CN114318577A - Using GO-SiO2Method for improving crystallization performance of polyester fiber by composite nucleus-forming additive - Google Patents
Using GO-SiO2Method for improving crystallization performance of polyester fiber by composite nucleus-forming additive Download PDFInfo
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Abstract
The invention discloses a method for preparing a graphene oxide film by using GO-SiO2A method for improving the crystallization performance of polyester fiber by using composite nuclear additive includes growing silicon dioxide (SiO) on the surface of Graphene Oxide (GO) in situ2) The block polymer (LMPET-PEG) was then grafted and the resulting hybrid particles were melt spun blended with polyethylene terephthalate (PET) and characterized. According to the invention, the compatibility of the additive and PET is increased by grafting the block polymer, so that the crystallization property and the thermal property of the PET fiber are increased by adding the block polymer into PET for spinning. The modified PET fiber has good thermodynamic stability, good crystallization performance and very good application prospect.
Description
Technical Field
The invention relates to the field of chemical modification and spinning, in particular to a method for improving the crystallization performance of polyester fiber by utilizing a nucleation additive of a graphene oxide and silicon dioxide composite material.
Background
Polyethylene terephthalate (PET), also known as Dacron or Dokura, is the most prominent type of thermoplastic polyester. It is prepared by exchanging terephthalic acid with glycol ester or synthesizing dihydroxy ethyl terephthalate by esterification of terephthalic acid and glycol ester and then carrying out polycondensation reaction. The PET has good mechanical properties, acid and alkali resistance, oil resistance, good low temperature resistance and high temperature resistance, no toxicity, no odor, good sanitation and good safety, and can be used for food packaging. It has wide application and excellent performance.
Silica acts as a nucleus during crystallization of the polyester and is an impurity that promotes crystallization. The addition of the silicon dioxide increases the number of heterogeneous nucleation, promotes the crystallization of molecules, accelerates the crystallization speed and can effectively improve the crystallization performance of the polyester. But the dispersibility of the filler in the polyester matrix is also a key factor affecting the performance of the composite.
Disclosure of Invention
The invention aims to provide a method for improving the crystallization performance and the thermal performance of PET fibers by using a nucleating additive containing graphene oxide.
The invention is realized by the following technical scheme:
using GO-SiO2A method for improving the crystallinity of polyester fibre by compounding core additive includes such steps as mixing GO-SiO2+ LMPET-PEG or GO-SiO2The + LMPET-PPG nano particles are granulated and blended with PET according to the proportion, and then the produced particles are melt spun to prepare the PET fiber containing the modified silicon dioxide;
GO-SiO2preparation of hybrid composite material: dissolving a small amount of GO nano-sheets in deionized water, performing ultrasonic dispersion, adding twice of absolute ethyl alcohol solution, performing ultrasonic treatment, adding ammonia water and TEOS solution, adopting an in-situ hydrolysis method, taking TEOS as a silicon source, and converting the TEOS into silicon dioxide on the GO nano-sheets after hydrolysis;
nucleating additive GO-SiO of graphene oxide and silicon dioxide composite material2+ LMPET-PEG or GO-SiO2Preparation of + LMPET-PPG: weighing 20mg of GO-SiO in the following proportion2Adding into 9.5mL ethanol +0.5mL water, ultrasonic pulverizing, dispersing, adding 1mL IPTES, adjusting pH to 4-5 with formic acid, refluxing at 70 deg.C, introducing N26 h; washing with ethanol for 2-3 times after the reaction is finished to obtain GO-SiO2-IPTES, dispersing GO-SiO2-IPTES into 10mL of DMF, dispersing 50mg of LMPET-PEG into 5mL of DMF, mixing the two, adding 50 mu L of dibutyltin dilaurate DBDU, heating to 70 ℃, and magnetically stirring for 10 hours to obtain GO-SiO2+ LMPET-PEG nanoparticles; the LMPET-PEG is replaced by LMPET-PPG to obtain GO-SiO2+ LMPET-PPG nanoparticles.
In the method, the GO nano-sheets are commercially available, the sheet diameter is 0.5-5 mu m, and the thickness is 0.8-1.2 nm; the molecular weight of LMPET is 5000-.
In the method, the PET used is commercially available fiber-grade PET, and the intrinsic viscosity is 0.65-0.68 dL/g.
The method, the synthesized GO-SiO2+ LMPET-PEG or GO-SiO2The proportion of the + LMPET-PPG nano particles in the PET fiber is 0.2-1%.
