CN106700043A - Direct polymerization preparation method of fiber-grade polyethylene glycol naphthalene-2,3-dicarboxylate material - Google Patents
Direct polymerization preparation method of fiber-grade polyethylene glycol naphthalene-2,3-dicarboxylate material Download PDFInfo
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- CN106700043A CN106700043A CN201611243989.4A CN201611243989A CN106700043A CN 106700043 A CN106700043 A CN 106700043A CN 201611243989 A CN201611243989 A CN 201611243989A CN 106700043 A CN106700043 A CN 106700043A
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- ethylene naphthalate
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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
- C08G63/185—Acids containing aromatic rings containing two or more aromatic rings
- C08G63/187—Acids containing aromatic rings containing two or more aromatic rings containing condensed aromatic rings
- C08G63/189—Acids containing aromatic rings containing two or more aromatic rings containing condensed aromatic rings containing a naphthalene ring
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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
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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
- D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
- D01F6/62—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyesters
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- 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
The invention relates to a direct polymerization preparation method of a fiber-grade polyethylene glycol naphthalene-2,3-dicarboxylate material. The direct polymerization preparation method comprises the following steps: preparing a slurry by using 2,3-naphthalene dicarboxylic acid and ethylene glycol as basic raw materials, uniformly stirring, adding the slurry into a reaction kettle by using a slurry pump, performing an esterification reaction to produce an oligomer, pumping the esterified oligomer together with additives on a pipeline, through which the oligomer enters a polycondensation reaction kettle, into a prepolycondensation reaction kettle with the reaction temperature of 258-290 DEG C and the vacuum degree of 0.3-25 mmHg, reacting for 1-6 hours, then enabling a reaction product to enter a final polycondensation reaction kettle with the reaction temperature of 280-290 DEG C and the vacuum degree being lower than or equal to 1 mmHg, reacting for 1-5 hours, rapidly cooling, granulating and drying to obtain polyethylene glycol naphthalene-2,3-dicarboxylate slices, or directly connecting a melt with a spinning workshop for spinning by using a booster pump. The direct polymerization preparation method has the advantages of high yield rate and low cost; the finished product has a good barrier property.
Description
Technical field
The present invention relates to a kind of preparation method of polyester material, and in particular to a kind of poly- 2,3- naphthalenedicarboxylic acids second two of fibre-grade
Alcohol ester material direct polymerization preparation method.
Background technology
Fiber polyester chip comprising extensively, with the continuous progress of science and technology, transport by the material with excellent barrier property
With more and more extensive.The barrier of common PET is 0.1 Mg/ (L24h0.1MPa）（It is 20 microns thin to be made thickness
Piece OTR oxygen transmission rate）, it is impossible to meet the product demand higher to barrier requirement.
PEN（PEN）, its chemical constitution is similar to PET, difference be in strand PEN by
The bigger naphthalene nucleus of rigidity instead of the phenyl ring in PET, and naphthalene ring makes PEN have physical and mechanical properties higher, gas than PET
The performance such as barrier property, chemical stability and heat-resisting, UV resistant, radiation hardness.It is by 2,6- naphthalene diformic acid dimethyl esters（NDC）
Or 2,6- naphthalenedicarboxylic acids（NDA）With ethylene glycol（EG）Polycondensation is formed, and is a kind of emerging smart polymeric.But existing poly- naphthalene
Naphthalate（PEN）In reaction, it is necessary to by Exchange Ester Process, product row yielding is low, and high cost.It is promoted
Reference brings limitation.Seek that a kind of low cost, row yielding be high and fiber polyester chip of good barrier property, be absorbed in as industry
Focus.
The content of the invention
It is an object of the invention to provide a kind of poly- 2,3- (ethylene naphthalate)s material of the excellent fibre-grade of barrier property
Direct polymerization preparation method, the method has row yielding high, the advantage of low cost.
