CN104099685A - Preparation method for hygroscopic polyester fiber, hygroscopic polyester fiber and application thereof - Google Patents
Preparation method for hygroscopic polyester fiber, hygroscopic polyester fiber and application thereof Download PDFInfo
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- CN104099685A CN104099685A CN201310129277.XA CN201310129277A CN104099685A CN 104099685 A CN104099685 A CN 104099685A CN 201310129277 A CN201310129277 A CN 201310129277A CN 104099685 A CN104099685 A CN 104099685A
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Abstract
The invention discloses a preparation method for hygroscopic polyester fiber and the hygroscopic polyester fiber prepared by using the method. The method comprises: taking an aliphatic dihydric alcohol, an aromatic dicarboxylic acid or a derivative thereof, an aliphatic dibasic acid or a derivative thereof, and a metal-sulfonate-containing isophthalic acid or a derivative thereof as main raw materials to prepare a copolyester, and adding sodium acetate during synthesis of the copolyester; then blending the obtained copolyester and a hygroscopic substance to obtain a hygroscopic master batch; and finally performing melt spinning on the obtained hygroscopic master batch and common polyester, so as to obtain the hygroscopic polyester fiber. The method is capable of improving the service life of a spinning assembly, and the obtained hygroscopic polyester fiber is excellent in hygroscopicity and tone, and is widely applicable to the field of dress materials of underwear, sport suits and the like.
Description
Technical field
The present invention relates to a kind of preparation method and moisture absorption type polyester fiber obtained by this method of moisture absorption type polyester fiber.
Background technology
Polyester, due to its excellent performance, has a wide range of applications in fields such as fiber, film, plastics.But due to the compound with regular structure of polyester, hydrophobicity is stronger, compared with the natural fabric such as cotton or fiber crops, water imbibition, the hygroscopicity of polyester fiber are poor, have greatly limited polyester fiber in the application requiring under hygroscopicity environment.When the textiles being obtained by polyester fiber is made underclothes, because the hygroscopicity of polyester fiber is poor, can bring feeling of oppression and heat to people, therefore polyester fiber is not suitable for being applied to summer clothing aspect especially.
At present, the method of improving polyester fiber moisture pick-up properties is mainly to pass through physical modification, utilize wicking to improve the hygroscopicity of fiber, as fine, hollow porous and cross section special-shapedization etc., wherein be most widely used with cross section special-shapedization of fiber, as the Coolmax odd-shaped cross section terylene that du pont company releases, its surperficial You Si road groove, there is wicking, thereby reach the effect of moisture absorption.But the processing technology to spinnerets when profiled filament spinning is had relatively high expectations, and production cost is high.
In addition, because common polyester fiber dyeability is poor, must under high temperature and high pressure, just can dye.Solving polyester fiber achromatic method has a lot, introduces that easily to dye point be one of main means by combined polymerization.For example, will after the poly alkylene glycol copolymerization of polyester raw material and polyethylene glycol and so on, form polymer, or with the copolymerization of the straight chain such as adipic acid, decanedioic acid aliphatic carboxylic acid after form polymer.But this method must be introduced polyether structure unit or other monomer copolymerization unit in polyester segment, certainly will cause the decline of polyester heat resistance.Another kind method is to add containing M-phthalic acid and the derivative thereof of sodium group to improve the stainability energy of fiber, but while causing fibre spinning due to the autohemagglutination of sodium group, filter presses liter, and filament spinning component life cycle shortens, and has reduced production efficiency.
Summary of the invention
The moisture absorption type polyester fiber that the object of the present invention is to provide a kind of preparation method of moisture absorption type polyester fiber and prepared by the method, this preparation method's technique is simple, when spinning filter press stable, cost is low, and the moisture absorption type polyester fiber obtaining has the advantages such as normal atmosphere cation-dyeable, tone are good.The fabric being made by this moisture absorption type polyester fiber can be widely used in the underclothes such as underwear, sweat shirt.
