CN111072938B - Low-melting-point polyester and preparation method thereof - Google Patents
Low-melting-point polyester and preparation method thereof Download PDFInfo
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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
- C08G63/66—Polyesters containing oxygen in the form of ether groups
- C08G63/668—Polyesters containing oxygen in the form of ether groups derived from polycarboxylic acids and polyhydroxy compounds
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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
- C08G63/20—Polyesters having been prepared in the presence of compounds having one reactive group or more than two reactive groups
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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
- C08G63/60—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from the reaction of a mixture of hydroxy carboxylic acids, polycarboxylic acids and polyhydroxy 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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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
- Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear
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Abstract
The invention relates to the field of polyester materials, and discloses low-melting-point polyester and a preparation method thereof, wherein the low-melting-point polyester comprises the following raw materials in parts by weight: 100 parts of terephthalic acid, 40-65 parts of ethylene glycol, 0.01-1 part of low-melting-point modifier and 0.02-0.12 part of catalyst. According to the invention, the melting point of the polyester can be effectively reduced only by adding a very small amount of modifier, the thermal stability and spinnability of the polyester are not affected, the synthesized polyester can be used for fiber spinning, and the obtained fiber has higher elongation at break and better dyeing property than the conventional fiber.
Description
Technical Field
The invention relates to the field of polyester materials, in particular to low-melting-point polyester and a preparation method thereof.
Background
The low-melting-point fiber and the non-woven fabric can be directly bonded by a hot bonding method, and the method is more environment-friendly and convenient compared with the traditional method for bonding by using a water-based adhesive, so that the method is always an important direction for the development of differentiated products in the chemical fiber industry. The melting point of the PET polyester fiber is about 260 ℃, and the melting point is relatively high, so that the energy consumption in the spinning process is increased, and the technical difficulty in the subsequent processing process is also increased.
The existing methods for preparing low-melting point polyester mainly comprise two methods: (1) the method can effectively reduce the crystallinity and the melting point, but in order to achieve the effect, the adding amount of the third monomer is generally higher, so that the spinnability of the polyester melt is poor, and the interference and the influence on the subsequent blending effect of spinning and fibers are easy to cause. Therefore, most low-melting polyesters cannot be used for fiber production (only as raw materials for other polyester products) at present. (2) Another method is the substitution of monomers, such as PTT polyesters obtained by substituting 1, 3-Propanediol (PDO) for ethylene glycol, which have a melting point of about 225 deg.C, by increasing the length of the soft segment to reduce crystallinity and melting point. However, large-scale industrialization of PDO has not been achieved in China, and the yield cannot meet the demand as a monomer at present. Meanwhile, the above two methods greatly change the chemical composition of PET polyester, which causes an increase in cost or complication of the process.
CN103102473 provides a method for preparing low-melting-point PET copolyester, the content of added isophthalic acid derivatives is 10-30% of the copolyester, the crystallinity is low, the transparency is good, and the method is mainly applied to the manufacture of injection molding products. CN104119521 also adopts a similar method, which adds 1-20% by weight of C6-C10 dibasic acid and/or C5-C10 dihydric alcohol third monomer, and reduces crystallization performance and melting point by adding linear block, and can be used for spinning fiber products and non-woven fabrics, considering that the melt strength is reduced due to too long flexible chain, the spinning performance of the product obtained by the method has risk. CN105063797 provides a method for preparing polyester composite fiber, which comprises adding polyether block to synthesize low-melting point copolymer, spinning to obtain low-melting point polyester composite fiber with conventional polyester as core layer and copolymer as skin layer. In summary, no low-melting PET polyester fiber with very low content of single component or additive component has been reported.
Disclosure of Invention
In order to solve the technical problems, the invention provides a low-melting-point polyester and a preparation method thereof. The invention can obviously reduce the melting point of the polyester by only adding a little amount of modifier, does not influence the thermal stability and spinnability of the polyester, can be used for fiber spinning, and has higher breaking elongation and better dyeing property compared with the conventional fiber.
The specific technical scheme of the invention is as follows: the low-melting-point polyester comprises the following raw materials in parts by weight:
100 parts of terephthalic acid, namely terephthalic acid,
40-65 parts of ethylene glycol,
0.01 to 1 part of low-melting point modifier,
0.02-0.12 part of catalyst.
