Deodorizing polyester fiber and preparation method thereof

By introducing sodium sulfonate and sodium carboxylate groups into the fibers and combining antibacterial masterbatches, the problem of insufficient stability and aging in existing deodorant fibers is solved, and under any light conditions is achieved The effective odor removal and antibacterial effect significantly improves the deodorization performance of the fiber.

CN119194661APending Publication Date: 2024-12-27FUJIAN HUAFENG NEW MATERIALS

Patent Information

Application Number
CN202411355640.4
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-09-27
Publication Date
2024-12-27

AI Technical Summary

Technical Problem

Existing anti-odor fiber products have defects in stability, aging and light dependence, and cannot effectively remove the odor of human secretions, especially if they fail in the absence of light or weak ultraviolet rays.

Method used

Modified polyester fibers containing sodium sulfonate and sodium carboxylate groups were prepared by melt spinning, and through pickling treatment, combined with antibacterial masterbatch, to form deodorizing fibers with acid-base buffering and hydrophilic properties, which can be combined with The odor components in sweat are neutralized and have antibacterial properties and long-term deodorization effects.

Benefits of technology

It effectively removes odor from sweat under any light conditions, has washing resistance and long-term antibacterial properties, and significantly improves the deodorization performance of the fiber.

✦ Generated by Eureka AI based on patent content.

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Patent Text Reader

Abstract

The invention relates to a deodorizing polyester fiber and a preparation method thereof.According to the preparation method of the deodorizing polyester fiber, modified polyester with sodium sulfonate and sodium carboxylate groups is subjected to melt spinning and then subjected to acid pickling, so that the fiber obtains an acid-base-like buffer group, the hydrophilicity is improved, and the deodorizing polyester fiber is prepared; a neutralization reaction with odor components such as ammonia gas, isovaleric acid and the like in sweat and the like can be carried out to achieve a deodorization effect; and the fiber contains the antibacterial master batch, so that the fiber has antibacterial property and can inhibit the proliferation of bacteria and fungi to prevent putrefaction odor. The deodorizing polyester fiber has washability and has a long-acting deodorizing effect.
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Description

Technical Field

[0001] The present application relates to the field of textiles, and in particular to a deodorizing polyester fiber and a preparation method thereof. Background Art

[0002] At present, the deodorizing fiber products on the market basically adopt masking deodorization, physical adsorption deodorization, biological deodorization, photocatalytic deodorization and chemical deodorization methods.

[0003] The masking deodorization method usually refers to using a fragrant smell to cover up unpleasant odors, which is deceptive. The mixture of the two odors may produce an even more uncomfortable smell.

[0004] Physical deodorization methods usually refer to the use of porous structure materials such as activated carbon to adsorb odor molecules, but the stability is poor. After the concentration is saturated or the carbon molecules decompose, the odor will be emitted again, and the odor is not actually eliminated.

[0005] The biological deodorization method usually refers to adding additives, particles or coatings with antibacterial and deodorizing effects to the deodorizing product. The advantage of this method is that it is easy to process, but the additives have poor timeliness and are easily ineffective. Antibacterial particles or coatings can inhibit the odor after bacterial corruption, but cannot immediately solve the odor of human secretions such as sweat and urine.

[0006] Photocatalytic deodorization is the use of substances with photocatalytic effects, such as nano-titanium dioxide, nano-zinc oxide, etc., which react with various organic substances to eliminate odors by decomposing free radicals under the irradiation of sunlight or ultraviolet rays. The limitation of photocatalytic deodorization is that it can only be used under the condition of light. For example, when shoes, socks and inner clothes are not exposed to light or when the ultraviolet rays are weak, there is no antibacterial and deodorizing effect.

[0007] The chemical deodorization method uses groups that can chemically react with odorous substances to decompose or neutralize the odorous substances, thereby reducing the concentration of odorous substances in the air, completely eliminating odorous substances, and realizing truly deodorizing textiles.