Technical solution of the present invention is as follows:
A preparation method for moisture absorption type polyester fiber, is made up through melt spinning of hygroscopicity master batch and conventional polyester, and the method mainly comprises the steps:
(1) prepare copolyesters taking the M-phthalic acid or derivatives thereof of aliphatic dihydroxy alcohol, aromatic binary carboxylic acid or derivatives thereof, aliphatic dibasic acid or derivatives thereof and containing metal sulfonate as main raw material, wherein the addition of aliphatic dibasic acid or derivatives thereof accounts for the 2.5mol%～15mol% of total acid composition, the addition of the M-phthalic acid or derivatives thereof of containing metal sulfonate accounts for the 0.3mol%～10mol% of total acid composition, is also added with sodium acetate in the process of synthetic copolyester;
(2) copolyesters and the hygroscopic matter blend that are mainly obtained by step (1) obtain hygroscopicity master batch, and wherein the addition of hygroscopic matter accounts for the 5wt%～40wt% of hygroscopicity master batch;
(3) the hygroscopicity master batch obtaining and conventional polyester are carried out to melt spinning by weight 1:1～1:5, obtain moisture absorption type polyester fiber.
In copolyesters segment, the introducing of aliphatic dibasic acid structure can improve the irregularity of polyester, makes polyester fiber dyestuff in the time of dyeing more easily enter amorphous field, improves the dyeability of polyester fiber.The addition of aliphatic dibasic acid or derivatives thereof accounts for the 2.5mol%～15mol% of total acid composition.When its addition is during lower than 2.5mol%, do not have and improve the effect that polyester fiber normal pressure can dye; And when its addition is during higher than 15mol%, the heat resistance of polyester fiber declines.
What above-mentioned aliphatic dibasic acid can be enumerated has malonic acid, succinic acid, adipic acid, decanedioic acid, dimethyl adipate, dimethyl sebacate etc., wherein preferred adipic acid.
In the time preparing copolyesters, be also one of polymerization single polymerization monomer containing M-phthalic acid and the derivative thereof of sodium group.Due to the existence of sodium group, this monomer can improve final polyester fiber dyeability.But containing M-phthalic acid and the easy autohemagglutination of derivative thereof of sodium group, can cause filter to press liter in the spinning process of follow-up hygroscopicity master batch and conventional polyester, shorten the service life of filament spinning component, reduce production efficiency.M-phthalic acid and derivative thereof containing sodium group can be 5-sodium sulfo isophthalate (SIPA), Sodium Dimethyl Isophthalate-5-sulfonate (SIPM) or ethylene isophthalate-5-sodium sulfonate (SIPE), its addition accounts for the 0.3mol%～10mol% of total acid composition, preferably 0.5～5mol%.
Problem is pressed in filter when improving polyester fiber fibroblast, also adds sodium acetate in the process of preparing copolyesters, can reduce the generation of ehter bond.Simultaneously, because sodium acetate has and the M-phthalic acid and the identical CATION of derivative thereof that contain sodium group, therefore sodium acetate can improve containing the M-phthalic acid of sodium group and the autohemagglutination of derivative thereof, improve the intermiscibility of itself and copolyesters, thereby the high problem of filter voltage rise can improve copolyesters spinning time, in the service life of improving filament spinning component, can reach more than 10 days.
Preferably the addition of sodium acetate accounts for the 400ppm～2000ppm of copolyesters total amount, the anti-etherificate better effects if that sodium acetate plays within the scope of this.Within the addition of sodium acetate need be controlled at the general interpolation scope of additive, also can accelerate the degraded of copolyesters if added too much in the time that copolyesters is synthetic, the polyester fiber finally obtaining is easily painted.
In the time of step (1) synthetic copolyester, can add compound containing titanium elements as catalyst.Because the catalyst activity of titanium-containing catalyst is high, easily promote side reaction, affect the tone stability of final polyester fiber, within its addition is preferably controlled at and is equivalent to the scope of copolyesters 3～20ppm in titanium elements while therefore selecting titanium-containing catalyst.
Feedstock fat of the present invention family dihydroxylic alcohols is the general aliphatic dihydroxy alcohols such as ethylene glycol, propylene glycol, butanediol, and aromatic binary carboxylic acid or derivatives thereof is the dicarboxylic acids or the dibasic acid ester that contain phenyl ring for pet reaction of the routines such as terephthalic acid (TPA), dimethyl terephthalate (DMT).In the present invention, can select as required different aliphatic dihydroxy alcohols and aromatic binary carboxylic acid or derivatives thereof, can not produce too much influence to moisture sorption effect of the present invention.
When hygroscopicity master batch is prepared in the copolyesters that step (1) is obtained and hygroscopic matter blend, the addition of hygroscopic matter accounts for the 5wt%～40wt% of hygroscopicity master batch.Described hygroscopic matter can be polyvinylpyrrolidone (PVP), polyvinyl alcohol (PVA) or polyether compound.Preferably polyethylene pyrrolidones of the present invention.
