CN106854262A - Moisture absorption can contaminate low melting point polyester chip and preparation method thereof - Google Patents
Moisture absorption can contaminate low melting point polyester chip and preparation method thereof Download PDFInfo
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- CN106854262A CN106854262A CN201611242980.1A CN201611242980A CN106854262A CN 106854262 A CN106854262 A CN 106854262A CN 201611242980 A CN201611242980 A CN 201611242980A CN 106854262 A CN106854262 A CN 106854262A
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- melting point
- low melting
- point polyester
- polyester chip
- moisture absorption
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/02—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polycarbonates or saturated polyesters
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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
- C08G63/68—Polyesters containing atoms other than carbon, hydrogen and oxygen
- C08G63/688—Polyesters containing atoms other than carbon, hydrogen and oxygen containing sulfur
- C08G63/6884—Polyesters containing atoms other than carbon, hydrogen and oxygen containing sulfur derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/6886—Dicarboxylic acids and dihydroxy compounds
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- 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
- D01F6/78—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolycondensation products
- D01F6/84—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolycondensation products from copolyesters
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Polyesters Or Polycarbonates (AREA)
Abstract
Low melting point polyester chip can be contaminated the present invention relates to polyester modification technical field, especially a kind of moisture absorption, its component matches and is by mass percentage：Low melting point polyester chip 92 97%, maleic anhydride 2.6 7.8%, initiator 0.2 0.4%；Its preparation method is：Low melting point polyester chip and maleic anhydride are weighed in reactor according to above-mentioned formula, start stirring, be warming up to 155 ~ 165 °C after material melts completely, add initiator, discharging, cooling, pelletizing, drying after 3h is reacted under normal pressure, you can.The present invention prepares moisture absorption can contaminate low melting point polyester chip, and due to destroying the rigid structure and regularity of PET molecules, fusing point is reduced to 135 160 DEG C；Sodium group, more easy dyeing are introduced on strand；Maleic anhydride is grafted on strand by the method for fusion-grafting, is made containing hydrophilic radical COOH on strand, obtained modified low-melting point polyester has good permanent moisture pick-up properties.Melt spinning is carried out to gained section carries out hydroscopicity measure, and hydroscopicity is 5.0 6.4%.
Description
Technical field
Low melting point polyester chip and its preparation side can be contaminated the present invention relates to polyester modification technical field, especially a kind of moisture absorption
Method.
Background technology
Since the appearance, it has a series of premium properties to polyester fiber, is preferable clothes material, it has also become development
Fastest, yield highest synthetic fibers.But current polyester single varieties, the traditional performance having can not meet people
Various demands.Therefore, polyester modification is particularly important.People can be modified by polyester, assign polyester new
Characteristic, to meet different demands, low-melting point polyester is a kind of polyester modification product.
Low-melting point polyester generally refers to a class modified copolyester of the fusing point at 100~210 °C, typically poly- in normal polyester
During conjunction, modified component is added, to change polyester molecule rigid structure, saboteur's chain regularity reduces molten so as to reach
The purpose of point.Low-melting point polyester have low fusing point, good fluidity, keep normal polyester part of properties on the premise of with normal polyester
There is preferable compatibility, be widely used in the industries such as Polyester color master batch, non-woven fabrics, weaving.In recent years, to low melting point
The report of polyester research is more, the low-melting point polyester preparation method having been reported, and is added in normal polyester production process
Three, the 4th modified components, make modified component with PTA, EG hybrid reaction and combined polymerization.Common third component has aliphatic two
First acid and aromatic acid, such as M-phthalic acid, phthalic acid, adipic acid, the 4th component such as butanediol, new penta 2
The dihydroxylic alcohols such as alcohol, hexylene glycol, cyclohexanedimethanol, polyethylene glycol.There is within 2003 scholar by 1,4- butanediols, hexylene glycol, hexamethylene
Alkane dimethanol is reacted in being added to PTA and EG, and the low-melting point polyester that fusing point is 100~130 °C has been obtained.Have within 2005
People has obtained the low melting point that fusing point is 110 °C and has gathered by PTA, EG, M-phthalic acid, butanediol hybrid reaction, through esterification, polycondensation
Ester.Researcher in 2006 replaces part EG with 1,6- hexylene glycols, is reacted with PTA, and obtained low-melting point polyester fusing point can
Up to 110 °C.Someone in 2007 replaces part PTA and EG with M-phthalic acid, adipic acid and neopentyl glycol, and fusing point has been obtained is
110 °C of low-melting point polyester.However, current preparation method is simple gathering less than the low melting point of normal polyester in order to fusing point is obtained
Ester, dyeability, hygroscopicity of the low-melting point polyester for obtaining etc., still without big difference, still can not meet people with normal polyester
Demand.
