CN105733093A - Special high-flowability resin for polypropylene fibers and preparation method thereof - Google Patents
Special high-flowability resin for polypropylene fibers and preparation method thereof Download PDFInfo
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- CN105733093A CN105733093A CN201610181375.1A CN201610181375A CN105733093A CN 105733093 A CN105733093 A CN 105733093A CN 201610181375 A CN201610181375 A CN 201610181375A CN 105733093 A CN105733093 A CN 105733093A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/14—Peroxides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
- C08K5/098—Metal salts of carboxylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/10—Esters; Ether-esters
- C08K5/101—Esters; Ether-esters of monocarboxylic acids
- C08K5/103—Esters; Ether-esters of monocarboxylic acids with polyalcohols
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/13—Phenols; Phenolates
- C08K5/134—Phenols containing ester groups
- C08K5/1345—Carboxylic esters of phenolcarboxylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/524—Esters of phosphorous acids, e.g. of H3PO3
- C08K5/526—Esters of phosphorous acids, e.g. of H3PO3 with hydroxyaryl 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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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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
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/46—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyolefins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/12—Applications used for fibers
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Abstract
The invention discloses a special high-flowability resin for polypropylene fibers. The resin is mainly prepared from a homopolymer polypropylene resin, organic peroxides, an antioxidant and processing aids. On the basis of the mass of the homopolymer polypropylene resin, the mass ratio of the homopolymer polypropylene resin to the organic peroxides is 100:(0.04-0.12), the mass ratio of the homopolymer polypropylene resin to the antioxidant is 100:(0.10-0.25), and the mass ratio of the homopolymer polypropylene resin to the processing aids is 100:(0.05-0.15). The special high-flowability resin for polypropylene fibers has the advantages of high melt index, narrow molecular weight distribution, excellent mechanical properties, higher elongation at break, low ash content, favorable chroma and other favorable fiber forming properties.
Description
Technical field
The present invention relates to a kind of acrylic resin, it is resin dedicated to be specifically related to a kind of high-flowability polypropylene fiber, meanwhile, the invention still further relates to the preparation method that this polypropylene fibre is resin dedicated.
Background technology
Fiber is the fourth-largest consumer field of acrylic resin, polypropylene fibre is a kind of fibre made for raw material by melt spinning with polypropylene, due to polypropylene fibre there is light weight, avirulence, wear-resisting, hydrophobic, bear dirty, the washable easily advantage such as dry, heat insulation, it is widely used in industry, agricultural, packaging, domestic, the various fields such as medical, it is kind with fastest developing speed in synthetic fibers in recent years, it has also become be only second to the second largest synthetic fiber products of terylene.Polypropylene fibre can be divided into flat filament, long filament, chopped fiber, bicomponent fibre etc. with fibre morphology classification；Divide by processing method and can be divided into spine silk, common long filament, composite fibre buiky yarn, chopped fiber, non-woven fabrics etc..Wherein non-woven fabrics is owing to having special performance, develop rapidly, the application and the demand that make polypropylene fibre constantly expand, except as industrial cloth, filtering material, geotextiles, agricultural fabric, covering material, it is also possible in aspects such as medical material, hygienic material, disposable material, clothing, decorations.
Along with polypropylene fibre is differential, the development of functionalization, the performance that fibrous polypropylene is resin dedicated be it is also proposed higher requirement, it must have high melt flow rate (MFR), Narrow Molecular Weight Distribution, high isotactic, high elongation at tear, low ash and gel particles etc., to improve Fiber spinning speeds, reduce processing temperature, so could improve service efficiency and reduce energy consumption；High tensile property then can reduce fibre number, and goods are thin, meets non-woven fabrics to the performance requirement such as feel, intensity.