The low-melting point modifier is selected from one or more of bis (trimethylolpropane), dipentaerythritol, dimethylolpropionic acid and ethoxylated pentaerythritol.
In research by the invention team, the polymer can form a special long-chain branched structure only by adding a trace amount of the low-melting-point modifier in the polyester synthesis process, so that the molecular regularity of the polyester is reduced, the crystallinity is reduced, the crystallization rate is slowed down, the melting point of the polyester is obviously reduced, and the lowest melting point can reach a level of 225 ℃. The addition amount of the modifier is far less than that of a modifying monomer used for reducing the melting point of polyester in the prior art, meanwhile, the addition of the low-melting-point modifier does not influence the spinnability of polyester melt, and the spinning temperature of the synthesized polyester is obviously lower than that of the conventional polyester.
The invention can realize good effect under the condition of trace amount of low-melting point modifier, because the selected low-melting point modifiers have a multi-functional group structure, and the polymer is subjected to branching modification to form a random structure, thereby reducing the crystallinity. More importantly, compared with common multifunctional branching agents such as pentaerythritol, trimethylolpropane, pyromellitic dianhydride and the like, the low-melting point modifiers have larger spacing between functional groups in molecules, reduce steric hindrance of a branched structure formed by reaction with a polyester PET monomer, and can form more long-chain branched structures under the condition of the same molar amount of the functional groups, so that the melting point of the obtained polymer is further reduced.
The melting point of the polyester PET decreases as the amount of low melting point modifier added increases. However, it should be noted that the content of the modifier should not be too high, otherwise, the reaction rate is too fast, stable control is difficult, and crosslinking is easy to occur, which results in difficult discharging of the product and damages to the reaction kettle.
Preferably, the low-melting point modifier is 0.1 to 0.6 part.
Preferably, the catalyst is selected from one or more of ethylene glycol antimony, antimony trioxide and antimony acetate.
A method for preparing low-melting point polyester comprises the following steps:
1) esterification reaction: adding terephthalic acid, ethylene glycol, a low-melting-point modifier and a catalyst into a preheated polymerization reaction kettle, and uniformly stirring and mixing. Pressurizing and heating under the protection of inert gas to perform esterification reaction until water is discharged.
2) And (3) polycondensation reaction: vacuumizing, heating to perform pre-polycondensation reaction, performing final polycondensation reaction, discharging after reaction, and granulating to obtain the low-melting-point polyester chip.
The intrinsic viscosity of the polyester chip prepared by the method is within the range of 0.60-0.90 dl/g, and the level of 0.64-0.68 dl/g of the conventional polyester fiber can be reached only by adjusting the reaction conditions. The melting point range is 225-245 ℃, and can be adjusted according to the type, concentration and reaction time of the low-melting point modifier, but the melting point is greatly lower than the melting point of 260 ℃ of the conventional polyester fiber.
Preferably, in the step 1), the preheating temperature of the polymerization reaction kettle is 50-100 ℃, and the stirring time is 10-30 min.
Preferably, in the step 1), the esterification reaction temperature is 220-260 ℃ and the pressure is 0-0.35 MPa.
Preferably, in the step 2), the vacuum is pumped for 30-90min to the absolute pressure of less than 1000Pa, and the pre-polycondensation temperature is 260-280 ℃.
Preferably, in the step 2), the final polycondensation temperature is 265-285 ℃, the pressure is 0-300 Pa, and the reaction time is 10-120 min.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention obviously reduces the melting point of polyester, has simple formula and extremely low content of low-melting point modifier, and does not influence the thermal stability and spinnability of the product. Meanwhile, the fluidity is enhanced, and the spinning speed is improved.
(2) The invention can realize the controllability of the viscosity and the melting point of the product by adjusting the concentration, the type and the reaction time of the modifier with low melting point, and the invention can be applied to different application fields to ensure that the production and the processing become more flexible. The high-melting-point polyester film can be made into bottles, films, plates, sheets and the like by using blow molding, injection molding and other forming methods, and compared with the conventional bottle-grade slices, the processes of adding a third monomer and performing solid-phase tackifying are reduced, and the polyester film is simpler and more convenient. The fiber-grade spinning fiber with a lower melting point can be used for fiber-grade spinning, and due to good fluidity brought by a branched structure, the spinning speed and the elongation at break of the fiber-grade spinning fiber are higher than those of conventional fibers. Meanwhile, the melting point is low, and the corresponding spinning temperature can be reduced by 10-20 ℃. The dyeing performance of the spun fiber is good.
