CN110438583A - A kind of polyester fiber and preparation method thereof - Google Patents
A kind of polyester fiber and preparation method thereof Download PDFInfo
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- CN110438583A CN110438583A CN201810407521.7A CN201810407521A CN110438583A CN 110438583 A CN110438583 A CN 110438583A CN 201810407521 A CN201810407521 A CN 201810407521A CN 110438583 A CN110438583 A CN 110438583A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
- C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
- C08G63/181—Acids containing aromatic rings
- C08G63/183—Terephthalic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
- C08G63/82—Preparation processes characterised by the catalyst used
- C08G63/85—Germanium, tin, lead, arsenic, antimony, bismuth, titanium, zirconium, hafnium, vanadium, niobium, tantalum, or compounds thereof
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Polyesters Or Polycarbonates (AREA)
- Artificial Filaments (AREA)
Abstract
The present invention provides a kind of polyester fibers and preparation method thereof, and addition hyper-branched polyester progress melt spinning obtains polyester fiber after polyester is produced under the conditions of Titanium series catalyst.After hyper-branched polyester is added in the present invention, since hyperbranched poly ester molecule has a large amount of terminal hydroxy groups, so that catalyst metal atom is also coordinated with the ester carbonyl group oxygen in hyperbranched poly ester terminal while coordination with oxygen on ester carbonyl group in polyester PET macromolecular chain, the activity that hyper-branched polyester of the present invention inhibits titanium catalyst later is added, so that the extent of thermal degradation of post-processing spinning process polyester substantially reduces, solves titanium polyester post-processing process viscosity because caused by thermal degradation is big and drop the problems such as more, the preceding spinning spinnability of large and small molecule precipitation is poor.Pass through the restraining function with catalyst metal atom coordination to backbone plus hyper-branched polyester simultaneously, and hyper-branched polyester reticular structure causes the amorphous region of gained fiber to increase the inhibition of PET polyester macromolecule chain, when alkali decrement treatment, reduction rate improves, and reduces production energy consumption.
Description
Technical field
The present invention relates to a kind of fibers, and in particular to a kind of polyester fiber and preparation method thereof.
Background technique
Polyester fiber is with PET polyester through fiber made of spinning and post-processing, and PET polyester mainly uses direct ester at present
Change method is synthesized, and direct esterification is with terephthalic acid (TPA) (PTA) and ethylene glycol (EG) for raw material, and direct esterification dehydration generates
Bishydroxyethyl terephthalate (BHET), polycondensation takes off EG generation PET or dehydration generation PET occurs with carboxyl end group BHET again.
Different catalysts catalyzed polycondensation and the rate constant of degradation are different, and it is fireballing that titanium compound is catalyzed positive reaction
Meanwhile the speed of catalytic degradation is also fast.Why to polycondensation reaction catalytic activity with higher, mainly due to titanium and BHET
The coordination ability of ester carbonyl group oxygen is stronger, thus shows very high activity.Titanium compound is equally because match ester carbonyl group oxygen
Capability is relatively strong and thermal degradation reaction is made to be easy to carry out.The products such as long filament, short fibre, film are carried out after titanium polyester melting at present
Preparation process, since its thermal stability is poor, when production and processing always exist melt viscosity drop large and small molecule more, preceding spinning is precipitated can
The property spun is poor, and irregular lumps is more when spinning spinning before being embodied in, and causes periodically to repair the raising of plate frequency, irregularly increase, seriously
When the problems such as causing curling round the roll because of lumps problem.The mode of generally addition heat stabilizer is subject in order to solve this problem in industry at present
Improve, but effect is less desirable.
In addition, the hygroscopicity and wearability of traditional dacron are poor, whether ordinary polyester or super fine polyester are knitted
Object, all processing Silk-Like Polyesters will carry out alkali decrement treatment, so that fabric is reached the feel of Silk, meet taking
The requirement of the indices such as energy.Caustic reduction processing, which refers to, handles dacron in high temperature and denseer soda bath, after processing,
Fiber attenuates, and moisture absorption regain improves, intensity decline.
