CN109137136A - A kind of preparation method and application of the compound fibrid of PET-PA66 - Google Patents

A kind of preparation method and application of the compound fibrid of PET-PA66 Download PDF

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Publication number
CN109137136A
CN109137136A CN201810814573.6A CN201810814573A CN109137136A CN 109137136 A CN109137136 A CN 109137136A CN 201810814573 A CN201810814573 A CN 201810814573A CN 109137136 A CN109137136 A CN 109137136A
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pet
compound
fibrid
preparation
paper
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CN201810814573.6A
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Chinese (zh)
Inventor
张素风
宋宝玉
张斌
张美娟
刘丽娜
李豪
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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Priority to CN201810814573.6A priority Critical patent/CN109137136A/en
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/14Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/12Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyamide as constituent

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Paper (AREA)

Abstract

The invention discloses a kind of preparation method and applications of the compound fibrid of PET-PA66, and PET and PA66 are dissolved in cosolvent first, obtain PET-PA66 mixed solution;Then PET-PA66 mixed solution is instilled in coagulating bath and is sheared, is washed with distilled water after shearing several times to get the compound fibrid of PET-PA66.The present invention has prepared the compound fibrid of PET-PA66 of different specific surface areas, hydrophilicity, good dispersion using precipitation method, and can be applied to the production of PET speciality paper, prepares the good paper base material of mechanical strength.

