CN102504224A - Hydrophilic copolyester slices prepared by continuous method and preparation method thereof - Google Patents
Hydrophilic copolyester slices prepared by continuous method and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a continuous method for preparing hydrophilic copolyester slices and the hydrophilic copolyester slices prepared by the preparation method. The preparation method of the hydrophilic copolyester slices prepared by the continuous method comprises the following steps: continuously and uniformly adding pure terephthalic acid, ethylene glycol, benzene dibasic acid binary alcohol ester-5-sodium sulfonate, polydibasic alcohol, other dibasic alcohols, a delustering agent and the like into a beating kettle in proportion, performing esterification, prepolycondensation and polycondensation reactions, discharging, pelletizing and drying to get the hydrophilic copolyester slices. A continuous polymerization device is adopted for synthesis; and in the prepared hydrophilic copolyester slices, the molecular structure of polyester is changed by adding hydroxyl-containing components and inorganic powder into copolyester slices, thus the hydrophilic property is good. The preparation method is simple, the manufacturing process has no special requirements on the polymerization device, and the hydrophilic copolyester slices can be produced on existing domestic or imported equipment, so that the production cost is slow and industrial production is easy to realize.
Description
Technical field
The present invention relates to a kind of hydrophilic copolyester section and preparation method thereof, belong to the technical field of polyester modification.
Background technology
The molecular structure of PET fiber has the tacticity of height, and molecular chain is arranged closely, contains characteristics such as inflexible phenyl ring in symmetrical configuration and the molecular chain, and this makes PET have good physical and mechanical property, resistance to chemical attack, antimicrobial erosion.The high-crystallinity of PET, the characteristics such as high orientation when becoming fine make its fiber and fabric that good conformality, stiffness and characteristics such as quick-drying washable arranged, thereby very popular.But the character of itself has also brought the wetting ability of PET fiber, yarn and fabric poor, is prone to produce shortcomings such as static, has hindered its further application and development.Therefore, when trevira came out, people had just begun the research work to the PET modification, and the shortcoming that is intended to overcome the PET fiber is with not enough.
The method of modifying of PET can be divided into chemical modification method and physical modification method, and wherein chemical modification method is more stable, lasting and effective means.Chemical modification has methods such as copolymerization, surface chemical reaction; Using the method modification of copolymerization is very important a kind of method in the chemical modification, and it is to be main raw material with pure terephthalic acid (PTA), terepthaloyl moietie (EG), adds a certain amount of the 3rd monomer component at synthesis phase; The 4th monomer component; Even the 5th set of monomers grade, carry out copolymerization, produce copolyesters.
1958, du pont company added monomer SIP when polymerization, invented cationic-dyeable polyester fibers, the English CDP that is called for short.CDP mainly is the dyeing behavior that has improved trevira, but the hydrophilicity of trevira is not had tangible improvement.
The eighties in 20th century, toray company adds monomer SIP and polyethers component when polymerization, develop normal pressure type cationic-dyeable polyester fibers, the English ECDP that is called for short.ECDP mainly is the dyeing behavior that has improved trevira, but not remarkable to the hydrophilicity raising of trevira, and the thermotolerance of fiber is relatively poor, has influenced the spinning property of fiber.
Since the nineties in 20th century, American-European, Japan and other countries passes through to improve monomer SIP content, develops novel atmospheric cation dye chromophil trevira, is called for short HCDP.This kind fiber has dye uptake and colour fastness preferably.But along with the increase of monomer SIP add-on, the interaction of ionic group strengthens, and melt viscosity sharply increases when causing polymerization, makes polyreaction be difficult to carry out, so the molecular weight of HCDP is generally lower, the HV during fusion also causes the post-treatment difficulty.
2000, Nichols Carl S, Humelsine Billy Mack [US] is with polyoxyethylene glycol and tetramethylolmethane C (CH
2OH)
4Come the modified PET polyester.Though having more obviously, the water absorbability of gained fiber improves, because the number-average molecular weight of the polyoxyethylene glycol of introducing is lower, so the poor heat resistance of fiber; And along with the increase of tetramethylolmethane content, melt viscosity increases violently during polymerization, and it is very big fluctuate, makes polymerization difficult, and spinning is difficult to carry out.
2003, Naruse Yoshihiro, Sasaki Toshihiro [JP] with the silicon-dioxide inorganic powder of 1-20wt%, utilizes the method for blend to add in the polyester, obtains wetting ability modified poly ester preferably.But because silicon-dioxide has a strong water-absorbent, so along with the increase of dioxide-containing silica, the water cut of PET Resin/Poyester Chips Bottle Grade increases, and makes the spinning property reduction of section.
2005, Ruzek Ivo Edward [DE] came modified polyester fiber with W 166, found that the blocked copolyester that makes has water absorbability preferably.But the number-average molecular weight of the W 166 of introducing is lower, so the thermostability of blocked copolyester is relatively poor, is unfavorable for carrying out postorder processing such as spinning.
2010, people such as Chen Bin through adding monomer SIP and the aliphatic dihydroxy alcohol that contains side chain, studied the preparation and the performance of normal temperature and pressure cation dye easy-dying copolyester and fiber thereof.Though the dyeability and the flexibility of this modified polyester fiber are improved, the moisture regain of fiber is not significantly improved.
Summary of the invention
The purpose of this invention is to provide a kind of copolyester section with excellent hydrophilic.
In order to achieve the above object, the invention provides a kind of preparation method of hydrophilic copolyester section of continuous processing preparation, it is characterized in that, may further comprise the steps:
The first step: will be input to equably continuously with transferpump with pure terephthalic acid (PTA) 1, terepthaloyl moietie (EG) 1.1-2.5, a benzene diprotic acid dibasic ester-5-sodium sulfonate 0.015-0.06, poly-dihydric alcohol 0.000166-0.01245, other divalent alcohol 0.005-0.08, matting agent 0.0104-0.0416, catalyzer 0.00007836-0.0005125 and the thermo-stabilizer 0.00004659-0.0007111 of molar ratio computing and carry out esterification in the esterifying kettle;
Second step: the carboxylate that the first step is obtained is transported to and carries out prepolymerization reaction in the precondensation still;
The 3rd step: second prepolycondensate that obtain of step is transported to carries out polycondensation in the whole polycondensation vessel;
The 4th step: go on foot polycondensate discharging, pelletizing, the drying that obtains with the 3rd.
Preferably, described benzene diprotic acid binary alcohol esters-5-sodium sulfonate is ethylene isophthalate-5-sodium sulfonate.
Preferably, described poly-dihydric alcohol is polyoxyethylene glycol, W 166 or polytetramethylene glycol, and number-average molecular weight is 4000-10000.
Further, the number-average molecular weight of described polyoxyethylene glycol is 5000-7000; The number-average molecular weight of W 166 is 4000-6000; The number-average molecular weight of polytetramethylene glycol is 4000-6000.
Preferably, described other divalent alcohol is 1,2-Ucar 35,1, ammediol, 1,2-butyleneglycol, 1,3 butylene glycol, 1,4-butyleneglycol, 1,2-pentanediol or 1,5-pentanediol.
Further, described other divalent alcohol is 1,2-Ucar 35,1,2-butyleneglycol or 1,2-pentanediol.
Preferably, described matting agent is titanium oxide (TiO
2) powder.
Preferably, described catalyzer is antimony glycol, antimony acetate or Antimony Trioxide: 99.5Min.
Preferably, described thermo-stabilizer is triphenylphosphate or trimethyl phosphite 99.
Preferably; The concrete steps of the esterification in the described the first step are: will join with pure terephthalic acid (PTA) 1, terepthaloyl moietie (EG) 1.1-2.5, other divalent alcohol 0.005-0.08 of molar ratio computing in the making beating still and pull an oar; After being delivered to the reaction of first esterifying kettle then equably; Be delivered in second esterifying kettle, a benzene diprotic acid dibasic ester-5-sodium sulfonate 0.015-0.06, poly-dihydric alcohol 0.000166-0.01245, matting agent 0.0104-0.0416, catalyzer 0.00007836-0.0005125 and thermo-stabilizer 0.00004659-0.0007111 added in second esterifying kettle continuously equably react simultaneously.
Preferably; The concrete steps of the esterification in the described the first step are: will join with pure terephthalic acid (PTA) 1, terepthaloyl moietie (EG) 1.1-2.5 of molar ratio computing in the making beating still and pull an oar; Then; After being delivered to the reaction of first esterifying kettle equably; Be delivered in second esterifying kettle, a benzene diprotic acid dibasic ester-5-sodium sulfonate 0.015-0.06, poly-dihydric alcohol 0.000166-0.01245, other divalent alcohol 0.005-0.08, matting agent 0.0104-0.0416, catalyzer 0.00007836-0.0005125 and thermo-stabilizer 0.00004659-0.0007111 added in second esterifying kettle continuously equably react simultaneously.
