CN109252243A - A kind of copolymerization preparation method of porous polyester fiber - Google Patents
A kind of copolymerization preparation method of porous polyester fiber Download PDFInfo
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- CN109252243A CN109252243A CN201810924581.6A CN201810924581A CN109252243A CN 109252243 A CN109252243 A CN 109252243A CN 201810924581 A CN201810924581 A CN 201810924581A CN 109252243 A CN109252243 A CN 109252243A
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- Prior art keywords
- esterification
- polyester fiber
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- raw material
- temperature
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Classifications
-
- 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
-
- 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
- C08G63/68—Polyesters containing atoms other than carbon, hydrogen and oxygen
- C08G63/685—Polyesters containing atoms other than carbon, hydrogen and oxygen containing nitrogen
-
- 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
- C08G63/68—Polyesters containing atoms other than carbon, hydrogen and oxygen
- C08G63/688—Polyesters containing atoms other than carbon, hydrogen and oxygen containing sulfur
-
- 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
-
- 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
- D01F1/07—Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments
Abstract
The invention discloses a kind of copolymerization preparation methods of porous polyester fiber, include the following steps: S100, raw material preparation, and the raw material prepared will be needed to be deployed after mixing in proportion and dried for the first time；Part material after drying is added reaction kettle of the esterification and carries out esterification by S200, esterification treatment；S300, polymerization reaction carry out redrying after esterification completion, and feed modified copolymer；S400, preparation is blended, fire-retardant master granule is added in obtained raw material, mixing is blended, spinning moulding, after by above-mentioned preparation step, obtained porous polyester fiber has good hydrophily and anti-flammability, and while performance reaches requirement in all respects, it is effectively improved its uvioresistant and ageing resistance, there is good service performance.
Description
Technical field
The present invention relates to polyester fiber manufacture technology field, specially a kind of copolymerization preparation method of porous polyester fiber.
Background technique
Polyester fiber is commonly called as " terylene ", is the polyester as made of organic dibasic acid and dihydric alcohol polycondensation through the resulting conjunction of spinning
At fiber, abbreviation PET fiber invents in nineteen forty-one, is the first big kind of current synthetic fibers, polyester fiber biggest advantage
It is that wrinkle resistance and conformality are fine, intensity with higher and elastic recovery capability.Its strong durable, wash and wear, not adhesive hair.
Nineteen forty-one, the J.R. Weinfield and J.T. Dixon of Britain are being tested using terephthalic acid (TPA) and ethylene glycol as raw material
Polyester fiber is succeeded in developing in interior first, is named as terylene (Terylene), and nineteen fifty-three trade name produced in USA reaches can synthetic fibre
(Dacron) polyester fiber, subsequent polyester fiber are rapidly developed in countries in the world, and is produced from the world of nineteen sixty polyester fiber
Amount is more than polyacrylonitrile fibre, and 1972 are more than again Fypro, becomes the first big kind of synthetic fibers, refers to by a variety of two
The polyester that first pure and mild aromatic binary carboxylic acid or its ester are generated through polycondensation is the general designation of fiber obtained by raw material.
Since dacron fibre is its principal item, therefore practises and polyester fiber is claimed to refer to this fiber.This
Fiber appearance is well-pressed, and thermal stability is good, but hygroscopicity is slightly worse, they be mainly used for making various clothing articles, bedding,
Upholstery etc.；Individual plants are such as: poly- two ester fiber of 2,6- naphthalene diacid second is mainly used for industrial aspect.
But the polyester fiber typically now produced is not very well, actually to make due to its anti-uv-ray and anti-flammability
The used time problem serious it is easy to appear aging leads to the reduction of polyester fiber service life, and its hydrophily is bad is easy to
Its surface is caused to be difficult to clean.
Summary of the invention
In order to overcome the shortcomings of that prior art, the present invention provide a kind of copolymerization preparation method of porous polyester fiber,
Porous polyester fiber obtained has good hydrophily and anti-flammability, and while performance reaches requirement in all respects, has
Effect improves its uvioresistant and ageing resistance, has good service performance, can effectively solve asking for background technique proposition
Topic.
The technical solution adopted by the present invention to solve the technical problems is:
A kind of copolymerization preparation method of porous polyester fiber, includes the following steps:
S100, raw material preparation, it would be desirable to which the raw material of preparation is dried for the first time after deploying mixing in proportion；
Part material after drying is added reaction kettle of the esterification and carries out esterification by S200, esterification treatment；
S300, polymerization reaction carry out redrying after esterification completion, and feed modified copolymer；
S400, preparation is blended, fire-retardant master granule is added in obtained raw material, mixing, spinning moulding is blended.
