Negative ion antibacterial polyester fiber fabric and preparation method thereof

Abstract

The present application relates to the technical field of fiber fabric, in particular to a kind of negative ion antibacterial polyester fiber fabric and preparation method thereof.The present application overcomes the problems of low mechanical strength and poor durable antibacterial performance of polyester fiber fabric.The synthetic raw materials of the negative ion antibacterial polyester fiber fabric in the present application include composite negative ion powder, composite antibacterial agent, modified dispersing agent, coupling agent mixture, terephthalic acid, ethylene glycol and catalytic aid.By controlling the proportion and particle size of the components in the composite negative ion powder, the negative ions of the fabric can be continuously released;By changing the amount of composite negative ion powder and composite antibacterial agent, the sustained antibacterial ability of the fabric is improved;By preparing modified dispersing agent and coupling agent mixture, the bursting strength of the fabric is improved;By controlling the parameter conditions of synthesizing terephthalate glycol and the time and temperature of polycondensation, the wear resistance of the fabric is improved;By controlling the parameter conditions in the process of spinning, the elongation at break of the fabric is improved.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of fiber fabrics, in particular to a negative ion antibacterial polyester fiber fabric and a preparation method thereof. BACKGROUND

[0002] Polyester fiber is a synthetic fiber obtained by spinning polyester which is obtained by polycondensation of organic dibasic acid and dibasic alcohol, and belongs to a high molecular compound. The polyester fiber has many advantages, including high breaking strength, moderate resilience, good heat resistance and light resistance. The polyester fiber can maintain stable shape under various use conditions, so that the fabric has the characteristics of washable and wear-resistant, so that the polyester fiber is widely used in home textiles and other fields. However, the polyester fiber has poor moisture absorption performance and is prone to bacterial growth, which limits the development of the polyester fiber in many occasions.

[0003] Introducing a negative ion additive into the polyester fiber is a common technology to improve the antibacterial ability. When the negative ion polyester fabric rubs against the human skin, it can continuously generate air negative ions, thereby playing the roles of eliminating odor, purifying air and resisting and inhibiting bacteria. However, there is still a problem of particle agglomeration in the synthesis process, which leads to unobvious modification effect.

[0004] Patent CN112442745B discloses a preparation method of polyester with temperature-responsive negative ion release antibacterial function and fiber thereof. The new negative ion release / antibacterial fiber is prepared by adopting a brand-new negative ion release / antibacterial mechanism, the fiber diameter can reach superfine fiber, the fiber can be made into white / light color, and has permanent negative ion release / antibacterial function. However, the negative ion release / antibacterial fiber of the application is prone to agglomeration when applied to the preparation of polyester fiber, thereby affecting the duration of negative ion release and the antibacterial effect, so that the polyester fiber has poor long-lasting antibacterial performance.

[0005] Patent CN107217325A discloses a negative ion, antibacterial and anti-mite composite polyester functional fiber and a manufacturing method thereof. The composite polyester functional fiber is light in quality and comfortable, has health care functions such as negative ion, antibacterial and anti-mite, and has wide application prospect. The preparation method of the polyester fiber is simple, low in cost, low in equipment requirement, and suitable for large-scale production. However, the polyester fiber prepared by the method has low mechanical strength and poor washing resistance, and is difficult to use for a long time.

[0006] In summary, after introducing the negative ion additive into the polyester fiber and weaving it into a fabric, the negative ion is difficult to be continuously released, the sterilization effect is unstable, and the fabric is easy to wear out, so that the polyester fiber fabric has problems of low mechanical strength and poor long-lasting antibacterial performance, which seriously affects its application in life.

[0007] Therefore, a negative ion antibacterial polyester fiber fabric and a preparation method thereof are provided. SUMMARY

[0008] The present application aims to design a kind of negative ion antibacterial polyester fiber fabric and its preparation method.The present application overcomes the problems of low mechanical strength and poor long-lasting antibacterial performance of polyester fiber fabric;The synthetic raw materials of the negative ion antibacterial polyester fiber include composite negative ion powder, composite antibacterial agent, modified dispersant, coupling agent mixture, terephthalic acid, ethylene glycol and catalytic aid.The present application controls the proportion of the components in the composite negative ion powder and the particle size, so that the negative ions of the fabric can be continuously released;By changing the amount of composite negative ion powder and the parameter conditions of synthesizing composite antibacterial agent, the long-lasting antibacterial capacity of the fabric is improved;By preparing modified dispersant, changing the amount of coupling agent mixture and the proportion of components in the coupling agent mixture, the bursting strength of the fabric is improved;By controlling the amount of ethylene glycol and catalytic aid and the temperature and time of esterification polycondensation reaction, the wear resistance of the fabric is improved;By controlling the parameter conditions in the process of spinning, the elongation at break of the fabric is improved.

[0009] To achieve the above object, the present application provides the following technical scheme:

[0010] The present application provides a kind of negative ion antibacterial polyester fiber fabric, and the negative ion antibacterial polyester fiber fabric includes the following raw materials by weight fraction:

[0011] Composite negative ion powder: 4-8 parts;

[0012] Composite antibacterial agent: 1.1-1.5 parts;

[0013] Modified dispersant: 0.7-1.5 parts;

[0014] Coupling agent mixture: 1-5 parts;

[0015] Terephthalic acid: 40 parts;

[0016] Ethylene glycol: 14-22 parts;

[0017] Catalytic aid: 0.08-0.12 parts.