The present invention the used technical scheme that solves the above problems is：A kind of poly- 2,3- (ethylene naphthalate)s of fibre-grade
Material direct polymerization preparation method, with 2,3- naphthalenedicarboxylic acids and ethylene glycol for base stock, in molar ratio 1:1 ~ 2.3 is prepared into slurry
Material, after stirring, being added to by mashing pump carries out esterification in reactor, and the reaction time is 1 ~ 6 hour, generates oligomerisation
Thing, the inherent viscosity for obtaining enters on polycondensation vessel pipeline the oligomer after esterification together with oligomer through pump in 0.3 ~ 0.4dL/g
Each additive injects prepolymerization reaction kettle together, there is INFRARED ABSORPTION particulate plasma device, prepolymerization reaction kettle on pipeline
Reaction temperature at 258 ~ 290 DEG C, vacuum is 0.3 ~ 25mmHg, and the reaction time is 1 ~ 6 hour, and then product enters most final minification
Poly- reactor, the reaction temperature of final polycondensation reactor is 280 ~ 290 DEG C, and vacuum≤1mmHg, the reaction time is 1 ~ 5 hour,
After through quick cooling, pelletizing, drying, poly- 2,3- (ethylene naphthalate)s section is obtained, also can be straight by melt by booster pump
Connecing spinning workshop in succession carries out spinning process.
The INFRARED ABSORPTION particulate plasma device includes：The housing of one closed vacuum-pumping, it is arranged in housing
Ultrasonic wave cell body and the infrared transmitting device and plasma producing apparatus that are arranged on ultrasonic wave cell body；
The working frequency of the ultrasonic unit is 30-50KH, and ultrasonic power is：800-1200W.
0.3-0.6 amperes of the infrared transmitting device output current, the Infrared irradiation of 750-850nm wavelength, every point
Clock 15-25 subpulses irradiate.
The supply frequency that the plasma producing apparatus are used is 30-50KHz, and discharge voltage is 15-25KV.
The 2,3- naphthalenedicarboxylic acids molecular structural formula is：
Between 10000 ~ 50000, structure such as formula is the number-average molecular weight of poly- 2, the 3- (ethylene naphthalate)s：
The additive that the oligomer enters on prepolymerization kettle pipeline includes one or more things in catalyst, toner and diethylene glycol (DEG)
Matter.
The catalyst is metallic compound；The metallic compound includes antimony system, germanium system, titanium system, aluminium system or cobalt system
Compound.
The toner uses cobalt acetate or red blue agent.
The additive is first dissolved in ethylene glycol respectively, normal temperature or be heated to 100 DEG C ± 10 DEG C and stir 5 ± 2 hours,
Respective mixed liquor is made, then is added in the oligomer by pump and injector, into prepolymerization kettle.
Preferably, described 2,3- naphthalenedicarboxylic acids and the molar ratio of ethylene glycol are preferably 1:2~2.2.
Preferably, the number-average molecular weight of described poly- 2,3- (ethylene naphthalate)s is between 15000 ~ 30000.
Compared with prior art, the advantage of the invention is that：
Using 2,3- naphthalenedicarboxylic acids for raw material and ethylene glycol directly carry out polymerisation in the application, it is not necessary to carry out ester exchange
Intermediate reaction step, production cost reduction；But when direct polymerization reacts, reaction speed is slow, is also easy to produce organic molecule, is esterified
Rate has much room for improvement, and after increasing INFRARED ABSORPTION particulate plasma device, reduces organic molecule by infrared effect and produces, and improves
Esterification yield, improves the transparency and intensity of finished product, while by INFRARED ABSORPTION particulate plasma device, ethylene glycol can be with negative
Electric charge, with the effect for accelerating reaction.
Brief description of the drawings
Fig. 1 is a kind of poly- 2,3- (ethylene naphthalate)s material direct polymerization preparation side of fibre-grade in the embodiment of the present invention
The process chart of method.
