CN111321485A - Preparation method of regenerated polyester wool tops - Google Patents
Preparation method of regenerated polyester wool tops Download PDFInfo
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- CN111321485A CN111321485A CN202010172294.1A CN202010172294A CN111321485A CN 111321485 A CN111321485 A CN 111321485A CN 202010172294 A CN202010172294 A CN 202010172294A CN 111321485 A CN111321485 A CN 111321485A
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- Prior art keywords
- polyester
- regenerated
- temperature
- bottle chips
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Classifications
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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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
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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
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
- D01D10/02—Heat treatment
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
- D01D5/088—Cooling filaments, threads or the like, leaving the spinnerettes
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/12—Stretch-spinning methods
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Organic Chemistry (AREA)
- Polymers & Plastics (AREA)
- Health & Medical Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Artificial Filaments (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
Abstract
The invention discloses a preparation method of regenerated polyester wool tops, which comprises the following steps: 1) carrying out alcoholysis on the recycled polyester bottle chips after cleaning, sorting and crushing, filtering an alcoholysis product to obtain BHET, adding a modified monomer into the BHET, and polymerizing to obtain functional regenerated PET; 2) after sorting, crushing and cleaning the recycled polyester bottle chips, mixing the recycled polyester bottle chips with the functional regenerated PET, drying the polyester bottle chips, and then melting the polyester bottle chips into a melt; 3) and conveying the melt into a spinning box to extrude and spin to prepare the regenerated polyester wool tops. The invention adopts a three-monomer modification technology, so that the easy-dyeing gene is grafted to a polyester macromolecular chain, and the addition of the fatty acid dibasic acid flexible gene obviously improves the dyeing property and the moisture absorption property of the wool top fiber, thereby leading the yarn fabric to be smooth, thin, full and comfortable, obviously enhancing the skin softening property, bright color and extremely strong anti-pilling property.
Description
Technical Field
The invention relates to a preparation method of regenerated polyester wool tops, and belongs to the technical field of textiles.
Background
Polyester is a renewable material, but when the polyester bottle chips are directly used for spinning, more impurities exist, and the quality of the formed yarn is influenced. Alcoholysis of polyesters also presents certain difficulties for high quality spinning, especially with difficulty in meeting fiber "zero defects" requirements.
Disclosure of Invention
The invention aims to blend sorted, crushed and cleaned bottle flakes with regenerated polyester and provides a preparation method of regenerated polyester tops.
The technical scheme of the invention is as follows:
a preparation method of regenerated polyester wool tops comprises the following steps:
1) carrying out alcoholysis on the recycled polyester bottle chips after cleaning, sorting and crushing, filtering an alcoholysis product to obtain BHET, adding a modified monomer into the BHET, polymerizing to obtain functional regenerated PET, and recycling redundant ethylene glycol in the polymerization process;
in the esterification process, some impurities (PP and the like after being melted) can be brought out in the vacuumizing process, and the melt is filtered, so that purer BHET can be obtained, the polymerization reaction efficiency is improved, and the performance of a polymerization product is improved.
2) After sorting, crushing and cleaning the recycled polyester bottle chips, mixing the recycled polyester bottle chips with the functional regenerated PET obtained in the step 1), drying the mixture, and then melting the mixture into a melt;
3) and conveying the melt into a spinning box to extrude and spin to prepare the regenerated polyester wool tops.
Preferably, the alcoholysis condition in the step 1) is that 300kg of MEG is added into each ton of polyester bottle chips, and Sb with the mass fraction of two ten-thousandth is added2O3A catalyst; alcoholysis reaction temperature: 250-260 ℃; alcoholysis time: for 4 hours.
Preferably, the modified monomers are SIPM (dimethyl isophthalate-5-sodium sulfonate) and saturated fatty acid, the adding amount of the SIPM is 120 kg/ton of polyester, the adding amount of the fatty acid is 50 kg/ton of polyester, the SIPM is esterified by ethylene glycol before being added, methanol is extracted in the esterification process, the extracting amount of the methanol is 150ml per ton of SIPM, and the fatty acid is directly added.
Preferably, the filtration is performed by using a special melt filter.