At present, the method for industrial production high-flowability polypropylene mainly has hydrogen to adjust method and controllable flow political reform two kinds.The former adopts new catalyst to combine the method regulating high polymerization inhibitor such as density of hydrogen, reduces polypropylene molecule amount, thus improving polypropylene melt index.The method is subject to the restriction such as catalyst system, reaction condition, and product molecular weight distribution is relatively wide, is unfavorable for improving the intensity of fiber；Additionally, during industrialized production, Transition Materials is many, polymerization reactor control difficulty is big.The latter is in extruding pelletization process, adds peroxide and degrades, to improve its melt index in polypropylene base resin.It is short that this method produces transformation process, and Transition Materials is few, and polyreaction is easily controlled, and its product has the advantages such as melt index controlled range width, narrow molecular weight distribution.
Although the domestic report having high-flowability polypropylene fiber resin dedicated, but it is big to there is melting means fluctuation in product quality, molecular weight distribution width, less stable, impurity content is higher, produce during thin product fracture of wire and the problem such as doubling phenomena is serious, can be only applied in the disposable diaper of industry cloth and low side, then rely primarily on import solve for producing the needed raw materials such as the fine-denier of high-end polypropylene fibre goods, super fine denier, slim fibre.Therefore, be badly in need of wanting a kind of method prepare high-flowability polypropylene resin, while there is high fusion index, Narrow Molecular Weight Distribution, moreover it is possible to generally maintain the mechanical property of product, it is ensured that resin there is homogeneous, stable fibre-forming performance, can be suitably used for slim textile fabrics.
Summary of the invention
An object of the present invention is to provide that a kind of high-flowability polypropylene fiber is resin dedicated, and it has high fusion index, Narrow Molecular Weight Distribution, is maintained with excellent mechanical property, the good fibre-forming performance such as have that higher elongation at break, ash be low and colourity is good.
The two of the purpose of the present invention are to provide the preparation method that above-mentioned high-flowability polypropylene fiber is resin dedicated, and this preparation method is simple, and polyreaction is easily controlled, and are suitable for industrialized production.
First purpose of the present invention is achieved through the following technical solutions: a kind of high-flowability polypropylene fiber is resin dedicated, it is prepared from HOPP resin, organic peroxide, antioxidant and processing aid for primary raw material, with the quality of HOPP resin for benchmark, the mass ratio between described raw material is:
HOPP resin organic peroxide=100 0.04～0.12；
HOPP resin antioxidant=100 0.10～0.25；
HOPP resin processing aid=100 0.05～0.15.
Molecular weight distribution≤3.0 that polypropylene fibre of the present invention is resin dedicated, melt index (MFR) 30～80g/10min, tension fracture elongation rate > 500%.
HOPP of the present invention, it is common to use propylene is carried out polyreaction by Ziegler-Natta catalyst, preparation method can be mass polymerization reaction, it is also possible to be body-gas phase polymerization reaction, it is also possible to be gas phase polymerization reaction.Melt index (the MFR of heretofore described HOPP2) it is 1～10g/10min.
For ensureing that organic peroxide can effectively react by triggered degradation, organic peroxide of the present invention adopts has the half-life organic peroxide that temperature is 130 DEG C ~ 150 DEG C corresponding when being 1h, the present invention includes but not limited to 2,5-dimethyl-2,5-di-tert-butyl peroxide hexane, di-t-butyl peroxide, cumyl peroxide, DIBHP, 2,5-dimethyl-2,5-di-tert-butyl peroxide alkynes and one or more the combination in two tertiary amyl peroxide.In addition, the material time of staying in screw extruder controls at 30 ~ 150 seconds, organic peroxide is needed to have trigger rate steady, rapid, to ensure that it decomposes completely in an extruder but not still has residual in the final acrylic resin of preparation, otherwise will cause extreme influence to the ageing-resistant performance of acrylic resin.Further, organic peroxide of the present invention preferably 2,5-dimethyl-2, the compound of 5-di-tert-butyl peroxide hexane and di-t-butyl peroxide, the mass ratio of the two is 6-8 2-5.
Antioxidant can improve acrylic resin heat aging property in processing and use procedure, and as one embodiment of the present of invention, described antioxidant can select the compound of Hinered phenols antioxidant and phosphite ester kind antioxidant.In compound, Hinered phenols antioxidant and phosphite ester kind antioxidant mass ratio can be 12.