Description

A kind of preparation method and application of the compound fibrid of PET-PA66
Technical field
The invention belongs to synthetic fiber technologies, and in particular to a kind of preparation method of the compound fibrid of PET-PA66 With application.
Background technique
Polyethylene terephthalate (PET) is used as the maximum synthetic fibers of current industrial production scale, uses extensively In fields such as packaging, filtering and electrical insulating materials.The high intensity of PET fiber production, heat resistance speciality paper can be applied to resistance to height Warm insulating paper, filtering material, reverse osmosis membrane backing material etc., but the polar group contained in PET self-molecules present is lower, it is fine Dimension dispersed poor, easy aggregation in water, thus limit the extensive use in speciality paper.
Summary of the invention
The purpose of the present invention is to provide the preparation methods and application of a kind of compound fibrid of PET-PA66, are made with overcoming The problem of paper PET fiber bad dispersibility, the present invention have prepared the PET- of different specific surface areas, hydrophilicity using precipitation method The compound fibrid of PA66, good dispersion, and can be applied to the production of PET speciality paper, prepare the good paper base of mechanical strength Material.
In order to achieve the above objectives, the present invention adopts the following technical scheme:
A kind of preparation method of the compound fibrid of PET-PA66, comprising the following steps:
(1) PET and PA66 are dissolved in cosolvent, obtain PET-PA66 mixed solution;
(2) PET-PA66 mixed solution is instilled in coagulating bath and is sheared, is washed with distilled water after shearing several It is secondary to get the compound fibrid of PET-PA66.
Further, PET and PA66 95:5~80:20 in mass ratio is dissolved in cosolvent in step (1).
Further, the mixture of 36.25g PET and PA66 is added in step (1) in every 300mL cosolvent.
Further, in step (1) cosolvent be phenol and tetrachloroethanes mixture, and the body of phenol and tetrachloroethanes Product is than being 1:1.
Further, solution temperature is 65 DEG C -75 DEG C in step (1).
Further, drop rate is 2~5mL/min in step (2).
Further, PET-PA66 mixed solution is instilled into stirring rate when being sheared in coagulating bath in step (2) For 1500-2000rpm, mixing time 30-60min.
Further, coagulating bath is made of glycerol and dehydrated alcohol in step (2), and the volume ratio of glycerol and dehydrated alcohol For (3~7): (1~3).
A kind of application of the compound fibrid of PET-PA66 mixes the compound fibrid of PET-PA66 with PET chopped strand After conjunction, using wet papermaking process at paper.
Further, the absolute dry mass ratio of the compound fibrid of the PET-PA66 and PET chopped strand is 1:1.
Compared with prior art, the invention has the following beneficial technical effects:
The present invention dissolves PET the and PA66 resin of different quality ratio in cosolvent, has been prepared not using precipitation method The compound fibrid of PET-PA66 of same specific surface area, hydrophilicity, and applied using wet papermaking technology in PET paper In preparation, the bonding between the compound fibrid of PET-PA66 and PET fiber is even closer, assigns the higher mechanical strength of PET paper, It prolongs its service life, widens its application field.The present invention, which utilizes, contains a large amount of polar group in polyamide 66 (PA66), and And have good compatibility between PET and PA66, the PET- of good dispersion has been prepared using polymer blend method and precipitation method The compound fibrid of PA66, in wet process in paper, fiber can be evenly dispersed and close with other fibres bonds, to generate tool There is high-intensitive, durothermic PET special type paper base material, used precipitation method is that polymer solution is instilled to coagulating for high speed shear Gu under the action of shear force, polymer solution droplets are gradually stretched parallel, and then are progressively solidified into a fixed length in bath The fiber of diameter ratio is a kind of fiber producing processes efficiently, controllable, inexpensive.
Using the compound fibrid of PET-PA66 prepared by the present invention have it is of uniform size it is tiny, specific surface area is larger, close The features such as aqueous good, the length of the compound fibrid of PET-PA66 of different quality ratio are 0.23-0.42mm, width 24.8- 26.5 μm, specific surface area 7.89-10.23m2/ g, contact angle is 83-92 °, by the compound fibrid of PET-PA66 of the invention Applied in the manufacturing paper with pulp of PET paper, the tensile index of paper is 34.82-39.43Nm/g, tear index 22.61- 30.24mN·m2/g。
Specific embodiment
Embodiments of the present invention are described in further detail below:
The present invention specifically realizes according to the following steps:
1) firstly, PET and PA66 resin to be added in three-necked flask according to certain mass ratio to (PET and PA66 are adopted 4*5*2 millimeters or so of sheet-like particle is used with slice, in present embodiment, but not limited to this), and phenol and tetrachloro is added Ethane cosolvent (phenol and tetrachloroethanes volume ratio be 1:1), three-necked flask is placed in 65 DEG C -75 DEG C of water-bath, is stirred medium It mixes under rate, by dissolving up to uniformly mixed PET-PA66 mixed solution for certain time.The wherein quality of PA66 and PET Than being the key that compound fibrid hydrophily and evenly dispersed in water, the mass ratio of PET and PA66 is 95:5- in the present invention The mixture of 36.25g PET and PA66 are added in every 300mL cosolvent by 80:20.
2) the PET-PA66 mixed solution of above-mentioned preparation is instilled into the solidifying of high-speed stirred with the drop rate of 2~5mL/min Gu in bath, 30-60min is stirred under the stirring rate of 1500-2000rpm, stretcher strain, final solidification, fibril occur for drop It is melted into the compound fibrid of PET-PA66, wherein coagulating bath is made of glycerol and dehydrated alcohol, and the body of glycerol and dehydrated alcohol Product is than being (3~7): (1~3).
Wherein stirring rate significantly affects the size of fiber, and stirring rate is preferably 1500rpm;The type of coagulating bath Influence fiber formation whether or its fibre crystallinity can difference, the present invention in coagulating bath be made of glycerol and dehydrated alcohol.
3) the compound fibrid of the PET-PA66 of above-mentioned formation is washed with distilled water 3 times, it is therefore an objective to remove fiber surface Extra solvent, finally the fiber of washing is dried, is saved.
4) table is carried out to the length of the compound fibrid of the PET-PA66 of above-mentioned preparation, width, specific surface area, contact angle Sign, the instrument used are followed successively by fiber quality analyzer, specific surface area analysis instrument and video optical contact angle meter.By what is characterized Each data of the compound fibrid of PET-PA66 can directly or indirectly show the difference of fiber dispersion performance in water, with And it can be used in wet papermaking, the bond enhancing material of paper base material.
5) the compound fibrid of PET-PA66 and PET fiber are manufactured paper with pulp into paper according to identical mass ratio, fibrous suspension PET paper is formed by techniques such as online, drainage and formation, drying, hot pressing.
6) tensile index and tear index of PET paper are carried out using automatic tensile strength tester, paper tear degree instrument Characterization, shows that specific surface area is larger, contact angle is smaller, the dispersed preferable compound fibrid of PET-PA66 is conducive to improve The mechanical performance of PET paper.
Below with reference to embodiment, the invention will be described in further detail:
Embodiment 1
1) PET and PA66 resin is weighed into 34.44g and 1.81g according to mass ratio 95:5 respectively first, be added to phenol and In the 300mL cosolvent of tetrachloroethanes, under 70 DEG C of water bath condition, 25min is persistently stirred, resin dissolves to obtain mass fraction For 10% PET-PA66 mixed solution;
2) the PET-PA66 mixed solution of 50mL step 1) preparation is measured, instilling shear velocity with 4mL/min rate is In the coagulating bath of 1000rpm, coagulating bath is made of the dehydrated alcohol of 600mL and the glycerol of 200mL, stops stirring after high speed shear 1h It mixes, obtains the mixed liquor containing the compound fibrid of PET-PA66;
3) mixed liquor of the compound fibrid of PET-PA66 formed in step 2) is filtered, obtained fiber distilled water Washing 3 times, finally drying simultaneously save;
4) size and hydrophilic characterization are carried out to the compound fibrid of the PET-PA66 prepared in step 3), obtains fiber Length be 0.42mm, width be 26.5 μm, specific surface area 7.89m2/ g, contact angle are 92 °, and the compound precipitating of PET-PA66 is fine The size and specific surface area of dimension meet wet process into the requirement of fiber size in paper, can preferably disperse in an aqueous medium;
5) by the compound fibrid of PET-PA66 of step 4) preparation and PET fiber according to mass ratio 5:5, using wet process at Paper and subsequent hot-pressing processing form quantification of 100g/m2PET paper;
6) PET paper prepared by step 5) is measured using automatic tensile strength tester, paper tear degree instrument, is obtained The tensile index of paper is 34.82Nm/g, tear index 22.61mNm2/g。
Embodiment 2
1) PET and PA66 resin is weighed into 32.62g and 3.63g according to mass ratio 90:10 first respectively, is added to phenol In the 300mL cosolvent of tetrachloroethanes, under 65 DEG C of water bath condition, 30min is persistently stirred, resin dissolves to obtain quality point The PET-PA66 mixed solution that number is 10%;
2) the PET-PA66 mixed solution of 50mL step 1) preparation is measured, instilling shear velocity with 5mL/min rate is In the coagulating bath of 1500rpm, coagulating bath is made of the dehydrated alcohol of 500mL and the glycerol of 300mL, is stopped after high speed shear 45min It only stirs, obtains the mixed liquor containing the compound fibrid of PET-PA66;