In the method, the rotation speed for centrifugation is 7000-10000r/min, and the time is 6-10 minutes.
The method is GO/SiO2Preparing a hybrid composite material, namely, adopting an in-situ hydrolysis method, taking TEOS as a silicon source, and converting the TEOS into silicon dioxide on GO nano-sheets after hydrolysis; firstly, dissolving 0.06g of GO nano-sheets in 60mL of deionized water for ultrasonic dispersion; 120mL of absolute ethanol solution was then added and sonicated. After the ultrasonic treatment is finished, adding 4mL of ammonia water and 0.6mL of TEOS solution; then, the mixed solution was magnetically stirred for 20 hours to allow it to react sufficiently; finally, the reaction solution was centrifugedAnd washed 2-3 times with a mixture of ethanol and water.
The preparation method of the LMPET-PEG comprises the following steps:
dissolving 18.3g of LMPET in a solution of phenol and tetrachloroethane with the mass ratio of 1: 1, reacting at 60 ℃, heating to 100 ℃ after the reaction is completely dissolved (1 hour), and adding a small amount of cross-linking agent ethylene glycol (about 5mL) for several times in the reaction process. Then, 0.03g of polycondensation catalyst Sb was added to the three-necked flask2O3And 32ml PEG400, heating to 100 ℃, and continuously stirring for reaction for 2-3 hours. Washing with phenol and carbon tetrachloride solution in the mass ratio of 1 to remove the residual LMPET, washing with acetone and ethanol twice, centrifuging to remove the residual impurities, and vacuum drying the obtained LMPET-PEG.
Compared with the original pure PET fiber, the invention has the following advantages:
1. according to the invention, the silicon dioxide grown on the surface of the graphene oxide is used as the nano nucleating agent, so that the heterogeneous nucleation times are increased, the crystallization of molecules is promoted, the crystallization rate is accelerated, and the crystallization performance of the polyester is effectively improved. However, the effect of improving the performance is easily affected by the self-agglomeration of pure silica particles, and the problem can be effectively solved by growing silica on the surface of graphene oxide. This is because GO is an oxide of graphene, with carboxyl and carbonyl groups on the edges, and hydroxyl and epoxide on the matrix. The presence of these functional groups makes GO extremely hydrophilic with good compatibility with the polar polymer PET.
2. The invention synthesizes GO-SiO2The hybrid composite material is added into PET, so that the nucleating agent is successfully and uniformly dispersed in the PET, the crystallization performance and the thermal performance of PET fibers are improved under the condition of less addition amount, wherein the crystallization temperature is increased from 184 ℃ to 225 ℃, and the thermal decomposition temperature is increased by 15 ℃.
Drawings
FIG. 1 is an SEM image of PET fibers prepared by the method of the present invention;
FIG. 2 is an XRD curve of PET fiber prepared by the method of the present invention;
FIG. 3 is a DSC curve of a PET fiber prepared by the method of the present invention;
Detailed Description
The present invention will be described in detail with reference to specific examples.
Example 1
The invention discloses a method for improving the crystallization performance of polyester fibers by using a nucleation additive of a graphene oxide and silicon dioxide composite material, which comprises the following specific steps:
preparing a nucleating additive of the graphene oxide and silicon dioxide composite material: weighing 20mg of GO-SiO2Adding into 9.5mL ethanol +0.5mL water, ultrasonic pulverizing, dispersing, adding 1mL IPTES, adjusting pH to 4-5 with formic acid, refluxing at 70 deg.C, introducing N2And 6 h. Washing with ethanol for 2-3 times after the reaction is finished to obtain a sample GO-SiO2-IPTES. Sample GO-SiO2IPTES was dispersed in 10mL of DMF, 50mg of LMPET-PEG was dispersed in another 5mL of DMF, and the two were mixed, 50. mu.L of dibutyltin dilaurate DBDU was added, heated to 70 ℃ and magnetically stirred for 10 hours. I.e. forming GO-SiO2+ LMPET-PEG nanoparticles.
Preparing a PET fiber by using a nucleating additive of a graphene oxide and silicon dioxide composite material: firstly, granulating and blending the obtained nucleating additive containing the graphene oxide and PET according to a certain proportion, and then preparing the PET fiber containing the modified silicon dioxide by utilizing melt spinning of the produced granules.