Processing aid of the present invention includes one or more combination of low molecule esters stearic acid, calcium stearate, zinc stearate and stearic acid complex ester apoplexy due to endogenous wind.As one embodiment of the present of invention, described processing aid is the combination of calcium stearate and tristerin.
The preparation method that high-flowability polypropylene fiber of the present invention is resin dedicated, comprises the following steps:
(1) HOPP resin, organic peroxide, antioxidant and processing aid are mixed by proportioning at 30～70 DEG C, obtain mixed material；
(2) mixed material addition extruder step (1) obtained carries out pelletize, namely obtains polypropylene fibre resin dedicated.
The present invention compared with prior art has the advantage that
(1) acrylic resin prepared by the present invention, with high fluidity, Narrow Molecular Weight Distribution, high elongation at tear, low ash, low colourity advantage.
(2) acrylic resin prepared by the present invention, according to GB3682(230 DEG C, 2.16kg) to test, it has melt index MFR is 30～80g/10min.
(3) acrylic resin prepared by the present invention, tests according to industry universal method, molecular weight distribution≤3.0.
(4) acrylic resin prepared by the present invention, tests according to GB/T1040-92, and rate of extension is 50mm/min, tension fracture elongation rate > 500%.
(5) preparation method of the present invention adopts controllable rheology degradation technique, uses a small amount of organic peroxide that HOPP is degraded, and between the trade mark, switching cycle is short, throughput rate is high, meet the processing characteristics of high fluidity, it is thus achieved that more Narrow Molecular Weight Distribution, there is good mechanical property simultaneously.
(6) acrylic resin provided by the invention, has good processing fluidity and fibre-forming performance, can be used for spun-bonded non-woven fabrics, SMS non-woven fabrics etc., the slim textile fabrics of particularly suitable high-speed spinning, can give goods flexility.
Detailed description of the invention
The weight of the HOPP according to the form below 1 and 2, organic peroxide, nucleator, antioxidant and processing aid takes each raw material respectively:
HOPP used by embodiment 1～4 and comparative example 1-3 is produced by Sinopec Maoming branch company, and the trade mark is PPH-T03, melt index 2.0～5.0g/10min.HOPP used by embodiment 5 is produced by Sinopec Maoming branch company, and the trade mark is S1003, melt index (MFR2) it is 2.0～5.0g/10min.
Embodiment 1～5 and comparative example 1-3 organic peroxide are 2,5-dimethyl-2, the compound of 5-di-tert-butyl peroxide hexane and di-t-butyl peroxide, 2,5-dimethyl-2,5-di-tert-butyl peroxide hexane and di-t-butyl peroxide mass ratio are 7:3, and it be 1 hour corresponding temperature is 130～150 DEG C that organic peroxide has a half-life.Processing aid is calcium stearate or glyceryl monostearate.
The antioxidant that embodiment 1～5 adopts is the compound antioxidant of Hinered phenols antioxidant 1010 and phosphite ester kind antioxidant 168, and the mass ratio of the two is 12.The antioxidant of comparative example 1-3 is similarly the compound antioxidant of Hinered phenols antioxidant 1010 and phosphite ester kind antioxidant 168, and the mass ratio of the two is 11.
The preparation method of above-mentioned high-fluidity high-toughness polypropylene resin is as follows:
(1) HOPP base resin, organic peroxide, antioxidant and processing aid being sufficiently mixed by the proportioning in table 1 respectively, mixing temperature controls at 30～70 DEG C.
(2) feed the mixture into double screw extruder melt blending extruding pelletization, obtain acrylic resin；Double screw extruder melt zone temperature is 230 DEG C, and die head temperature is 180 DEG C, screw speed 180 revs/min, and the mixture time of staying in double screw extruder controlled at 60 seconds.
The concrete test result of acrylic resin after pelletize is in Table 3.From result, the polypropylene fibre of embodiment 1-5 is resin dedicated has original text melt index, Narrow Molecular Weight Distribution, yellow colour index and content of ashes are low, it is maintained with excellent mechanical property, wherein tensile break strength and tension fracture elongation rate are higher, there is the fibre-forming performance of stable homogeneous, it is adaptable to slim textile fabrics.