3) mixed liquor of the compound fibrid of PET-PA66 formed in step 2) is filtered, obtained fiber distilled water Washing 3 times, finally drying simultaneously save;
4) size and hydrophilic characterization are carried out to the compound fibrid of the PET-PA66 prepared in step 3), obtains fiber Length be 0.33mm, width be 25.8 μm, specific surface area 8.18m2/ g, contact angle are 89 °, and the compound precipitating of PET-PA66 is fine The size and specific surface area of dimension meet wet process into the requirement of fiber size in paper, can preferably disperse in an aqueous medium;
5) by the compound fibrid of PET-PA66 of step 4) preparation and PET fiber according to mass ratio 5:5, using wet process at Paper and subsequent hot-pressing processing form quantification of 100g/m2PET paper;
6) PET paper prepared by step 5) is measured using automatic tensile strength tester, paper tear degree instrument, is obtained The tensile index of paper is 35.52Nm/g, tear index 24.03mNm2/g。
Embodiment 3
1) PET and PA66 resin is weighed into 30.81g and 5.44g according to mass ratio 85:15 first respectively, is added to phenol In the 300mL cosolvent of tetrachloroethanes, under 67 DEG C of water bath condition, 28min is persistently stirred, resin dissolves to obtain quality point The PET-PA66 mixed solution that number is 10%;
2) the PET-PA66 mixed solution of 50mL step 1) preparation is measured, instilling shear velocity with 3mL/min rate is In the coagulating bath of 1500rpm, coagulating bath is made of the dehydrated alcohol of 700mL and the glycerol of 100mL, stops stirring after high speed shear 1h It mixes, obtains the mixed liquor containing the compound fibrid of PET-PA66;
3) mixed liquor of the compound fibrid of PET-PA66 formed in step 2) is filtered, obtained fiber distilled water Washing 3 times, finally drying simultaneously save;
4) size and hydrophilic characterization are carried out to the compound fibrid of the PET-PA66 prepared in step 3), obtains fiber Length be 0.28mm, width be 25.5 μm, specific surface area 9.57m2/ g, contact angle are 87 °, and the compound precipitating of PET-PA66 is fine The size and specific surface area of dimension meet wet process into the requirement of fiber size in paper, can preferably disperse in an aqueous medium, Its mechanical property can be significantly improved by being added in paper;
5) by the compound fibrid of PET-PA66 of step 4) preparation and PET fiber according to mass ratio 5:5, using wet process at Paper and subsequent hot-pressing processing form quantification of 100g/m2PET paper;
6) PET paper prepared by step 5) is measured using automatic tensile strength tester, paper tear degree instrument, is obtained The tensile index of paper is 36.67Nm/g, tear index 28.92mNm2/g。
Embodiment 4
1) PET and PA66 resin is weighed into 29.00g and 7.25g according to mass ratio 80:20 first respectively, is added to phenol In the 300mL cosolvent of tetrachloroethanes, under 75 DEG C of water bath condition, 20min is persistently stirred, resin dissolves to obtain quality point The PET-PA66 mixed solution that number is 10%;
2) the PET-PA66 mixed solution of 50mL step 1) preparation is measured, instilling shear velocity with 2mL/min rate is In the coagulating bath of 2000rpm, coagulating bath is made of the dehydrated alcohol of 550mL and the glycerol of 250mL, is stopped after high speed shear 30min It only stirs, obtains the mixed liquor containing the compound fibrid of PET-PA66;
3) mixed liquor of the compound fibrid of PET-PA66 formed in step 2) is filtered by vacuum, obtained fiber It is washed with distilled water 3 times, finally drying simultaneously saves;
4) size and hydrophilic characterization are carried out to the compound fibrid of the PET-PA66 prepared in step 3), obtains fiber Length be 0.23mm, width be 24.8 μm, specific surface area 10.23m2/ g, contact angle are 83 °, the compound precipitating of PET-PA66 The size and specific surface area of fiber meet wet process into the requirement of fiber size in paper, can preferably be dispersed in aqueous medium In, its mechanical property can be significantly improved by being added in paper;
5) by the compound fibrid of PET-PA66 of step 4) preparation and PET fiber according to mass ratio 5:5, using wet process at Paper and subsequent hot-pressing processing form quantification of 100g/m2PET paper;
6) PET paper prepared by step 5) is measured using automatic tensile strength tester, paper tear degree instrument, is obtained The tensile index of paper is 39.43Nm/g, tear index 30.24mNm2/g。
It is obtained by above-mentioned 4 embodiments, with the increase of PA66 content contained in the compound fibrid of PET-PA66, warp The size for crossing the fiber of precipitation process preparation becomes smaller, and original fiber degree increases, hydrophily enhancing, can uniformly be situated between in water Disperse in matter, to preferably be applied in wet papermaking, is added in PET paper or other paper base materials, effectively improves paper Whole mechanical strength is opened, its application range is widened.