Specific embodiment
Embodiment 1：
The present embodiment provides a kind of preparation method of poly- 2,3- (ethylene naphthalate)s, and it comprises the following steps：
（1）By 2,3- naphthalenedicarboxylic acids and ethylene glycol in molar ratio 1:2 are prepared into slurry, after stirring, are added by mashing pump
Esterification, 220 DEG C of reaction temperature are carried out in reactor, the reaction time is 2.5 hours, generates oligomer；
（2）The oligomer after esterification is injected pre- together with the catalyst glycol antimony that oligomer enters on polycondensation vessel pipeline through pump
Batch condensation polymerization reactor, there is INFRARED ABSORPTION particulate plasma device on pipeline, the reaction temperature of prepolymerization reaction kettle at 280 DEG C,
Vacuum is 15mmHg, and the reaction time is 1.5 hours, obtains precondensation product；
Catalyst is heated to 100 DEG C ± 10 DEG C and stirs 5 ± 2 hours using being preceding dissolved in ethylene glycol, then by pump and note
Enter device to be added in the oligomer, into prepolymerization kettle；
The INFRARED ABSORPTION particulate plasma device includes：The housing of one closed vacuum-pumping, be arranged at it is super in housing
Sound wave cell body and the infrared transmitting device and plasma producing apparatus that are arranged on ultrasonic wave cell body；The ultrasonic wave
The working frequency of device is 40KH, and ultrasonic power is：1000W；0.5 ampere of infrared transmitting device output current, 800nm ripples
Infrared irradiation long, 20 subpulse irradiation per minute；The supply frequency that the plasma producing apparatus are used is 40KHz,
Discharge voltage is 20KV；
（3）, precondensation product is passed through whole batch condensation polymerization reactor, in 285 DEG C of temperature, under vacuum 0.7mmHg, the reaction time is
1.5 hours, go tank quickly to cool down through end of extruded band, pelletizing, be obtained after drying, obtain poly- 2,3- (ethylene naphthalate)s section
（Direct polymerization method quality index is shown in Table 1）, GPC method molecular weight is 23000.
Table 1
Also melt can be directly connected into spinning workshop by booster pump carries out spinning process.
Embodiment 2：
The present embodiment provides a kind of preparation method of poly- 2,3- (ethylene naphthalate)s, and it comprises the following steps：
（1）By 2,3- naphthalenedicarboxylic acids and ethylene glycol in molar ratio 1:2.1 are prepared into slurry, after stirring, by mashing pump plus
Enter in reactor to carry out esterification, 220 DEG C of reaction temperature, the reaction time is 2.5 hours, generates oligomer；
（2）The oligomer after esterification is injected pre- together with the catalyst glycol antimony that oligomer enters on polycondensation vessel pipeline through pump
Batch condensation polymerization reactor, there is INFRARED ABSORPTION particulate plasma device on pipeline, the reaction temperature of prepolymerization reaction kettle at 275 DEG C,
Vacuum is 10mmHg, and the reaction time is 2 hours, obtains precondensation product；
Catalyst is heated to 100 DEG C ± 10 DEG C and stirs 5 ± 2 hours using being preceding dissolved in ethylene glycol, then by pump and note
Enter device to be added in the oligomer, into prepolymerization kettle；
The INFRARED ABSORPTION particulate plasma device includes：The housing of one closed vacuum-pumping, be arranged at it is super in housing
Sound wave cell body and the infrared transmitting device and plasma producing apparatus that are arranged on ultrasonic wave cell body；The ultrasonic wave
The working frequency of device is 40KH, and ultrasonic power is：1000W；0.5 ampere of infrared transmitting device output current, 800nm ripples
Infrared irradiation long, 20 subpulse irradiation per minute；The supply frequency that the plasma producing apparatus are used is 40KHz,
Discharge voltage is 20KV；
（3）, precondensation product is passed through whole batch condensation polymerization reactor, in 280 DEG C of temperature, under vacuum 0.8mmHg, the reaction time is
1.5 hours, go tank quickly to cool down through end of extruded band, pelletizing, be obtained after drying, obtain poly- 2,3- (ethylene naphthalate)s section
（Direct polymerization method quality index is shown in Table 2）, GPC method molecular weight is 22000.
Table 2
Also melt can be directly connected into spinning workshop by booster pump carries out spinning process.