The content of the invention
Being there is provided the invention aims to solve the deficiency of above-mentioned technology a kind of has low fusing point, good hygroscopicity and can
The moisture absorption of the characteristic of deep dye can contaminate low melting point polyester chip and preparation method thereof.
In order to achieve the above object, a kind of moisture absorption designed by the present invention can contaminate low melting point polyester chip, and its component presses matter
Amount percentage matches and is：Low melting point polyester chip 92-97%, maleic anhydride 2.6-7.8%, initiator 0.2-0.4%；Described draws
Sending out agent is：Benzoyl peroxide or di-t-butyl peroxide.
Described low melting point polyester chip by PTA, EG, glycol modified dose, M-phthalic acid binaryglycol ester sodium sulfonate,
Antimony glycol is constituted, and the mass ratio of wherein PTA and EG is 60-65：35-40, it is 10 that glycol modified dose accounts for EG mass percents
~20%, it is 2~7% that M-phthalic acid binaryglycol ester sodium sulfonate accounts for PTA mass percents, and antimony glycol accounts for PTA mass percentages
Than being 0.15%.Wherein glycol modified dose is dipropylene glycol.
A kind of moisture absorption can contaminate the preparation method of low melting point polyester chip, comprise the following steps：（1）Weighed according to above-mentioned formula
PTA, EG, M-phthalic acid binaryglycol ester sodium sulfonate, glycol modified dose and antimony glycol are added in 5L polymerization reaction kettles,
Replaced with N2, stirring, heat temperature raising under the N2 pressure of 0.1 ~ 0.3MPA, using pressure in still top regulation valve regulation kettle
It is 0.3 ~ 0.5MPA, the outer temperature of still is heated to 175 ~ 250 DEG C, as the zero point of esterification when thering is esterification water to distillate,
1.5h is reacted at 225-260 DEG C, water to be distillated is significantly reduced, pressure is decreased obviously in kettle, pressure is let out to normal pressure, complete esterification
Reaction；Next enter intensification buck stage, in 45Min, reactor temperature is risen to 265 ~ 285 DEG C, while by pressure
50 ~ 100pa is dropped to, now as the zero point of high vacuum polycondensation reaction, is entered under 285 DEG C, pressure 100pa, constant agitation rotating speed
Row polycondensation reaction, power to be mixed increases to 40W, terminates reaction, and polyester fondant is pressed into tank with N2, cooling, pelletizing, does
It is dry, obtain final product described low melting point polyester chip；（2）Low melting point polyester chip and maleic anhydride are weighed in reaction according to above-mentioned formula
In kettle, start stirring, be warming up to 155 ~ 165 °C after material melts completely, add initiator, go out after 3h is reacted under normal pressure
Material, cooling, pelletizing, drying, obtaining final product described moisture absorption can deeply contaminate low melting point polyester chip.
Moisture absorption obtained by the present invention can contaminate low melting point polyester chip and preparation method thereof, and preparing moisture absorption by the present invention can contaminate
Low melting point polyester chip, due to destroying the rigid structure and regularity of PET molecules, fusing point is reduced to 135-160 DEG C；In molecule
Sodium group, more easy dyeing are introduced on chain；Maleic anhydride is grafted on strand by the method for fusion-grafting, makes molecule
Contain hydrophilic radical-COOH on chain, obtained modified low-melting point polyester has good permanent moisture pick-up properties.Gained is cut into slices into
Row melt spinning carries out hydroscopicity measure, and hydroscopicity is 5.0-6.4%, and conventional PET highest hydroscopicity is 0.3-0.5%.
Specific embodiment
The present invention is further described by the following embodiment.
Embodiment 1：
A kind of moisture absorption of the present embodiment description can contaminate low melting point polyester chip, and it is by 96.8 parts of low melting point polyester chip, maleic acid
3 parts of acid anhydride, 0.2 part of composition of di-t-butyl peroxide, wherein low-melting point polyester is by PTA60 parts, EG40 parts, dipropylene glycol 4
Part, 0.06 part of 1.2 parts of M-phthalic acid binaryglycol ester sodium sulfonate and antimony glycol are obtained through esterification, polymerisation.The above part
Number is mass fraction.