Detailed Description
The present invention will be further described with reference to the following examples.
General examples
The low-melting-point polyester comprises the following raw materials in parts by weight:
100 parts of terephthalic acid, namely terephthalic acid,
40-65 parts of ethylene glycol,
0.01 to 0.5 part, preferably 0.1 to 0.6 part, of a low-melting modifier,
0.02-0.12 part of catalyst (ethylene glycol antimony, antimony trioxide or antimony acetate).
The low-melting point modifier is selected from one or more of bis (trimethylolpropane), dipentaerythritol, dimethylolpropionic acid and ethoxylated pentaerythritol.
A method for preparing low-melting point polyester comprises the following steps:
1) esterification reaction: adding terephthalic acid, ethylene glycol, a low-melting-point modifier and a catalyst into a polymerization reaction kettle preheated at 50-100 ℃, and stirring for 10-30min to mix uniformly; pressurizing and heating under the protection of inert gas, and carrying out esterification reaction at 220-260 ℃ and under the pressure of 0-0.35 MPa until water outlet is finished.
2) And (3) polycondensation reaction: vacuumizing for 30-90min to below absolute pressure of 1000Pa, and simultaneously heating to perform pre-polycondensation reaction at the pre-polycondensation temperature of 260-280 ℃. And then carrying out final polycondensation reaction at 265-285 ℃ under 0-300 Pa for 10-120min, discharging after the reaction, and pelletizing to obtain the low-melting-point polyester.
Example 1
664g of terephthalic acid, 310g of ethylene glycol, 2.0g of dipentaerythritol and 0.3g of ethylene glycol antimony are added into a 2L reaction kettle, stirred at the temperature of 50-100 ℃ for 15min and then N is introduced2The esterification reaction was started at 230 ℃ and 0.3 MPa. After the water discharge is finished, low vacuum is pumped, and simultaneously, the kettle temperature is set to 280 ℃. And (3) vacuumizing the vacuum instrument after the vacuum instrument reaches-101 kPa, recording the current readings after the vacuum degree reaches below 100Pa, and taking 45min from the beginning of current rise to the current corresponding to the fiber-grade polyester sample. Stopping the reaction, discharging and pelletizing.
Example 2
664g of terephthalic acid, 310g of ethylene glycol, 2.0g of dipentaerythritol and 0.3g of ethylene glycol antimony were added to 2L of the reaction mixtureStirring the mixture in a kettle at 50-100 ℃ for 15min, and introducing N2The esterification reaction was started at 233 ℃ under 0.28 MPa. After the water outlet is finished, low vacuum is pumped, and the temperature of the kettle is set to 280 ℃. After the vacuum meter reaches-101 kPa, high vacuum is pumped, after the vacuum degree reaches below 100Pa, current readings are recorded, and the reaction is carried out for 90min from the beginning of the current rise. Stopping the reaction, discharging and pelletizing.
Comparative example 1
664g of terephthalic acid, 310g of ethylene glycol and 0.3g of ethylene glycol antimony are added into a 2L reaction kettle, stirred at the temperature of 50-100 ℃ for 15min and then N is introduced2The esterification reaction was started at 235 ℃ and 0.27 MPa. After the water discharge is finished, low vacuum is pumped, and simultaneously, the kettle temperature is set to 280 ℃. And (3) vacuumizing the vacuum instrument after the vacuum instrument reaches-101 kPa, recording the current readings after the vacuum degree reaches below 100Pa, and taking 150min from the beginning of current rise to the current corresponding to the fiber-grade polyester sample. Stopping the reaction, discharging and pelletizing.
Example 3
1660g of terephthalic acid, 977g of ethylene glycol, 5.0g of bis (trimethylolpropane) propane and 0.9g of ethylene glycol antimony are added into a 5L reaction kettle, stirred at 50-100 ℃ for 15min and then N is introduced2The esterification reaction was started at 226 ℃ and 0.33 MPa. After the water discharge is finished, low vacuum is pumped, and simultaneously, the kettle temperature is set to 280 ℃. And (3) after the vacuum instrument reaches-101 kPa, vacuumizing, recording torque readings, and taking 55min from the moment when the torque rises to reach the torque corresponding to the fiber-grade polyester sample. Stopping the reaction, discharging and pelletizing.