[0008] As the most widely used chemical fiber, polyester fiber has good fiber-forming properties and mechanical properties, high strength, good light resistance, heat resistance and acid and alkali resistance, and good processability and easy spinning. At present, there is no public deodorizing polyester fiber using a chemical deodorization method. Summary of the invention

[0009] In view of the above problems, the present invention provides a deodorizing polyester fiber that uses a chemical deodorizing method to deodorize. The fiber is produced by a melt spinning method and can effectively eliminate the odor of human secretions.

[0010] A first aspect of the present invention provides a method for preparing a deodorizing polyester fiber, comprising the following steps:

[0011] The modified polyester containing sodium sulfonate and sodium carboxylate groups, the antibacterial masterbatch and the polyester are uniformly mixed and melt-spun to obtain polyester fibers; the polyester fibers are acid-washed to obtain the deodorizing polyester fibers.

[0012] Different from the prior art, the deodorizing polyester fiber provided by the present invention is prepared by melt spinning modified polyester with sodium sulfonate and sodium carboxylate groups and then acid washing, so that the fiber has acid-base buffer groups and improved hydrophilicity, and can react with odor components such as ammonia and isovaleric acid in sweat to achieve a deodorizing effect; the fiber contains antibacterial masterbatch, which also makes the fiber antibacterial and can inhibit the proliferation of bacteria and fungi to prevent corruption odor. The polyester fiber is washable and has a long-lasting deodorizing effect.

[0013] Furthermore, the mass ratio of the modified polyester, the antibacterial masterbatch and the polyester is 10-40:0-5:55-90.

[0014] Furthermore, the preparation of the modified polyester comprises the following steps:

[0015] Preparation of the first esterification mixture: esterification reaction of the first dibasic acid and the first dibasic ester to obtain the first esterification mixture; the molar ratio of the first dibasic acid to the first diol is 10:12-18; the esterification temperature is 240-260°C;

[0016] Preparation of the second esterification mixture: esterify the sodium salt of the polyacid with the second dibasic acid and the second diol to obtain the second esterification mixture; the molar ratio of the sodium salt of the polyacid to the second dibasic acid and the second diol is 10:10:12-18; the esterification temperature is 180-250°C;

[0017] Preparation of diol toluene 5-sulfonic acid alkali metal salt: heating isophthalic acid 5-sulfonic acid alkali metal salt and ethylene glycol to 170-180° C. for esterification reaction to obtain a third esterification mixture; separating and purifying the third esterification mixture to obtain diol toluene 5-sulfonic acid alkali metal salt; the molar ratio of the isophthalic acid 5-sulfonic acid alkali metal salt to the diol is 10:12-18;

[0018] Pre-polycondensation: the first esterification mixture, the second esterification mixture, the alkali metal salt of diol toluene ester-5-sulfonic acid, the catalyst and the heat stabilizer are mixed, and the temperature is gradually increased, the vacuum is slowly drawn, and the mixture is stirred at a starting temperature of 160° C.; the pre-polycondensation is carried out at a low vacuum of 2 KPa and a temperature of 180 to 265° C. for 30 to 60 minutes to obtain a prepolymer;

[0019] Polycondensation: the prepolymer is gradually heated, slowly vacuumed, and stirred; polycondensation is carried out at 265-280° C. under a low vacuum below 100 Pa to obtain the modified polyester.

[0020] Furthermore, the esterification reaction is carried out at a pressure of 0 to 0.3 MPa.

[0021] Furthermore, the esterification reaction, pre-polycondensation reaction and polycondensation reaction are carried out in a nitrogen atmosphere.

[0022] Furthermore, the first dibasic acid is an aromatic dibasic acid; preferably terephthalic acid, isophthalic acid or furandicarboxylic acid;

[0023] The first dibasic ester is at least one of ethylene glycol, 1,3-propylene glycol, neopentyl glycol and 1,4-cyclohexanedimethanol.

[0024] Furthermore, the polyacid sodium salt is disodium citrate.

[0025] Furthermore, the second diol is an aliphatic diol, preferably ethylene glycol or butanediol.

[0026] Furthermore, the second dibasic acid is an aliphatic dibasic acid, preferably adipic acid.

[0027] Furthermore, the content of 5-sodium sulfophthalate in the modified polyester is 5 to 20 wt %, and the content of disodium citrate is 10 to 30 wt %.