The present invention can summarizing without prejudice to the spirit of the present invention or the concrete form of principal character with other, the above embodiment of the present invention all can only think the description of the invention rather than restriction, every any trickle amendment, equivalent variations and modification above example made according to the substantial technological of the present invention, belongs in the scope of technical solution of the present invention.
Claims (10)
1. a high-flowability polypropylene fiber is resin dedicated, it is characterized in that, being prepared from HOPP resin, organic peroxide, antioxidant and processing aid for primary raw material, with the quality of HOPP resin for benchmark, the mass ratio between described raw material is:
HOPP resin organic peroxide=100 0.04～0.12；
HOPP resin antioxidant=100 0.10～0.25；
HOPP resin processing aid=100 0.05～0.15.
2. high-flowability polypropylene fiber according to claim 1 is resin dedicated, it is characterised in that molecular weight distribution≤3.0 that described polypropylene fibre is resin dedicated, melt index 30～80g/10min, tension fracture elongation rate > 500%.
3. high-flowability polypropylene fiber according to claim 1 and 2 is resin dedicated, it is characterised in that the melt index of described HOPP is 1～10g/10min.
4. high-flowability polypropylene fiber according to claim 1 and 2 is resin dedicated, it is characterised in that described organic peroxide adopts has the half-life organic peroxide that temperature is 130 DEG C ~ 150 DEG C corresponding when being 1h.
5. high-flowability polypropylene fiber according to claim 4 is resin dedicated, it is characterized in that, described organic peroxide includes but not limited to 2,5-dimethyl-2,5-di-tert-butyl peroxide hexane, di-t-butyl peroxide, cumyl peroxide, DIBHP, 2,5-dimethyl-2,5-di-tert-butyl peroxide alkynes and one or more the combination in two tertiary amyl peroxide.
6. high-flowability polypropylene fiber according to claim 5 is resin dedicated, it is characterised in that described organic peroxide is 2,5-dimethyl-2, the compound of 5-di-tert-butyl peroxide hexane and di-t-butyl peroxide, and the mass ratio of the two is 6-8 2-5.
7. high-flowability polypropylene fiber according to claim 4 is resin dedicated, it is characterised in that described antioxidant is the compound of Hinered phenols antioxidant and phosphite ester kind antioxidant；Described processing aid includes one or more combination of low molecule esters stearic acid, calcium stearate, zinc stearate and stearic acid complex ester apoplexy due to endogenous wind.
8. high-flowability polypropylene fiber according to claim 7 is resin dedicated, it is characterised in that described Hinered phenols antioxidant and phosphite ester kind antioxidant mass ratio are 12.
9. high-flowability polypropylene fiber according to claim 7 is resin dedicated, it is characterised in that described processing aid is the combination of calcium stearate and tristerin.