Preparation method：（1）According to mass ratio weigh a certain amount of PTA, EG, M-phthalic acid binaryglycol ester sodium sulfonate,
Glycol modified dose is added in 2L polymerization reaction kettles with antimony glycol, is replaced with N2, stirred under the N2 pressure of 0.15MPA,
Heat temperature raising.It is 0.35MPA using pressure in still top regulation valve regulation kettle, the outer temperature of still is heated to 175 DEG C, has treated
As the zero point of esterification when esterification water is distillated, 1.5h is reacted at 225 DEG C, water to be distillated is significantly reduced, pressure is bright in kettle
It is aobvious to decline, pressure is let out to normal pressure, complete esterification.Next intensification buck stage is entered, in 45Min, by reactor
Interior temperature rises to 265 DEG C, while pressure is dropped into 100pa, now as the zero point of high vacuum polycondensation reaction.In 285 DEG C, pressure
Carry out polycondensation reaction under 100pa, constant agitation rotating speed, power to be mixed increases to 40W, terminate reaction, with N2 by polyester fondant
Press-in tank, cooling, pelletizing, drying obtain final product described low melting point polyester chip；
（2）A certain amount of low melting point polyester chip and maleic anhydride are weighed in reactor according to mass ratio, starts stirring, heat up
To 155 °C after material melts completely, add di-t-butyl peroxide, under normal pressure react 3h after discharging, cooling, pelletizing, do
Dry, obtaining final product described moisture absorption can contaminate low melting point polyester chip.
The fusing point that the moisture absorption can contaminate low melting point polyester chip is 135 °C, to the section melt spinning of gained, measures hydroscopicity
It is 6.4%, dyeability there has also been larger raising.
Embodiment 2：
A kind of moisture absorption of the present embodiment description can contaminate low melting point polyester chip, and it is by 92 parts of low melting point polyester chip, maleic anhydride
7.6 parts, 0.4 part of benzoyl peroxide composition, wherein low-melting point polyester are 7 parts of the dipropylene glycols by PTA65 parts, EG35 parts,
0.065 part of 4.55 parts of M-phthalic acid binaryglycol ester sodium sulfonate and antimony glycol are obtained through esterification, polymerisation.Above number
It is mass fraction.
Preparation method：A certain amount of PTA, EG, M-phthalic acid binaryglycol ester sodium sulfonate, binary are weighed according to mass ratio
Alcohol modifying agent and antimony glycol are added in 2L polymerization reaction kettles, are replaced with N2, stirred under the N2 pressure of 0.1MPA, are heated liter
Temperature.It is 0.3MPA using pressure in still top regulation valve regulation kettle, the outer temperature of still is heated to 200 DEG C, esterification water to be had
As the zero point of esterification when distillating, 2h is reacted at 250 DEG C, water to be distillated is significantly reduced, pressure is decreased obviously in kettle, will
Pressure is let out to normal pressure, completes esterification.Next enter intensification buck stage, in 45Min, reactor temperature is risen to
280 DEG C, while pressure is dropped into 80pa, now as the zero point of high vacuum polycondensation reaction.285 DEG C, it is pressure 100pa, constant
Polycondensation reaction is carried out under speed of agitator, power to be mixed increases to 40W, terminates reaction, and polyester fondant is pressed into tank with N2, cold
But, pelletizing, drying, obtain final product described low melting point polyester chip；；
（2）A certain amount of low melting point polyester chip and maleic anhydride are weighed in reactor according to mass ratio, starts stirring, heat up
To 165 °C after material melts completely, add benzoyl peroxide, under normal pressure react 3h after discharging, cooling, pelletizing, drying,
Obtaining final product described moisture absorption can contaminate low melting point polyester chip.
The fusing point that the moisture absorption can contaminate low melting point polyester chip is 158 °C, to the section melt spinning of gained, measures hydroscopicity
It is 5.0%, dyeability there has also been larger raising.
Embodiment 3：
A kind of moisture absorption can contaminate low melting point polyester chip, and it is by 95 parts of low melting point polyester chip, 4.7 parts of maleic anhydride, benzoyl peroxide
0.3 part of composition of formyl, wherein low melting point polyester chip is by PTA60 parts, EG40 parts, 8 parts of dipropylene glycol, M-phthalic acid
0.06 part of 1.2 parts of binaryglycol ester sodium sulfonate and antimony glycol are obtained through esterification, polymerisation.Above number is mass fraction.