[0028] Furthermore, the antibacterial masterbatch is prepared by melt granulation of 10-30wt% antibacterial agent and 70-90wt% polyester.

[0029] Furthermore, the antibacterial agent is copper-loaded zirconium phosphate and / or zinc-loaded zirconium phosphate.

[0030] Furthermore, the pickling is performed using an acetic acid solution.

[0031] The second aspect of the present invention provides a deodorizing polyester fiber, which is prepared by the method described in the first aspect of the present invention.

[0032] The above-mentioned records related to the invention content are only an overview of the technical solution of the present application. In order to enable ordinary technicians in the field to more clearly understand the technical solution of the present application, and then implement it according to the written contents of the specification, and to make the above-mentioned purpose and other purposes, features and advantages of the present application easier to understand, the specific implementation methods of the present application are explained below. DETAILED DESCRIPTION

[0033] In order to explain the technical content, structural features, achieved objectives and effects of the technical solution in detail, the following is a detailed description in conjunction with specific embodiments.

[0034] In order to explain in detail the possible application scenarios, technical principles, specific schemes that can be implemented, and the purposes and effects that can be achieved, the following is a detailed description in conjunction with the specific embodiments listed. The embodiments described herein are only used to more clearly illustrate the technical solutions of the present application, and are therefore only used as examples, and cannot be used to limit the scope of protection of the present application.

[0035] Reference to "embodiment" herein means that the specific features, structures or characteristics described in conjunction with the embodiment may be included in at least one embodiment of the present application. The term "embodiment" appearing in various places in the specification does not necessarily refer to the same embodiment, nor does it particularly limit its independence or association with other embodiments. In principle, in the present application, as long as there is no technical contradiction or conflict, the various technical features mentioned in the embodiments can be combined in any way to form a corresponding implementable technical solution.

[0036] Unless otherwise defined, the technical terms used in this document have the same meanings as those generally understood by those skilled in the art to which this application belongs; the use of relevant terms in this document is only for describing specific embodiments and is not intended to limit this application.

[0037] In the description of this application, the term "and / or" is an expression used to describe the logical relationship between objects, indicating that three relationships may exist, for example, A and / or B, which means: A exists, B exists, and A and B exist at the same time. In addition, the character " / " in this article generally indicates that the objects before and after are in an "or" logical relationship.

[0038] In the present application, terms such as “first” and “second” are merely used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any actual relationship of quantity, priority or sequence between these entities or operations.

[0039] Without further limitations, in this application, the words "include", "comprises", "has" or other similar expressions used in the sentences are intended to cover non-exclusive inclusion. These expressions do not exclude the presence of additional elements in the process, method or product including the elements, so that the process, method or product including a series of elements may include not only those limited elements, but also other elements not explicitly listed, or also include elements inherent to such process, method or product.

[0040] Similar to the understanding in the Examination Guidelines, in this application, expressions such as "greater than", "less than", "exceed" and the like are understood to exclude the number itself; expressions such as "above", "below", "within" and the like are understood to include the number itself. In addition, in the description of the embodiments of this application, "multiple" means more than two (including two), and similar expressions related to "multiple" are also understood in this way, such as "multiple groups", "multiple times", etc., unless otherwise clearly and specifically limited.

[0041] A first aspect of the present invention provides a method for preparing a deodorizing polyester fiber, comprising the following steps:

[0042] The modified polyester containing sodium sulfonate and sodium carboxylate groups, the antibacterial masterbatch and the polyester are uniformly mixed and melt-spun to obtain polyester fibers; the polyester fibers are acid-washed to obtain the deodorizing polyester fibers.

[0043] Different from the prior art, the modified polyester provided by the present invention has sodium sulfonate and sodium carboxylate groups, which are melt-spun and then acid-washed, so that the fiber has acid-base buffer groups and improved hydrophilicity, and can react with odor components such as ammonia and isovaleric acid in sweat to achieve a deodorizing effect; the fiber contains antibacterial masterbatch, which also makes the fiber antibacterial and can inhibit the proliferation of bacteria and fungi to prevent corruption odor. Polyester fiber is washable and has a long-lasting deodorizing effect.