Alkali decrement treatment brings many merits to dacron, but the waste water COD concentration of Alkali reduction process discharge may be up to
90000mg/L, pH value are up to 13 or more, containing a large amount of TA (terephthalic acid (TPA)) or its sodium salt and on a small quantity with Bu Tong poly- in waste water
Right existing polymer.Alkali decrement waste water can recycle most of TA by the treatment processes such as acid out, but still containing TA and
Macromolecule organic belongs to high concentration hard-degraded organic waste water, the alkali-minimization dyeing wastewater formed after being mixed with dyeing waste water at
Divide complicated, COD concentration height, pH value height, biodegradability poor.
Currently, there are mainly two types of the alkali deweightings of conventional polyester fabric: first is that high-temperature high-pressure craft, processing temperature is general
Greater than 100 DEG C, to the more demanding of equipment；Another kind is atmospheric processes, and processing temperature is generally also greater than 95 DEG C, and to lye
Concentration and the dosage of promotor are more demanding.As can be seen that current alkali deweighting method, one side energy consumption is high, another party
The contaminated wastewater that face process generates is serious.
Summary of the invention
Goal of the invention: in view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a kind of polyester fiber and its preparation
Method asks the thermal degradation of gained titanium polyester post-processing process using the collective effect of Titanium series catalyst and hyper-branched polyester
Topic is greatly improved, and the reduction rate of gained fiber is improved, and can weaken caustic reduction processing, energy-saving, reduces simultaneously
Alkali decrement waste water is to the pollution level of environment, and polyester use environment friendly titanium polyester of the present invention, eliminates a huge sum of money
Harm of the metal catalyst to environment and human body.
Technical solution: a kind of polyester fiber, addition hyper-branched polyester carries out after polyester is produced under the conditions of Titanium series catalyst
Melt spinning obtains.
A kind of preparation method of polyester fiber using binary acid and dihydric alcohol as primary raw material, and is added Titanium series catalyst, is adopted
With direct esterification raw materials for production polyester, mixing hyper-branched polyester carries out melt spinning after obtaining Starting Material Polyester.
Further, the Titanium series catalyst is STiC-01.
Further, the additive amount of the Titanium series catalyst is 5-10mg/kg relative to the accounting of Starting Material Polyester quality.
Further, the Titanium series catalyst is added before esterification or after esterification.
Further, the production process of polyester includes esterification, prepolymerization reaction and final polycondensation reaction；Wherein esterification temperature
255 DEG C~265 DEG C, pressure is normal pressure；270 DEG C~278 DEG C of precondensation temperature, pressure 2KPa~24KPa；Whole condensation temperature 278
DEG C~283 DEG C, pressure 90Pa~150Pa；By pelletizing, drying, polyester slice is made.
Further, the additive amount of the hyper-branched polyester accounts for the 1~5% of Starting Material Polyester quality.
Further, delustering agent TiO is added after esterification2, additive amount accounts for the 0.3% of Starting Material Polyester quality.
Further, using slice indirectly spin FDY filament preparation process: by Starting Material Polyester be sliced dry, and with it is dried
Hyper-branched polyester mixing carries out spinning through spinneret, spinning process adds hyper-branched polyester after squeezing out fusion plastification；Screw rod
285-300 DEG C of temperature, 282-288 DEG C of spinning body temperature, 20-25 DEG C of cooling wind temperature, 90-95 DEG C of drawing temperature, setting temperature
160-165 DEG C, winding speed 4500-4800m/min.
Further, the hyper-branched polyester is to pass through A2+B3System is made by polycondensation reaction, has fragrance-lard type point
Sub- skeleton structure, using M-phthalic acid and trimethylolpropane as raw material, p-methyl benzenesulfonic acid is catalyst, at 120-150 DEG C
It is prepared by condensation, the hyper-branched polyester number average molecular weight 3000-5000 of preparation, end group is hydroxyl.