Preparation method：A certain amount of PTA, EG, M-phthalic acid binaryglycol ester sodium sulfonate, binary are weighed according to mass ratio
Alcohol modifying agent and antimony glycol are added in 2L polymerization reaction kettles, are replaced with N2, stirred under the N2 pressure of 0.2MPA, are heated liter
Temperature.It is 0.4MPA using pressure in still top regulation valve regulation kettle, the outer temperature of still is heated to 220 DEG C, esterification water to be had
As the zero point of esterification when distillating, 2.5h is reacted at 255 DEG C, water to be distillated is significantly reduced, pressure is decreased obviously in kettle,
Pressure is let out to normal pressure, esterification is completed.Next intensification buck stage is entered, in 45Min, by reactor temperature liter
To 280 DEG C, while pressure is dropped into 70pa, now as the zero point of high vacuum polycondensation reaction.285 DEG C, pressure 100pa, perseverance
Determine to carry out polycondensation reaction under speed of agitator, power to be mixed increases to 40W, terminates reaction, and polyester fondant is pressed into tank with N2,
Cooling, pelletizing, drying, obtain final product described low melting point polyester chip；；
（2）A certain amount of low melting point polyester chip and maleic anhydride are weighed in reactor according to mass ratio, starts stirring, heat up
To 165 °C after material melts completely, add benzoyl peroxide, under normal pressure react 3h after discharging, cooling, pelletizing, drying,
Obtaining final product described moisture absorption can contaminate low melting point polyester chip.
The fusing point that the moisture absorption can contaminate low melting point polyester chip is 151 °C, to the section melt spinning of gained, measures hydroscopicity
It is 6.3 %, dyeability there has also been larger raising.
Embodiment 4：
A kind of moisture absorption can contaminate low melting point polyester chip, and it is by 93.5 parts of low melting point polyester chip, 6.15 parts of maleic anhydride, peroxidating
0.35 part of composition of di-t-butyl, wherein low-melting point polyester is by PTA65 parts, EG35 parts, 3.5 parts of dipropylene glycol, isophthalic two
0.065 part of 3.25 parts of formic acid binaryglycol ester sodium sulfonate and antimony glycol are obtained through esterification, polymerisation.Above number is quality
Number.
Preparation method：A certain amount of PTA, EG, M-phthalic acid binaryglycol ester sodium sulfonate, binary are weighed according to mass ratio
Alcohol modifying agent and antimony glycol are added in 2L polymerization reaction kettles, are replaced with N2, stirred under the N2 pressure of 0.3MPA, are heated liter
Temperature.It is 0.5MPA using pressure in still top regulation valve regulation kettle, the outer temperature of still is heated to 250 DEG C, esterification water to be had
As the zero point of esterification when distillating, 1.5h is reacted at 260 DEG C, water to be distillated is significantly reduced, pressure is decreased obviously in kettle,
Pressure is let out to normal pressure, esterification is completed.Next intensification buck stage is entered, in 45min, by reactor temperature liter
To 285 DEG C, while pressure is dropped into 50pa, now as the zero point of high vacuum polycondensation reaction.285 DEG C, pressure 100pa, perseverance
Determine to carry out polycondensation reaction under speed of agitator, power to be mixed increases to 40W, terminates reaction, and polyester fondant is pressed into tank with N2,
Cooling, pelletizing, drying, obtain final product described low melting point polyester chip；
（2）A certain amount of low melting point polyester chip and maleic anhydride are weighed in reactor according to mass ratio, starts stirring, heat up
To 160 °C after material melts completely, add di-t-butyl peroxide, under normal pressure react 3h after discharging, cooling, pelletizing, do
Dry, obtaining final product described moisture absorption can contaminate low melting point polyester chip.
The fusing point that the moisture absorption can contaminate low melting point polyester chip is 141 °C, to the section melt spinning of gained, measures hydroscopicity
It is 5.8 %, dyeability there has also been larger raising.
Claims (5)
1. a kind of moisture absorption can contaminate low melting point polyester chip, it is characterised in that：Its component matches and is by mass percentage：Low melting point is gathered
Ester section 92-97%, maleic anhydride 2.6-7.8%, initiator 0.2-0.4%.
2. a kind of moisture absorption according to claim 1 can contaminate low melting point polyester chip, it is characterized in that：Described initiator is：
Benzoyl peroxide or di-t-butyl peroxide.