Further, the temperature of reaction of described first esterifying kettle is 240-260 ℃, and the reaction times is 90-240 minute; The temperature of reaction of second esterifying kettle is 242-265 ℃, and the reaction times is 60-120 minute.
Preferably, the concrete steps of prepolymerization reaction in described second step are: the carboxylate that the first step is obtained is transported in the first precondensation still after the reaction, is transported in the second precondensation still and reacts.
Further, the temperature of reaction of the described first precondensation still is 260-275 ℃, and the reaction times is 30-60 minute, and vacuum tightness is 5000-9000Pa; The temperature of reaction of the second precondensation still is 262-275 ℃, and the reaction times is 35-60 minute, and vacuum tightness is 500-1500Pa.
Preferably, the temperature of reaction of described whole polycondensation vessel is 265-280 ℃, and the reaction times is 120-200 minute, and vacuum tightness is 0-50Pa.
Principle of the present invention is in macromolecular chain, to have introduced the feminine gender with sulfonate groups to dye seat; Introduced poly-dihydric alcohol again with higher number average molecular weight; Also introduced the side chain alkane group of divalent alcohol.This fiber that makes this kind copolyester section make is used cationic dye capable of dyeing at normal temperatures and pressures, and chromatogram is complete, and is beautiful in colour, and colour fastness is good.The number-average molecular weight of poly-dihydric alcohol is higher, has increased the thermostability of copolyester section.Poly-dihydric alcohol increases the hydroxyl value in the molecular chain, and ether oxygen base and water molecules in the molecular chain have affinity interaction, and the moisture regain of copolyester fiber is improved.And, because the volume effect of the side-chain radical of divalent alcohol, reduced the crystal properties such as percent crystallinity of this kind copolyesters, reduced the second-order transition temperature of copolyesters, make fiber have ultra soft feel and good hydrophilicity.Matting agent makes copolyester fiber have soft gloss and warm sense, thereby has improved the wax sense and the creeping chill of common PET fiber.
Hydrophilic copolyester section provided by the invention is in copolyester section, to have added component and the inorganic powder that contains hydroxyl, has changed the molecular structure of polyester, has the good hydrophilicity ability.The preparation method is simple, and manufacturing processed does not have special requirement to polymerization unit, can on the existing installation of homemade or import, produce, thus its low production cost, easy realization of industrial production.The hydrophilic copolyester fiber that utilizes this copolyester section to make has been realized the comprehensive improvement on multiple performances such as wetting ability, water absorbability.
Description of drawings
Fig. 1 is the synoptic diagram of successive polymerization reaction unit.
The molecular structure of the hydrophilic copolyester section that Fig. 2 provides for embodiment 25.
Among the figure:
1, first opening for feed;
2, making beating still;
3, heating plant;
4, first esterifying kettle;
5, separation column;
6, second opening for feed;
7, second esterifying kettle;
8, the first precondensation still;
9, vacuum system;
10, the second precondensation still;
11, whole polycondensation vessel;
12, discharge port.
Embodiment
Below in conjunction with concrete embodiment, further set forth the present invention.
Among the embodiment 1-24, the pure terephthalic acid abbreviates PTA as; Terepthaloyl moietie abbreviates EG as; 1, the 2-Ucar 35 abbreviates 1 as, 2-PDO; 1, the 2-butyleneglycol abbreviates 1 as, 2-BDO; Ethylene isophthalate-5-sodium sulfonate abbreviates SIPE as; Polyoxyethylene glycol selects for use number-average molecular weight to be respectively 4000,6000,10000 polyoxyethylene glycol, abbreviates PEG4000, PEG6000, PEG10000 respectively as; W 166 selects for use number-average molecular weight to be respectively 4000,6000,10000 W 166, abbreviates PPG4000, PPG6000, PPG10000 respectively as; Polytetramethylene glycol selects for use number-average molecular weight to be respectively 4000,6000,10000 polytetramethylene glycol, abbreviates PBG4000, PBG6000, PBG10000 respectively as; Matting agent is selected titanium oxide (TiO for use
2) powder; Catalyzer is selected antimony acetate for use; Thermo-stabilizer is selected triphenylphosphate for use.
The reaction unit of embodiment 1-24 is the successive polymerization reaction unit, and is as shown in Figure 1.
Embodiment 1
With the input speed of PTA with 20000kg/h (120481.93mol/h); EG is with the input speed and 1 of 8590.36kg/h (138554.22mol/h); 2-PDO joins making beating the making beating still 2 from first opening for feed 1 respectively with the input speed of 183.35kg/h (2409.64mol/h); Above-mentioned slurry is delivered in first esterifying kettle 4 continuously equably carries out esterification, the temperature of reaction of first esterifying kettle 4 is 240 ℃, and the reaction times is 200 minutes; Be transported in second esterifying kettle 7 through transferpump, simultaneously, with the input speed of SIPE with 643.90kg/h (1807.23mol/h), PEG6000 is with the input speed of 2000kg/h (333.33mol/h), TiO respectively again
2Input speed with 100kg/h (1251.88mol/h); Antimony acetate is with the input speed of 6kg/h (20.07mol/h) and the triphenylphosphate input speed with 4kg/h (12.26mol/h); Add to equably second esterifying kettle 7 from second opening for feed 6; The temperature of reaction of second esterifying kettle 7 is 250 ℃, and the reaction times is 90 minutes; Carboxylate is transported in the first precondensation still 8 through transferpump, and the temperature of reaction of the first precondensation still 8 is 265 ℃, and the reaction times is 45 minutes, and vacuum tightness is 7000Pa; The temperature of reaction that is transported to 10, the second precondensation stills 10 in the second precondensation still again is 270 ℃, and the reaction times is 50 minutes, and vacuum tightness is 500Pa; Prepolycondensate is transported in the whole polycondensation vessel 11, and the temperature of reaction of whole polycondensation vessel 11 is 275 ℃, and the reaction times is 150 minutes, and vacuum tightness is 10Pa; Reaction finishes the back from discharge port 12 dischargings, and pelletizing, drying, makes copolyester section.The intrinsic viscosity of section is 0.628 dL/g, and fusing point is 244.5 ℃.The hydrophilic copolyester section that makes behind crystallization in advance, drying, spinning process, is made the hydrophilic copolyester fiber, and its moisture regain is 1.04%.
With PTA with the input speed of 20000kg/h (120481.93mol/h) and EG with the input speed of 8590.36kg/h (138554.22mol/h), join making beating the making beating still 2 from opening for feed 1 respectively; Above-mentioned slurry is delivered in first esterifying kettle 4 continuously equably, and the temperature of reaction of first esterifying kettle 4 is 240 ℃, and the reaction times is 200 minutes; Be transported in second esterifying kettle 7 through transferpump again; Simultaneously; With the input speed of SIPE with 643.90kg/h (1807.23mol/h), PEG6000 is with the input speed of 2000kg/h (333.33mol/h), 1 respectively; 2-PDO is with the input speed of 183.35kg/h (2409.64mol/h), TiO
2Input speed with 100kg/h (1251.88mol/h); Antimony acetate is with the input speed of 6kg/h (20.07mol/h) and the triphenylphosphate input speed with 4kg/h (12.26mol/h); Add to equably second esterifying kettle 7 from second opening for feed 6; The temperature of reaction of second esterifying kettle 7 is 250 ℃, and the reaction times is 90 minutes; Carboxylate is transported in the first precondensation still 8 through transferpump, and the temperature of reaction of the first precondensation still 8 is 265 ℃, and the reaction times is 45 minutes, and vacuum tightness is 7000Pa; The temperature of reaction that is transported to 10, the second precondensation stills 10 in the second precondensation still again is 270 ℃, and the reaction times is 50 minutes, and vacuum tightness is 500Pa; Prepolycondensate is transported in the whole polycondensation vessel 11, and the temperature of reaction of whole polycondensation vessel 11 is 275 ℃, and the reaction times is 150 minutes, and vacuum tightness is 10Pa; Reaction finishes the back from discharge port 12 dischargings, and pelletizing, drying, makes copolyester section.The intrinsic viscosity of section is 0.630dL/g, and fusing point is 244.8 ℃.The hydrophilic copolyester section that makes behind crystallization in advance, drying, spinning process, is made the hydrophilic copolyester fiber, and its moisture regain is 1.06%.