The selected polyvinylpyrrolidone of the present invention be vinylpyrrolidone monomer by known polymerization as the homopolymer that bulk polymerization, polymerisation in solution, suspension polymerization, emulsion polymerisation etc. obtain, can be linear structure, dendritic morphology or cross-linked structure.The K value of polyvinylpyrrolidone is 15～90, and concrete can select in 17,30,60,85,90,115.If the K value of polyvinylpyrrolidone is too low, the complexing power of polyvinylpyrrolidone and copolyesters is not strong, and the easy stripping of PVP in the Cooling Process after blend is extruded, causes final polyester fiber to can not get good hygroscopicity; And if its K value is too high, the viscosity of blend system increases greatly, mixing spue bad, be difficult to granulation, cause production efficiency low.
When preparation hygroscopicity master batch, the addition of hygroscopic matter accounts for the 5wt%～40wt% of hygroscopicity master batch.If hygroscopic matter content is too low, the moisture sorption effect that fiber does not reach; If hygroscopic matter too high levels, excessive hygroscopic matter can destroy light resistance, the feel etc. of the fabric being obtained by fiber.In master batch, the addition of hygroscopic matter accounts for moisture absorption master batch and is preferably 5wt%～20wt%.
Hygroscopic matter particularly polyvinylpyrrolidone is easily painted, affects the tone of final polyester fiber.Sodium acetate in copolyesters can prevent that hygroscopic matter is painted.
In order further to improve the tone of polyester fiber, the polyester blending preferably making in hygroscopic matter and step (1) adds antioxidant phosphorus compound while preparing hygroscopicity master batch.The present invention is two (2,6-di-t-butyl-4-aminomethyl phenyl) pentaerythritol diphosphate more preferably, its structural formula as shown in Equation 1,
formula 1.
Add antioxidant phosphorus compound in hygroscopicity master batch time, its addition had better not exceed 20000ppm in P elements with respect to hygroscopicity master batch, adds the performance that too much can affect final polyester fiber.
The hygroscopicity master batch and the conventional polyester that obtain the most at last obtain moisture absorption type polyester fiber through melt spinning.Conventional polyester wherein can be half common delustring polyester, can be also the polyester that contains one or more copolymer compositions in metal sulfonate, polyether compound, aliphatic dibasic acid and derivative thereof, aliphatic dihydroxy alcohol and derivative thereof.
In the preparation method of moisture absorption type polyester fiber of the present invention, can also add the multiple additives such as stabilizing agent, delustering agent.
The present invention also wants the claimed a kind of moisture absorption type polyester fiber being prepared by said method, and the △ MR of this fiber is more than 2%; The tone L value of fiber is more than 80, and b value is below 6, and light fastness can reach more than 4 grades, and when spinning, assembly life-span reaches more than 10 days.
Fiber of the present invention can be used for making fabric, and gained fabric can be widely used in the aspects such as the clothing that underwear, sweat shirt etc. directly contact with skin.
The method of testing of each index involved in the present invention is as follows:
(1) moisture absorption parameter
△ MR refers to while wearing the clothes, and the moisture in clothes is discharged and index that human body is felt comfortably cool.△ MR is with 30 DEG C, the hydroscopicity (MR of 90%RH
2) deduct 20 DEG C, the hydroscopicity (MR of 65%RH
1) difference (△ the MR(%)=MR that obtains
2-MR
1).△ MR is larger, and wettability power is stronger, and the comfortableness while dress is better;
MR
1, MR
2computing formula as follows:
MR
1（%）＝（W
1－W
3）/W
3，MR
2（%）＝（W
2－W
3）/W
3
W
1: in the atmosphere of 20 DEG C × 65%RH, place the quality (g) of test film after 24 hours,
W
2: in the atmosphere of 30 DEG C × 90%RH, place the quality (g) of test film after 24 hours,
W
3: the quality of test film (g) under over dry state.
(2) filament spinning component life cycle
31M/C spinning machine carries out spinning and studies, the mensuration of unit replacement number of days.
(3) mensuration of tone L, b value
Carry out after the calibration of white standard plate with colour difference meter (SM-T45), carry out L, a, b measures (L value (lightness index), a value (red/green index), b value (cyan/yellow colour index)).
(4) color fastness to light
According to standard GB/T8427-2008, the color fastness to light of test textiles under artificial light COLOR FASTNESS xenon arc, the grade of COLOR FASTNESS have 3 grades following, 3 grades, 3 grades above, 4 grades following, 4 grades, 4 grades with first-class.