3. a kind of moisture absorption according to claim 1 and 2 can contaminate low melting point polyester chip, it is characterized in that：Described low melting point
Polyester slice is made up of PTA, EG, glycol modified dose, M-phthalic acid binaryglycol ester sodium sulfonate, antimony glycol, wherein PTA
It is 60-65 with the mass ratio of EG：35-40, it is 10~20%, M-phthalic acid diethyl that glycol modified dose accounts for EG mass percents
It is 2~7% that diol ester sodium sulfonate accounts for PTA mass percents, and it is 0.15% that antimony glycol accounts for PTA mass percents.
4. a kind of moisture absorption according to claim 3 can contaminate low melting point polyester chip, it is characterized in that：Described is glycol modified
Agent is dipropylene glycol.
5. a kind of moisture absorption as claimed in claim 3 can contaminate the preparation method of low melting point polyester chip, it is characterized in that：Including following
Step：（1）PTA, EG, M-phthalic acid binaryglycol ester sodium sulfonate, glycol modified dose and antimony glycol are weighed according to formula
It is added in 5L polymerization reaction kettles, is replaced with N2, stirring, heat temperature raising under the N2 pressure of 0.1 ~ 0.3MPA, using still
Pressure is 0.3 ~ 0.5MPA in top regulation valve regulation kettle, and the outer temperature of still is heated to 175 ~ 250 DEG C, when having esterification water to distillate
As the zero point of esterification, 1.5h is reacted at 225-260 DEG C, water to be distillated is significantly reduced, pressure is decreased obviously in kettle, will
Pressure is let out to normal pressure, completes esterification；Next enter intensification buck stage, in 45Min, reactor temperature is risen to
265 ~ 285 DEG C, while pressure is dropped into 50 ~ 100pa, now as the zero point of high vacuum polycondensation reaction, in 285 DEG C, pressure
Carry out polycondensation reaction under 100pa, constant agitation rotating speed, power to be mixed increases to 40W, terminate reaction, with N2 by polyester fondant
Press-in tank, cooling, pelletizing, drying obtain final product described low melting point polyester chip；（2）Low-melting point polyester is weighed according to formula to cut
Piece and maleic anhydride start stirring in reactor, are warming up to 155 ~ 165 °C after material melts completely, add initiator,
Discharging, cooling, pelletizing, drying after 3h is reacted under normal pressure, obtaining final product described moisture absorption can deeply contaminate low melting point polyester chip.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111607843A (en) * | 2020-06-24 | 2020-09-01 | 江苏微笑新材料科技有限公司 | Preparation method of anhydride modified sheath-core composite fiber |
| CN112981610A (en) * | 2021-03-08 | 2021-06-18 | 江苏江南高纤股份有限公司 | Environment-friendly hydrophilic low-melting-point PET composite short fiber and preparation method thereof |
| CN113403843A (en) * | 2021-06-07 | 2021-09-17 | 宜禾股份有限公司 | Special work clothes in dangerous place based on flexible sensing |
| CN113861638A (en) * | 2021-12-02 | 2021-12-31 | 富维薄膜（山东）有限公司 | Preparation method of modified polyester and application of modified polyester in polyester film for dry film resist |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104497222A (en) * | 2014-12-18 | 2015-04-08 | 桐乡中欣化纤有限公司 | Hygroscopic deep-dyeable low-melting point polyester chip and preparation method thereof |
-
2016
- 2016-12-29 CN CN201611242980.1A patent/CN106854262A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104497222A (en) * | 2014-12-18 | 2015-04-08 | 桐乡中欣化纤有限公司 | Hygroscopic deep-dyeable low-melting point polyester chip and preparation method thereof |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111607843A (en) * | 2020-06-24 | 2020-09-01 | 江苏微笑新材料科技有限公司 | Preparation method of anhydride modified sheath-core composite fiber |
| CN112981610A (en) * | 2021-03-08 | 2021-06-18 | 江苏江南高纤股份有限公司 | Environment-friendly hydrophilic low-melting-point PET composite short fiber and preparation method thereof |
| CN113403843A (en) * | 2021-06-07 | 2021-09-17 | 宜禾股份有限公司 | Special work clothes in dangerous place based on flexible sensing |
| CN113861638A (en) * | 2021-12-02 | 2021-12-31 | 富维薄膜（山东）有限公司 | Preparation method of modified polyester and application of modified polyester in polyester film for dry film resist |
| CN113861638B (en) * | 2021-12-02 | 2022-03-29 | 富维薄膜（山东）有限公司 | Preparation method of modified polyester and application of modified polyester in polyester film for dry film resist |
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