With the input speed of PTA with 20000kg/h (120481.93mol/h); EG is with the input speed and 1 of 8590.36kg/h (138554.22mol/h); 2-PDO joins making beating the making beating still 2 from opening for feed 1 respectively with the input speed of 733.4kg/h (9638.56mol/h); Above-mentioned slurry is delivered in first esterifying kettle 4 continuously equably, and the temperature of reaction of first esterifying kettle 4 is 240 ℃, and the reaction times is 200 minutes; Be transported in second esterifying kettle 7 through transferpump, simultaneously, with the input speed of SIPE with 2575.6kg/h (7228.92mol/h), PEG6000 is with the input speed of 200kg/h (33.33mol/h), TiO respectively again
2Input speed with 400kg/h (5007.51mol/h); Antimony acetate is with the input speed of 6kg/h (20.07mol/h) and the triphenylphosphate input speed with 4kg/h (12.26mol/h); Add to equably second esterifying kettle 7 from second opening for feed 6; The temperature of reaction of second esterifying kettle 7 is 250 ℃, and the reaction times is 90 minutes; Be transported in the first precondensation still 8 through transferpump, the temperature of reaction of the first precondensation still 8 is 265 ℃ again, and the reaction times is 45 minutes, and vacuum tightness is 7000Pa; The temperature of reaction that prepolycondensate is transported to 10, the second precondensation stills 10 in the second precondensation still is 270 ℃, and the reaction times is 50 minutes, and vacuum tightness is 500Pa; Then prepolycondensate is transported in the whole polycondensation vessel 11, the temperature of reaction of whole polycondensation vessel 11 is 275 ℃, and the reaction times is 150 minutes, and vacuum tightness is 10Pa; Reaction finishes the back from discharge port 12 dischargings, and pelletizing, drying, makes copolyester section.The intrinsic viscosity of section is 0.615dL/g, and fusing point is 241.4 ℃.The hydrophilic copolyester section that makes behind crystallization in advance, drying, spinning process, is made the hydrophilic copolyester fiber, and its moisture regain is 1.07%.
Embodiment 4
With PTA with the input speed of 20000kg/h (120481.93mol/h) and EG with the input speed of 8590.36kg/h (138554.22mol/h), join making beating the making beating still 2 from opening for feed 1 respectively; Above-mentioned slurry is delivered in first esterifying kettle 4 continuously equably, and the temperature of reaction of first esterifying kettle 4 is 240 ℃, and the reaction times is 200 minutes; Be transported in second esterifying kettle 7 through transferpump again, simultaneously, respectively with the input speed of SIPE with 2575.6kg/h (7228.92mol/h); PEG6000 is with the input speed of 200kg/h (33.33mol/h); 1,2-PDO is with the input speed of 733.4kg/h (9638.56mol/h), TiO
2Input speed with 400kg/h (5007.51mol/h); Antimony acetate is with the input speed of 6kg/h (20.07mol/h) and the triphenylphosphate input speed with 4kg/h (12.26mol/h); Add to equably second esterifying kettle 7 from second opening for feed 6; The temperature of reaction of second esterifying kettle 7 is 250 ℃, and the reaction times is 90 minutes; Carboxylate is transported in the first precondensation still 8 through transferpump, and the temperature of reaction of the first precondensation still 8 is 265 ℃, and the reaction times is 45 minutes, and vacuum tightness is 7000Pa; The temperature of reaction that then prepolycondensate is transported to 10, the second precondensation stills 10 in the second precondensation still is 270 ℃, and the reaction times is 50 minutes, and vacuum tightness is 500Pa; Then prepolycondensate is transported in the whole polycondensation vessel 11, the temperature of reaction of whole polycondensation vessel 11 is 275 ℃, and the reaction times is 150 minutes, and vacuum tightness is 10Pa; Reaction finishes the back from discharge port 12 dischargings, and pelletizing, drying, makes copolyester section.The intrinsic viscosity of section is 0.618dL/g, and fusing point is 241.6 ℃.The hydrophilic copolyester section that makes behind crystallization in advance, drying, spinning process, is made the hydrophilic copolyester fiber, and its moisture regain is 1.10%.
Embodiment 5
With the input speed of PTA with 20000kg/h (120481.93mol/h); EG is with the input speed and 1 of 8590.36kg/h (138554.22mol/h); 2-PDO joins making beating the making beating still 2 from opening for feed 1 respectively with the input speed of 45.84kg/h (602.41mol/h); Above-mentioned slurry is delivered in first esterifying kettle 4 continuously equably, and the temperature of reaction of first esterifying kettle 4 is 240 ℃, and the reaction times is 200 minutes; Be transported in second esterifying kettle 7 through transferpump, simultaneously, with the input speed of SIPE with 643.90kg/h (1807.23mol/h), PEG6000 is with the input speed of 6000kg/h (1000mol/h), TiO respectively again
2Input speed with 100kg/h (1251.88mol/h); Antimony acetate is with the input speed of 6kg/h (20.07mol/h) and the triphenylphosphate input speed with 4kg/h (12.26mol/h); Add to equably second esterifying kettle 7 from second opening for feed 6; The temperature of reaction of second esterifying kettle 7 is 250 ℃, and the reaction times is 90 minutes; Carboxylate is transported in the first precondensation still 8 through transferpump, and the temperature of reaction of the first precondensation still 8 is 265 ℃, and the reaction times is 45 minutes, and vacuum tightness is 7000Pa; The temperature of reaction that then prepolycondensate is transported to 10, the second precondensation stills 10 in the second precondensation still is 270 ℃, and the reaction times is 50 minutes, and vacuum tightness is 500Pa; Then prepolycondensate is transported in the whole polycondensation vessel 11, the temperature of reaction of whole polycondensation vessel 11 is 275 ℃, and the reaction times is 150 minutes, and vacuum tightness is 10Pa; Reaction finishes the back from discharge port 12 dischargings, and pelletizing, drying, makes copolyester section.The intrinsic viscosity of section is 0.566dL/g, and fusing point is 229.6 ℃.The hydrophilic copolyester section that makes behind crystallization in advance, drying, spinning process, is made the hydrophilic copolyester fiber, and its moisture regain is 1.83%.
With PTA with the input speed of 20000kg/h (120481.93mol/h) and EG with the input speed of 8590.36kg/h (138554.22mol/h), join making beating the making beating still 2 from opening for feed 1 respectively; Above-mentioned slurry is delivered in first esterifying kettle 4 continuously equably, and the temperature of reaction of first esterifying kettle 4 is 240 ℃, and the reaction times is 200 minutes; Be transported in second esterifying kettle 7 through transferpump again, simultaneously, respectively with the input speed of SIPE with 643.90kg/h (1807.23mol/h); PEG6000 is with the input speed of 6000kg/h (1000mol/h); 1,2-PDO is with the input speed of 45.84kg/h (602.41mol/h), TiO
2Input speed with 100kg/h (1251.88mol/h); Antimony acetate is with the input speed of 6kg/h (20.07mol/h) and the triphenylphosphate input speed with 4kg/h (12.26mol/h); Add to equably second esterifying kettle 7 from second opening for feed 6; The temperature of reaction of second esterifying kettle 7 is 250 ℃, and the reaction times is 90 minutes; Carboxylate is transported in the first precondensation still 8 through transferpump, and the temperature of reaction of the first precondensation still 8 is 265 ℃, and the reaction times is 45 minutes, and vacuum tightness is 7000Pa; The temperature of reaction that then prepolycondensate is transported to 10, the second precondensation stills 10 in the second precondensation still is 270 ℃, and the reaction times is 50 minutes, and vacuum tightness is 500Pa; Then prepolycondensate is transported in the whole polycondensation vessel 11, the temperature of reaction of whole polycondensation vessel 11 is 275 ℃, and the reaction times is 150 minutes, and vacuum tightness is 10Pa; Reaction finishes the back from discharge port 12 dischargings, and pelletizing, drying, makes copolyester section.The intrinsic viscosity of section is 0.572dL/g, and fusing point is 229.0 ℃.The hydrophilic copolyester section that makes behind crystallization in advance, drying, spinning process, is made the hydrophilic copolyester fiber, and its moisture regain is 1.85%.