Comparative example 2
1660g of terephthalic acid, 977g of ethylene glycol, 2.7g of pentaerythritol and 0.9g of ethylene glycol antimony are added into a 5L reaction kettle, stirred at 50-100 ℃ for 15min and then N is introduced2The esterification reaction was started at 232 ℃ under 0.33 MPa. After the water discharge is finished, low vacuum is pumped, and simultaneously, the kettle temperature is set to 280 ℃. After the vacuum meter reaches-101 kPa, the vacuum is pumped, the torque reading is recorded, and the reaction is started for 55min from the rise of the current reading. Stopping the reaction, discharging and granulating.
Example 4
1660g of terephthalic acid, 977g of ethylene glycol, 16.6g of bis (trimethylolpropane) propane, 0g of ethylene glycolAdding 9g of ethylene glycol antimony into a 5L reaction kettle, stirring at 50-100 ℃ for 15min, and introducing N2The esterification reaction was started at 225 ℃ and 0.3 MPa. After the water discharge is finished, low vacuum is pumped, and simultaneously, the kettle temperature is set to 280 ℃. After the vacuum meter reached-101 kPa, the vacuum was pulled high, the torque reading was recorded, and the reaction was carried out for 55min from the start of the torque increase. Stopping the reaction, discharging and pelletizing.
Example 5
1660g of terephthalic acid, 977g of ethylene glycol, 2.5g of dimethylolpropionic acid and 0.9g of ethylene glycol antimony are added into a 5L reaction kettle, stirred at 50-100 ℃ for 15min and then N is introduced2The esterification reaction was started at 232 ℃ under 0.3 MPa. After the water discharge is finished, low vacuum is pumped, and simultaneously, the kettle temperature is set to 280 ℃. And (3) after the vacuum instrument reaches-101 kPa, vacuumizing, recording torque readings, and taking 60min from the moment when the torque rises to reach the torque corresponding to the fiber-grade polyester sample. Stopping the reaction, discharging and pelletizing.
Example 6
Adding 100kg of terephthalic acid, 48kg of ethylene glycol, 300g of ditrimethylolpropane and 45g of ethylene glycol antimony into a 300L reaction kettle, stirring at 50-100 ℃ for 15min, and introducing N2The esterification reaction was started at 235 ℃ and 0.3 MPa. After the water discharge is finished, vacuumizing is carried out, and meanwhile, the kettle temperature is set to 285 ℃. After the vacuum meter reaches-101 kPa, the vacuum is pumped, the torque reading is recorded, and the reaction is carried out for 50min from the moment when the torque rises. Stopping the reaction, discharging and pelletizing.
Comparative example 3
Adding 100kg of terephthalic acid, 48kg of ethylene glycol and 45g of ethylene glycol antimony into a 300L reaction kettle, stirring at 50-100 ℃ for 15min, and introducing N2The esterification reaction was started at 236 ℃ under 0.3 MPa. After the water outlet is finished, low vacuum pumping is carried out, and meanwhile, the kettle temperature is set to 285 ℃. After the vacuum meter reaches-101 kPa, the vacuum is pumped, the torque reading is recorded, and the reaction lasts for 150min from the moment when the torque rises. Stopping the reaction, discharging and pelletizing.
The polyester chips obtained in each example and comparative example were subjected to performance tests, and the data are shown in Table 1.
TABLE 1 sample parameter comparison Table
The test method comprises the following steps:
(1) intrinsic viscosity: polyester samples were dissolved in phenol: in a mixed solvent of tetrachloroethane at a mass ratio of 3: 2, the intrinsic viscosity of the sample was measured at room temperature using an Ubbelohde viscometer.
(2) Melting point and crystallization temperature: and (3) adopting a differential scanning calorimeter to scan the sample for heating and cooling cycles between 30 and 280 ℃ to determine the melting point of the polymer.
As can be seen from the data in Table 1, the invention can effectively reduce the melting point of polyester PET and accelerate the reaction rate by only adding a trace amount of low-melting point modifier. Examples 1 and 2 show that the longer the polymerization time, the higher the viscosity and the lower the melting point. Examples 3 and 4 show that the higher the concentration of the low-melting modifier, the higher the viscosity and the lower the melting point for the same reaction time.