[0018] Preferably, the composite negative ion powder is a mixture of tourmaline powder, quartz powder and carbon fiber;The weight fraction ratio of the tourmaline powder, the quartz powder and the carbon fiber is 3-9:2:1;The particle size of the composite negative ion powder is 450nm-650nm.

[0019] Preferably, the coupling agent mixture is a mixture of γ-aminopropyl triethoxysilane, tetrabutyl titanate and aluminum acid tris (2-vinylphenyl) ester;The weight fraction ratio of the γ-aminopropyl triethoxysilane, the tetrabutyl titanate and the aluminum acid tris (2-vinylphenyl) ester is 5-7:3:7-5.

[0020] Preferably, the catalytic aid is one of antimony trioxide, titanium tetrachloride and zinc chloride.

[0021] Another aspect of the present application provides a preparation method of the anion antibacterial polyester fiber fabric, which comprises the following steps:

[0022] S1: 40 parts of terephthalic acid, 14-22 parts of ethylene glycol and 0.08-0.12 parts of a catalytic aid are put into a beaker and stirred for 1 h to obtain a mixture A; the mixture A is transferred into an esterification polycondensation reactor and reacted at a temperature TE1 for 1.5 h to obtain an ethylene glycol terephthalate;

[0023] S2: 4-8 parts of a composite anion powder, 1.1-1.5 parts of a composite antibacterial agent, 0.7-1.5 parts of a modified dispersant and 1-5 parts of a coupling agent mixture are added into the ethylene glycol terephthalate, and after stirring and uniformly mixing, a mixture B is obtained; the mixture B is transferred into an esterification polycondensation reactor and reacted at 260℃ for 50 min, then the esterification polycondensation reactor is adjusted to vacuum, and the temperature is increased to a temperature TE2 for a polycondensation TI1 time, and after cooling and granulation, a polyester chip is obtained;

[0024] S3: the polyester chip is dried and transferred into a vacuum drum, slowly heated to a temperature TE3 for pre-crystallization for 100 min, then heated to a temperature TE4 for TI2 time, and then put into a spinning machine for spinning treatment at a temperature TE5, and the spinning speed is 3100 m / min, to obtain an anion antibacterial polyester fiber; after weaving the anion antibacterial polyester fiber, the anion antibacterial polyester fiber fabric is obtained.

[0025] Preferably, the temperature TE1 in S1 is 220℃-232℃.

[0026] Preferably, the preparation method of the composite antibacterial agent in S2 is: 6-10 parts of nano titanium dioxide, 1-5 parts of silver ions and 2-6 parts of copper nitrate are put into 15 parts of deionized water and stirred for 1 h, then transferred into a reactor and reacted at 175℃-190℃ for 10 h, and after cooling to room temperature, centrifugal drying is performed to obtain the composite antibacterial agent.

[0027] Preferably, the preparation method of the modified dispersant in S2 is: 1-9 parts of polyvinyl alcohol fatty acid ester and 5 parts of polyvinyl alcohol are put into 10 parts of deionized water, and after stirring and uniformly mixing, a dispersant mixture is obtained; 0.6-1 parts of glutaraldehyde is added into the dispersant mixture, and after stirring and uniformly mixing, a precursor is obtained; the precursor is put into a reactor for crosslinking reaction, the temperature is 125℃-140℃, the time is 150 min, and after cooling to room temperature, centrifugal drying is performed to obtain the modified dispersant.

[0028] Preferably, the vacuum in S2 is 100 Pa or less; the temperature TE2 is 275 DEG C - 290 DEG C; and the TI1 time is 0.5 h - 2 h.

[0029] Preferably, the slow heating rate in S3 is 2 DEG C / min; the temperature TE3 is 100 DEG C - 106 DEG C; the temperature TE4 is 170 DEG C - 176 DEG C; the TI2 time is 1 h - 3 h; and the temperature TE5 is 290 DEG C - 296 DEG C.

[0030] Compared with the prior art, the present application has the following beneficial effects:

[0031] 1、The present application controls the proportion and particle size of the composite negative ion powder to enable the negative ions of the fabric to be continuously released. The introduction of the negative ion powder into the fabric can eliminate odors and play an antibacterial role. The appropriate proportion can enable the performance of the composite negative ion powder to be the highest and to be released stably and durably, and the antibacterial effect is improved. If the particle size of the composite negative ion powder is too large, the specific surface area of the composite negative ion powder in contact with air is reduced, which can result in a reduction in the release efficiency of the negative ions. If the particle size is too small, agglomeration can occur, which can affect the final release of the negative ions and reduce the continuous antibacterial performance. The negative ion release amount of the final fabric before washing is 8000 pieces / cm 3 , and the negative ion release amount after 30 washes is 5500 pieces / cm 3 .

[0032] 2、The present application changes the amount of the composite negative ion powder and the parameter conditions of the synthesis of the composite antibacterial agent to improve the antibacterial ability of the fabric. A single antibacterial agent has insufficient antibacterial ability and cannot achieve good antibacterial effect. The composite antibacterial agent prepared by reacting nano-titanium dioxide, silver ions and copper nitrate in a reaction kettle can effectively improve the antibacterial effect of the antibacterial agent. Controlling the amount of the composite antibacterial agent can effectively inhibit bacterial growth, reduce odors, and at the same time maintain good air permeability and softness of the fabric. The composite negative ion powder and the composite antibacterial agent have a synergistic effect, and both can promote the improvement of the antibacterial performance of the fabric, so that the antibacterial effect of the fabric after washing is still very good. The bactericidal rate of the final fabric on Escherichia coli before washing is 100%, and the bactericidal rate on Staphylococcus aureus is 99.9%. The bactericidal rate of the fabric on Escherichia coli after 50 washes is 99.4%, and the bactericidal rate on Staphylococcus aureus is 95.7%.