Detailed description of the invention
Below in conjunction with specific embodiment, the invention will be further described.The concrete numerical value of each embodiment and comparative example is in table 1.
In the embodiment of the present invention, the abbreviation of related part material is as follows:
(1) dimethyl adipate: DMA;
(2) dimethyl sebacate: DMS;
(3) Sodium Dimethyl Isophthalate-5-sulfonate: SIPM;
(4) polyvinylpyrrolidone: PVP;
(5) polyvinyl alcohol: PVA;
(6) polyethylene glycol: PEG;
(7) two (2,6-di-t-butyl-4-aminomethyl phenyl) pentaerythritol diphosphate: PEP36;
(8) lithium acetate: LAH.
Embodiment 1
Step 1: dimethyl terephthalate (DMT) 111.2Kg and ethylene glycol 69.8Kg are dropped in esterifying kettle, add Sodium Dimethyl Isophthalate-5-sulfonate (SIPM) 4.4Kg simultaneously, dimethyl adipate (DMA) 5.4Kg, with respect to the catalyst metatitanic acid four butyl ester 10ppm of copolyesters weight, sodium acetate 500ppm, stirring is warming up to 230 DEG C and carries out travelling to polycondensation vessel after ester exchange reaction, cross the stabilizing agent trimethyl phosphate 100ppm adding with respect to copolyesters weight for 5 minutes, TITANIUM DIOXIDE DELUSTRANT 0.07wt%, after 5 minutes, start decompression, heat up, reach final temperature, after final pressure, be back to normal pressure to importing nitrogen in reaction system, stop polycondensation reaction and obtain copolyesters.
Step 2: the polyvinylpyrrolidone (PVP), two (2 that the copolyesters being obtained by step (1) and K value are 30,6-di-t-butyl-4-aminomethyl phenyl) pentaerythritol diphosphate (PEP36) blending extrusion on two axle extruders (φ 44mm, L/D:52), wherein the addition of PVP accounts for the 20wt% of hygroscopicity master batch, and the addition of PEP36 is equivalent to the 0.3wt% of master batch in P elements.The Temperature Setting of extruder is 245 DEG C of fusing departments, 200 DEG C of kneading parts, extrudes in order.
Step 3: the master batch that above-mentioned steps (2) is obtained and conventional polyester (can be the simple polyester only being obtained by binary acid and diol reaction, also can be the polyester that contains various functional monomers or additive) carry out melt spinning and batch obtaining undrawn yarn under the hauling speed of the spinning temperature of 290 DEG C, 3000m by weight 1:2, then the undrawn yarn obtaining is stretched under the condition of 90 DEG C of draft temperatures, 1.65 times of stretching ratios, finally at 130 DEG C, after HEAT SETTING, batch the polyester fiber that obtains 56dtex ∕ 24f.After tested, the hygroscopicity parameter △ MR of gained fiber is 2.0wt%, and tone L value is that 85, b value is 4.5; Filament spinning component life-span when hygroscopicity master batch and conventional polyester melt spinning is 12 days.
Embodiment 2～embodiment 15
Select different raw material and addition, other steps prepare moisture absorption type polyester fiber with embodiment 1, and concrete numerical parameter is in table 1 and table 2.
Embodiment 16
In the time of synthetic hygroscopicity master batch (step 2), do not add antioxidant phosphorus compound, other prepare moisture absorption type polyester fiber with embodiment 1, and concrete numerical parameter is in table 2.
Comparative example 1
The M-phthalic acid or derivatives thereof that does not add containing metal sulfonate in the time of step 1 synthetic copolyester, other prepare polyester fiber with embodiment 1, and concrete numerical parameter is in table 2.
Comparative example 2
In the time of step 1 synthetic copolyester, do not add aliphatic dibasic acid or derivatives thereof, other prepare polyester fiber with embodiment 1, and concrete numerical parameter is in table 2.
Comparative example 3
In the process of step 1 synthetic copolyester, do not add sodium acetate, other prepare polyester fiber with embodiment 1, and concrete numerical parameter is in table 2.
Comparative example 4
In the process of step 1 synthetic copolyester, change sodium acetate into lithium acetate, its addition is equivalent to the 500ppm of final copolyesters, and other prepare polyester fiber with embodiment 1, and concrete numerical parameter is in table 2.