Comparative examples 1 and 3 belong to the polymerization process of conventional fiber grade polyesters, with low reaction rate and high melting point of the product in the absence of low melting point modifiers. Example 3 and comparative example 2 used the same molar amount of functional group modifier, and the sample obtained in example 3 had a lower melting point, indicating that the degree of branching of the molecule is higher and the modifier works better. Although the melting point can be further lowered by increasing the mass of pentaerythritol in comparative example 2, a high content of pentaerythritol makes the reaction rate too fast, difficult to control in actual operation, easily forms cross-links, causes difficulty in discharging and damages to the reaction vessel.
Example 7
The low-melting-point polyester chip prepared in the embodiment 6 is used for melt spinning, the spinning temperature is 220-260 ℃, the spinning speed is 4000m/min, the FDY filament sample is obtained by stretching, winding and elasticizing, a dyeing test is carried out,
comparative example 4
And (3) applying the low-melting-point polyester chip prepared in the comparative example 3 to melt spinning at the spinning temperature of 250-290 ℃ and the spinning speed of 3500m/min, stretching, winding and elasticizing to obtain an FDY filament sample, and performing a dyeing test.
As can be seen from the above, the modified polyester has lower spinning temperature and higher spinning speed. The dyeing properties of the samples obtained in example 7 and comparative example 4 were compared, as shown in table 2.
TABLE 2 sample dyeing Properties vs. Table
| Numbering | Elongation at break | Dye uptake | M rate of dyeing |
| Example 7 | 45％ | 88％ | 94％ |
| Comparative example 4 | 30％ | 75％ | 90％ |
As shown in the table, the polyester PET fiber added with the low melting point modifier of the invention in example 7 has better toughness and higher elongation at break than the unmodified sample. The dye uptake and dye uniformity were also higher than for the unmodified sample, due to more random areas.
The raw materials and equipment used in the invention are common raw materials and equipment in the field if not specified; the methods used in the present invention are conventional in the art unless otherwise specified.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and all simple modifications, alterations and equivalents of the above embodiments according to the technical spirit of the present invention are still within the protection scope of the technical solution of the present invention.
Claims (6)
1. The application of the low-melting point modifier in the preparation of low-melting point polyester is characterized in that: the low-melting-point polyester comprises the following raw materials in parts by weight:
100 parts of terephthalic acid, namely terephthalic acid,
40-65 parts of ethylene glycol,
0.01 to 0.15 portion of low-melting point modifier,
0.02-0.12 part of catalyst;
the low-melting point modifier is selected from one or more of bis (trimethylolpropane), dipentaerythritol, dimethylolpropionic acid and ethoxylated pentaerythritol;
the preparation method of the low-melting-point polyester comprises the following steps:
1) esterification reaction: adding terephthalic acid, ethylene glycol, a low-melting-point modifier and a catalyst into a preheated polymerization reaction kettle, and uniformly stirring and mixing; pressurizing and heating under the protection of inert gas to carry out esterification reaction until water outlet is finished;
2) and (3) polycondensation reaction: vacuumizing, heating to perform pre-polycondensation reaction, vacuumizing to perform final polycondensation reaction, discharging after reaction, and granulating to obtain the low-melting-point polyester chip.
2. The use of claim 1, wherein the catalyst is selected from one or more of ethylene glycol antimony, antimony trioxide and antimony acetate.
3. The use according to claim 1, wherein in step 1), the preheating temperature of the polymerization reactor is 50 to 100 ℃ and the stirring time is 10 to 30 min.
4. The use of claim 1, wherein in step 1), the esterification reaction temperature is 220 to 260 ℃ and the pressure is 0 to 0.35 MPa.
5. The use according to claim 1, wherein in step 2), a vacuum is applied for 30-60min to a pressure below 1000Pa absolute and the prepolycondensation temperature is 260-280 ℃.
6. The use according to claim 1, wherein in step 2), the final polycondensation temperature is 265 to 285 ℃, the pressure is 0 to 300Pa, and the reaction time is 10 to 120 min.
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| CN115897001A (en) * | 2022-12-15 | 2023-04-04 | 浙江绿龙新材料有限公司 | Antimony-free low-melting-point parallel nano yarn and preparation method thereof |
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|---|---|
| CN111072938A (en) | 2020-04-28 |
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