CN105733093B - A kind of high-flowability polypropylene fiber is resin dedicated and preparation method thereof - Google Patents
A kind of high-flowability polypropylene fiber is resin dedicated and preparation method thereof Download PDFInfo
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- CN105733093B CN105733093B CN201610181375.1A CN201610181375A CN105733093B CN 105733093 B CN105733093 B CN 105733093B CN 201610181375 A CN201610181375 A CN 201610181375A CN 105733093 B CN105733093 B CN 105733093B
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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 kind of high-flowability polypropylene fiber is resin dedicated, it is prepared using homopolypropylene resin, organic peroxide, antioxidant and processing aid as primary raw material, on the basis of the quality of homopolypropylene resin, mass ratio between the raw material are as follows: homopolypropylene Shu Zhi ﹕ organic peroxide=100 ﹕ 0.04~0.12, homopolypropylene Shu Zhi ﹕ antioxidant=100 ﹕ 0.10~0.25, homopolypropylene Shu Zhi ﹕ processing aid=100 ﹕ 0.05~0.15.High-flowability polypropylene fiber provided by the invention is resin dedicated to have high fusion index, Narrow Molecular Weight Distribution, while keeping excellent mechanical property, and elongation at break with higher, ash content be low and the good fibre-forming performances such as coloration is good.
Description
Technical field
The present invention relates to a kind of acrylic resins, and in particular to and a kind of high-flowability polypropylene fiber is resin dedicated, meanwhile,
The invention further relates to the resin dedicated preparation methods of the polypropylene fibre.
Background technique
Fiber is the fourth-largest consumer field of acrylic resin, and polypropylene fibre is to be spun using polypropylene as raw material by melting
A kind of fibre made of silk, due to polypropylene fibre have light, non-toxic, wear-resisting, hydrophobic, bear dirty, it is easy to wash it is easily dry, every
The advantages that hot, is widely used in the various fields such as industry, agricultural, packaging, household, medical, is to send out in synthetic fibers in recent years
Open up most fast kind, it has also become be only second to the second largest synthetic fiber products of terylene.Polypropylene fibre can with fibre morphology classification
It is divided into flat filament, long filament, staple fiber, bicomponent fibre etc.；It is swollen that spine silk, common long filament, composite fibre can be divided by processing method point
Body yarn, staple fiber, non-woven fabrics etc..Wherein non-woven fabrics is rapidly developed due to unique energy, makes the application neck of polypropylene fibre
Domain and demand constantly expand, other than being used as industrial cloth, filtering material, geotextiles, agricultural fabric, covering material,
It can be used for medical material, hygienic material, disposable material, clothes, decoration etc..
As polypropylene fibre is differential, the development of functionalization, the performance resin dedicated to fibrous polypropylene it is also proposed that
Higher requirement, must have high melt flow rate (MFR), Narrow Molecular Weight Distribution, high isotactic, high elongation at tear, a low ash
Point and gel particles etc. to improve Fiber spinning speeds reduce processing temperature, could improve service efficiency and reduction energy in this way
Consumption；And high tensile property can then reduce fibre number, product is thin, meets non-woven fabrics to performance requirements such as feel, intensity.
Currently, industrially the method for production high-flowability polypropylene mainly has hydrogen-regulating method and two kinds of controllable flow political reform.The former
It is that the method for adjusting high polymerization inhibitor such as density of hydrogen is combined using new catalyst, to reduce polypropylene molecule amount, to improve
Polypropylene melt index.This method is limited by catalyst system, reaction condition etc., and product molecular weight distribution is wider, unfavorable
In the intensity for improving fiber；In addition, Transition Materials are more when industrialized production, polymerization reactor control difficulty is big.The latter is made in extrusion
During grain, peroxide is added into polypropylene base resin and is degraded, to improve its melt index.The production conversion of this method
Process is short, and Transition Materials are few, and polymerization reaction is easy to control, and product has wide, narrow molecular weight distribution of melt index controlled range etc.
Advantage.