Embodiment 3：
The present embodiment provides a kind of preparation method of poly- 2,3- (ethylene naphthalate)s, and it comprises the following steps：
（1）By 2,3- naphthalenedicarboxylic acids and ethylene glycol in molar ratio 1:1.6 are prepared into slurry, after stirring, by mashing pump plus
Enter in reactor to carry out esterification, 220 DEG C of reaction temperature, the reaction time is 2.5 hours, generates oligomer；
（2）The oligomer after esterification is injected pre- together with the catalyst glycol antimony that oligomer enters on polycondensation vessel pipeline through pump
Batch condensation polymerization reactor, there is INFRARED ABSORPTION particulate plasma device on pipeline, the reaction temperature of prepolymerization reaction kettle at 275 DEG C,
Vacuum is 10mmHg, and the reaction time is 2 hours, obtains precondensation product；
Catalyst is stirred 5 ± 2 hours, then be added to by pump and injector at normal temperatures using being preceding dissolved in ethylene glycol
In the oligomer, into prepolymerization kettle；
The INFRARED ABSORPTION particulate plasma device includes：The housing of one closed vacuum-pumping, be arranged at it is super in housing
Sound wave cell body and the infrared transmitting device and plasma producing apparatus that are arranged on ultrasonic wave cell body；The ultrasonic wave
The working frequency of device is 40KH, and ultrasonic power is：1000W；0.5 ampere of infrared transmitting device output current, 800nm ripples
Infrared irradiation long, 20 subpulse irradiation per minute；The supply frequency that the plasma producing apparatus are used is 40KHz,
Discharge voltage is 20KV；
（3）, precondensation product is passed through whole batch condensation polymerization reactor, in 280 DEG C of temperature, under vacuum 0.6mmHg, the reaction time is 2
Hour, go tank quickly to cool down through end of extruded band, pelletizing, be obtained after drying, obtain poly- 2,3- (ethylene naphthalate)s section（Directly
Connect polymerization quality index and be shown in Table 2）, GPC method molecular weight is 26000.
Table 3
Also melt can be directly connected into spinning workshop by booster pump carries out spinning process.
Comparative example 1：
This comparative example is differed only in embodiment 1, does not use the INFRARED ABSORPTION particulate plasma to fill in comparative example 1
Put, the Product checking being made the results are shown in Table 4.
Table 4
Comparative example 2：
This comparative example is differed only in embodiment 1, and 2,3- naphthalenedicarboxylic acids are replaced using NDA in comparative example 2,
The Product checking being made the results are shown in Table 5.
Table 5
Comparative example 3：
This comparative example is differed only in comparative example 1, and 2,3- naphthalenedicarboxylic acids are replaced using NDA in comparative example 3,
The Product checking being made the results are shown in Table 6.
Table 6
Commercially available PET, PEN performance is shown in Table 7.
Table 7
Poly- 2, the 3- (ethylene naphthalate)s prepared by Data Comparison, this method, barrier property is good, and row yielding
It is high；Further, since poly- 2,3- (ethylene naphthalate)s carboxyl-content is low, reaction is abundant, with short production cycle, small molecule product
Few, row yielding is high, low production cost, and the OTR oxygen transmission rate of product is low, and under the conditions of identical OTR oxygen transmission rate, PEN is just more
Height, PEN synthesis is more difficult, and some use ester-interchange methods are produced and batch process, and yield is low, and the production cycle is more long, because for poly-
For 2,3- (ethylene naphthalate)s are using the synthesis for direct polymerization method one-step method, than PEN with regard to lower cost.
In addition to the implementation, present invention additionally comprises having other embodiment, all use equivalents or equivalence replacement
The technical scheme that mode is formed, all should fall within the scope of the hereto appended claims.
Claims (10)
1. poly- 2, the 3- (ethylene naphthalate)s material direct polymerization preparation method of a kind of fibre-grade, it is characterised in that：With 2,3-
Naphthalenedicarboxylic acid and ethylene glycol are base stock, are made into slurry, and being added to carries out esterification in reactor, generate oligomerisation
Thing, injects prepolymerization reaction kettle together with each additive, has INFRARED ABSORPTION particulate plasma device on pipeline, then product
Polycondensation reaction is carried out into final polycondensation reactor.
2. the poly- 2,3- (ethylene naphthalate)s material direct polymerization preparation side of a kind of fibre-grade according to claim 1
Method, it is characterised in that：Methods described is for base stock in molar ratio 1 with 2,3- naphthalenedicarboxylic acids and ethylene glycol:1 ~ 2.3 prepares
Into slurry, after stirring, being added to by mashing pump carries out esterification in reactor, and the reaction time is 1 ~ 6 hour, generation
Oligomer, by the oligomer after esterification injects precondensation anti-through pump together with each additive that oligomer enters on polycondensation vessel pipeline
Answer kettle, there is INFRARED ABSORPTION particulate plasma device on pipeline, the reaction temperature of prepolymerization reaction kettle at 258 ~ 290 DEG C, very
Reciprocal of duty cycle is 0.3 ~ 25mmHg, and the reaction time is 1 ~ 6 hour, and then product enters final polycondensation reactor, final polycondensation reactor
Reaction temperature be 280 ~ 290 DEG C, vacuum≤1mmHg, the reaction time is 1 ~ 5 hour, through quick cooling, pelletizing, drying after,
Obtain the section of poly- 2,3- (ethylene naphthalate)s, or melt be directly connected into spinning workshop by booster pump carrying out spinning work
Sequence.