With the input speed of PTA with 20000kg/h (120481.93mol/h); EG is with the input speed and 1 of 8590.36kg/h (138554.22mol/h); 2-BDO joins making beating the making beating still 2 from opening for feed 1 respectively with the input speed of 868.63kg/h (9638.56mol/h); Above-mentioned slurry is delivered in first esterifying kettle 4 continuously equably, and the temperature of reaction of first esterifying kettle 4 is 240 ℃, and the reaction times is 200 minutes; Be transported in second esterifying kettle 7 through transferpump, simultaneously, with the input speed of SIPE with 2575.6kg/h (7228.92mol/h), PEG4000 is with the input speed of 200kg/h (50mol/h), TiO respectively again
2Input speed with 200kg/h (2503.76mol/h); Antimony acetate is with the input speed of 6kg/h (20.07mol/h) and the triphenylphosphate input speed with 4kg/h (12.26mol/h); Add to equably second esterifying kettle 7 from second opening for feed 6; The temperature of reaction of second esterifying kettle 7 is 250 ℃, and the reaction times is 90 minutes; Carboxylate is transported in the first precondensation still 8 through transferpump, and the temperature of reaction of the first precondensation still 8 is 265 ℃, and the reaction times is 45 minutes, and vacuum tightness is 7000Pa; The temperature of reaction that then prepolycondensate is transported to 10, the second precondensation stills 10 in the second precondensation still is 270 ℃, and the reaction times is 50 minutes, and vacuum tightness is 500Pa; Then prepolycondensate is transported in the whole polycondensation vessel 11, the temperature of reaction of whole polycondensation vessel 11 is 275 ℃, and the reaction times is 150 minutes, and vacuum tightness is 10Pa; Reaction finishes the back from discharge port 12 dischargings, and pelletizing, drying, makes copolyester section.The intrinsic viscosity of section is 0.617dL/g, and fusing point is 242.3 ℃.The hydrophilic copolyester section that makes behind crystallization in advance, drying, spinning process, is made the hydrophilic copolyester fiber, and its moisture regain is 1.09%.
With PTA with the input speed of 20000kg/h (120481.93mol/h) and EG with the input speed of 8590.36kg/h (138554.22mol/h), join making beating the making beating still 2 from opening for feed 1 respectively; Above-mentioned slurry is delivered in first esterifying kettle 4 continuously equably, and the temperature of reaction of first esterifying kettle 4 is 240 ℃, and the reaction times is 200 minutes; Be transported in second esterifying kettle 7 through transferpump again, simultaneously, respectively with the input speed of SIPE with 2575.6kg/h (7228.92mol/h); PEG4000 is with the input speed of 200kg/h (50mol/h); 1,2-BDO is with the input speed of 868.63kg/h (9638.56mol/h), TiO
2Input speed with 200kg/h (2503.76mol/h); Antimony acetate is with the input speed of 6kg/h (20.07mol/h) and the triphenylphosphate input speed with 4kg/h (12.26mol/h); Add to equably second esterifying kettle 7 from second opening for feed 6; The temperature of reaction of second esterifying kettle 7 is 250 ℃, and the reaction times is 90 minutes; Carboxylate is transported in the first precondensation still 8 through transferpump, and the temperature of reaction of the first precondensation still 8 is 265 ℃, and the reaction times is 45 minutes, and vacuum tightness is 7000Pa; The temperature of reaction that then prepolycondensate is transported to 10, the second precondensation stills 10 in the second precondensation still is 270 ℃, and the reaction times is 50 minutes, and vacuum tightness is 500Pa; Then prepolycondensate is transported in the whole polycondensation vessel 11, the temperature of reaction of whole polycondensation vessel 11 is 275 ℃, and the reaction times is 150 minutes, and vacuum tightness is 10Pa; Reaction finishes the back from discharge port 12 dischargings, and pelletizing, drying, makes copolyester section.The intrinsic viscosity of section is 0.624dL/g, and fusing point is 242.6 ℃.The hydrophilic copolyester section that makes behind crystallization in advance, drying, spinning process, is made the hydrophilic copolyester fiber, and its moisture regain is 1.12%.
Embodiment 9
With the input speed of PTA with 20000kg/h (120481.93mol/h); EG is with the input speed and 1 of 8590.36kg/h (138554.22mol/h); 2-BDO joins making beating the making beating still 2 from opening for feed 1 respectively with the input speed of 54.29kg/h (602.41mol/h) per hour; Above-mentioned slurry is delivered in first esterifying kettle 4 continuously equably, and the temperature of reaction of first esterifying kettle 4 is 240 ℃, and the reaction times is 200 minutes; Be transported in second esterifying kettle 7 through transferpump, simultaneously, with the input speed of SIPE with 643.90kg/h (1807.23mol/h), PEG4000 is with the input speed of 6000kg/h (1500mol/h), TiO respectively again
2Input speed with 100kg/h (1251.88mol/h); Antimony acetate is with the input speed of 6kg/h (20.07mol/h) and the triphenylphosphate input speed with 4kg/h (12.26mol/h); Add to equably second esterifying kettle 7 from second opening for feed 6; The temperature of reaction of second esterifying kettle 7 is 250 ℃, and the reaction times is 90 minutes; Carboxylate is transported in the first precondensation still 8 through transferpump, and the temperature of reaction of the first precondensation still 8 is 265 ℃, and the reaction times is 45 minutes, and vacuum tightness is 7000Pa; The temperature of reaction that then prepolycondensate is transported to 10, the second precondensation stills 10 in the second precondensation still is 270 ℃, and the reaction times is 50 minutes, and vacuum tightness is 500Pa; Then prepolycondensate is transported in the whole polycondensation vessel 11, the temperature of reaction of whole polycondensation vessel 11 is 275 ℃, and the reaction times is 150 minutes, and vacuum tightness is 10Pa; Reaction finishes the back from discharge port 12 dischargings, and pelletizing, drying, makes copolyester section.The intrinsic viscosity of section is 0.575dL/g, and fusing point is 228.2 ℃.The hydrophilic copolyester section that makes behind crystallization in advance, drying, spinning process, is made the hydrophilic copolyester fiber, and its moisture regain is 1.85%.
With PTA with the input speed of 20000kg/h (120481.93mol/h) and EG with the input speed of 8590.36kg/h (138554.22mol/h), join making beating the making beating still 2 from opening for feed 1 respectively; Above-mentioned slurry is delivered in first esterifying kettle 4 continuously equably, and the temperature of reaction of first esterifying kettle 4 is 240 ℃, and the reaction times is 200 minutes; Be transported in second esterifying kettle 7 through transferpump again, simultaneously, respectively with the input speed of SIPE with 643.90kg/h (1807.23mol/h); PEG4000 is with the input speed of 6000kg/h (1500mol/h); 1,2-BDO is with the input speed of 54.29kg/h (602.41mol/h), TiO
2Input speed with 100kg/h (1251.88mol/h); Antimony acetate is with the input speed of 6kg/h (20.07mol/h) and the triphenylphosphate input speed with 4kg/h (12.26mol/h); Add to equably second esterifying kettle 7 from second opening for feed 6; The temperature of reaction of second esterifying kettle 7 is 250 ℃, and the reaction times is 90 minutes; Carboxylate is transported in the first precondensation still 8 through transferpump, and the temperature of reaction of the first precondensation still 8 is 265 ℃, and the reaction times is 45 minutes, and vacuum tightness is 7000Pa; The temperature of reaction that then prepolycondensate is transported to 10, the second precondensation stills 10 in the second precondensation still is 270 ℃, and the reaction times is 50 minutes, and vacuum tightness is 500Pa; Then prepolycondensate is transported in the whole polycondensation vessel 11, the temperature of reaction of whole polycondensation vessel 11 is 275 ℃, and the reaction times is 150 minutes, and vacuum tightness is 10Pa; Reaction finishes the back from discharge port 12 dischargings, and pelletizing, drying, makes copolyester section.The intrinsic viscosity of section is 0.578dL/g, and fusing point is 228.5 ℃.The hydrophilic copolyester section that makes behind crystallization in advance, drying, spinning process, is made the hydrophilic copolyester fiber, and its moisture regain is 1.87%.
With the input speed of PTA with 20000kg/h (120481.93mol/h); EG is with the input speed and 1 of 8590.36kg/h (138554.22mol/h); 2-BDO joins making beating the making beating still 2 from opening for feed 1 respectively with the input speed of 217.16kg/h (2409.64mol/h); Above-mentioned slurry is delivered in first esterifying kettle 4 continuously equably, and the temperature of reaction of first esterifying kettle 4 is 240 ℃, and the reaction times is 200 minutes; Be transported in second esterifying kettle 7 through transferpump, simultaneously, with the input speed of SIPE with 1287.8kg/h (3614.46mol/h), PEG4000 is with the input speed of 2000kg/h (500mol/h), TiO respectively again
2Input speed with 200kg/h (2503.76mol/h); Antimony acetate is with the input speed of 6kg/h (20.07mol/h) and the triphenylphosphate input speed with 4kg/h (12.26mol/h); Add to equably second esterifying kettle 7 from second opening for feed 6; The temperature of reaction of second esterifying kettle 7 is 250 ℃, and the reaction times is 90 minutes; Carboxylate is transported in the first precondensation still 8 through transferpump, and the temperature of reaction of the first precondensation still 8 is 265 ℃, and the reaction times is 45 minutes, and vacuum tightness is 7000Pa; The temperature of reaction that then prepolycondensate is transported to 10, the second precondensation stills 10 in the second precondensation still is 270 ℃, and the reaction times is 50 minutes, and vacuum tightness is 500Pa; Then prepolycondensate is transported in the whole polycondensation vessel 11, the temperature of reaction of whole polycondensation vessel 11 is 275 ℃, and the reaction times is 150 minutes, and vacuum tightness is 10Pa; Reaction finishes the back from discharge port 12 dischargings, and pelletizing, drying, makes copolyester section.The intrinsic viscosity of section is 0.612dL/g, and fusing point is 240.5 ℃.The hydrophilic copolyester section that makes behind crystallization in advance, drying, spinning process, is made the hydrophilic copolyester fiber, and its moisture regain is 1.41%.