[0044] Furthermore, the mass ratio of the modified polyester, the antibacterial masterbatch and the polyester is 10-40:0-5:55-90.

[0045] Furthermore, the preparation of the modified polyester comprises the following steps:

[0046] Preparation of the first esterification mixture: esterifying the first dibasic acid with the first dibasic ester to obtain the first esterification mixture; the molar ratio of the first dibasic acid to the first diol is 10:12-18;

[0047] Preparation of the second esterification mixture: esterifying the sodium salt of the polyacid with the second dibasic acid and the second diol to obtain the second esterification mixture; the molar ratio of the sodium salt of the polyacid to the second dibasic acid and the second diol is 10:10:12-18;

[0048] Preparation of diol toluene 5-sulfonic acid alkali metal salt: esterify isophthalic acid 5-sulfonic acid alkali metal salt and ethylene glycol to obtain a third esterification mixture; separate and purify the third esterification mixture to obtain diol toluene 5-sulfonic acid alkali metal salt; the molar ratio of the isophthalic acid 5-sulfonic acid alkali metal salt to the diol is 10:12-18;

[0049] Pre-polycondensation: the first esterification mixture, the second esterification mixture, the alkali metal salt of diol toluene ester-5-sulfonic acid, the catalyst and the heat stabilizer are mixed, and the temperature is gradually increased, the vacuum is slowly drawn, and the mixture is stirred at a starting temperature of 160° C.; the pre-polycondensation is carried out at a low vacuum of 2 KPa and a temperature of 180 to 265° C. for 30 to 60 minutes to obtain a prepolymer;

[0050] Polycondensation: the prepolymer is gradually heated, slowly vacuumed, and stirred; polycondensation is carried out at 265-280° C. under a low vacuum below 100 Pa to obtain the modified polyester.

[0051] Furthermore, the esterification reaction is carried out at a pressure of 0 to 0.3 MPa.

[0052] Furthermore, the esterification reaction, the pre-polycondensation reaction and the polycondensation reaction are carried out in a nitrogen atmosphere.

[0053] Furthermore, the preparation of the modified polyester comprises the following steps:

[0054] Preparation of the first esterification mixture: adding the first dibasic acid and the first dibasic ester into the first reaction kettle, stirring and beating at below 129° C., filling with nitrogen and pressurizing to 0.3 MPa, and gradually heating to 240-260° C. for esterification reaction to obtain the first esterification mixture; the molar ratio of the first dibasic acid to the first diol is 10:12-18;

[0055] Preparation of the second esterification mixture: adding the sodium salt of the polyacid, the second dibasic acid and the second diol into the second reaction kettle, heating to 180-250° C. in a nitrogen atmosphere for esterification reaction to obtain the second esterification mixture; the molar ratio of the sodium salt of the polyacid to the second dibasic acid and the second diol is 10:10:12-18;

[0056] Preparation of 5-sulfonic acid alkali metal salt of diol toluene: adding 5-sulfonic acid alkali metal salt of isophthalic acid and ethylene glycol into a third reaction kettle, introducing nitrogen, raising the temperature to 170-180° C. for esterification reaction; obtaining a third esterification mixture after 1.5-2 hours at 170-180° C.; distilling the third esterification mixture at 170-180° C., stopping the reaction when the amount of distilled liquid reaches 80-90% of the theoretical value, and collecting the distillate;

[0057] The distillate is a diol toluene ester-5-sulfonic acid alkali metal salt solution; the molar ratio of the isophthalic acid-5-sulfonic acid alkali metal salt to ethylene glycol is 10:12-18;

[0058] Pre-polycondensation: the first reaction kettle after the esterification reaction is cooled to 160°C, the second esterification mixture, diol toluene ester-5 sulfonic acid alkali metal salt solution, catalyst and heat stabilizer are added to the first reaction kettle, and stirred and mixed with the first esterification mixture; the first reaction kettle is gradually heated and slowly evacuated; pre-polycondensation is carried out at a low vacuum of 2KPa and a temperature of 180-265°C for 30-60min to obtain a prepolymer;

[0059] Polycondensation: The first reaction kettle continues to gradually heat up, slowly evacuates and stirs, and the prepolymer is polycondensed at 265-280° C. under a low vacuum below 100 Pa to obtain the modified polyester.