Preferably, the polymerization conditions in step 1) are as follows: the low vacuum temperature is more than or equal to 260 ℃, the vacuum degree is 70Pa, and the time is 50 minutes;
the high vacuum temperature is more than or equal to 265 ℃, the vacuum degree is 60Pa, and the time is 60 minutes;
the temperature reduction point is 266 ℃;
reaction final temperature: 282 ℃;
the discharge pressure (N2) is less than or equal to 0.4 MPa. The reaction system is an exothermic reaction, the temperature-raising valve is closed after the temperature-lowering point is reached, and finally the temperature of the reaction system is raised to about 282 ℃.
Preferably, the feeding ratio in the step 2) is that the functional recycled PET350kg is added in every 650kg of polyester bottle chips.
Preferably, the drying time after mixing in step 2) is 12 hours, the maximum temperature is 150 +/-2 ℃, and the moisture after drying is below 50 PPM.
Preferably, the regenerated polyester wool top is prepared by carrying out circular blowing cooling, oiling, winding, traction, feeding, drafting, curling, drying and packaging after spinning in the step 3), wherein the temperature of a spinning screw is 278 ℃ in a first zone, 285 ℃ in a second zone, 290 ℃ in a third zone, 287 ℃ in a fourth zone, 285 ℃ in a fifth zone, 285 ℃ in a sixth zone, 285 ℃ in a box body, the cooling distance is 2-3cm, the cooling air temperature is 20-30 ℃, the air speed is 1-2m/s, the spinning speed is 1200-1400 m/min, the stretching multiple is 3.0-3.5 times, and the drafting temperature is 60-80 ℃.
Has the advantages that: the invention adopts a three-monomer modification technology, regenerated easy-to-dye fibers (wool tops) are chemically modified, so that easy-to-dye genes are grafted to a polyester macromolecular chain, and the addition of fatty acid dibasic acid flexible genes obviously improves the dyeing property and the moisture absorption property of the wool top fibers, so that the yarn fabric is smooth, fine, full and comfortable, the skin softening property is obviously enhanced, the color is bright, and the yarn fabric can be applied to semi-worsted, single-mark spinning and blended fabrics of acrylic fibers and wool and is also suitable for knitted fabrics. The fabric has strong wool and pilling resistance. The invention solves the difficult problem of the functionalization of the regenerated fiber; meanwhile, the bottle flakes (PET) and the regenerated functional polyester are blended, so that the quality is stable, the cost is low, the fiber meets the functional requirements, and different products can be developed according to the blending proportion to meet the market demand. The prepared wool top and wool blended fabric can be dyed in one bath, and the dyeing property is consistent with that of wool.
Detailed Description
Examples 1 to 3
The preparation method of the regenerated polyester wool tops comprises the following steps:
1) carrying out alcoholysis on the recycled polyester bottle chips after cleaning, sorting and crushing, filtering an alcoholysis product to obtain BHET, adding a modified monomer into the BHET, polymerizing to obtain functional regenerated PET, and recycling redundant ethylene glycol in the polymerization process;
2) after sorting, crushing and cleaning the recycled polyester bottle chips, mixing the recycled polyester bottle chips with the functional regenerated PET obtained in the step 1), drying the mixture, and then melting the mixture into a melt;
3) and conveying the melt into a spinning box to extrude and spin to prepare the regenerated polyester wool tops.
The properties of the obtained regenerated polyester tops were measured, and the results are shown in table 2.
The spinning screw temperature is 278 ℃ in the first zone, 285 ℃ in the second zone, 290 ℃ in the third zone, 287 ℃ in the fourth zone, 285 ℃ in the fifth zone and 285 ℃ in the sixth zone.
TABLE 1 Process parameters for examples 1-3
| Index (I) | Example 1 | Example 2 | Example 3 | Comparative example |
| Temperature of the tank (. degree. C.) | 282 | 285 | 287 | 295 |
| Cooling distance (cm) | 2 | 4 | 3 | 6 |
| Wind temperature (. degree. C.) | 28 | 32 | 30 | 22 |
| Speed division (m/s) | 1.0 | 1.5 | 1.2 | 1.8 |
| Spinning speed (meter/minute) | 1280 | 1350 | 1420 | 1490 |
| Stretching ratio | 3.0 | 3.1 | 3.2 | 3.5 |
| Draft temperature (. degree. C.) | 68.0 | 72.0 | 70.0 | 75 |
TABLE 2 product indices for examples 1-3
Claims (8)
1. A preparation method of regenerated polyester wool tops comprises the following steps:
1) carrying out alcoholysis on the recycled polyester bottle chips after cleaning, sorting and crushing, filtering an alcoholysis product to obtain BHET, adding a modified monomer into the BHET, and polymerizing to obtain functional regenerated PET;
2) after sorting, crushing and cleaning the recycled polyester bottle chips, mixing the recycled polyester bottle chips with the functional regenerated PET obtained in the step 1), drying the mixture, and then melting the mixture into a melt;
3) and conveying the melt into a spinning box to extrude and spin to prepare the regenerated polyester wool tops.