PTA is joined making beating the making beating still 2 from opening for feed 1 with the input speed of 20000kg/h (120481.93mol/h) and EG respectively with the input speed of 8590.36kg/h (138554.22mol/h); Above-mentioned slurry is delivered in first esterifying kettle 4 continuously equably, and the temperature of reaction of first esterifying kettle 4 is 240 ℃, and the reaction times is 200 minutes; Be transported in second esterifying kettle 7 through transferpump again, simultaneously, respectively with the input speed of SIPE with 1287.8kg/h (3614.46mol/h); PEG4000 is with the input speed of 2000kg/h (500mol/h); 1,2-BDO is with the input speed of 217.16kg/h (2409.64mol/h), TiO
2Input speed with 200kg/h (2503.76mol/h); Antimony acetate is with the input speed of 6kg/h (20.07mol/h) and the triphenylphosphate input speed with 4kg/h (12.26mol/h); Add to equably second esterifying kettle 7 from second opening for feed 6; The temperature of reaction of second esterifying kettle 7 is 250 ℃, and the reaction times is 90 minutes; Carboxylate is transported in the first precondensation still 8 through transferpump, and the temperature of reaction of the first precondensation still 8 is 265 ℃, and the reaction times is 45 minutes, and vacuum tightness is 7000Pa; The temperature of reaction that then prepolycondensate is transported to 10, the second precondensation stills 10 in the second precondensation still is 270 ℃, and the reaction times is 50 minutes, and vacuum tightness is 500Pa; Then prepolycondensate is transported in the whole polycondensation vessel 11, the temperature of reaction of whole polycondensation vessel 11 is 275 ℃, and the reaction times is 150 minutes, and vacuum tightness is 10Pa; Reaction finishes the back from discharge port 12 dischargings, and pelletizing, drying, makes copolyester section.The intrinsic viscosity of section is 0.617dL/g, and fusing point is 240.8 ℃.The hydrophilic copolyester section that makes behind crystallization in advance, drying, spinning process, is made the hydrophilic copolyester fiber, and its moisture regain is 1.47%.
Embodiment 13
With the input speed of PTA with 20000kg/h (120481.93mol/h); EG is with the input speed and 1 of 8590.36kg/h (138554.22mol/h); The 2-pentanediol joins making beating the making beating still 2 from opening for feed 1 respectively with the input speed of 1003.86kg/h (9638.56mol/h); Above-mentioned slurry is delivered in first esterifying kettle 4 continuously equably, and the temperature of reaction of first esterifying kettle 4 is 240 ℃, and the reaction times is 200 minutes; Be transported in second esterifying kettle 7 through transferpump, simultaneously, with the input speed of SIPE with 2575.6kg/h (7228.92mol/h), PEG10000 is with the input speed of 200kg/h (20mol/h), TiO respectively again
2Input speed with 200kg/h (2503.76mol/h); Antimony acetate is with the input speed of 6kg/h (20.07mol/h) and the triphenylphosphate input speed with 4kg/h (12.26mol/h); Add to equably second esterifying kettle 7 from second opening for feed 6; The temperature of reaction of second esterifying kettle 7 is 250 ℃, and the reaction times is 90 minutes; Carboxylate is transported in the first precondensation still 8 through transferpump, and the temperature of reaction of the first precondensation still 8 is 265 ℃, and the reaction times is 45 minutes, and vacuum tightness is 7000Pa; The temperature of reaction that then prepolycondensate is transported to 10, the second precondensation stills 10 in the second precondensation still is 270 ℃, and the reaction times is 50 minutes, and vacuum tightness is 500Pa; Then prepolycondensate is transported in the whole polycondensation vessel 11, the temperature of reaction of whole polycondensation vessel 11 is 275 ℃, and the reaction times is 150 minutes, and vacuum tightness is 10Pa; Reaction finishes the back from discharge port 12 dischargings, and pelletizing, drying, makes copolyester section.The intrinsic viscosity of section is 0.622dL/g, and fusing point is 242.6 ℃.The hydrophilic copolyester section that makes behind crystallization in advance, drying, spinning process, is made the hydrophilic copolyester fiber, and its moisture regain is 1.08%.
Embodiment 14
With PTA with the input speed of 20000kg/h (120481.93mol/h) and EG with the input speed of 8590.36kg/h (138554.22mol/h), join making beating the making beating still 2 from opening for feed 1 respectively; Above-mentioned slurry is delivered in first esterifying kettle 4 continuously equably, and the temperature of reaction of first esterifying kettle 4 is 240 ℃, and the reaction times is 200 minutes; Be transported in second esterifying kettle 7 through transferpump again; Simultaneously; With the input speed of SIPE with 2575.6kg/h (7228.92mol/h), PEG10000 is with the input speed of 200kg/h (20mol/h), 1 respectively; The 2-pentanediol is with the input speed of 1003.86kg/h (9638.56mol/h), TiO
2Input speed with 200kg/h (2503.76mol/h); Antimony acetate is with the input speed of 6kg/h (20.07mol/h) and the triphenylphosphate input speed with 4kg/h (12.26mol/h); Add to equably second esterifying kettle 7 from second opening for feed 6; The temperature of reaction of second esterifying kettle 7 is 250 ℃, and the reaction times is 90 minutes; Carboxylate is transported in the first precondensation still 8 through transferpump, and the temperature of reaction of the first precondensation still 8 is 265 ℃, and the reaction times is 45 minutes, and vacuum tightness is 7000Pa; The temperature of reaction that then prepolycondensate is transported to 10, the second precondensation stills 10 in the second precondensation still is 270 ℃, and the reaction times is 50 minutes, and vacuum tightness is 500Pa; Then prepolycondensate is transported in the whole polycondensation vessel 11, the temperature of reaction of whole polycondensation vessel 11 is 275 ℃, and the reaction times is 150 minutes, and vacuum tightness is 10Pa; Reaction finishes the back from discharge port 12 dischargings, and pelletizing, drying, makes copolyester section.The intrinsic viscosity of section is 0.625dL/g, and fusing point is 242.9 ℃.The hydrophilic copolyester section that makes behind crystallization in advance, drying, spinning process, is made the hydrophilic copolyester fiber, and its moisture regain is 1.13%.
Embodiment 15
With the input speed of PTA with 20000kg/h (120481.93mol/h); EG is with the input speed and 1 of 8590.36kg/h (138554.22mol/h); The 2-pentanediol joins making beating the making beating still 2 from opening for feed 1 respectively with the input speed of 62.74kg/h (602.41mol/h); Above-mentioned slurry is delivered in first esterifying kettle 4 continuously equably, and the temperature of reaction of first esterifying kettle 4 is 240 ℃, and the reaction times is 200 minutes; Be transported in second esterifying kettle 7 through transferpump, simultaneously, with the input speed of SIPE with 643.90kg/h (1807.23mol/h), PEG10000 is with the input speed of 6000kg/h (600mol/h), TiO respectively again
2Input speed with 100kg/h (1251.88mol/h); Antimony acetate is with the input speed of 6kg/h (20.07mol/h) and the triphenylphosphate input speed with 4kg/h (12.26mol/h); Add to equably second esterifying kettle 7 from second opening for feed 6; The temperature of reaction of second esterifying kettle 7 is 250 ℃, and the reaction times is 90 minutes; Carboxylate is transported in the first precondensation still 8 through transferpump, and the temperature of reaction of the first precondensation still 8 is 265 ℃, and the reaction times is 45 minutes, and vacuum tightness is 7000Pa; The temperature of reaction that then prepolycondensate is transported to 10, the second precondensation stills 10 in the second precondensation still is 270 ℃, and the reaction times is 50 minutes, and vacuum tightness is 500Pa; Then prepolycondensate is transported in the whole polycondensation vessel 11, the temperature of reaction of whole polycondensation vessel 11 is 275 ℃, and the reaction times is 150 minutes, and vacuum tightness is 10Pa; Reaction finishes the back from discharge port 12 dischargings, and pelletizing, drying, makes copolyester section.The intrinsic viscosity of section is 0.585dL/g, and fusing point is 229.4 ℃.The hydrophilic copolyester section that makes behind crystallization in advance, drying, spinning process, is made the hydrophilic copolyester fiber, and its moisture regain is 1.81%.