[0033] 3、The present application improves the bursting strength of the fabric by preparing improved dispersant, changing the amount of coupling agent mixture and the proportion of components in the coupling agent mixture. The cross-linking reaction of adding glutaraldehyde in the mixture of polyvinyl alcohol fatty acid ester and polyvinyl alcohol can effectively improve the performance of the dispersant, so that the dispersion of each component in the synthetic fiber process is uniform, and the agglomeration phenomenon does not occur; the coupling agent mixture can enhance the bonding force between each component, improve the physical strength of the fabric, and if the amount of the coupling agent mixture is too large, it may have an adverse effect on the structure of the fiber itself, resulting in a decrease in the strength of the fiber, and long-term use may reduce the durability of the fabric. The final fabric bursting strength is 366N.

[0034] 4、The present application improves the wear resistance of the fabric by controlling the amount of ethylene glycol and catalytic aid and the temperature and time of esterification polycondensation reaction. Controlling the parameter conditions of synthesizing terephthalate glycol, the material can maintain good performance; too high esterification polycondensation temperature may cause thermal degradation of polymer chain, molecular chain breakage, resulting in a decrease in the molecular weight of the final product, affecting the strength of the fabric, and too low temperature will cause the esterification reaction to proceed slowly, the polycondensation rate is reduced, and the polymerization reaction may not be completely performed, resulting in insufficient molecular weight of the product, poor wear resistance and durability of the fabric. The fabric is not damaged after 50 times of washing.

[0035] 5、The present application improves the elongation at break of the fabric by controlling the parameter conditions in the spinning process. When the temperature is too high, the molecular chain of the polymer is prone to thermal degradation, resulting in a decrease in the molecular weight, thereby affecting the mechanical properties of the fiber, and high temperature will also cause some components in the polymer to decompose, producing volatile substances, which may cause uneven solidification during the cooling process, forming surface defects; when the temperature of the melt is too low, the viscosity of the polymer increases, resulting in poor flowability of the melt, making it difficult to uniformly stretch into fibers, and problems such as jet hole blockage and melt fracture may occur, and even spinning failure. The final fabric elongation at break is 9.5%. BRIEF DESCRIPTION OF DRAWINGS

[0036] Figure 1 The elongation at break of the present application is shown in the following table. DETAILED DESCRIPTION

[0037] The technical solutions in the embodiments of the present application will be described clearly and completely below with reference to the drawings in the embodiments of the present application. Obviously, the described embodiments are only a part of the embodiments of the present application, not all. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor are within the scope of protection of the present application.

[0038] Specific referenceFigure 1 The application provides a negative ion antibacterial polyester fiber fabric and a preparation method thereof.

[0039] Example 1

[0040] The tourmaline powder, the quartz powder and the carbon fiber are uniformly mixed according to a weight ratio of 3:2:1 to obtain a composite negative ion powder, and the particle size of the composite negative ion powder is 450 nm.

[0041] The gamma-aminopropyl triethoxysilane, the tetrabutyl titanate and the tris(2-vinylphenyl)aluminate are uniformly mixed according to a weight ratio of 5:3:7 to obtain a coupling agent mixture.

[0042] Preparation of a composite antibacterial agent

[0043] The 6 parts of nanometer titanium dioxide, 1 part of silver ions and 2 parts of copper nitrate are put into 15 parts of deionized water and stirred for 1 h, and then transferred to a reaction kettle for reaction at 175 ℃ for 10 h, and then centrifuged and dried after cooling to room temperature to obtain the composite antibacterial agent.

[0044] Preparation of an improved dispersant

[0045] The 1 part of polyvinyl alcohol fatty acid ester and 5 parts of polyvinyl alcohol are put into 10 parts of deionized water, and the mixture is stirred uniformly to obtain a dispersant mixture; 0.6 parts of glutaraldehyde are added to the dispersant mixture, and the mixture is stirred uniformly to obtain a precursor; the precursor is put into a reaction kettle for crosslinking reaction, the temperature is 125 ℃, the time is 150 min, and the mixture is centrifuged and dried after cooling to room temperature to obtain the improved dispersant.

[0046] Preparation of a negative ion antibacterial polyester fiber fabric

[0047] S1: 40 parts of terephthalic acid, 14 parts of ethylene glycol and 0.08 parts of a catalytic aid are put into a beaker and stirred for 1 h to obtain a mixture A; the mixture A is transferred to an esterification polycondensation reaction kettle, and reacted at 220 ℃ for 1.5 h to obtain ethylene glycol terephthalate;

[0048] S2: 4 parts of the composite negative ion powder, 1.1 parts of the composite antibacterial agent, 0.7 parts of the improved dispersant and 1 part of the coupling agent mixture are added to the ethylene glycol terephthalate, and the mixture is stirred until uniformly mixed to obtain a mixture B; the mixture B is transferred to an esterification polycondensation reaction kettle, and reacted at 260 ℃ for 50 min, and then the esterification polycondensation reaction kettle is adjusted to vacuum, and the temperature is increased to 275 ℃ for polycondensation for 0.5 h, and then the mixture is cooled and granulated to obtain polyester chips;

[0049] S3 transfers the polyester chips after drying treatment to a vacuum drum, slowly heats to 100℃ for pre-crystallization for 100min, then heats to 170℃ for 1h, and then is put into a spinning machine for spinning treatment at 290℃, with a spinning speed of 3100m / min, to obtain anion antibacterial polyester fiber; after weaving the anion antibacterial polyester fiber, the anion antibacterial polyester fiber fabric is obtained.