Further, in the step S100, the raw material of required preparation include PTA, triphenyl phosphate, titanium dioxide,
Double benzoxazoles talan, anion polyester master particle, Third monomer M-phthalic acid diethyl alcohol ester -5- sodium sulfonate.
Further, primary drying process uses 10~20min of heated-air drying after raw material mixing, and drying temperature control exists
110~135 DEG C.
Further, in the step S200, detailed process is as follows for esterification:
Reaction kettle of the esterification is heated by Electric heating first, temperature reaches 230~250 DEG C, and pressure is 0.3~
0.4MPa, controlling the fractionation capital temperature inside reaction kettle of the esterification is 125~130 DEG C；
The theoretical water yield of raw material reaction is calculated, and detects the water yield of real reaction, reaches theoretical in detection water yield
When water yield 80%, start pressure release to reach normal condition；
After pressure release terminates, when water yield reaches theoretical water yield 90%, be added the 4th monomer polyethylene glycol and
5th monomer hydrophilic agent continues 50~60min of esterification, until esterification is completed.
Further, in esterification, judge that the condition that esterification is completed is that detection water yield reaches 95% or more.
Further, in the step S300, redrying process is as follows:
In the pre-crystallized stage, treated, and raw material heats 8~15min in ebullated bed, and temperature is 160~180 DEG C, drops later
For low temperature to 125~145 DEG C, stirring-type fills 1~1.5h；
In the high temperature drying stage, rotary-drum vacuum is dry, and temperature continues 10~20min at 120~140 DEG C.
Further, in the step S300, modified copolymer includes the following steps:
Start the decompression that vacuumizes and heat up, within 42~47min time, reaction kettle of the esterification internal temperature improves to 250~
260 DEG C, while reaction kettle of the esterification internal vacuum reaches 60Pa or less；
It is separately added into antioxidant, delustering agent and antimony acetate, reacts 110~130min under the above conditions；
It is stirred within the set time with setting power, until reaching setting time, stops stirring, nitrogen vacuum breaker is simultaneously
Discharging, obtains polyester slice.
Further, in the step S400, the fire-retardant master granule ratio of obtained raw material and addition is 100:7~13, tool
Body mixing step is as follows:
The pre-crystallized 5h under 130~135 DEG C of vacuum condition；
Subsequent to be warming up to 145~150 DEG C, dry 12~16h obtains blended slice；
Spinning on obtained blended slice twin-screw high speed compound spinning machine, spinning temperature are 250~270 DEG C.
Further, as-spun fibre 6~8h of balance after spinning is completed, drawing-off processing is carried out on parallel drafting machine.
Further, the condition of drawing-off processing are as follows: 65 DEG C of heat roller temperature, 150 DEG C of setting temperature, draft speed 300m/
Min, drafting multiple 3.2.
Compared with prior art, the beneficial effects of the present invention are:
By adding double benzoxazoles talan in the present invention, while guaranteeing polyester fiber basic nature energy, effectively
Its anti-uv-ray and ageing resistance are improved, while by blending polymerization between fire-retardant master granule and molding materials, into one
Step improves the fire retardancy of molding of polyester fiber, while Third monomer M-phthalic acid diethyl alcohol ester -5- sodium sulfonate, the 4th monomer
The addition of polyethylene glycol and the 5th monomer hydrophilic agent effectively enhances the hydrophily of Finished polyester fiber, so that its surface cleaning
Degree greatly improves.
Detailed description of the invention
Fig. 1 is overall flow schematic diagram of the invention.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
As shown in Figure 1, including the following steps: the present invention provides a kind of copolymerization preparation method of porous polyester fiber
S100, raw material preparation, it would be desirable to which the raw material of preparation is dried for the first time after deploying mixing in proportion；
In the step S100, the raw material of required preparation includes PTA, triphenyl phosphate, titanium dioxide, double benzoxazoles
Talan, anion polyester master particle, Third monomer M-phthalic acid diethyl alcohol ester -5- sodium sulfonate, pass through double benzos of addition
Oxazole talan raw material, introduces polyester system, while viscosity reaches requirement, substantially increases the anti-purple of finished fiber
Outside line ability and ageing resistance, while the anion of anion polyester master particle has certain bactericidal effect.
Primary drying process uses 10~20min of heated-air drying after raw material mixing, and drying temperature is controlled 110~135
DEG C, dry effect for the first time is that the crystallization water for preventing from containing in the raw material being added or surface water generate shadow to subsequent processing
It rings.