Inventive principle: after hyper-branched polyester is added in the present invention, since hyperbranched poly ester molecule has a large amount of terminal hydroxy groupsSo that catalyst metal atom and oxygen on ester carbonyl group in polyester PET macromolecular chain
It is also coordinated with the ester carbonyl group oxygen in hyperbranched poly ester terminal while coordination:
It is added of the present invention hyperbranched
The activity of titanium catalyst is inhibited after polyester, so that the extent of thermal degradation of post-processing spinning process polyester substantially reduces, is solved
Titanium polyester post-processing process viscosity because caused by thermal degradation is big, which drops large and small molecule more, preceding spinning spinnability difference etc. is precipitated, asks
Topic.Simultaneously plus hyper-branched polyester by with catalyst metal atom coordination to the restraining function of backbone and hyperbranched
Polyester mesh structure causes the amorphous region of gained fiber to increase, alkali decrement treatment the inhibition of PET polyester macromolecule chain
When, reduction rate improves, or while reaching the reduction rate of pure titanium system fabric can obviously weaken caustic reduction processing, reduce production energy consumption.
The utility model has the advantages that when (1) is using polyester mixture melt spinning post-processing of the present invention, it is poly- compared to using pure titanium system
When ester, extent of thermal degradation is greatly decreased, specific manifestation are as follows: oil-free silk viscosity drop reduces, and is reduced to 0.02- by 0.030dL/g
0.01dL/g, range of decrease 33.3-66.6%.Spinnability improvement is further shown as, specifically: preceding spinning small molecule, which is precipitated, to be reduced, no
Plate reduction is periodically repaired, irregular average value is reduced to 1-4 times/day by 6 times/day, periodically repairs plate frequency by 1 time/12h and extend to 1
Secondary 24-60h.
(2) suspenders being made into simultaneously using the FDY filament of mixture production of polyester of the present invention compares pure titanium system terylene
Product, under identical caustic reduction processing, 14-60% is can be improved in reduction rate.
Specific embodiment
Technical solution of the present invention is described in detail below, but protection scope of the present invention is not limited to the implementation
Example.
Embodiment:
Comparative example: carrying out the preparation of titanium polyester slice first, then carry out the preparation of FDY filament, specifically: spinning institute
It is 30,000 tons/year of five autoclaves process polyester device productions with polyester raw material, binary acid is p-phthalic acid, and dihydric alcohol is ethylene glycol,
Molar ratio of alcohol to acid is 1.1:1, product type be it is semi-dull, used catalyst is STiC-01 Titanium series catalyst, addition before being esterified,
Additive amount is 5mg/kg (relative to polyester PET quality)；Delustering agent TiO2It is added after esterification, additive amount 0.3% is (relative to polyester
PET mass).Concrete technology is the first 265 DEG C of esterifying kettle temperature, and 262 DEG C of second esterification kettle temperature, esterification process is normal pressure ester
Change；First 273 DEG C of preshrunk kettle temperature degree, pressure 24KPa, the second 278 DEG C of preshrunk kettle temperature degree, pressure 4KPa；Whole condensation temperature 283
DEG C, pressure 150Pa.By pelletizing, drying, obtained polyester slice carries out the preparation that slice spins FDY filament, specifically: screw rod one
Area~six area's temperature are respectively 285 DEG C, 288 DEG C, 290 DEG C, 293 DEG C, 295 DEG C, 300 DEG C, 288 DEG C of spinning body temperature, are cooled down
23 DEG C of wind-warm syndrome, wind speed: 1.2m/s, 95 DEG C of drawing temperature, 160 DEG C of setting temperature, winding speed 4500m/min.Without silk noil viscosity
It is reduced to 0.03dL/g, the average plate number of irregularly repairing of 24 spinning stations of single line is 6 times/day, and periodically repairing the plate period is 1 time/12 small
When.