[0050] Examples 2-8

[0051] Referring to the parameter conditions of the preparation method in Example 1, the specific differences are shown in Table 1.

[0052] Comparative Example 1

[0053] Referring to the parameter conditions of the preparation method in Example 1, the difference is that only tourmaline powder is added as anion powder.

[0054] Example 9 Anion release amount test

[0055] The anion release amount of Examples 1-8 and Comparative Example 1 is determined according to GB / T 30128-2013 "Textiles - Determination and evaluation of anion generation amount", and the results are shown in Table 1.

[0056] Table 1 Parameter conditions and anion release amount test of Examples 1-8 and Comparative Example 1

[0057]

[0058]

[0059] As can be seen from Table 1, in Comparative Example 1, only tourmaline powder is added as anion powder, and the anion release amount is obviously lower than that of the fabric added with composite anion powder, because single tourmaline powder cannot provide enough anions, so the performance of the anion powder is improved by mixing with quartz powder and carbon fiber and changing the ratio. In Examples 1-8, when the weight fraction ratio of tourmaline powder, quartz powder and carbon fiber is changed, and the particle size of the composite anion powder remains unchanged, the anion release amount of the fabric before washing first increases and then decreases, from 5400 / cm 3 to 6700 / cm 3 and then to 4400 / cm 3 When the weight fraction ratio of tourmaline powder, quartz powder and carbon fiber is 5:2:1, the anion release amount of Example 2 reaches the highest, the anion release amount before washing is 6700 / cm 3 , and the anion release amount after 30 times of washing is 3300 / cm 3, this is because by mixing the three materials, the performance of releasing negative ions can be effectively improved, the odor can be eliminated and the antibacterial effect can be achieved. The appropriate ratio can make the performance of the composite negative ion powder reach the highest and release stably and durably. When the weight ratio of tourmaline powder, quartz powder and carbon fiber is 5:2:1, the negative ion release amount of the fabric before washing changes from 6700 / cm 3 to 8000 / cm 3 and then decreases to 6900 / cm 3 When the particle size of the composite negative ion powder is 550 nm, the negative ion release amount of Example 6 reaches the highest, which is 8000 / cm 3 before washing and 5500 / cm 3 after 30 times of washing. This is because the specific surface area of the composite negative ion powder contacting with the air decreases when the particle size is too large, resulting in the decrease of the release efficiency of the negative ions. When the particle size is too small, the agglomeration phenomenon occurs, affecting the final release of the negative ions and thus reducing the sustained antibacterial performance.

[0060] Examples 10-22

[0061] Referring to the parameter conditions of the preparation method in Example 6, the difference lies in changing the amount of the composite negative ion powder, the parameter conditions of synthesizing the composite antibacterial agent and the amount of the composite antibacterial agent. The specific differences are shown in Table 2.

[0062] Table 2 Parameter conditions of Example 6 and Examples 10-22

[0063]

[0064]

[0065] Comparative Example 2

[0066] Referring to the parameter conditions of the preparation method in Example 6, the difference lies in not adding the composite negative ion powder.

[0067] Comparative Example 3

[0068] Referring to the parameter conditions of the preparation method in Example 6, the difference lies in using only nano titanium dioxide as the antibacterial agent.

[0069] Example 23 Antibacterial ability test

[0070] The antibacterial performance of Examples 6, 10-22 and Comparative Examples 2-3 was tested according to GB / T 20944.3-2008 “Evaluation of the antibacterial performance of textiles”. The results are shown in Table 3.

[0071] Table 3 Antibacterial ability test of Example 6, Examples 10-22 and Comparative Examples 2-3

[0072]

[0073]