Part material after drying is added reaction kettle of the esterification and carries out esterification by S200, esterification treatment；
In the step S200, detailed process is as follows for esterification:
Reaction kettle of the esterification is heated by Electric heating first, temperature reaches 230~250 DEG C, and pressure is 0.3~
0.4MPa, controlling the fractionation capital temperature inside reaction kettle of the esterification is 125~130 DEG C；
The theoretical water yield of raw material reaction is calculated, and detects the water yield of real reaction, reaches theoretical in detection water yield
When water yield 80%, starts pressure release to reach normal condition, the ratio of water yield and theoretical water yield is detected by judgement,
To judge the response situation inside reaction kettle of the esterification, it is ensured that reach reaction and require；
After pressure release terminates, when water yield reaches theoretical water yield 90%, be added the 4th monomer polyethylene glycol and
5th monomer hydrophilic agent continues 50~60min of esterification, until esterification is completed, it is poly- by the 4th monomer being newly added
Ethylene glycol and the 5th monomer hydrophilic agent cooperate Third monomer M-phthalic acid diethyl alcohol ester -5- sodium sulfonate, so that finished fiber
Hydrophily improves, and has good hydrophilicity in actual use, and use is more comfortable.
In esterification, judges that the condition that esterification is completed is that detection water yield reaches 95% or more, be discharged in detection
It is monitored simultaneously when amount using multiple detection devices, to reduce error caused by folk prescription planar survey, so that it is guaranteed that esterification
It is properly completed.
S300, polymerization reaction carry out redrying after esterification completion, and feed modified copolymer；
The purpose of redrying is as follows: redrying is the softening point of the material in order to improve, and prevents polyester fiber
Softening point is low and ring knot clogging occurs；The moisture wherein contained is removed simultaneously, to prevent in subsequent polyester fiber
The problem of strand generates violent hydrolysis during the spinning process, and molecular weight is caused to reduce, be also prevented to be formed cavity filament, lousiness or
The problem of person is floatd thread.
In the step S300, redrying process is as follows:
In the pre-crystallized stage, treated, and raw material heats 8~15min in ebullated bed, and temperature is 160~180 DEG C, drops later
For low temperature to 125~145 DEG C, stirring-type fills 1~1.5h, so that the material of everywhere can be by good dry water removal；
In the high temperature drying stage, rotary-drum vacuum is dry, and temperature continues 10~20min at 120~140 DEG C.
To water removal is dried in such a way that pre-crystallized and high temperature drying is mutually handled, subsequent product quality is improved.
It should be added that the drying mode in the present embodiment is not limited in aforesaid way, it is also possible to other
Drying mode.
In the step S300, modified copolymer includes the following steps:
Start the decompression that vacuumizes and heat up, within 42~47min time, reaction kettle of the esterification internal temperature improves to 250~
260 DEG C, while reaction kettle of the esterification internal vacuum reaches 60Pa or less；
It is separately added into antioxidant, delustering agent and antimony acetate, reacts 110~130min under the above conditions；
It is stirred within the set time with setting power, until reaching setting time, stops stirring, nitrogen vacuum breaker is simultaneously
Discharging, obtained high polymer molten obtain polyester slice through Cast Strip pelletizing by cold rinse bank.
S400, preparation is blended, fire-retardant master granule is added in obtained raw material, mixing, spinning moulding is blended.
Before fire-retardant master granule is added, the limit oxygen index of hydrophilic polyesters slice is 27.0%, and the poly- of fire-retardant master granule is added
The limit oxygen index of ester batten reaches 30.1%~34.2%, both greater than 27%, is fire retardant grade material, and flame retardant property has very big
Promotion.
The test polyester fiber and common contrast sample polyester fiber obtained simultaneously to this programme compares, and comparison is tied
Fruit is as follows:
| Reduced parameter | The uvioresistant time | Resistance combustion temperature | Hydrophily |
| Test polyester fiber | 1000h | 600℃ | It is excellent |
| Contrast sample | 600h | 400℃ | Generally |
By above-mentioned comparison, the polyester fiber that this programme obtains, anti-uv-ray, ageing resistance, anti-flammability and
It is all significantly improved in hydrophily, substantially increases its performance.
In the step S400, the fire-retardant master granule ratio of obtained raw material and addition is 100:7~13, specific mixing step
It is as follows:
The pre-crystallized 5h under 130~135 DEG C of vacuum condition；
Subsequent to be warming up to 145~150 DEG C, dry 12~16h obtains blended slice；
Spinning on obtained blended slice twin-screw high speed compound spinning machine, spinning temperature are 250~270 DEG C.
As-spun fibre 6~8h of balance after spinning is completed, the purpose of balance is primarily to improve subsequent drawing-off effect
Fruit prevents the case where local fracture occur when drawing-off, and drawing-off processing is carried out on parallel drafting machine.