[0060] Furthermore, the first dibasic acid is an aromatic dibasic acid; preferably terephthalic acid, isophthalic acid or furandicarboxylic acid;

[0061] The first dibasic ester is at least one of ethylene glycol, 1,3-propylene glycol, neopentyl glycol and 1,4-cyclohexanedimethanol.

[0062] Furthermore, the polyacid sodium salt is disodium citrate.

[0063] Furthermore, the second diol is an aliphatic diol, preferably ethylene glycol or butanediol.

[0064] Furthermore, the second dibasic acid is an aliphatic dibasic acid, preferably adipic acid.

[0065] Furthermore, the catalyst is at least one of an antimony-based catalyst, a titanium-based catalyst, a germanium-based catalyst and a tin-based catalyst.

[0066] Furthermore, the amount of the catalyst added is 50 to 300 ppm of the total amount of the dibasic acid added in the preparation of the modified polyester.

[0067] Furthermore, the stabilizer is at least one of phosphoric acid, polyphosphoric acid, and triphenyl phosphate.

[0068] Furthermore, the phosphorus content in the stabilizer is 300 to 1000 ppm of the total amount of dibasic acid added in the preparation of the modified polyester.

[0069] Furthermore, the content of 5-sodium sulfophthalate in the modified polyester is 5 to 20 wt %, and the content of disodium citrate is 10 to 30 wt %.

[0070] Furthermore, the antibacterial masterbatch is prepared by melt granulation of 10-30wt% antibacterial agent and 70-90wt% polyester.

[0071] Furthermore, the antibacterial agent is copper-loaded zirconium phosphate and / or zinc-loaded zirconium phosphate.

[0072] When trace copper / zinc ions with positive charge come into contact with the negatively charged cell membrane of microorganisms, Coulomb attraction occurs, and metal ions penetrate the cell membrane, enter the bacteria, and react with the sulfhydrylamino groups on the proteins in the bacteria, destroying the cell proteins and causing the microorganisms to die or lose their ability to divide and proliferate. At the same time, phosphate has certain deodorizing properties; and zirconium phosphate carriers also have certain deodorizing properties such as isovaleric acid and ammonia.

[0073] Furthermore, the pickling is performed using an acetic acid solution.

[0074] The acetic acid solution is used because the acetic acid is weak in acidity and can replace the sodium salt in the sodium carboxylate under low temperature conditions without causing degradation of the polyester fiber. If a strong acid is used, it will be corrosive and the process requirements will be strict. High concentration or long time will cause serious degradation of the polyester acid, thus affecting the strength of the polyester fiber.

[0075] The second aspect of the present invention provides a deodorizing polyester fiber, which is prepared by the method described in the first aspect of the present invention.

[0076] All raw materials in this embodiment are commercially available. The antibacterial agents copper-loaded zirconium phosphate and zinc-loaded zirconium phosphate were purchased from Fujian Ruisen New Materials Co., Ltd.

[0077] Example 1 A deodorizing polyester fiber and its preparation

[0078] 1. Preparation of modified polyester:

[0079] Preparation of the first esterification mixture: adding isophthalic acid and ethylene glycol into a first reaction kettle, stirring and beating at below 129° C., filling with nitrogen and pressurizing to 0.3 MPa, and gradually heating to 240-260° C. for esterification reaction to obtain a first esterification mixture; the molar ratio of isophthalic acid to ethylene glycol is 10:15;

[0080] Preparation of the second esterification mixture: adding disodium citrate, adipic acid and ethylene glycol into a second reaction kettle, heating to 180-250° C. in a nitrogen atmosphere for esterification reaction to obtain a second esterification mixture; the molar ratio of disodium citrate to adipic acid and ethylene glycol is 10:10:15;