Wherein, GO-SiO2The method for preparing the hybrid composite material comprises the following steps:
0.06g of GO nanoplates were first dissolved in 60mL of deionized water and ultrasonically dispersed. 120mL of absolute ethanol solution was then added and sonicated. After the completion of the sonication, 4mL of ammonia and 4mL of TEOS solution were added. Then, the mixed solution was magnetically stirred for 20 hours to allow it to react sufficiently. Finally, the reaction solution was centrifuged and washed 2-3 times with a mixture of ethanol and water.
The preparation method of the LMPET-PEG comprises the following steps:
dissolving 18.3g of LMPET in a solution of phenol and tetrachloroethane with the mass ratio of 1: 1, reacting at 60 ℃, heating to 100 ℃ after the reaction is completely dissolved (1 hour), and adding a small amount of cross-linking agent ethylene glycol (about 5mL) for several times in the reaction process. Then, 0.03g of polycondensation catalyst Sb2O3 and 32mLPEG400 were added to the three-necked flask, and the mixture was heated to 100 ℃ and stirred to react for 2 to 3 hours. Washing with phenol and carbon tetrachloride solution in the mass ratio of 1 to remove the residual LMPET, washing with acetone and ethanol twice, centrifuging to remove the residual impurities, and vacuum drying the obtained LMPET-PEG.
By scanning image analysis of the PET fiber, see FIG. 1, wherein a is pure PET fiber, and b is PET fiber with the content of 1 wt% of graphene oxide and silicon dioxide composite material. It is seen from the figure that the fibers are in the micron size and the fiber surface is smooth, indicating that the nucleating additive containing graphene oxide is more uniformly dispersed in the PET.
By the analysis of XRD and DSC, which are respectively shown in figure 2 and figure 3, the addition of the nucleation additive containing the graphene oxide improves the crystallinity of the PET fiber, and the crystallization temperature is improved by about 41 ℃, so that the improvement effect of the addition of the nucleation additive of the graphene oxide and silicon dioxide composite material on the performance of the PET fiber is obvious.
Example 2
Preparing a nucleating additive of the graphene oxide and silicon dioxide composite material: weighing 20mg of GO-SiO2Mixing the hybrid composite material with 9.5mL of ethanol and 0.5mL of water, ultrasonically crushing and dispersing, adding 1mL of IPTES, adjusting the pH value to 4-5 with formic acid, refluxing at 70 ℃, introducing N2And 6 h. After the reaction is finished, washing the reaction product for 2 to 3 times by using ethanol. The previous experiment obtains a sample GO-SiO2IPTES was dispersed in DMF (10mL), 50mg of LMPET-PPG (polypropylene glycol) was dispersed in DMF (5mL), and the two were mixed, 50. mu.L of BDU (dibutyltin dilaurate) was added, and the mixture was heated to 70 ℃ and stirred magnetically for 10 hours. I.e. forming GO-SiO2+ LMPET-PPG nanoparticles.
Preparing a PET fiber by using a nucleating additive of a graphene oxide and silicon dioxide composite material: firstly, granulating and blending the obtained nucleating additive containing the graphene oxide and PET according to a certain proportion, and then preparing the PET fiber containing the modified silicon dioxide by utilizing melt spinning of the produced granules.
Wherein, GO-SiO2Methods for the preparation of hybrid composites such asThe following:
0.06g of GO nanoplates were first dissolved in 60mL of deionized water and ultrasonically dispersed. 120mL of absolute ethanol solution was then added and sonicated. After the sonication was completed, 4mL of ammonia and 0.6mL of TEOS solution were added. Then, the mixed solution was magnetically stirred for 20 hours to allow it to react sufficiently. Finally, the reaction solution was centrifuged and washed 2-3 times with a mixture of ethanol and water.
The preparation method of the LMPET-PPG comprises the following steps:
dissolving 18.3g of LMPET in a solution of phenol and tetrachloroethane with the mass ratio of 1: 1, reacting at 60 ℃, heating to 100 ℃ after the reaction is completely dissolved (1 hour), and adding a small amount of cross-linking agent ethylene glycol (about 5mL) for several times in the reaction process. Then, 0.03g of polycondensation catalysts Sb2O3 and 32mLPPG were added to the three-necked flask, and the mixture was heated to 100 ℃ and stirred to react for 2 to 3 hours. Washing with a solution of phenol and carbon tetrachloride in a mass ratio of 1: 1 to remove the residual LMPET, washing with acetone and ethanol twice, centrifuging to remove the residual impurities, and vacuum drying the prepared LMPET-PPG.