Claims (10)

1. a kind of preparation method of the compound fibrid of PET-PA66, which comprises the following steps:
(1) PET and PA66 are dissolved in cosolvent, obtain PET-PA66 mixed solution;
(2) PET-PA66 mixed solution is instilled in coagulating bath and is sheared, is washed with distilled water after shearing several times, i.e., Obtain the compound fibrid of PET-PA66.
2. a kind of preparation method of the compound fibrid of PET-PA66 according to claim 1, which is characterized in that step (1) PET and PA66 95:5~80:20 in mass ratio is dissolved in cosolvent in.
3. a kind of preparation method of the compound fibrid of PET-PA66 according to claim 2, which is characterized in that step (1) mixture of 36.25g PET and PA66 is added in every 300mL cosolvent.
4. a kind of preparation method of the compound fibrid of PET-PA66 according to claim 1, which is characterized in that step (1) cosolvent is the mixture of phenol and tetrachloroethanes in, and the volume ratio of phenol and tetrachloroethanes is 1:1.
5. a kind of preparation method of the compound fibrid of PET-PA66 according to claim 1, which is characterized in that step (1) solution temperature is 65 DEG C -75 DEG C in.
6. a kind of preparation method of the compound fibrid of PET-PA66 according to claim 1, which is characterized in that step (2) drop rate is 2~5mL/min in.
7. a kind of preparation method of the compound fibrid of PET-PA66 according to claim 1, which is characterized in that step (2) it is 1500-2000rpm that PET-PA66 mixed solution, which is instilled stirring rate when being sheared in coagulating bath, in, when stirring Between be 30-60min.
8. a kind of preparation method of the compound fibrid of PET-PA66 according to claim 1, which is characterized in that step (2) coagulating bath is made of glycerol and dehydrated alcohol in, and the volume ratio of glycerol and dehydrated alcohol is (3~7): (1~3).
9. a kind of application of the compound fibrid of PET-PA66, the compound fibrid of PET-PA66 uses claim 1 institute A kind of preparation method for the compound fibrid of PET-PA66 stated is prepared, which is characterized in that by the compound precipitating of PET-PA66 After fiber is mixed with PET chopped strand, using wet papermaking process at paper.
10. a kind of application of the compound fibrid of PET-PA66 according to claim 9, which is characterized in that the PET- The absolute dry mass ratio of the compound fibrid of PA66 and PET chopped strand is 1:1.
CN201810814573.6A 2018-07-23 2018-07-23 A kind of preparation method and application of the compound fibrid of PET-PA66 Pending CN109137136A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110184677A (en) * 2019-06-03 2019-08-30 江苏扬农化工集团有限公司 A kind of preparation method of PPTA-MPIA In-situ reaction fibrid
CN110820424A (en) * 2019-10-16 2020-02-21 陕西科技大学 Novel filter paper and preparation method thereof
CN113481627A (en) * 2021-07-05 2021-10-08 陕西科技大学 Preparation method of PET-PVA composite fibrid

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Publication number Priority date Publication date Assignee Title
CN103889675A (en) * 2011-11-04 2014-06-25 伊士曼化工公司 Processes for recycling carpet and products of such processes
CN104559174A (en) * 2015-01-29 2015-04-29 北京科方创业科技企业孵化器有限公司 Preparation method of unenhanced halogen-free flame retardant nylon 66
CN106751806A (en) * 2016-12-29 2017-05-31 上海普利特复合材料股份有限公司 A kind of reactive compatibilizer prepares the alloy material for reclaiming carpet PA66 resins and recycled PET

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Publication number Priority date Publication date Assignee Title
CN103889675A (en) * 2011-11-04 2014-06-25 伊士曼化工公司 Processes for recycling carpet and products of such processes
CN104559174A (en) * 2015-01-29 2015-04-29 北京科方创业科技企业孵化器有限公司 Preparation method of unenhanced halogen-free flame retardant nylon 66
CN106751806A (en) * 2016-12-29 2017-05-31 上海普利特复合材料股份有限公司 A kind of reactive compatibilizer prepares the alloy material for reclaiming carpet PA66 resins and recycled PET

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Title
张素风: "实验部分、结果与讨论部分", 《PET-PA66相容性及其复合沉析纤维的制备方法》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110184677A (en) * 2019-06-03 2019-08-30 江苏扬农化工集团有限公司 A kind of preparation method of PPTA-MPIA In-situ reaction fibrid
CN110184677B (en) * 2019-06-03 2021-11-26 江苏瑞盛新材料科技有限公司 Preparation method of PPTA-MPIA in-situ composite fibrid
CN110820424A (en) * 2019-10-16 2020-02-21 陕西科技大学 Novel filter paper and preparation method thereof
CN113481627A (en) * 2021-07-05 2021-10-08 陕西科技大学 Preparation method of PET-PVA composite fibrid

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Application publication date: 20190104