Although the report that the country has high-flowability polypropylene fiber resin dedicated, there are melting means fluctuations for product quality greatly,
Molecular weight distribution is wide, and stability is poor, and impurity content is higher, fracture of wire and the problems such as serious doubling phenomena when producing thin product,
It can be only applied in the disposable diaper of industry cloth and low side, and be used to produce the fine-denier, ultra-fine of high-end polypropylene fibre product
Raw material needed for denier, slim fibre etc. then relies primarily on import solution.Therefore, it is badly in need of wanting a kind of method preparation high fluidity poly-
Allyl 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 tree
Rouge has uniform, stable fibre-forming performance, can be suitably used for slim textile fabrics.
Summary of the invention
It is resin dedicated that an object of the present invention is to provide a kind of high-flowability polypropylene fiber, and there is high melting to refer to
Number, Narrow Molecular Weight Distribution, while keeping excellent mechanical property, and elongation at break with higher, ash content are low and coloration is good etc.
Good fibre-forming performance.
The second object of the present invention is to provide above-mentioned high-flowability polypropylene fiber resin dedicated preparation method, the preparation
Method is simple, and polymerization reaction is easy to control, and is suitble to industrialized production.
The first purpose of this invention is achieved through the following technical solutions: a kind of high-flowability polypropylene fiber is special
With resin, it is prepared using homopolypropylene resin, organic peroxide, antioxidant and processing aid as primary raw material, with equal
Mass ratio on the basis of the quality of poly- acrylic resin, between the raw material are as follows:
Homopolypropylene Shu Zhi ﹕ organic peroxide=100 ﹕ 0.04~0.12；
Homopolypropylene Shu Zhi ﹕ antioxidant=100 ﹕ 0.10~0.25；
Homopolypropylene Shu Zhi ﹕ processing aid=100 ﹕ 0.05~0.15.
Resin dedicated molecular weight distribution≤3.0 of polypropylene fibre of the present invention, melt index (MFR) 30~80g/
10min, tension fracture elongation rate > 500%.
Homopolypropylene of the present invention carries out polymerization reaction, system to propylene usually using Ziegler-Natta catalyst
Preparation Method can be mass polymerization reaction, is also possible to ontology-gas phase polymerization reaction, can also be that gas phase polymerization is anti-
It answers.Melt index (the MFR of heretofore described homopolypropylene2) it is 1~10g/10min.
To guarantee that organic peroxide can effectively cause degradation reaction, organic peroxide of the present invention, which uses, to be had
The organic peroxide that corresponding temperature is 130 DEG C ~ 150 DEG C when half-life period is 1h, the present invention in include but is not limited to 2,5-
Dimethyl -2,5- di-tert-butyl peroxide hexane, di-t-butyl peroxide, cumyl peroxide, diisopropylbenzene hydroperoxide,
The combination of 2,5- dimethyl -2,5- di-tert-butyl peroxide one or more of alkynes and two tertiary amyl peroxide.
In addition, residence time of the material in screw extruder controlled at 30 ~ 150 seconds, organic peroxide is needed to have steady, rapid
Trigger rate, with guarantee its in an extruder completely decompose rather than still have residual in the final acrylic resin of preparation, it is no
To then extreme influence be caused to the ageing-resistant performance of acrylic resin.Further, organic peroxide of the present invention is excellent
The compound of 2,5- dimethyl -2,5- di-tert-butyl peroxide hexane and di-t-butyl peroxide is selected, the mass ratio of the two is 6-
8 ﹕ 2-5.
The heat aging property of acrylic resin in the process of processing and using can be improved in antioxidant, as of the invention
One embodiment, the antioxidant can select the compound of Hinered phenols antioxidant and phosphite ester antioxidant.Compounding
In object, Hinered phenols antioxidant and phosphite ester antioxidant mass ratio can be 1 ﹕ 2.
Processing aid of the present invention includes that low molecule esters stearic acid, calcium stearate, zinc stearate and stearic acid are multiple
Close the combination of one or more of esters.As an embodiment of the present invention, the processing aid is calcium stearate
With the combination of tristerin.
The resin dedicated preparation method of high-flowability polypropylene fiber of the present invention, comprising the following steps:
(1) by homopolypropylene resin, organic peroxide, antioxidant and processing aid according to the ratio at 30~70 DEG C
Mixing, obtains mixed material；
(2) mixed material that step (1) obtains is added in extruder and is granulated to get dedicated to polypropylene fibre
Resin.
Compared with the prior art, the present invention has the following advantages:
(1) acrylic resin prepared by the present invention, with high fluidity, Narrow Molecular Weight Distribution, high elongation at tear,
The advantages of low ash point, low coloration.
