requires specific conditions to obtain a product with anti-wicking effect and stable mechanical properties; the direct mixing method cannot achieve the same effect.
[0099] In the same preparation process, the blank group (No. 3 in Table 6) without adding the anti-wicking component of the present application has a lower oil content and also shows basically no wicking effect. This shows that the anti-wicking effect of the oil agent requires the anti-wicking component and the antistatic agent, smoothing agent, antibacterial agent and other components to work together.
[0100] Comparative Example 1
[0101] This case uses a common anti-wicking oil agent for oiling. Compared with Example 1, the main differences are as follows:
[0102] Table 7: Performance comparison of functional oils from different sources
[0103]
[0104] Compared with Japan's Daikin's TG-5574 fluorine-containing oil, XF5537C fluorine-free oil and the United States' fluorine-free oil FT-621, the oil provided in this case can not only achieve the same wicking level as imported fluorine-containing oils, but also use green, environmentally friendly, fluorine-free and easily available substances as raw materials, and are formulated after emulsion polymerization. Its cost, safety and preparation method are better than imported fluorine-containing oils; compared with imported fluorine-free oils, the average wicking height is significantly lower, basically meeting the standard of 0 wicking, and the number of breakages within 8 hours is also at a low level. The comprehensive effect of spinning condition and wicking is better than that of imported fluorine-free oils.
[0105] Comparative Example 2
[0106] Taking CN1493601A as comparative example 2, CN1493601A uses two monomers, an emulsifier and water to obtain a fluorinated copolymer in an aqueous medium through pre-emulsification and polymerization as an emulsion of a water-based fluorinated poly-water-and-oil-polymer. This solution uses a fluorinated copolymer, which is mainly used for water-repellent and oil-repellent finishing of oilfield labor protection clothing fabrics, and is added during the fabric finishing process. If it is used in the spinning stage, it will have defects such as poor cohesion of the yarn bundle and low mechanical properties; while the anti-wicking component of this case needs to be blended with the basic oil agent, which is mainly used for water repellency without oil repellency.
[0107] Comparative Example 3
[0108] CN105887487A is used as comparative example 3, which uses acrylic latex, emulsifier, hexafluorocarbon waterproof and oil-proof agent and water to obtain a water-repellent and oil-repellent modified acrylic adhesive. The formula provided by this scheme is mainly used for polyester spunbond non-woven fabrics, and is used in combination with other components as an adhesive. However, for the application object of this case, polyester industrial yarn, due to the special processing requirements such as high temperature and high-ratio stretching during the spinning process, comparative example 3 cannot meet the comprehensive properties such as temperature resistance, lubrication, and antistatic.
[0109] The above-mentioned embodiments only express several feasible implementation methods of the present invention, and the description is relatively specific and detailed, but it cannot be understood as limiting the scope of the patent of the present invention, and the embodiments are not used to limit the scope of protection in the claims of the present invention. For ordinary technicians in this field, several modifications and improvements can be made without departing from the concept of the present invention, and all equivalent implementations or changes that do not depart from the present invention should be included in the technology of the present invention.
Claims
1. Anti-wicking components, It is characterized in that The anti-wicking component is resistant to high temperatures of 236-265°C and includes the following components: First monomer: di-trimethylolpropane tetraacrylate, methyl methacrylate or hydroxyethyl acrylate, 20-40%; Second monomer: methyl methacrylate or butyl acrylate, 4~10%; Catalyst: ammonium persulfate or potassium persulfate, 0.1~0.8%; Emulsifier: Tween-20, fatty alcohol polyoxyethylene ether, sorbitan fatty acid ester or lauryl alcohol polyoxyethylene ether, 1~5%; The balance is water.
2. The anti-wicking component according to claim 1, Features: The addition amount of the first monomer is 25-30%, the addition amount of the second monomer is 4-6%, the addition amount of the catalyst is 0.4-0.5%, and the addition amount of the emulsifier is 2-3%.
3. A method for preparing the anti-wicking component according to claim 1, It is characterized in that Here are the steps: Step 1, weigh the emulsifier and catalyst respectively, add them into deionized water, and heat them at 70-85°C with stirring for 15-30 minutes; Step 2: After the first monomer and the second monomer are evenly mixed, they are slowly added dropwise to the reaction system of step 1 using a constant pressure dropping funnel, and the reaction is continued for 1 to 3 hours; Step 3: After cooling to room temperature to complete the reaction, filtering is performed and the pH is adjusted to 7-8 to obtain the anti-wicking component.
4. The method for preparing the anti-wicking component according to claim 3, Features: In step 1, the stirring speed is 200~400 r / min.
5. The method for preparing the anti-wicking component according to claim 3, Features: In step 3, the filtration mesh size is 200~300 mesh.
6. Use of the anti-wicking component according to claim 1, It is characterized in that The anti-wicking component is mixed with a smoothing agent, an emulsifier, an antistatic agent, an antibacterial agent and water to form a functional oil, and the composition of each component is as follows: Anti-wicking component: 25~40%, Smoothing agent: 12~25%, Emulsifier: 10~18%, Antistatic agent: 2~8%, Antimicrobial agent: 1~5%, Water: 20~40%.
7. Use of the anti-wicking component according to claim 6, Features: The lubricant is polyethylene glycol laurate or polyethylene glycol sorbitan oleate, and the emulsifier is POE polyol alkyl ester ether.
8. Use of the anti-wicking component according to claim 6, Features: The antistatic agent is any one of alkyl sulfonate, alkyl phosphate, docusate sodium and quaternary ammonium salt.
9. Use of the anti-wicking component according to claim 6, Features: The antibacterial agent is methylparaben or butylparaben.
10. Use of the anti-wicking component according to claim 6, It is characterized in that The preparation method of the functional oil is as follows: adding water to the anti-wicking component and heating it to 30-45° C., first adding a smoothing agent and an emulsifier under stirring, then adding an antistatic agent and an antibacterial agent, stirring until a transparent homogeneous state, and cooling to room temperature to obtain the functional oil.