[0074] As can be seen from Table 3, in Comparative Example 2, no composite negative ion powder is added, and the antibacterial performance of the fabric is poor; in Comparative Example 3, only nano titanium dioxide is added, and it is found that the antibacterial effect is obviously poorer than that of other examples, the E. coli sterilization rate before washing is 98.7%, the S. aureus sterilization rate is 97.3%, the E. coli sterilization rate after 50 times of washing is 91.2%, and the S. aureus sterilization rate is 85.4%, which is because the antibacterial ability of a single antibacterial agent is insufficient, and a good antibacterial effect cannot be achieved, and the antibacterial performance can be improved by synthesizing a composite antibacterial agent. In Example 6 and Examples 10-22, when the amount of the composite negative ion powder is changed, the amounts of nano titanium dioxide, silver ions and copper nitrate, the reaction temperature and the amount of the composite antibacterial agent are unchanged, the antibacterial effect of the fabric first increases and then decreases, when the amount of the composite negative ion powder is 6 parts, the antibacterial effect of Example 10 is the best, the E. coli sterilization rate before washing is 99.4%, the S. aureus sterilization rate is 98.9%, the E. coli sterilization rate after 50 times of washing is 98.7%, and the S. aureus sterilization rate is 94.7%; when the amount of the composite negative ion powder is 6 parts, the amount of nano titanium dioxide is changed, the amounts of silver ions and copper nitrate, the reaction temperature and the amount of the composite antibacterial agent are unchanged, the antibacterial effect of the fabric first increases and then decreases, when the amount of nano titanium dioxide is 8 parts, the antibacterial effect of Example 12 is the best, the E. coli sterilization rate before washing is 99.5%, the S. aureus sterilization rate is 99.1%, the E. coli sterilization rate after 50 times of washing is 98.8%, and the S. aureus sterilization rate is 94.8%; when the amount of the composite negative ion powder is 6 parts and the amount of nano titanium dioxide is 8 parts, the amount of silver ions is changed, the amounts of copper nitrate, the reaction temperature and the amount of the composite antibacterial agent are unchanged, the antibacterial effect of the fabric is the best when the amount of silver ions is 3 parts, the E. coli sterilization rate before washing of Example 14 is 99.6%, the S. aureus sterilization rate is 99.3%, the E. coli sterilization rate after 50 times of washing is 99.0%, and the S. aureus sterilization rate is 95.0%; when the amount of the composite negative ion powder is 6 parts, the amount of nano titanium dioxide is 8 parts and the amount of silver ions is 3 parts, the amount of copper nitrate is changed, the reaction temperature and the amount of the composite antibacterial agent are unchanged, the antibacterial effect of the fabric is the best when the amount of copper nitrate is 4 parts, the E. coli sterilization rate before washing of Example 16 is 99.8%, the S. aureus sterilization rate is 99.5%, the E. coli sterilization rate after 50 times of washing is 99.1%, and the S. aureus sterilization rate is 95.2%; when the amount of the composite negative ion powder is 6 parts, the amount of nano titanium dioxide is 8 parts, the amount of silver ions is 3 parts and the amount of copper nitrate is 4 parts, the reaction temperature is changed, and the amount of the composite antibacterial agent is unchanged, the antibacterial effect of the fabric is the best when the reaction temperature is 180°C, the E. coli sterilization rate before washing of Example 18 is 99.9%, the S. aureus sterilization rate is 99.7%, the E. coli sterilization rate after 50 times of washing was 99.3%, and the S. aureus sterilization rate was 95.5%; when the amount of the composite negative ion powder was 6 parts, the amount of the nano titanium dioxide was 8 parts, the amount of the silver ion was 3 parts, the amount of the copper nitrate was 4 parts, and the reaction temperature was 180 DEG C, the antibacterial effect of the fabric was the best when the amount of the composite antibacterial agent was 1.3 parts, the E. coli sterilization rate before washing of Example 21 was 100%, the S. aureus sterilization rate was 99.9%, the E. coli sterilization rate after 50 times of washing was 99.4%, and the S. aureus sterilization rate was 95.7%, because too much composite negative ion powder may make the fabric hard or rough, affecting the wearing comfort, and too little composite negative ion powder may cause the release effect of negative ions to be not obvious, the antibacterial ability of the fabric is weak, the long-lasting antibacterial performance after washing is poor, and the expected effect is difficult to achieve; the composite antibacterial agent prepared by reacting the nano titanium dioxide, the silver ion and the copper nitrate in the reaction kettle can effectively improve the antibacterial effect of the antibacterial agent, so that the fabric can still effectively resist bacteria after washing, controlling the amount of the composite antibacterial agent can effectively inhibit the growth of bacteria, reduce odor, and at the same time make the fabric maintain good air permeability and softness, too little composite antibacterial agent cannot achieve effective antibacterial effect, and too much composite antibacterial agent may make the fabric hard, and even irritate the skin; the composite negative ion powder and the composite antibacterial agent have a synergistic effect, and both can promote the improvement of the antibacterial performance of the fabric, so that the antibacterial effect of the fabric after washing is still very good.

[0075] Examples 24-40

[0076] Referring to the parameter conditions of the preparation method in Example 21, the difference is that the parameter conditions for preparing the modified dispersant are controlled, the amount of the coupling agent mixture and the proportion of the components in the coupling agent mixture are changed, and the specific differences are shown in Table 4.

[0077] Table 4 Parameter conditions of Example 21 and Examples 24-40

[0078]

[0079]

[0080]

[0081] Comparative Example 4

[0082] Referring to the parameter conditions of the preparation method in Example 21, the difference is that the modified dispersant is not added.

[0083] Comparative Example 5

[0084] Referring to the parameter conditions of the preparation method in Example 21, the difference is that the coupling agent mixture is not added.

[0085] Top burst strength test

[0086] The top burst strength of Examples 21, 24-40 and Comparative Examples 4-5 was tested according to GB / T 19976-2005 as the standard, and the results are shown in Table 5.