(2) acrylic resin prepared by the present invention, according to GB3682(230 DEG C, 2.16kg) it is tested, have molten
Melting index M FR is 30~80g/10min.
(3) acrylic resin prepared by the present invention is tested, molecular weight distribution≤3.0 according to industry universal method.
(4) acrylic resin prepared by the present invention is tested according to GB/T 1040-92, rate of extension 50mm/
Min, tension fracture elongation rate > 500%.
(5) preparation method of the present invention uses controllable rheology degradation technique, poly- to homopolymerization using a small amount of organic peroxide
Propylene is degraded, and switching cycle is short between the trade mark, and throughput rate is high, is met the processing performance of high fluidity, is obtained narrower molecule
Amount distribution, while there is good mechanical property.
(6) acrylic resin provided by the invention has good processing fluidity and fibre-forming performance, can be used for spunbond
Non-woven fabrics, SMS non-woven fabrics etc., the slim textile fabrics of particularly suitable high-speed spinning, can assign product flexility.
Specific embodiment
The weight of homopolypropylene, organic peroxide, nucleating agent, antioxidant and processing aid in difference according to the form below 1 and 2
Part proportion is measured to take each raw material:
Homopolypropylene used in Examples 1 to 4 and comparative example 1-3 is produced by Sinopec Maoming branch company, and the trade mark is
PPH-T03,2.0~5.0 g/10min of melt index.Homopolypropylene used in embodiment 5 is by Sinopec Maoming branch company
Production, the trade mark is S1003, melt index (MFR2) it is 2.0~5.0 g/10min.
Examples 1 to 5 and comparative example 1-3 organic peroxide are 2,5- dimethyl -2,5- di-tert-butyl peroxide hexane
With the compound of di-t-butyl peroxide, 2,5- dimethyl -2,5- di-tert-butyl peroxide hexanes and di-t-butyl peroxide matter
For amount than being 7:3, it be temperature corresponding to 1 hour is 130~150 DEG C that organic peroxide, which has half-life period,.Processing aid is hard
Resin acid calcium or glycerin monostearate.
The antioxidant that Examples 1 to 5 uses compounds for Hinered phenols antioxidant 1010 and phosphite ester antioxidant 168
Antioxidant, the mass ratio of the two are 1 ﹕ 2.The antioxidant of comparative example 1-3 is similarly Hinered phenols antioxidant 1010 and phosphite ester
The compound antioxidant of kind antioxidant 168, the mass ratio of the two are 1 ﹕ 1.
Above-mentioned high-fluidity high-toughness polypropylene resin the preparation method is as follows:
(1) by homopolypropylene base resin, organic peroxide, antioxidant and processing aid respectively by matching in table 1
Than being sufficiently mixed, mixing temperature is controlled at 30~70 DEG C.
(2) double screw extruder melt blending and extruding pelletization are fed the mixture into, acrylic resin is obtained；Twin-screw squeezes
Machine melt zone temperature is 230 DEG C out, and die head temperature is 180 DEG C, and 180 revs/min of screw speed, mixture is in double screw extruder
Residence time control at 60 seconds.
The specific test result of acrylic resin after granulation is shown in Table 3.By result as it can be seen that the polypropylene fibre of embodiment 1-5
Resin dedicated to have original text melt index, Narrow Molecular Weight Distribution, yellow colour index and content of ashes are low, maintain excellent mechanics
Performance, wherein tensile break strength and tension fracture elongation rate are higher, and the fibre-forming performance with stable homogeneous is suitable for slim spinning
Fabric products.
The present invention can be summarized with others without prejudice to the concrete form of spirit or essential characteristics of the invention, of the invention
Above-described embodiment can only all be considered the description of the invention rather than limit that all substantial technologicals according to the present invention are to above
Any subtle modifications, equivalent variations and modifications, belong in the range of technical solution of the present invention made by embodiment.