[0081] Preparation of 5-sulfonic acid alkali metal salt of diol toluene: adding sodium 5-sulfonate of isophthalic acid and ethylene glycol into a third reaction kettle, introducing nitrogen, raising the temperature to 170-180° C. for esterification reaction; obtaining a third esterification mixture after 2 hours at 170-180° C.; distilling the third esterification mixture at 170-180° C., stopping the reaction when the amount of distilled liquid reaches 90% of the theoretical value, and collecting a light-colored distillate as sodium 5-sulfonate solution of ethylene glycol isophthalate; the molar ratio of the 5-sulfonic acid alkali metal salt of isophthalic acid to ethylene glycol is 10:14;

[0082] Pre-polycondensation: After the first reactor after the esterification reaction is cooled to 160° C., the second esterification mixture, diol toluene ester-5-sulfonic acid alkali metal salt solution, ethylene glycol antimony and phosphoric acid are added to the first reactor, and stirred for 10 minutes with the first esterification mixture to mix evenly; then the first reactor is gradually heated and slowly evacuated until the pressure in the reactor is lower than 2Kpa, and pre-polycondensation is performed at a temperature of 180-265° C. for 30-60 minutes to obtain a prepolymer;

[0083] Polycondensation: The first reaction kettle continues to gradually heat up and stir, and slowly evacuates to below 100 Pa, and the prepolymer is polycondensed at 265-280° C. to obtain the modified polyester. The molar ratios of terephthalic acid, 5-sodium sulfoisophthalic acid, disodium citrate and adipic acid in the modified polyester are 5:1:2:2, respectively. The content of 5-sodium sulfoisophthalic acid in the modified polyester is about 11wt%, and the content of disodium citrate is about 20wt%.

[0084] The modified polyester is subjected to strip drawing, water tank cooling and pelletizing under nitrogen protection to obtain modified polyester chips.

[0085] 2. Preparation of antibacterial masterbatch

[0086] 20 parts of dried copper ion zirconium phosphate antibacterial agent, 79 parts of 10 mesh polyester powder and 1 part of DP310 dispersant were placed in a mixer, mixed at a speed of 150r / min for 10 minutes and then added to a twin-screw extruder for melt extrusion granulation and then dried. The twin-screw extruder adopts 11-zone temperature setting, and the temperatures are set to 160℃-220℃-240℃-250℃-260℃-260℃-240℃-230℃-230℃-240℃-260℃ in sequence. The cooling temperature is 15-30℃. The twin-screw extruder speed is 500r / min to obtain the antibacterial masterbatch, which contains 20% copper-loaded zirconium phosphate.

[0087] 3. Melt spinning

[0088] The dried modified polyester chips, antibacterial masterbatch and polyester chips are weighed and mixed evenly in a mass ratio of 20:5:75, and then the antibacterial polyester fibers are obtained by sequentially performing melt extrusion, mixing, metering, filtering and spinning, cooling and molding, and oiling and winding processes.

[0089] 4. Pickling:

[0090] The fiber was neutralized and washed with acetic acid water to obtain a polyester fiber that can be deodorized chemically. The textile made from the fiber was marked as sample A. The content of copper zirconium phosphate in the fabric was 1wt%, the content of citric acid in disodium citrate was about 4wt%, and the content of sodium 5-sulfonate of isophthalic acid was about 2.2wt%.

[0091] Example 2

[0092] The difference from Example 1 is that the antibacterial agent is zinc zirconium phosphate, and the textile made of deodorizing fiber is marked as B.

[0093] Example 3

[0094] The difference from Example 1 is that the molar ratios of terephthalic acid, sodium 5-sulfoisophthalic acid, disodium citrate and adipic acid in the synthesized modified polyester are 3:1:3:3 respectively. (The content of sodium 5-sulfoisophthalic acid in the modified polyester is about 12.3wt%, and the content of disodium citrate is about 34.5wt%)

[0095] The content of copper zirconium phosphate in the deodorizing fiber and the fabric woven from the deodorizing fiber is 1wt%, the content of citric acid in disodium citrate is about 6.9wt%, and the content of 5-sodium sulfoisophthalate is about 2.5wt%. The textiles prepared from the deodorizing fiber are marked as C.