3. the poly- 2,3- (ethylene naphthalate)s material direct polymerization preparation side of a kind of fibre-grade according to claim 2
Method, it is characterised in that：The additive that the oligomer enters on prepolymerization kettle pipeline includes in catalyst, toner and diethylene glycol (DEG)
Plant or several materials.
4. the poly- 2,3- (ethylene naphthalate)s material direct polymerization preparation side of a kind of fibre-grade according to claim 3
Method, it is characterised in that：The catalyst is metallic compound；The metallic compound include antimony system, germanium system, titanium system, aluminium system or
Cobalt based compound.
5. the poly- 2,3- (ethylene naphthalate)s material direct polymerization preparation side of a kind of fibre-grade according to claim 2
Method, it is characterised in that：Described 2,3- naphthalenedicarboxylic acids and the molar ratio of ethylene glycol are preferably 1:2~2.2.
6. the poly- 2,3- (ethylene naphthalate)s material direct polymerization preparation side of a kind of fibre-grade according to claim 2
Method, it is characterised in that：The additive is first dissolved in ethylene glycol respectively, normal temperature or be heated to 100 DEG C ± 10 DEG C and stir 5 ±
2 hours, respective mixed liquor is made, then is added in the oligomer by pump and injector, into prepolymerization kettle.
7. the poly- 2,3- (ethylene naphthalate)s material direct polymerization preparation side of a kind of fibre-grade according to claim 2
Method, it is characterised in that：The inherent viscosity of the oligomer is in 0.3 ~ 0.4dL/g.
8. the poly- 2,3- (ethylene naphthalate)s material direct polymerization preparation side of a kind of fibre-grade according to claim 2
Method, it is characterised in that：The number-average molecular weight of the poly- 2,3- (ethylene naphthalate)s is between 10000 ~ 50000.
9. the poly- 2,3- (ethylene naphthalate)s material direct polymerization preparation side of a kind of fibre-grade according to claim 8
Method, it is characterised in that：The number-average molecular weight of described poly- 2,3- (ethylene naphthalate)s is between 15000 ~ 30000.
10. according to a kind of poly- 2,3- (ethylene naphthalate)s material direct polymerization of the described fibre-grades of one of claim 1-9
Preparation method, it is characterised in that：The INFRARED ABSORPTION particulate plasma device includes：The housing of one closed vacuum-pumping,
The ultrasonic wave cell body being arranged in housing and the infrared transmitting device being arranged on ultrasonic wave cell body and plasma occur
Device；
The working frequency of the ultrasonic unit is 30-50KH, and ultrasonic power is：800-1200W；
0.3-0.6 amperes of the infrared transmitting device output current, the Infrared irradiation of 750-850nm wavelength, 15- per minute
25 subpulses irradiate；
The supply frequency that the plasma producing apparatus are used is 30-50KHz, and discharge voltage is 15-25KV.
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| CN2016108523779 | 2016-09-27 | ||
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2014012796A (en) * | 2012-07-05 | 2014-01-23 | Teijin Dupont Films Japan Ltd | Polyester and producing method thereof |
| CN104530396A (en) * | 2015-01-05 | 2015-04-22 | 福建省鑫东华实业有限公司 | Polyethylene glycol terephthalate preparation method |
| WO2015194526A1 (en) * | 2014-06-18 | 2015-12-23 | 東洋紡株式会社 | Polyester preform and method for manufacturing polyester preform |
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2016
- 2016-12-29 CN CN201611243989.4A patent/CN106700043B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2014012796A (en) * | 2012-07-05 | 2014-01-23 | Teijin Dupont Films Japan Ltd | Polyester and producing method thereof |
| WO2015194526A1 (en) * | 2014-06-18 | 2015-12-23 | 東洋紡株式会社 | Polyester preform and method for manufacturing polyester preform |
| CN104530396A (en) * | 2015-01-05 | 2015-04-22 | 福建省鑫东华实业有限公司 | Polyethylene glycol terephthalate preparation method |
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