[0087] Table 5 Top burst strength test of Examples 21, 24-40 and Comparative Examples 4-5

[0088]

[0089] It can be found from Table 5 that the bursting strength of the fabric of Comparative Example 4 is low and the mechanical property is poor because no dispersant is added, and the components are prone to agglomeration during synthesis, which ultimately affects the mechanical property of the fabric; the bursting strength of the fabric of Comparative Example 5 is also low because no coupling agent mixture is added, and the components are not tightly combined, which ultimately reduces the mechanical property of the fabric. In Example 21 and Examples 24-40, when the amount of polyvinyl alcohol fatty acid ester, the amount of glutaraldehyde, the reaction temperature, the amount of modified dispersant, the weight fraction ratio of γ-aminopropyl triethoxysilane, tetrabutyl titanate and tris(2-vinylphenyl)aluminate, and the amount of coupling agent mixture are unchanged, the bursting strength of the fabric first increases and then decreases from 326N to 334N and then decreases to 325N. When the amount of polyvinyl alcohol fatty acid ester is 5 parts, the bursting strength of Example 25 is the highest, and the bursting strength is 334N. When the amount of polyvinyl alcohol fatty acid ester is 5 parts, the amount of glutaraldehyde, the reaction temperature, the amount of modified dispersant, the weight fraction ratio of γ-aminopropyl triethoxysilane, tetrabutyl titanate and tris(2-vinylphenyl)aluminate, and the amount of coupling agent mixture are unchanged, the bursting strength of the fabric is the highest when the amount of glutaraldehyde is 0.8 parts, and the bursting strength of Example 28 is 338N. When the amount of polyvinyl alcohol fatty acid ester is 5 parts, the amount of glutaraldehyde is 0.8 parts, the reaction temperature is changed, the amount of modified dispersant, the weight fraction ratio of γ-aminopropyl triethoxysilane, tetrabutyl titanate and tris(2-vinylphenyl)aluminate, and the amount of coupling agent mixture are unchanged, the bursting strength of the fabric is the highest when the reaction temperature is 130°C, and the bursting strength of Example 30 is 344N. When the amount of polyvinyl alcohol fatty acid ester is 5 parts, the amount of glutaraldehyde is 0.8 parts, the reaction temperature is 130°C, the amount of modified dispersant is changed, the weight fraction ratio of γ-aminopropyl triethoxysilane, tetrabutyl titanate and tris(2-vinylphenyl)aluminate, and the amount of coupling agent mixture are unchanged, the bursting strength of the fabric is the highest when the amount of modified dispersant is 1.1 parts, and the bursting strength of Example 34 is 355N. When the amount of polyvinyl alcohol fatty acid ester is 5 parts, the amount of glutaraldehyde is 0.8 parts, the reaction temperature is 130°C, and the amount of modified dispersant is 1.1 parts, the weight fraction ratio of γ-aminopropyl triethoxysilane, tetrabutyl titanate and tris(2-vinylphenyl)aluminate is changed, and the amount of coupling agent mixture is unchanged, the bursting strength of the fabric is the highest when the weight fraction ratio is 6:3:6, and the bursting strength of Example 37 is 360N. When the amount of polyvinyl alcohol fatty acid ester is 5 parts, the amount of glutaraldehyde is 0.8 parts, the reaction temperature is 130°C, the amount of modified dispersant is 1.1 part, the weight ratio of γ-aminopropyl triethoxysilane, tetrabutyl titanate and tris(2-vinylphenyl)aluminate is 6:3:6, when the amount of the coupling agent mixture is changed, the bursting strength of the fabric first increases and then decreases, and the highest is obtained when the amount of the coupling agent mixture is 3 parts, the bursting strength of Example 39 is 366N, because glutaraldehyde is added to the mixture of polyvinyl alcohol fatty acid ester and polyvinyl alcohol to carry out crosslinking reaction, which can effectively improve the performance of the dispersant, so that the dispersion of each component in the synthetic fiber process is more uniform, and the agglomeration phenomenon does not occur, thereby improving the mechanical properties of the fabric; the coupling agent mixture can enhance the bonding force between each component and improve the physical strength of the fabric, if the amount of the coupling agent mixture is too large, it may have an adverse effect on the structure of the fiber itself, resulting in a decrease in the strength of the fiber, and long-term use may reduce the durability of the fabric.

[0090] Examples 42-58

[0091] Referring to the parameter conditions of the preparation method in Example 39, the difference lies in changing the amount and type of ethylene glycol, catalytic aid and the temperature and time of esterification and polycondensation reaction, and the specific differences are shown in Table 6.

[0092] Table 6 Parameter conditions of Example 39 and Examples 42-58

[0093]

[0094]

[0095] Comparative Example 6

[0096] Referring to the parameter conditions of the preparation method in Example 39, the difference lies in that the temperature TE1 is 300℃, the temperature TE2 is 350℃, and the TI1 time is 4h.

[0097] Comparative Example 7

[0098] Referring to the parameter conditions of the preparation method in Example 39, the difference lies in that the temperature TE1 is 150℃, the temperature TE2 is 200℃, and the TI1 time is 0.1h.

[0099] Example 59 Wear resistance test

[0100] According to the standard of GBPT 8629-2001, Examples 39, Examples 42-58 and Comparative Examples 6-7 are washed, and the wear degree of the fabric after 50 times of washing is tested, and the results are shown in Table 7.