Next the FDY filament of above-mentioned preparation is made into suspenders on dye test braider (model KU483B), then
Alkali reduction test is carried out by following alkali deweighting technique: alkali deweighting is carried out to it with sodium hydroxide using impregnation technology,
Alkali deweighting process flow are as follows: sodium hydroxide is made into the solution that concentration is 20g/L, pure titanium system suspenders is then put into lye
In, then Alkali reduction bath raio 1:50 is warming up to 100 DEG C with the heating rate of 3.75 DEG C/min, 60min is kept the temperature, after heat preservation
Suspenders is taken out with originally washing 3 times, dry 1h is subsequently placed in 60 DEG C of convection ovens, then be warming up to 105 DEG C of baking 4h, then in electricity
It weighs rapidly on sub- balance, (1) calculates reduction rate as follows:
Embodiment 1: polymerization, spinning technique, alkali deweighting process route are identical as comparative example, except that when polymerization
Concrete technology is the first 265 DEG C of esterifying kettle temperature, 262 DEG C of second esterification kettle temperature；First 273 DEG C of preshrunk kettle temperature degree, pressure
24KPa, the second 278 DEG C of preshrunk kettle temperature degree, pressure 4KPa；283 DEG C of whole condensation temperature, pressure 150Pa.Addition accounts for polyester when spinning
The hyper-branched polyester of quality 1%, hyper-branched polyester number average molecular weight 3000.One area of screw rod~six area's temperature are respectively 285 DEG C,
288 DEG C, 290 DEG C, 293 DEG C, 295 DEG C, 300 DEG C, 288 DEG C of spinning body temperature, 25 DEG C of cooling wind temperature, wind speed: 1.2m/s, drawing-off
95 DEG C of temperature, 160 DEG C of setting temperature, winding speed 4500m/min.No silk noil viscosity is reduced to 0.02dL/g, 24 spinning of single line
The average plate number of irregularly repairing in position is 4 times/day, and periodically repairing the plate period is 1 time/24 hours.
Embodiment 2: polymerization, spinning technique, alkali deweighting process route are identical as comparative example, except that when polymerization
Concrete technology is to add after catalyst esterification, the first 265 DEG C of esterifying kettle temperature, 261 DEG C of second esterification kettle temperature；First preshrunk
272 DEG C of kettle temperature degree, pressure 20KPa, the second 277 DEG C of preshrunk kettle temperature degree, pressure 3KPa；282 DEG C of whole condensation temperature, pressure 140Pa.
Addition accounts for the hyper-branched polyester of polyester quality 2%, hyper-branched polyester number average molecular weight 3500 when spinning.One area of screw rod~six Qu Wen
Degree is respectively 285 DEG C, 286 DEG C, 288 DEG C, 290 DEG C, 291 DEG C, 295 DEG C, 285 DEG C of spinning body temperature, 23 DEG C of cooling wind temperature, is led
Stretch 95 DEG C of temperature, 162 DEG C of setting temperature, winding speed 4600m/min.No silk noil viscosity is reduced to 0.015dL/g, 24, single line spinnings
The average plate number of irregularly repairing in silk position is 3 times/day, and periodically repairing the plate period is 1 time/36 hours.
Embodiment 3: polymerization, spinning technique, alkali deweighting process route are identical as comparative example, except that when polymerization
Concrete technology is catalyst loading 7mg/kg, the first 263 DEG C of esterifying kettle temperature, 259 DEG C of second esterification kettle temperature；First is pre-
271 DEG C of contracting kettle temperature degree, pressure 22KPa, the second 276 DEG C of preshrunk kettle temperature degree, pressure 3KPa；280 DEG C of whole condensation temperature, pressure
100Pa.Addition accounts for the hyper-branched polyester of polyester quality 3.5%, hyper-branched polyester number average molecular weight 4000 when spinning.One area of screw rod
~six area's temperature are respectively 285 DEG C, 286 DEG C, 287 DEG C, 289 DEG C, 291 DEG C, 293 DEG C, and 285 DEG C of spinning body temperature, cooling wind
22 DEG C of temperature, 92 DEG C of drawing temperature, 164 DEG C of setting temperature, winding speed 4700m/min.No silk noil viscosity is reduced to 0.010dL/g,
The average plate number of irregularly repairing of 24 spinning stations of single line is 2 times/day, and periodically repairing the plate period is 1 time/48 hours.