The condition of drawing-off processing are as follows: 65 DEG C of heat roller temperature, 150 DEG C of setting temperature, draft speed 300m/min, drafting multiple
3.2。
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie
In the case where without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Benefit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent elements of the claims
Variation is included within the present invention.Any reference signs in the claims should not be construed as limiting the involved claims.
Claims (10)
1. a kind of copolymerization preparation method of porous polyester fiber, characterized by the following steps:
S100, raw material preparation, it would be desirable to which the raw material of preparation is dried for the first time after deploying mixing in proportion；
Part material after drying is added reaction kettle of the esterification and carries out esterification by S200, esterification treatment；
S300, polymerization reaction carry out redrying after esterification completion, and feed modified copolymer；
S400, preparation is blended, fire-retardant master granule is added in obtained raw material, mixing, spinning moulding is blended.
2. a kind of copolymerization preparation method of porous polyester fiber according to claim 1, it is characterised in that: the step
In S100, the raw material of required preparation includes PTA, triphenyl phosphate, titanium dioxide, double benzoxazoles talan, anion
Polyester master particle, Third monomer M-phthalic acid diethyl alcohol ester -5- sodium sulfonate.
3. a kind of copolymerization preparation method of porous polyester fiber according to claim 2, it is characterised in that: raw material mixes it
Primary drying process uses 10~20min of heated-air drying afterwards, and drying temperature is controlled at 110~135 DEG C.
4. a kind of copolymerization preparation method of porous polyester fiber according to claim 1, it is characterised in that: the step
In S200, detailed process is as follows for esterification:
Reaction kettle of the esterification is heated by Electric heating first, temperature reaches 230~250 DEG C, and pressure is 0.3~0.4MPa,
Controlling the fractionation capital temperature inside reaction kettle of the esterification is 125~130 DEG C；
The theoretical water yield of raw material reaction is calculated, and detects the water yield of real reaction, reaches theoretical water outlet in detection water yield
When measuring 80%, start pressure release to reach normal condition；
After pressure release terminates, when water yield reaches theoretical water yield 90%, the 4th monomer polyethylene glycol and the 5th is added
Monomer hydrophilic agent continues 50~60min of esterification, until esterification is completed.
5. a kind of copolymerization preparation method of porous polyester fiber according to claim 4, it is characterised in that: esterification
In, judge that the condition that esterification is completed is that detection water yield reaches 95% or more.
6. a kind of copolymerization preparation method of porous polyester fiber according to claim 1, it is characterised in that: the step
In S300, redrying process is as follows:
In the pre-crystallized stage, treated, and raw material heats 8~15min in ebullated bed, and temperature is 160~180 DEG C, reduces temperature later
It spends to 125~145 DEG C, stirring-type fills 1~1.5h；
In the high temperature drying stage, rotary-drum vacuum is dry, and temperature continues 10~20min at 120~140 DEG C.
7. a kind of copolymerization preparation method of porous polyester fiber according to claim 1, it is characterised in that: the step
In S300, modified copolymer includes the following steps:
Start the decompression that vacuumizes and heat up, within 42~47min time, reaction kettle of the esterification internal temperature is improved to 250~260
DEG C, while reaction kettle of the esterification internal vacuum reaches 60Pa or less；
It is separately added into antioxidant, delustering agent and antimony acetate, reacts 110~130min under the above conditions；
It is stirred within the set time with setting power, until reaching setting time, stops stirring, nitrogen vacuum breaker simultaneously goes out
Material, obtains polyester slice.
8. a kind of copolymerization preparation method of porous polyester fiber according to claim 1, it is characterised in that: the step
In S400, the fire-retardant master granule ratio of obtained raw material and addition is 100:7~13, and specific mixing step is as follows:
The pre-crystallized 5h under 130~135 DEG C of vacuum condition；
Subsequent to be warming up to 145~150 DEG C, dry 12~16h obtains blended slice；
Spinning on obtained blended slice twin-screw high speed compound spinning machine, spinning temperature are 250~270 DEG C.
9. a kind of copolymerization preparation method of porous polyester fiber according to claim 8, it is characterised in that: complete spinning it
As-spun fibre afterwards balances 6~8h, and drawing-off processing is carried out on parallel drafting machine.
10. a kind of copolymerization preparation method of porous polyester fiber according to claim 9, it is characterised in that: drawing-off processing
Condition are as follows: 65 DEG C of heat roller temperature, 150 DEG C of setting temperature, draft speed 300m/min, drafting multiple 3.2.
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| CN201810924581.6A CN109252243A (en) | 2018-08-14 | 2018-08-14 | A kind of copolymerization preparation method of porous polyester fiber |
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Application publication date: 20190122 |