[0101] Table 7 Wear resistance test of Example 39, Examples 42-58 and Comparative Examples 6-7

[0102]

[0103]

[0104] It can be found from Table 7 that the too high esterification and polycondensation temperature and too long time in Comparative Example 6 result in the decrease of the wear resistance of the fabric after 50 times of washing, because the too high esterification and polycondensation temperature can cause thermal degradation of the polymer chain, molecular chain breakage, decrease of the molecular weight of the final product, and influence on the strength of the fabric; the too low esterification and polycondensation temperature and too short time in Comparative Example 7 also influence the wear resistance of the fabric, because the too low temperature causes slow esterification reaction, decrease of the polycondensation rate, and incomplete polycondensation reaction, resulting in insufficient molecular weight of the product and poor wear resistance and durability of the fabric. In Example 39 and Examples 42-58, when the amount of ethylene glycol, the type of catalytic aid, the amount of catalytic aid, the temperature TE1, the temperature TE2 and the TI1 time are unchanged, the wear resistance of the fabric is the strongest when the amount of ethylene glycol is 18 parts; when the amount of ethylene glycol is 8 parts, the type of catalytic aid, the amount of catalytic aid, the temperature TE1, the temperature TE2 and the TI1 time are unchanged, the wear resistance of Example 46 is the highest when the catalytic aid is titanium tetrachloride, because the suitable catalytic aid can promote the esterification reaction and finally improve the strength of the fiber fabric; when the amount of ethylene glycol is 8 parts, the catalytic aid is titanium tetrachloride, the amount of catalytic aid is changed, the temperature TE1, the temperature TE2 and the TI1 time are unchanged, the wear resistance of the fabric is the highest when the amount of catalytic aid is 0.1 part, because the suitable amount of catalytic aid can ensure the sufficient esterification reaction and make the properties of the ethylene terephthalate reach the highest; when the amount of ethylene glycol is 8 parts, the catalytic aid is titanium tetrachloride, the amount of catalytic aid is 0.1 part, the temperature TE1 is changed, the temperature TE2 and the TI1 time are unchanged, the wear resistance of Example 50 is the highest, the fabric has less broken yarns and fewer holes; when the amount of ethylene glycol is 8 parts, the catalytic aid is titanium tetrachloride, the amount of catalytic aid is 0.1 part, the temperature TE1 is 224°C, the temperature TE2 is changed, and the TI1 time is unchanged, the wear resistance of Example 54 is the highest, the fabric has no broken yarns and no holes; when the amount of ethylene glycol is 8 parts, the catalytic aid is titanium tetrachloride, the amount of catalytic aid is 0.1 part, the temperature TE1 is 224°C, the temperature TE2 is 285°C, and the TI1 time is changed, the wear resistance of Example 56 is the highest, the fabric is not damaged after 50 times of washing, because the parameters for synthesizing the ethylene terephthalate are controlled to make the material maintain good properties, and the suitable reaction temperature and time are helpful for the smooth reaction, which can avoid the problems of molecular weight reduction caused by too high or too low temperature and ensure the sufficient reaction to obtain the polymer with high molecular weight, finally improve the wear resistance of the fabric and enhance the mechanical properties.

[0105] Examples 60-70

[0106] The parameters of the preparation method in Example 56 were used as reference, except that the parameters in the spinning process were changed, and the specific differences are shown in Table 8.

[0107] Table 8 Parameters of Example 56 and Examples 60-70

[0108] Example temperature TE3 / °C temperature TE4 / °C [CAT] TI2 time / h temperature TE5 / °C Example 56 100 170 1 290 Example 60 102 170 1 290 Example 61 104 170 1 290 Example 62 106 170 1 290 Example 63 104 172 1 290 Example 64 104 174 1 290 Example 65 104 176 1 290 Example 66 104 174 2 290 Example 67 104 174 3 290 Example 68 104 174 2 292 Example 69 104 174 2 294 Example 70 104 174 2 296

[0109] Comparative Example 8

[0110] The parameters of the preparation method in Example 56 were used as reference, except that the temperature TE3 was 150℃, the temperature TE4 was 250℃, the TI2 time was 5h, and the temperature TE5 was 400℃.

[0111] Comparative Example 9

[0112] The parameters of the preparation method in Example 56 were used as reference, except that the temperature TE3 was 50℃, the temperature TE4 was 100℃, the TI2 time was 0.5h, and the temperature TE5 was 200℃.

[0113] Example 71 Elongation at Break Test

[0114] The elongation at break of Example 56, Examples 60-70, and Comparative Examples 8-9 was tested according to GB / T 3916-1997 “Test Method for Breaking Strength and Elongation of Single Yarn”, and the results are shown in Table 9 and Figure 1 .

[0115] Table 9 Elongation at Break Test of Example 56, Examples 60-70, and Comparative Examples 8-9

[0116] Example % Elongation at break Example 56 7.9 Example 60 8.2 Example 61 8.4 Example 62 8.1 Example 63 8.6 Example 64 8.7 Example 65 8.5 Example 66 9.0 Example 67 8.9 Example 68 9.2 Example 69 9.5 Example 70 9.3 Comparative Example 8 6.8 Comparative Example 9 7.3