Claims (5)
1. a kind of high-flowability polypropylene fiber is resin dedicated, which is characterized in that with homopolypropylene resin, organic peroxy
Object, antioxidant and processing aid are prepared for primary raw material, on the basis of the quality of homopolypropylene resin, between the raw material
Mass ratio are as follows:
Homopolypropylene Shu Zhi ﹕ organic peroxide=100 ﹕ 0.04~0.12；
Homopolypropylene Shu Zhi ﹕ antioxidant=100 ﹕ 0.10~0.25；
Homopolypropylene Shu Zhi ﹕ processing aid=100 ﹕ 0.05~0.15,
The melt index of the homopolypropylene be 1~10g/10min, the organic peroxide use with half-life period for
The organic peroxide that corresponding temperature is 130 DEG C ~ 150 DEG C when 1h, the resin dedicated molecular weight of the polypropylene fibre point
Cloth≤3.0,30~80g/10min of melt index, tension fracture elongation rate > 500%；
The antioxidant is the compound of Hinered phenols antioxidant and phosphite ester antioxidant, the Hinered phenols antioxidant
It is 1 ﹕ 2 with phosphite ester antioxidant mass ratio；
The high-flowability polypropylene fiber is resin dedicated to be prepared by the following method:
(1) homopolypropylene resin, organic peroxide, antioxidant and processing aid are mixed at 30~70 DEG C according to the ratio,
Obtain mixed material；
(2) mixed material that step (1) obtains is added in extruder and is granulated, double screw extruder melt zone temperature is
230 DEG C, die head temperature be 180 DEG C, material in screw extruder residence time control 30 ~ 150 seconds to get arrive polypropylene
Fiber is resin dedicated.
2. high-flowability polypropylene fiber according to claim 1 is resin dedicated, which is characterized in that the organic peroxy
Object includes but is not limited to 2,5- dimethyl -2,5- di-tert-butyl peroxide hexane, di-t-butyl peroxide, peroxidating diisopropyl
Benzene, diisopropylbenzene hydroperoxide, 2,5- dimethyl -2,5- di-tert-butyl peroxide in alkynes and two tertiary amyl peroxide one
Kind or two or more combinations.
3. high-flowability polypropylene fiber according to claim 2 is resin dedicated, which is characterized in that the organic peroxy
Compound is the compound of 2,5- dimethyl -2,5- di-tert-butyl peroxide hexane and di-t-butyl peroxide, the mass ratio of the two
For 6-8 ﹕ 2-5.
4. high-flowability polypropylene fiber according to claim 1 is resin dedicated, which is characterized in that the processing aid
Group including one or more of low molecule esters stearic acid, calcium stearate, zinc stearate and the compound esters of stearic acid
It closes.
5. high-flowability polypropylene fiber according to claim 4 is resin dedicated, which is characterized in that the processing aid is
The combination of calcium stearate and tristerin.
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| CN201610181375.1A CN105733093B (en) | 2016-03-28 | 2016-03-28 | A kind of high-flowability polypropylene fiber is resin dedicated and preparation method thereof |
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Families Citing this family (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 |
| KR102388031B1 (en) * | 2018-11-06 | 2022-04-19 | 주식회사 엘지화학 | Polypropylene resin pellet and method for preparing the 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 |
| CN112239896B (en) * | 2019-07-18 | 2023-05-09 | 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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| US5122593A (en) * | 1989-02-22 | 1992-06-16 | The B. F. Goodrich Company | Stabilized gamma-irradiatable polypropylene fibers and sterilizable articles thereof |
| CN1351086A (en) * | 2000-10-26 | 2002-05-29 | 上海塑杰科技有限公司 | Functional polypropylene for special purpose and its preparing process and application |
| CN102040774A (en) * | 2010-12-20 | 2011-05-04 | 深圳市科聚新材料有限公司 | PP (polypropylene) filled masterbatch and method for preparing same |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1217989C (en) * | 2003-05-09 | 2005-09-07 | 东华大学 | Superhigh melt index polypropene and preparing process thereof |
| CN101429308B (en) * | 2007-11-08 | 2011-04-20 | 中国石油天然气股份有限公司 | Process for producing polypropylene degradation master batch |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5122593A (en) * | 1989-02-22 | 1992-06-16 | The B. F. Goodrich Company | Stabilized gamma-irradiatable polypropylene fibers and sterilizable articles thereof |
| CN1351086A (en) * | 2000-10-26 | 2002-05-29 | 上海塑杰科技有限公司 | Functional polypropylene for special purpose and its preparing process and application |
| CN102040774A (en) * | 2010-12-20 | 2011-05-04 | 深圳市科聚新材料有限公司 | PP (polypropylene) filled masterbatch and method for preparing same |
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