Embodiment 16
With PTA with the input speed of 20000kg/h (120481.93mol/h) and EG with the input speed of 8590.36kg/h (138554.22mol/h), join making beating the making beating still 2 from opening for feed 1 respectively; Above-mentioned slurry is delivered in first esterifying kettle 4 continuously equably, and the temperature of reaction of first esterifying kettle 4 is 240 ℃, and the reaction times is 200 minutes; Be transported in second esterifying kettle 7 through transferpump again; Simultaneously; With the input speed of SIPE with 643.90kg/h (1807.23mol/h), PEG10000 is with the input speed of 6000kg/h (600mol/h), 1 respectively; The 2-pentanediol is with the input speed of 62.74kg/h (602.41mol/h), TiO
2Input speed with 100kg/h (1251.88mol/h); Antimony acetate is with the input speed of 6kg/h (20.07mol/h) and the triphenylphosphate input speed with 4kg/h (12.26mol/h); Add to equably second esterifying kettle 7 from second opening for feed 6; The temperature of reaction of second esterifying kettle 7 is 250 ℃, and the reaction times is 90 minutes; Carboxylate is transported in the first precondensation still 8 through transferpump, and the temperature of reaction of the first precondensation still 8 is 265 ℃, and the reaction times is 45 minutes, and vacuum tightness is 7000Pa; The temperature of reaction that then prepolycondensate is transported to 10, the second precondensation stills 10 in the second precondensation still is 270 ℃, and the reaction times is 50 minutes, and vacuum tightness is 500Pa; Then prepolycondensate is transported in the whole polycondensation vessel 11, the temperature of reaction of whole polycondensation vessel 11 is 275 ℃, and the reaction times is 150 minutes, and vacuum tightness is 10Pa; Reaction finishes the back from discharge port 12 dischargings, and pelletizing, drying, makes copolyester section.The intrinsic viscosity of section is 0.600dL/g, and fusing point is 229.8 ℃.The hydrophilic copolyester section that makes behind crystallization in advance, drying, spinning process, is made the hydrophilic copolyester fiber, and its moisture regain is 1.84%.
Embodiment 17
With the input speed of PTA with 20000kg/h (120481.93mol/h); EG is with the input speed and 1 of 8590.36kg/h (138554.22mol/h); The 2-pentanediol joins making beating the making beating still 2 from opening for feed 1 respectively with the input speed of 250.96kg/h (2409.64mol/h); Above-mentioned slurry is delivered in first esterifying kettle 4 continuously equably, and the temperature of reaction of first esterifying kettle 4 is 240 ℃, and the reaction times is 200 minutes; Be transported in second esterifying kettle 7 through transferpump, simultaneously, with the input speed of SIPE with 1287.8kg/h (3614.46mol/h), PEG10000 is with the input speed of 2000kg/h (200mol/h), TiO respectively again
2Input speed with 200kg/h (2503.76mol/h); Antimony acetate is with the input speed of 6kg/h (20.07mol/h) and the triphenylphosphate input speed with 4kg/h (12.26mol/h); Add to equably second esterifying kettle 7 from second opening for feed 6; The temperature of reaction of second esterifying kettle 7 is 250 ℃, and the reaction times is 90 minutes; Carboxylate is transported in the first precondensation still 8 through transferpump, and the temperature of reaction of the first precondensation still 8 is 265 ℃, and the reaction times is 45 minutes, and vacuum tightness is 7000Pa; The temperature of reaction that then prepolycondensate is transported to 10, the second precondensation stills 10 in the second precondensation still is 270 ℃, and the reaction times is 50 minutes, and vacuum tightness is 500Pa; Then prepolycondensate is transported in the whole polycondensation vessel 11, the temperature of reaction of whole polycondensation vessel 11 is 275 ℃, and the reaction times is 150 minutes, and vacuum tightness is 10Pa; Reaction finishes the back from discharge port 12 dischargings, and pelletizing, drying, makes copolyester section.The intrinsic viscosity of section is 0.614dL/g, and fusing point is 242.0 ℃.The hydrophilic copolyester section that makes behind crystallization in advance, drying, spinning process, is made the hydrophilic copolyester fiber, and its moisture regain is 1.43%.
Embodiment 18
With PTA with the input speed of 20000kg/h (120481.93mol/h) and EG with the input speed of 8590.36kg/h (138554.22mol/h), join making beating the making beating still 2 from opening for feed 1 respectively; Above-mentioned slurry is delivered in first esterifying kettle 4 continuously equably, and the temperature of reaction of first esterifying kettle 4 is 240 ℃, and the reaction times is 200 minutes; Be transported in second esterifying kettle 7 through transferpump again; Simultaneously; With the input speed of kg SIPE with 1287.8kg/h (3614.46mol/h), PEG10000 is with the input speed of 2000kg/h (200mol/h), 1 respectively; The 2-pentanediol is with the input speed of 250.96kg/h (2409.64mol/h), TiO
2Input speed with 200kg/h (2503.76mol/h); Antimony acetate is with the input speed of 6kg/h (20.07mol/h) and the triphenylphosphate input speed with 4kg/h (12.26mol/h); Add to equably second esterifying kettle 7 from second opening for feed 6; The temperature of reaction of second esterifying kettle 7 is 250 ℃, and the reaction times is 90 minutes; Carboxylate is transported in the first precondensation still 8 through transferpump, and the temperature of reaction of the first precondensation still 8 is 265 ℃, and the reaction times is 45 minutes, and vacuum tightness is 7000Pa; The temperature of reaction that then prepolycondensate is transported to 10, the second precondensation stills 10 in the second precondensation still is 270 ℃, and the reaction times is 50 minutes, and vacuum tightness is 500Pa; Then prepolycondensate is transported in the whole polycondensation vessel 11, the temperature of reaction of whole polycondensation vessel 11 is 275 ℃, and the reaction times is 150 minutes, and vacuum tightness is 10Pa; Reaction finishes the back from discharge port 12 dischargings, and pelletizing, drying, makes copolyester section.The intrinsic viscosity of section is 0.617dL/g, and fusing point is 242.2 ℃.The hydrophilic copolyester section that makes behind crystallization in advance, drying, spinning process, is made the hydrophilic copolyester fiber, and its moisture regain is 1.48%.
Embodiment 19
With PTA with the input speed of 20000kg/h (120481.93mol/h) and EG with the input speed of 8590.36kg/h (138554.22mol/h), join making beating the making beating still 2 from opening for feed 1 respectively; Above-mentioned slurry is delivered in first esterifying kettle 4 continuously equably, and the temperature of reaction of first esterifying kettle 4 is 240 ℃, and the reaction times is 200 minutes; Be transported in second esterifying kettle 7 through transferpump again, simultaneously, respectively with the input speed of SIPE with 1287.8kg/h (3614.46mol/h); PPG4000 is with the input speed of 2000kg/h (500mol/h); 1,2-PDO is with the input speed of 183.35kg/h (2409.64mol/h), TiO
2Input speed with 200kg/h (2503.76mol/h); Antimony acetate is with the input speed of 6kg/h (20.07mol/h) and the triphenylphosphate input speed with 4kg/h (12.26mol/h); Add to equably second esterifying kettle 7 from second opening for feed 6; The temperature of reaction of second esterifying kettle 7 is 250 ℃, and the reaction times is 90 minutes; Carboxylate is transported in the first precondensation still 8 through transferpump, and the temperature of reaction of the first precondensation still 8 is 265 ℃, and the reaction times is 45 minutes, and vacuum tightness is 7000Pa; The temperature of reaction that then prepolycondensate is transported to 10, the second precondensation stills 10 in the second precondensation still is 270 ℃, and the reaction times is 50 minutes, and vacuum tightness is 500Pa; Then prepolycondensate is transported in the whole polycondensation vessel 11, the temperature of reaction of whole polycondensation vessel 11 is 275 ℃, and the reaction times is 150 minutes, and vacuum tightness is 10Pa; Reaction finishes the back from discharge port 12 dischargings, and pelletizing, drying, makes copolyester section.The intrinsic viscosity of section is 0.606dL/g, and fusing point is 241.3 ℃.The hydrophilic copolyester section that makes behind crystallization in advance, drying, spinning process, is made the hydrophilic copolyester fiber, and its moisture regain is 1.49%.