Embodiment 4: polymerization, spinning technique, alkali deweighting process route are identical as comparative example, except that when polymerization
Concrete technology is catalyst loading 10mg/kg, the first 260 DEG C of esterifying kettle temperature, 255 DEG C of second esterification kettle temperature；First is pre-
270 DEG C of contracting kettle temperature degree, pressure 20KPa, the second 274 DEG C of preshrunk kettle temperature degree, pressure 2KPa；278 DEG C of whole condensation temperature, pressure
90Pa.Addition accounts for the hyper-branched polyester of polyester quality 5%, hyper-branched polyester number average molecular weight 5000 when spinning.One area of screw rod~
Six area's temperature are respectively 285 DEG C, 285 DEG C, 286 DEG C, 288 DEG C, 289 DEG C, 292 DEG C, and 282 DEG C of spinning body temperature, cooling wind temperature
20 DEG C, 90 DEG C of drawing temperature, 165 DEG C of setting temperature, winding speed 4800m/min.No silk noil viscosity is reduced to 0.010dL/g, single
The average plate number of irregularly repairing of 24 spinning stations of line is 1 times/day, and periodically repairing the plate period is 1 time/60 hours.
Comparative example and the preparation of Examples 1 to 4 fiber and alkali deweighting data see the table below:
Claims (10)
1. a kind of polyester fiber, it is characterised in that: addition hyper-branched polyester carries out after producing polyester under the conditions of Titanium series catalyst
Melt spinning obtains.
2. a kind of preparation method of polyester fiber, it is characterised in that: using binary acid and dihydric alcohol as primary raw material, and add titanium system
Catalyst, using direct esterification raw materials for production polyester, mixing hyper-branched polyester carries out melt spinning after obtaining Starting Material Polyester.
3. the preparation method of polyester fiber according to claim 2, it is characterised in that: the Titanium series catalyst is STiC-
01。
4. the preparation method of polyester fiber according to claim 2 or 3, it is characterised in that: the Titanium series catalyst adds
Dosage is 5-10mg/kg relative to the accounting of Starting Material Polyester quality.
5. the preparation method of polyester fiber according to claim 2 or 3, it is characterised in that: the Titanium series catalyst is in ester
It is added before changing or after esterification.
6. the preparation method of polyester fiber according to claim 2, it is characterised in that: the production process of polyester includes esterification
Reaction, prepolymerization reaction and final polycondensation reaction；Wherein 255 DEG C ~ 265 DEG C of esterification temperature, pressure is normal pressure；Precondensation temperature 270
DEG C ~ 278 DEG C, pressure 2KPa ~ 24KPa；278 DEG C ~ 283 DEG C of whole condensation temperature, pressure 90Pa ~ 150Pa；By pelletizing, drying, system
Obtain polyester slice.
7. the preparation method of polyester fiber according to claim 2, it is characterised in that: the additive amount of the hyper-branched polyester
Account for the 1 ~ 5% of Starting Material Polyester quality.
8. the preparation method of polyester fiber according to claim 2, it is characterised in that: add delustering agent after esterification
TiO2, additive amount accounts for the 0.3% of Starting Material Polyester quality.
9. the preparation method of polyester fiber according to claim 6, it is characterised in that: spin FDY filament indirectly using slice
Preparation process: Starting Material Polyester being sliced and is dried, and is mixed with dried hyper-branched polyester, after squeezing out fusion plastification, warp
Spinneret carries out spinning, and spinning process adds hyper-branched polyester；285-300 DEG C of extruder temperature, 282-288 DEG C of spinning body temperature,
20-25 DEG C of cooling wind temperature, 90-95 DEG C of drawing temperature, 160-165 DEG C of setting temperature, winding speed 4500-4800m/min.
10. the preparation method of polyester fiber according to claim 2, it is characterised in that: the hyper-branched polyester is to pass through A2
+B3System is made by polycondensation reaction, has fragrance-lard type molecular structure, with M-phthalic acid and trihydroxy methyl third
Alkane is raw material, and p-methyl benzenesulfonic acid is catalyst, passes through condensation preparation, the hyper-branched polyester data point of preparation at 120-150 DEG C
Son amount 3000-5000, end group is hydroxyl.
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| CN114574981A (en) * | 2021-12-07 | 2022-06-03 | 浙江恒逸高新材料有限公司 | Preparation method of polyester staple fiber special for vortex spinning |
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| CN114574981B (en) * | 2021-12-07 | 2023-02-28 | 浙江恒逸高新材料有限公司 | Preparation method of polyester staple fiber special for vortex spinning |
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