[0117] From Table 9 and Figure 1 it can be found that the high temperature and long time of spinning in Comparative Example 8 can seriously affect the strength of the fabric, and the elongation at break is only 6.8%, because when the temperature is too high, the molecular chains of the polymer are prone to thermal degradation, resulting in a decrease in molecular weight, thereby affecting the mechanical properties of the fiber, and high temperature can also cause the decomposition of some components in the polymer, producing volatile substances, which may not be uniformly solidified during cooling, forming surface defects; the low temperature and short time in Comparative Example 9 can also affect the elongation at break of the fabric, because when the temperature of the melt is too low, the viscosity of the polymer increases, which can cause poor melt flowability, making it difficult to uniformly stretch into fibers, and may cause problems such as jet hole blockage, melt fracture, etc., or even lead to spinning failure. From Table 9 and Figure 1It is found that in Example 56 and Examples 60-70, when the temperature TE3 is changed, the elongation at break of the fabric first increases and then decreases from 7.9% to 8.4% and then to 8.1%, the elongation at break of Example 61 is the highest, which is 8.4% when the temperature TE3 is 104℃; when the temperature TE3 is 104℃, the temperature TE4 is changed, and the elongation at break of the fabric increases from 8.4% to 8.7% and then decreases to 8.5%, the elongation at break of Example 64 is the highest, which is 8.7% when the temperature TE4 is 174℃; when the temperature TE3 is 104℃ and the temperature TE4 is 174℃, the TI2 time is changed, and the elongation at break of the fabric is the highest when the TI2 time is 2h, the elongation at break of Example 66 is 9.0%; when the temperature TE3 is 104℃, the temperature TE4 is 174℃, and the TI2 time is 2h, the temperature TE5 is changed, and the elongation at break of the fabric is the highest when the temperature TE5 is 294℃, the elongation at break of Example 69 is 9.5%, because too high or too low temperature can cause the quality of the fiber to decrease, and the appropriate temperature and time ensure that the melt has good fluidity and the fiber is uniform, so that the elongation at break is high, the mechanical properties are improved, and the melt degradation or equipment damage is avoided.

[0118] Although the embodiments of the present application have been shown and described, it is to be understood that for the purpose of the present application, the embodiments can be substantially changed without departing from the spirit and the scope of the present application, the scope of the present application being defined by the appended claims and their equivalents.

Claims

1. A method for preparing a negative ion antibacterial polyester fiber fabric, characterized by: The preparation method comprises the following steps in terms of weight parts: S1: 40 parts of terephthalic acid, 14-22 parts of ethylene glycol and 0.08-0.12 parts of a catalytic aid are stirred in a beaker for 1 h to obtain a mixture A; the mixture A is transferred into an esterification polycondensation reactor, and is reacted at 220-232℃ for 1.5 h to obtain an ethylene glycol terephthalate; S2: 4-8 parts of a composite negative ion powder, 1.1-1.5 parts of a composite antibacterial agent, 0.7-1.5 parts of an improved dispersant and 1-5 parts of a coupling agent mixture are added into the ethylene glycol terephthalate, and are stirred until uniformly mixed to obtain a mixture B; the mixture B is transferred into an esterification polycondensation reactor, and is reacted at 260℃ for 50 min, then the esterification polycondensation reactor is adjusted to below 100 Pa, and is heated to 275-290℃ for polycondensation for 0.5-2 h, and is cooled and cut into pieces to obtain polyester chips; S3: the polyester chips are dried, transferred into a vacuum drum, heated to 100-106℃ at a rate of 2℃ / min for pre-crystallization for 100 min, then heated to 170-176℃ for 1-3 h, and then fed into a spinning machine for spinning treatment at 290-296℃, and a spinning speed is 3100 m / min to obtain anionic antibacterial polyester fibers; after the anionic antibacterial polyester fibers are knitted, the anionic antibacterial polyester fiber fabric is obtained; The composite negative ion powder is a mixture of tourmaline powder, quartz powder and carbon fiber; the weight part ratio of the tourmaline powder, the quartz powder and the carbon fiber is 3-9:2:1, and the particle size of the composite negative ion powder is 450-650 nm; The coupling agent mixture is a mixture of γ-aminopropyl triethoxysilane, tetrabutyl titanate and tri(2-vinylphenyl)aluminate; the weight part ratio of the γ-aminopropyl triethoxysilane, the tetrabutyl titanate and the tri(2-vinylphenyl)aluminate is 5-7:3:7-5; The preparation method of the composite antibacterial agent is as follows: 6-10 parts of nano titanium dioxide, 1-5 parts of silver ions and 2-6 parts of copper nitrate are stirred in 15 parts of deionized water for 1 h, then transferred into a reactor for reaction at 175-190℃ for 10 h, centrifuged and dried after cooling to room temperature to obtain the composite antibacterial agent; The preparation method of the improved dispersant is as follows: 1-9 parts of polyvinyl alcohol fatty acid ester and 5 parts of polyvinyl alcohol are stirred in 10 parts of deionized water to obtain a dispersant mixture; 0.6-1 parts of glutaraldehyde is added into the dispersant mixture, and stirred to obtain a precursor; the precursor is put into a reactor for crosslinking reaction at a temperature of 125-140℃ for 150 min, and centrifuged and dried after cooling to room temperature to obtain the improved dispersant.

2. A negative ion antibacterial polyester fiber fabric, characterized by: The anionic antibacterial polyester fiber fabric is prepared by the preparation method in claim 1, and the anionic antibacterial polyester fiber fabric comprises the following raw materials in terms of weight parts: Composite negative ion powder: 4-8 parts; Composite antibacterial agent: 1.1-1.5 parts; Improved dispersant: 0.7-1.5 parts; Coupling agent mixture: 1-5 parts; terephthalic acid: 40 parts; ethylene glycol: 14-22 parts; catalytic aid: 0.08-0.12 parts.

3. The anion antibacterial polyester fiber fabric according to claim 2, characterized in that: The catalytic aid is one of antimony trioxide, titanium tetrachloride and zinc chloride.

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