Embodiment 20
With PTA with the input speed of 20000kg/h (120481.93mol/h) and EG with the input speed of 8590.36kg/h (138554.22mol/h), join making beating the making beating still 2 from opening for feed 1 respectively; Above-mentioned slurry is delivered in first esterifying kettle 4 continuously equably, and the temperature of reaction of first esterifying kettle 4 is 240 ℃, and the reaction times is 200 minutes; Be transported in second esterifying kettle 7 through transferpump again; Simultaneously; With the input speed of SIPE with 1287.8kg/h (3614.46mol/h), PPG6000 is with the input speed of 2000kg/h (333.33mol/h), 1 respectively; 2-PDO is with the input speed of 183.35kg/h (2409.64mol/h) per hour, TiO
2Input speed with 200kg/h (2503.76mol/h); The kg antimony acetate is with the input speed of 6kg/h (20.07mol/h) and the triphenylphosphate input speed with 4kg/h (12.26mol/h); Add to equably second esterifying kettle 7 from second opening for feed 6; The temperature of reaction of second esterifying kettle 7 is 250 ℃, and the reaction times is 90 minutes; Carboxylate is transported in the first precondensation still 8 through transferpump, and the temperature of reaction of the first precondensation still 8 is 265 ℃, and the reaction times is 45 minutes, and vacuum tightness is 7000Pa; The temperature of reaction that then prepolycondensate is transported to 10, the second precondensation stills 10 in the second precondensation still is 270 ℃, and the reaction times is 50 minutes, and vacuum tightness is 500Pa; Then prepolycondensate is transported in the whole polycondensation vessel 11, the temperature of reaction of whole polycondensation vessel 11 is 275 ℃, and the reaction times is 150 minutes, and vacuum tightness is 10Pa; Reaction finishes the back from discharge port 12 dischargings, and pelletizing, drying, makes copolyester section.The intrinsic viscosity of section is 0.604dL/g, and fusing point is 241.4 ℃.The hydrophilic copolyester section that makes behind crystallization in advance, drying, spinning process, is made the hydrophilic copolyester fiber, and its moisture regain is 1.45%.
Embodiment 21
With PTA with the input speed of 20000kg/h (120481.93mol/h) and EG with the input speed of 8590.36kg/h (138554.22mol/h), join making beating the making beating still 2 from opening for feed 1 respectively; Above-mentioned slurry is delivered in first esterifying kettle 4 continuously equably, and the temperature of reaction of first esterifying kettle 4 is 240 ℃, and the reaction times is 200 minutes; Be transported in second esterifying kettle 7 through transferpump again; Simultaneously; With the input speed of SIPE with 1287.8kg/h (3614.46mol/h), PPG10000 is with the input speed of 2000kg/h (200mol/h), 1 respectively; 2-PDO is with the input speed of 183.35kg/h (2409.64mol/h) per hour, TiO
2Input speed with 200kg/h (2503.76mol/h); The kg antimony acetate is with the input speed of 6kg/h (20.07mol/h) and the triphenylphosphate input speed with 4kg/h (12.26mol/h); Add to equably second esterifying kettle 7 from second opening for feed 6; The temperature of reaction of second esterifying kettle 7 is 250 ℃, and the reaction times is 90 minutes; Carboxylate is transported in the first precondensation still 8 through transferpump, and the temperature of reaction of the first precondensation still 8 is 265 ℃, and the reaction times is 45 minutes, and vacuum tightness is 7000Pa; The temperature of reaction that then prepolycondensate is transported to 10, the second precondensation stills 10 in the second precondensation still is 270 ℃, and the reaction times is 50 minutes, and vacuum tightness is 500Pa; Then prepolycondensate is transported in the whole polycondensation vessel 11, the temperature of reaction of whole polycondensation vessel 11 is 275 ℃, and the reaction times is 150 minutes, and vacuum tightness is 10Pa; Reaction finishes the back from discharge port 12 dischargings, and pelletizing, drying, makes copolyester section.The intrinsic viscosity of section is 0.600dL/g, and fusing point is 241.6 ℃.The hydrophilic copolyester section that makes behind crystallization in advance, drying, spinning process, is made the hydrophilic copolyester fiber, and its moisture regain is 1.42%.
Embodiment 22
With PTA with the input speed of 20000kg/h (120481.93mol/h) and EG with the input speed of 8590.36kg/h (138554.22mol/h), join making beating the making beating still 2 from opening for feed 1 respectively; Above-mentioned slurry is delivered in first esterifying kettle 4 continuously equably, and the temperature of reaction of first esterifying kettle 4 is 240 ℃, and the reaction times is 200 minutes; Be transported in second esterifying kettle 7 through transferpump again; Simultaneously; With the input speed of SIPE with 1287.8kg/h (3614.46mol/h), PBG4000 is with the input speed of 2000kg/h (500mol/h), 1 respectively; 2-PDO is with the input speed of 183.35kg/h (2409.64mol/h) per hour, TiO
2Input speed with 200kg/h (2503.76mol/h); Antimony acetate is with the input speed of 6kg/h (20.07mol/h) and the triphenylphosphate input speed with 4kg/h (12.26mol/h); Add to equably second esterifying kettle 7 from second opening for feed 6; The temperature of reaction of second esterifying kettle 7 is 250 ℃, and the reaction times is 90 minutes; Carboxylate is transported in the first precondensation still 8 through transferpump, and the temperature of reaction of the first precondensation still 8 is 265 ℃, and the reaction times is 45 minutes, and vacuum tightness is 7000Pa; The temperature of reaction that then prepolycondensate is transported to 10, the second precondensation stills 10 in the second precondensation still is 270 ℃, and the reaction times is 50 minutes, and vacuum tightness is 500Pa; Then prepolycondensate is transported in the whole polycondensation vessel 11, the temperature of reaction of whole polycondensation vessel 11 is 275 ℃, and the reaction times is 150 minutes, and vacuum tightness is 10Pa; Reaction finishes the back from discharge port 12 dischargings, and pelletizing, drying, makes copolyester section.The intrinsic viscosity of section is 0.599dL/g, and fusing point is 240.7 ℃.The hydrophilic copolyester section that makes behind crystallization in advance, drying, spinning process, is made the hydrophilic copolyester fiber, and its moisture regain is 1.50%.
Embodiment 23
With PTA with the input speed of 20000kg/h (120481.93mol/h) and EG with the input speed of 8590.36kg/h (138554.22mol/h), join making beating the making beating still 2 from opening for feed 1 respectively; Above-mentioned slurry is delivered in first esterifying kettle 4 continuously equably, and the temperature of reaction of first esterifying kettle 4 is 240 ℃, and the reaction times is 200 minutes; Be transported in second esterifying kettle 7 through transferpump again; Simultaneously; With the input speed of SIPE with 1287.8kg/h (3614.46mol/h), PBG6000 is with the input speed of 2000kg/h (333.33mol/h), 1 respectively; 2-PDO is with the input speed of 183.35kg/h (2409.64mol/h) per hour, TiO
2Input speed with 200kg/h (2503.76mol/h); The kg antimony acetate is with the input speed of 6kg/h (20.07mol/h) and the triphenylphosphate input speed with 4kg/h (12.26mol/h); Add to equably second esterifying kettle 7 from second opening for feed 6; The temperature of reaction of second esterifying kettle 7 is 250 ℃, and the reaction times is 90 minutes; Carboxylate is transported in the first precondensation still 8 through transferpump, and the temperature of reaction of the first precondensation still 8 is 265 ℃, and the reaction times is 45 minutes, and vacuum tightness is 7000Pa; The temperature of reaction that then prepolycondensate is transported to 10, the second precondensation stills 10 in the second precondensation still is 270 ℃, and the reaction times is 50 minutes, and vacuum tightness is 500Pa; Then prepolycondensate is transported in the whole polycondensation vessel 11, the temperature of reaction of whole polycondensation vessel 11 is 275 ℃, and the reaction times is 150 minutes, and vacuum tightness is 10Pa; Reaction finishes the back from discharge port 12 dischargings, and pelletizing, drying, makes copolyester section.The intrinsic viscosity of section is 0.601dL/g, and fusing point is 241.2 ℃.The hydrophilic copolyester section that makes behind crystallization in advance, drying, spinning process, is made the hydrophilic copolyester fiber, and its moisture regain is 1.48%.