It will be understood that modifications and variations can be made by persons skilled in the art in light of the above teachings and all such modifications and variations are intended to be included within the scope of the invention as defined in the appended claims.
Claims (7)
1. Using GO-SiO2The method for improving the crystallization performance of the polyester fiber by compounding the core forming additive is characterized in that GO-SiO2+ LMPET-PEG or GO-SiO2The + LMPET-PPG nano particles are granulated and blended with PET according to the proportion, and then the produced particles are melt spun to prepare the PET fiber containing the modified silicon dioxide;
GO-SiO2preparation of hybrid composite material: according to the following proportion: dissolving 0.06g of GO nano-sheets in 60mL of deionized water, performing ultrasonic dispersion, then adding 120mL of absolute ethyl alcohol, performing ultrasonic treatment, adding 4mL of ammonia water and 4mL of TEOS solution, adopting an in-situ hydrolysis method, taking TEOS as a silicon source, and converting the TEOS into silicon dioxide on the GO nano-sheets after hydrolysis;
graphene oxide and bisNucleating additive GO-SiO of silicon oxide composite material2+ LMPET-PEG or GO-SiO2Preparation of + LMPET-PPG: weighing 20mg of GO-SiO in the following proportion2Adding into 9.5mL ethanol +0.5mL water, ultrasonic pulverizing, dispersing, adding 1mL IPTES, adjusting pH to 4-5 with formic acid, refluxing at 70 deg.C, introducing N26 h; washing with ethanol for 2-3 times after the reaction is finished to obtain GO-SiO2-IPTES, dispersing GO-SiO2-IPTES into 10mL of DMF, dispersing 50mg of LMPET-PEG into 5mL of DMF, mixing the two, adding 50 mu L of dibutyltin dilaurate DBDU, heating to 70 ℃, and magnetically stirring for 10 hours to obtain GO-SiO2+ LMPET-PEG nanoparticles; the LMPET-PEG is replaced by LMPET-PPG to obtain GO-SiO2+ LMPET-PPG nanoparticles.
2. The method of claim 1, wherein: the GO nano-sheet is commercially available, the sheet diameter is 0.5-5 mu m, and the thickness is 0.8-1.2 nm; the molecular weight of LMPET is 5000-.
3. The method of claim 1, wherein: the PET used was a commercially available fiber grade PET having an intrinsic viscosity of 0.65 to 0.68 dL/g.
4. The method of claim 1, wherein: synthetic GO-SiO2+ LMPET-PEG or GO-SiO2The proportion of the + LMPET-PPG nano particles in the PET fiber is 0.2-1%.
5. The method of claim 1, wherein: the rotation speed for centrifugation is 7000-10000r/min, and the time is 6-10 minutes.
6. The method of claim 1, wherein: the GO/SiO2Preparing a hybrid composite material, namely, adopting an in-situ hydrolysis method, taking TEOS as a silicon source, and converting the TEOS into silicon dioxide on GO nano-sheets after hydrolysis; firstly, dissolving 0.06g of GO nano-sheets in 60mL of deionized water for ultrasonic dispersion; 120mL of absolute ethanol solution was then added and sonicated. After the ultrasonic treatment is finished, adding 4mL of ammonia water and 0.6mL of TEOS solution; then, mixingMagnetically stirring the mixed solution for 20 hours to fully react; finally, the reaction solution was centrifuged and washed 2-3 times with a mixture of ethanol and water.
7. The method of claim 1, wherein: the preparation method of LMPET-PEG is as follows:
dissolving 18.3g of LMPET in a mixed solution of phenol and tetrachloroethane with the mass ratio of 1: 1, reacting at 60 ℃, heating to 100 ℃ after complete dissolution, and adding a small amount of cross-linking agent ethylene glycol for several times in the reaction process; then, 0.03g of polycondensation catalyst Sb was added to the three-necked flask2O3And 32ml PEG400, heating to 100 ℃, and continuously stirring for reaction for 2-3 hours; washing with phenol and carbon tetrachloride solution in the mass ratio of 1 to remove the residual LMPET, washing with acetone and ethanol twice, centrifuging to remove the residual impurities, and vacuum drying the obtained LMPET-PEG.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114959942A (en) * | 2022-07-15 | 2022-08-30 | 浙江桐昆新材料研究院有限公司 | Antistatic anti-pilling moisture permeable heavy denier polyester drawn yarn and preparation method thereof |
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