[0096] Example 4

[0097] The difference from Example 1 is that no antibacterial masterbatch containing copper zirconium phosphate is added, and the textile prepared from the prepared fiber is marked as D.

[0098] Example 5

[0099] The difference from Example 1 is that the first esterification mixture is prepared by using terephthalic acid and 1,3-propylene glycol for esterification reaction.

[0100] Example 6

[0101] The difference from Example 1 is that the first esterification mixture is prepared by using furandicarboxylic acid and 1,4-cyclohexanedimethanol for esterification reaction.

[0102] Example 7

[0103] The difference from Example 1 is that the second esterification mixture is prepared by using disodium citrate to carry out esterification reaction with butanediol and adipic acid.

[0104] Comparative Example 1

[0105] The difference from Example 1 is that the fiber is prepared by melt spinning of copper-loaded zirconium phosphate antibacterial masterbatch and polyester chips, and the textile made of the obtained fiber is marked as E.

[0106] Comparative Example 2

[0107] The difference from Example 1 is that the woven textile is not subjected to acid washing after melt spinning, and is marked as F.

[0108] Performance testing:

[0109] 1. Antibacterial property test: The durability evaluation of the antibacterial property of fiber products is carried out in accordance with "GBT20944.3-2008 Evaluation of the antibacterial property of textiles Part 3 Oscillation method". Before the fiber product is tested, it is washed 50 times according to the method 10.1.2 of the standard. The test bacteria used in the standard are Staphylococcus aureus (ATCC6538), Escherichia coli (8099) and Candida albicans (ATCC10231). The higher the antibacterial rate measured by washing 50 times using the above method, the better the antibacterial property and durability of the fiber product.

[0110] 2. Deodorization test: The standard method of "GB / T 33610.2-2017 Deodorization performance of textiles Part 2: Detection tube method" was used to determine the reduction rate of ammonia in the textiles made of the fibers in the examples and comparative examples. The standard method of "GB / T 33610.3-2019 Deodorization performance of textiles Part 3: Gas chromatography" was used to determine the reduction rate of acetic acid and isovaleric acid in the textiles made of the fibers in the examples and comparative examples. "GB / T 33610.1-2019 Deodorization of textiles Part 1: General rules" was used as the basis for judgment.

[0111] The antibacterial and deodorizing test results of all examples and comparative examples are shown in Table 1, and the antibacterial and deodorizing test results after washing with water 50 times are shown in Table 2.

[0112] Table 1 Test results of antibacterial and deodorizing properties

[0113]

[0114] Table 2 Antibacterial and deodorizing test results after washing 50 times

[0115]

[0116]

[0117] 1. As can be seen from Examples 1 to 4, adding modified polyester to the fiber can neutralize ammonia, isovaleric acid, etc. to achieve a good deodorizing effect, and can eliminate the odor components in sweat, etc. The zirconium phosphate carrying zinc ions or copper ions in Examples 1-3 makes the polyester fiber have good antibacterial properties, and can inhibit the proliferation of bacteria and fungi to prevent corruption odor; the deodorizing effect is better.

[0118] 2. In Comparative Example 1, only adding zirconium phosphate carrying copper ions can also reduce isovaleric acid and ammonia, but the deodorizing effect cannot be achieved. This may be because the porous structure of zirconium phosphate adsorbs isovaleric acid and ammonia, and the acid can combine with antibacterial ions such as copper and zinc ions. In addition, the antibacterial effect of Comparative Example 1 is slightly reduced, which is because the polyester itself is hydrophobic, and the contact surface between the antibacterial agent and bacteria is reduced. The modified polyester introduces sodium sulfonate and sodium carboxylate groups through in-situ polymerization, which increases the hydrophilicity of the polyester.

[0119] 3. In Comparative Example 3, the fiber was not acid-washed, and only the elimination rate of isovaleric acid reached 90%, which met the national standard, but it had no effect on removing ammonia. This is because sodium sulfonate and sodium carboxylate are weakly alkaline and can adsorb isovaleric acid through ion exchange, but cannot absorb ammonia.