10. the preparation method that high-flowability polypropylene fiber described in any one of claim 1-9 is resin dedicated, comprises the following steps:
(1) HOPP resin, organic peroxide, antioxidant and processing aid are mixed by proportioning at 30～70 DEG C, obtain mixed material；
(2) mixed material addition extruder step (1) obtained carries out pelletize, namely obtains polypropylene fibre resin dedicated.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109354770A (en) * | 2018-10-25 | 2019-02-19 | 中国石油化工股份有限公司 | A kind of non-woven cloth acrylic resin and preparation method thereof |
| CN110183559A (en) * | 2019-04-04 | 2019-08-30 | 东华能源股份有限公司 | A kind of production method of high fluidity spun-bonded non-woven acrylic resin |
| CN110218273A (en) * | 2019-04-04 | 2019-09-10 | 东华能源股份有限公司 | A kind of production method of the spun-bonded non-woven acrylic resin of the color inhibition of Narrow Molecular Weight Distribution |
| CN111472100A (en) * | 2019-01-23 | 2020-07-31 | 广东维弈科技有限公司 | Polypropylene non-woven fabric material with ultrahigh fluidity and ultralow gel content |
| CN111849075A (en) * | 2020-08-07 | 2020-10-30 | 常州市天王塑业有限公司 | High-melt index polypropylene and preparation process thereof |
| CN112080072A (en) * | 2020-09-15 | 2020-12-15 | 惠州莹光塑胶颜料有限公司 | Polypropylene composition |
| CN112239896A (en) * | 2019-07-18 | 2021-01-19 | 中国石油化工股份有限公司 | Preparation method and application of polypropylene fiber |
| CN112266535A (en) * | 2020-10-28 | 2021-01-26 | 中国石油化工股份有限公司 | Polypropylene material for non-woven fabric and preparation method thereof |
| EP3733724A4 (en) * | 2018-11-06 | 2021-10-13 | Lg Chem, Ltd. | Pellet-type polypropylene resin and method for manufacturing same |
| CN113683838A (en) * | 2020-05-19 | 2021-11-23 | 中国石油天然气股份有限公司 | Polypropylene fiber resin and preparation method thereof |
| CN114717675A (en) * | 2021-01-06 | 2022-07-08 | 中国石油天然气股份有限公司 | Special resin for homo-polypropylene fiber and preparation method thereof |
| CN118087080A (en) * | 2024-04-22 | 2024-05-28 | 万华化学集团股份有限公司 | Polypropylene fiber material and preparation method and application thereof |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109354770A (en) * | 2018-10-25 | 2019-02-19 | 中国石油化工股份有限公司 | A kind of non-woven cloth acrylic resin and preparation method thereof |
| US11759977B2 (en) | 2018-11-06 | 2023-09-19 | Lg Chem, Ltd. | Polypropylene resin pellet and method for preparing the same |
| EP3733724A4 (en) * | 2018-11-06 | 2021-10-13 | Lg Chem, Ltd. | Pellet-type polypropylene resin and method for manufacturing same |
| CN111472100A (en) * | 2019-01-23 | 2020-07-31 | 广东维弈科技有限公司 | Polypropylene non-woven fabric material with ultrahigh fluidity and ultralow gel content |
| CN110183559B (en) * | 2019-04-04 | 2021-07-23 | 东华能源(宁波)新材料有限公司 | Production method of polypropylene resin for high-fluidity spun-bonded non-woven fabric |
| CN110218273A (en) * | 2019-04-04 | 2019-09-10 | 东华能源股份有限公司 | A kind of production method of the spun-bonded non-woven acrylic resin of the color inhibition of Narrow Molecular Weight Distribution |
| CN110183559A (en) * | 2019-04-04 | 2019-08-30 | 东华能源股份有限公司 | A kind of production method of high fluidity spun-bonded non-woven acrylic resin |
| CN112239896A (en) * | 2019-07-18 | 2021-01-19 | 中国石油化工股份有限公司 | Preparation method and application of polypropylene fiber |
| CN113683838A (en) * | 2020-05-19 | 2021-11-23 | 中国石油天然气股份有限公司 | Polypropylene fiber resin and preparation method thereof |
| CN111849075A (en) * | 2020-08-07 | 2020-10-30 | 常州市天王塑业有限公司 | High-melt index polypropylene and preparation process thereof |
| CN112080072A (en) * | 2020-09-15 | 2020-12-15 | 惠州莹光塑胶颜料有限公司 | Polypropylene composition |
| CN112266535A (en) * | 2020-10-28 | 2021-01-26 | 中国石油化工股份有限公司 | Polypropylene material for non-woven fabric and preparation method thereof |
| CN114717675A (en) * | 2021-01-06 | 2022-07-08 | 中国石油天然气股份有限公司 | Special resin for homo-polypropylene fiber and preparation method thereof |
| CN118087080A (en) * | 2024-04-22 | 2024-05-28 | 万华化学集团股份有限公司 | Polypropylene fiber material and preparation method and application thereof |
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| CN105733093B (en) | 2018-12-04 |
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