Comparative example 5
In the time of step 1 synthetic copolyester, add polyethylene glycol, other prepare polyester fiber with embodiment 1, and concrete numerical parameter is in table 2.
When in form, the amount of aliphatic dibasic acid or derivatives thereof refers to synthetic copolyester in step 1, aliphatic dibasic acid or derivatives thereof is with respect to the addition of total acid composition, when the amount of SIPM refers to synthetic copolyester in rapid 1, SIPM is with respect to the addition of total acid composition, when the amount of NaAc refers to synthetic copolyester in step 1, NaAc is with respect to the addition of copolyesters total amount, the amount of PEP36 refers in step 2 that PEP36 is with respect to the addition of hygroscopicity master batch, the amount of hygroscopic matter refers in step 2 that hygroscopic matter is with respect to the addition of hygroscopicity master batch, the weight ratio of hygroscopicity master batch and conventional polyester when the ratio of hygroscopicity master batch and polyester refers to melt spinning in step 3.
Claims (8)
1. a preparation method for moisture absorption type polyester fiber, is made up through melt spinning of hygroscopicity master batch and conventional polyester, it is characterized in that: the method mainly comprises the steps:
(1) prepare copolyesters taking the M-phthalic acid or derivatives thereof of aliphatic dihydroxy alcohol, aromatic binary carboxylic acid or derivatives thereof, aliphatic dibasic acid or derivatives thereof and containing metal sulfonate as main raw material, wherein the addition of aliphatic dibasic acid or derivatives thereof accounts for the 2.5mol%～15mol% of total acid composition, the addition of the M-phthalic acid or derivatives thereof of containing metal sulfonate accounts for the 0.3mol%～10mol% of total acid composition, is also added with sodium acetate in the process of synthetic copolyester;
(2) copolyesters and the hygroscopic matter blend that are mainly obtained by step (1) obtain hygroscopicity master batch, and wherein the addition of hygroscopic matter accounts for the 5wt%～40wt% of hygroscopicity master batch;
(3) the hygroscopicity master batch obtaining and conventional polyester are carried out to melt spinning by weight 1:1～1:5, obtain moisture absorption type polyester fiber.
2. the preparation method of moisture absorption type polyester fiber according to claim 1, is characterized in that: step (2) is added antioxidant phosphorus compound in hygroscopicity master batch preparation process, and its addition accounts for the 1000ppm～20000ppm of hygroscopicity master batch in P elements.
3. the preparation method of moisture absorption type polyester fiber according to claim 1 and 2, is characterized in that: in step (1), the addition of sodium acetate accounts for 400～2000ppm of copolyesters total amount.
4. the preparation method of moisture absorption type polyester fiber according to claim 1 and 2, is characterized in that: described hygroscopic matter is polyvinylpyrrolidone, polyvinyl alcohol or polyether compound.
5. the preparation method of moisture absorption type polyester fiber according to claim 1 and 2, is characterized in that: the described M-phthalic acid or derivatives thereof containing sodium group is 5-sodium sulfo isophthalate, Sodium Dimethyl Isophthalate-5-sulfonate or ethylene isophthalate-5-sodium sulfonate.
6. the preparation method of moisture absorption type polyester fiber according to claim 1 and 2, is characterized in that: described antioxidant phosphorus compound is two (2,6-di-t-butyl-4-aminomethyl phenyl) pentaerythritol diphosphate.
7. the moisture absorption type polyester fiber that described in claim 1, the preparation method of moisture absorption type polyester fiber obtains, is characterized in that: the △ MR of this polyester fiber is more than 2%, and tone L value is more than 80, and b value is below 6.
Described in a claim 7 moisture absorption type polyester fiber in the application of making on fabric.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109163496A (en) * | 2018-09-04 | 2019-01-08 | 广州创链科技有限公司 | A kind of energy saving high-low temperature chamber |
| CN111350017A (en) * | 2020-02-03 | 2020-06-30 | 江苏银兆新材料科技有限公司 | Moisture-absorbing warm-keeping knitted fabric |
-
2013
- 2013-04-15 CN CN201310129277.XA patent/CN104099685A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109163496A (en) * | 2018-09-04 | 2019-01-08 | 广州创链科技有限公司 | A kind of energy saving high-low temperature chamber |
| CN111350017A (en) * | 2020-02-03 | 2020-06-30 | 江苏银兆新材料科技有限公司 | Moisture-absorbing warm-keeping knitted fabric |
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Application publication date: 20141015 |