2. The method for preparing the regenerated polyester tops according to claim 1, characterized in that: step 1) alcoholysis conditions are that 300kg of MEG is added into each ton of polyester bottle chips, and Sb with the mass fraction of two ten-thousandth is added2O3A catalyst; alcoholysis reaction temperature: 250-260 ℃; alcoholysis time: for 4 hours.
3. The method for preparing the regenerated polyester tops according to claim 2, characterized in that: the filtration is carried out by adopting a special melt filter.
4. The method for preparing the regenerated polyester tops according to claim 3, characterized in that: the modified monomer is SIPM and fatty acid, the adding amount of the SIPM is 120 kg/ton of polyester, the adding amount of the fatty acid is 50 kg/ton of polyester, the SIPM is esterified by ethylene glycol before being added, methanol is extracted in the esterification process, and the extracting amount is 150ml of methanol per ton of SIPM.
5. The method for preparing the regenerated polyester tops according to claim 4, characterized in that: the polymerization reaction conditions in the step 1) are as follows: the low vacuum temperature is more than or equal to 260 ℃, the vacuum degree is 70Pa, and the time is 50 minutes;
the high vacuum temperature is more than or equal to 265 ℃, the vacuum degree is 60Pa, and the time is 60 minutes;
the temperature reduction point is 266 ℃;
reaction final temperature: 282 ℃;
the discharge pressure is less than or equal to 0.4 MPa.
6. The method for preparing the regenerated polyester tops according to any one of claims 1 to 5, wherein: the feeding ratio in the step 2) is 350kg of functional recycled PET added into every 650kg of polyester bottle chips.
7. The method for preparing the regenerated polyester tops according to claim 6, characterized in that: the drying time after mixing in the step 2) is 12 hours, the highest temperature is 150 +/-2 ℃, and the moisture after drying is below 50 PPM.
8. The method for preparing the regenerated polyester tops according to claim 6, characterized in that: and 3) carrying out circular blowing cooling, oiling, winding, traction, feeding, drafting, curling, drying and packaging after spinning to prepare the regenerated polyester wool tops, wherein the temperature of a spinning screw is 278 ℃ in a first zone, 285 ℃ in a second zone, 290 ℃ in a third zone, 287 ℃ in a fourth zone, 285 ℃ in a fifth zone, 285 ℃ in a sixth zone, 285 ℃ in a box body, the cooling distance is 2-3cm, the cooling air temperature is 20-30 ℃, the air speed is 1-2m/s, the spinning speed is 1200-1400 m/min, the stretching multiple is 3.0-3.5 times, and the drafting temperature is 60-80 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010172294.1A CN111321485A (en) | 2020-03-12 | 2020-03-12 | Preparation method of regenerated polyester wool tops |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010172294.1A CN111321485A (en) | 2020-03-12 | 2020-03-12 | Preparation method of regenerated polyester wool tops |
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| Publication Number | Publication Date |
|---|---|
| CN111321485A true CN111321485A (en) | 2020-06-23 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010172294.1A Pending CN111321485A (en) | 2020-03-12 | 2020-03-12 | Preparation method of regenerated polyester wool tops |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116180285A (en) * | 2023-02-01 | 2023-05-30 | 张家港市荣昌涤纶毛条有限公司 | Composite polyester ultra-soft long cilia strip and preparation method thereof |
-
2020
- 2020-03-12 CN CN202010172294.1A patent/CN111321485A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116180285A (en) * | 2023-02-01 | 2023-05-30 | 张家港市荣昌涤纶毛条有限公司 | Composite polyester ultra-soft long cilia strip and preparation method thereof |
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Application publication date: 20200623 |