[0120] From the antibacterial effects of Examples 1-4 and Comparative Examples 1\2 in Table 1, it can be found that the fiber textiles with added antibacterial agents all have antibacterial effects; from the deodorization results, by comparing Table 1 with the test results in Table 2 after washing 50 times, it can be found that the deodorizing fiber is also resistant to washing and has a long-lasting deodorizing effect.

[0121] Finally, it should be noted that although the above embodiments have been described in the text of the specification of this application, this does not limit the scope of patent protection of this application. All technical solutions generated by replacing or modifying equivalent structures or equivalent processes based on the essential concept of this application using the contents recorded in the text of the specification of this application, as well as directly or indirectly implementing the technical solutions of the above embodiments in other related technical fields, are included in the scope of patent protection of this application.

Claims

1. A method for preparing a deodorizing polyester fiber, characterized in that: The following steps are involved: The modified polyester containing sodium sulfonate and sodium carboxylate groups, antibacterial masterbatch and polyester are uniformly mixed and melt-spun to obtain modified polyester fibers; the modified polyester fibers are acid-washed to obtain the deodorizing polyester fibers.

2. The preparation method according to claim 1, characterized in that: The mass ratio of the modified polyester, the antibacterial masterbatch and the polyester is 10-40:0-5:55-90.

3. The preparation method according to claim 1, characterized in that: The preparation of the modified polyester comprises the following steps: Preparation of the first esterification mixture: esterifying the first dibasic acid with the first dibasic ester to obtain the first esterification mixture; the molar ratio of the first dibasic acid to the first diol is 10:12-18; Preparation of the second esterification mixture: esterifying the sodium salt of the polyacid with the second dibasic acid and the second diol to obtain the second esterification mixture; the molar ratio of the sodium salt of the polyacid to the second dibasic acid and the second diol is 10:10:12-18; Preparation of diol toluene 5-sulfonic acid alkali metal salt: esterify isophthalic acid 5-sulfonic acid alkali metal salt and ethylene glycol to obtain a third esterification mixture; separate and purify the third esterification mixture to obtain diol toluene 5-sulfonic acid alkali metal salt; the molar ratio of isophthalic acid 5-sulfonic acid alkali metal salt to ethylene glycol is 10:12-18; Pre-polycondensation: the first esterification mixture, the second esterification mixture, the alkali metal salt of diol toluene ester-5-sulfonic acid, the catalyst and the heat stabilizer are mixed, and the temperature is gradually increased, the vacuum is slowly drawn, and the mixture is stirred at a starting temperature of 160° C.; the pre-polycondensation is carried out at a low vacuum of 2 KPa and a temperature of 180 to 265° C. for 30 to 60 minutes to obtain a prepolymer; Polycondensation: the prepolymer is gradually heated, slowly vacuumed, and stirred; polycondensation is carried out at 265-280° C. under a low vacuum below 100 Pa to obtain the modified polyester.

4. The preparation method according to claim 3, characterized in that: The first dibasic acid is an aromatic dibasic acid; the first dibasic ester is at least one of ethylene glycol, 1,3-propylene glycol, neopentyl glycol and 1,4-cyclohexanedimethanol.

5. The preparation method according to claim 3, characterized in that: The polyacid sodium salt is disodium citrate, and the second diol is an aliphatic diol.

6. The preparation method according to claim 3, characterized in that: The content of 5-sodium sulfophthalate in the modified polyester is 5-20 wt %, and the content of disodium citrate is 10-30 wt %.

7. The preparation method according to claim 1, characterized in that: The antibacterial masterbatch is prepared by melt granulation of 10-30wt% antibacterial agent and 70-90wt% polyester.

8. The preparation method according to claim 7, characterized in that: The antibacterial agent is copper-loaded zirconium phosphate and / or zinc-loaded zirconium phosphate.

9. The preparation method according to claim 1, characterized in that: The pickling is carried out using an acetic acid solution.

10. A deodorizing polyester fiber, characterized in that: The deodorizing polyester fiber is prepared by the preparation method according to any one of claims 1 to 9.

Citation Information

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