Embodiment 24
With PTA with the input speed of 20000kg/h (120481.93mol/h) and EG with the input speed of 8590.36kg/h (138554.22mol/h), join making beating the making beating still 2 from opening for feed 1 respectively; Above-mentioned slurry is delivered in first esterifying kettle 4 continuously equably, and the temperature of reaction of first esterifying kettle 4 is 240 ℃, and the reaction times is 200 minutes; Be transported in second esterifying kettle 7 through transferpump again; Simultaneously; With the input speed of SIPE with 1287.8kg/h (3614.46mol/h), PBG10000 is with the input speed of 2000kg/h (200mol/h), 1 respectively; 2-PDO is with the input speed of 183.35kg/h (2409.64mol/h) per hour, TiO
2Input speed with 200kg/h (2503.76mol/h); The kg antimony acetate is with the input speed of 6kg/h (20.07mol/h) and the triphenylphosphate input speed with 4kg/h (12.26mol/h); Add to equably second esterifying kettle 7 from second opening for feed 6; The temperature of reaction of second esterifying kettle 7 is 250 ℃, and the reaction times is 90 minutes; Carboxylate is transported in the first precondensation still 8 through transferpump, and the temperature of reaction of the first precondensation still 8 is 265 ℃, and the reaction times is 45 minutes, and vacuum tightness is 7000Pa; The temperature of reaction that then prepolycondensate is transported to 10, the second precondensation stills 10 in the second precondensation still is 270 ℃, and the reaction times is 50 minutes, and vacuum tightness is 500Pa; Then prepolycondensate is transported in the whole polycondensation vessel 11, the temperature of reaction of whole polycondensation vessel 11 is 275 ℃, and the reaction times is 150 minutes, and vacuum tightness is 10Pa; Reaction finishes the back from discharge port 12 dischargings, and pelletizing, drying, makes copolyester section.The intrinsic viscosity of section is 0.604dL/g, and fusing point is 241.8 ℃.The hydrophilic copolyester section that makes behind crystallization in advance, drying, spinning process, is made the hydrophilic copolyester fiber, and its moisture regain is 1.46%.
The recipe ingredient of embodiment 1-24 is as shown in table 1:
Table 1
Annotate: in the table 1, wt% is add component and pure terephthalic acid's weight ratio; Mol% is add component and pure terephthalic acid's mol ratio.
The hydrophilic copolyester section that embodiment 1-24 makes is tested its performance by GB/T 14189-2008, and the hydrophilic copolyester fiber that embodiment 1-24 makes is by its performance of GB/T 6503-2008 test, and data are as shown in table 2:
Table 2
Embodiment 25
As shown in Figure 2, be the molecular structure of the hydrophilic copolyester section that adopts the preparation method preparation that provides of the present invention.This section mainly is made up of pure terephthalic acid, terepthaloyl moietie, benzene diprotic acid binary alcohol esters-5-sodium sulfonate, poly-dihydric alcohol and other divalent alcohol.Wherein, benzene diprotic acid dibasic ester-5-sodium sulfonate is selected ethylene isophthalate-5-sodium sulfonate for use; Poly-dihydric alcohol is selected polyoxyethylene glycol for use; Other divalent alcohol selects 1 for use, the 2-Ucar 35.
Among the figure, X is the molar content of ethylene isophthalate-5-sodium sulfonate, is 1.5-6% for pure terephthalic acid's molar percentage; Y is the mass content of polyoxyethylene glycol, is 1-30% for pure terephthalic acid's mass percent; Z is 1, and the molar content of 2-Ucar 35 is 0.5-8% for pure terephthalic acid's molar percentage.Wherein, separate between X, Y, the Z; N is the polymerization degree of polyoxyethylene glycol.
Claims (15)
1. the preparation method of the hydrophilic copolyester section of a continuous processing preparation is characterized in that, may further comprise the steps:
The first step: will be input to equably continuously with transferpump with pure terephthalic acid 1, terepthaloyl moietie 1.1-2.5, a benzene diprotic acid dibasic ester-5-sodium sulfonate 0.015-0.06, poly-dihydric alcohol 0.000166-0.01245, other divalent alcohol 0.005-0.08, matting agent 0.0104-0.0416, catalyzer 0.00007836-0.0005125 and the thermo-stabilizer 0.00004659-0.0007111 of molar ratio computing and carry out esterification in the esterifying kettle;
Second step: the carboxylate that the first step is obtained is transported to and carries out prepolymerization reaction in the precondensation still;
The 3rd step: second prepolycondensate that obtain of step is transported to carries out polycondensation in the whole polycondensation vessel;
The 4th step: go on foot polycondensate discharging, pelletizing, the drying that obtains with the 3rd.
2. the preparation method of the hydrophilic copolyester section of a kind of continuous processing preparation as claimed in claim 1 is characterized in that described benzene diprotic acid binary alcohol esters-5-sodium sulfonate is ethylene isophthalate-5-sodium sulfonate.
3. the preparation method of the hydrophilic copolyester section of a kind of continuous processing preparation as claimed in claim 1 is characterized in that described poly-dihydric alcohol is polyoxyethylene glycol, W 166 or polytetramethylene glycol, and number-average molecular weight is 4000-10000.
4. the preparation method of the hydrophilic copolyester section of a kind of continuous processing preparation as claimed in claim 3 is characterized in that the number-average molecular weight of described polyoxyethylene glycol is 5000-7000; The number-average molecular weight of W 166 is 4000-6000; The number-average molecular weight of polytetramethylene glycol is 4000-6000.
5. the preparation method of the hydrophilic copolyester section of a kind of continuous processing preparation as claimed in claim 1 is characterized in that described other divalent alcohol is 1,2-Ucar 35,1; Ammediol, 1,2-butyleneglycol, 1,3 butylene glycol, 1; 4-butyleneglycol, 1,2-pentanediol or 1,5-pentanediol.
6. the preparation method of the hydrophilic copolyester section of a kind of continuous processing preparation as claimed in claim 5 is characterized in that described other divalent alcohol is 1,2-Ucar 35,1,2-butyleneglycol or 1,2-pentanediol.
7. the preparation method of the hydrophilic copolyester section of a kind of continuous processing preparation as claimed in claim 1 is characterized in that described matting agent is a titania powder.
8. the preparation method of the hydrophilic copolyester section of a kind of continuous processing preparation as claimed in claim 1 is characterized in that described catalyzer is antimony glycol, antimony acetate or Antimony Trioxide: 99.5Min.
9. the preparation method of the hydrophilic copolyester section of a kind of continuous processing preparation as claimed in claim 1 is characterized in that described thermo-stabilizer is triphenylphosphate or trimethyl phosphite 99.
10. the preparation method of the hydrophilic copolyester section of a kind of continuous processing preparation as claimed in claim 1; It is characterized in that; The concrete steps of the esterification in the described the first step are: will join with pure terephthalic acid 1, terepthaloyl moietie 1.1-2.5, other divalent alcohol 0.005-0.08 of molar ratio computing in the making beating still and pull an oar; After being delivered to the reaction of first esterifying kettle then equably; Be delivered in second esterifying kettle, a benzene diprotic acid dibasic ester-5-sodium sulfonate 0.015-0.06, poly-dihydric alcohol 0.000166-0.01245, matting agent 0.0104-0.0416, catalyzer 0.00007836-0.0005125 and thermo-stabilizer 0.00004659-0.0007111 added in second esterifying kettle continuously equably react simultaneously.
11. the preparation method of the hydrophilic copolyester section of a kind of continuous processing preparation as claimed in claim 1; It is characterized in that; The concrete steps of the esterification in the described the first step are: will join with pure terephthalic acid 1, the terepthaloyl moietie 1.1-2.5 of molar ratio computing in the making beating still and pull an oar; Then; After being delivered to the reaction of first esterifying kettle equably; Be delivered in second esterifying kettle, a benzene diprotic acid dibasic ester-5-sodium sulfonate 0.015-0.06, poly-dihydric alcohol 0.000166-0.01245, other divalent alcohol 0.005-0.08, matting agent 0.0104-0.0416, catalyzer 0.00007836-0.0005125 and thermo-stabilizer 0.00004659-0.0007111 added in second esterifying kettle continuously equably react simultaneously.
12. the preparation method like the hydrophilic copolyester section of claim 10,11 described a kind of continuous processings preparations is characterized in that the temperature of reaction of described first esterifying kettle is 240-260 ℃, the reaction times is 90-240 minute; The temperature of reaction of second esterifying kettle is 242-265 ℃, and the reaction times is 60-120 minute.
13. the preparation method of the hydrophilic copolyester section of a kind of continuous processing preparation as claimed in claim 1; It is characterized in that; The concrete steps of prepolymerization reaction in described second step are: the carboxylate that the first step is obtained is transported in the first precondensation still after the reaction, is transported in the second precondensation still and reacts.
14. the preparation method of the hydrophilic copolyester section of a kind of continuous processing preparation as claimed in claim 13 is characterized in that the temperature of reaction of the described first precondensation still is 260-275 ℃, the reaction times is 30-60 minute, and vacuum tightness is 5000-9000Pa; The temperature of reaction of the second precondensation still is 262-275 ℃, and the reaction times is 35-60 minute, and vacuum tightness is 500-1500Pa.
15. the preparation method of the hydrophilic copolyester section of a kind of continuous processing preparation as claimed in claim 1 is characterized in that the temperature of reaction of described whole polycondensation vessel is 265-280 ℃, the reaction times is 120-200 minute, and vacuum tightness is 0-50Pa.
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