CN106554569A - A kind of random copolymer of propylene for super soft non-woven fabrics and preparation method thereof - Google Patents
A kind of random copolymer of propylene for super soft non-woven fabrics and preparation method thereof Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
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- C08K5/524—Esters of phosphorous acids, e.g. of H3PO3
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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- B29C2948/00—Indexing scheme relating to extrusion moulding
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Abstract
The present invention relates to a kind of preparation method of the random copolymer of propylene for super soft non-woven fabrics, comprises the steps：Polypropylene random copolymer is added in double screw extruder together with antioxidant 1010, irgasfos 168, antioxidant DHT, stabilizer, slipping agent, peroxide and is granulated, the random copolymer of propylene for obtaining.The present invention adopts polypropylene Innovene polymerization techniques, by controlling ethene addition, added hydrogen, determine catalyst charge, Al/Mg ratios, Al/Si than Optimal Control value, it is 201.0～300.0g/10min to realize melt index, and ethylene contents are the industrialized production of 3.3～4.0% random copolymer of propylene.Obtained random copolymer of propylene has excellent physical and mechanical properties, spinning properties, is particularly suited for super soft non-woven fabrics.
Description
Technical field
The present invention relates to cast film field, and in particular to a kind of random copolymer of propylene for super soft non-woven fabrics
Preparation method.
Background technology
The market capacity of domestic polypropylene non-woven fabric is very big, at present, high-end polypropylene (PP) fiber (as fine-denier,
Super fine denier and melt spraying non-woven fabrics etc.) the resin dedicated overwhelming majority needs import, the main trade mark to have Hyosung Corporation of Korea
The PP185 of S905, great Lin company, HP462S of 3155 and company of Basel of Exxon companies of the U.S. etc..
These imported raw materials are mainly for the production of exported product, and the higher hygienic protection articles for use of quality requirements and medical treatment
Amenities etc..
The production of domestic spinning PP Pipe Compound (random copolymer of propylene) at present is mainly produced using edman degradation Edman, production
During generally need to add peroxide, and peroxide can produce the material with stink in decomposable process,
Peculiar Smell is brought to product；Simultaneously because the wider distribution of molecular weight, melt flow rate (MFR) scope distribution width,
It is larger with import material gap, cause performance difference larger, which is affected in the application of high-end market.
For soft polypropylene non-woven fabrics, 30% or so acrylic is generally blended both at home and abroad using HOPP
Producing, (Vistamaxx as increased Exxonmobil productions) is mainly used in amenities to elastomer, into
This is costly.
The content of the invention
Present invention aim to address the deficiencies in the prior art, there is provided a kind of propylene random for super soft non-woven fabrics
Copolymer, which is avoided that the Peculiar Smell that the addition of peroxide brings, and good spinnability, Jing melt spinnings
Resulting polypropylene fibre has soft feel and excellent mechanical strength afterwards.
The concrete technical scheme of the present invention is as follows：
A kind of random copolymer of propylene for super soft non-woven fabrics, which is prepared from by the raw material of following weight portion：
1000 parts of random polypropylenes, 0.4～1.0 part of antioxidant 1010,0.4～1.0 part of irgasfos 168,0.4～0.8 part
Antioxidant BHT, 0.5～1.5 part of stabilizer, 0.5～1.5 part of slipping agent；
The preparation method of the random polypropylene is as follows：By the way of two horizontal type agitated bed reactor series connection,
With Ziegler-Natta catalyst as major catalyst, triethyl aluminum is co-catalyst, diisobutyl methoxy silane
For external electron donor, propylene is raw material, enters the first horizontal type agitated bed reactor, while being passed through second after prepolymerization
Alkene and H2, random polypropylene after polymerisation, is obtained；Wherein, in the first horizontal type agitated bed reactor, ethene：
The mol ratio of propylene is 0.015～0.018：1, hydrogen is 0.02～0.03 with the mol ratio of propylene：1, second crouches
In formula agitated bed reactor, ethene is 0.015～0.018 with the mol ratio of propylene：1, hydrogen and propylene mole
Than for 0.2～0.3：1.
Further, the random copolymer of propylene for super soft non-woven fabrics, is prepared by the raw material of following weight portion
Form：1000 parts of random polypropylenes, 0.4～0.6 part of antioxidant 1010,0.6～0.9 part of irgasfos 168,0.4～0.5
Part antioxidant BHT, 0.6～0.8 part of stabilizer, 0.5～0.8 part of slipping agent.
Further, the prepolymerized reaction temperature is 10～13 DEG C, and the reaction time is 1～10min.
Further, in the first horizontal type agitated bed reactor and the second horizontal type agitated bed reactor, the temperature of polymerisation
Degree is 70～80 DEG C.
Further, the dosage of the Ziegler-Natta catalyst, triethyl aluminum and diisobutyl methoxy silane
Meet Al/Mg (mol/mol)=10～14：1, Al/Si (mol/mol)=9:1.
Further, the stabilizer is calcium stearate or zinc stearate, can be made in high temperature screw rod granulation process not
Easily there is degraded.
Further, the slipping agent is erucyl amide or oleamide, can reduce the surface tension of film article,
Be conducive to improving film feel.
The Ziegler-Natta catalyst is selected from the CD/CDI catalyst of Amoco companies, Beijing chemical industry and grinds
Study carefully NG/NA catalyst, Beijing one kind up in the SAL catalyst of catalyst Co. difficult to understand of institute.
In the present invention, the antioxidant 1010 chemical name is four [B- (3,5- di-tert-butyl-hydroxy phenyl) third
Acid] pentaerythrite, the irgasfos 168 chemical name is three (2,4- di-tert-butyl phenyl) phosphite, described
Antioxidant BHT chemical name is DBPC 2,6 ditertiary butyl p cresol.
Preparation method of the present invention for the random copolymer of propylene of super soft non-woven fabrics：By random polypropylene, antioxygen
Agent 1010, irgasfos 168, antioxidant BHT, stabilizer, slipping agent together add Co rotating Twin Screw Extrusion
In machine, extrusion, granulation, obtain final product.
Further, the temperature in each area of the parallel dual-screw extruding machine is：One area：180～200 DEG C, 2nd area：
220～240 DEG C, 3rd area：190～210 DEG C, template：185～205 DEG C.
The present invention adopts polypropylene Innovene polymerization techniques, by controlling ethene addition, added hydrogen,
Determine catalyst charge, Al/Mg ratios, Al/Si than Optimal Control value, realize melt index for 201.0～
300.0g/10min, ethylene contents are the industrialized production of 3.3～4.0% random copolymer of propylene.It is obtained
Random copolymer of propylene Jing after melt spinning obtained by polypropylene fibre there is soft feel and excellent
Mechanical strength, is particularly suited for super soft non-woven fabrics.
Specific embodiment
Below in conjunction with specific embodiment, the invention will be further described.
Remarks：In the present invention, the test reference GB/T3682-2000 standards of melt index, test condition is
230℃、2.160Kg；Ethylene contents are determined with Fourier transform infrared spectrometry；The test reference of bending modulus
GB/T9341-2000 standards；The test reference GB/T2546.2-2003 standards of tensile property, draw speed is
50mm/min；The test reference GB/T 1043.1-2008 standards of simple beam impact strength (23 DEG C).Spinning
Experiment is using self-control plug type melt spinning machine, orifice diameter 0.03mm, spinneret orifice 6, spinning temperature
210-230℃。
Embodiment 1
Prepare random polypropylene：Connected using two horizontal type agitated bed reactors, test load is set as 25.0t/h,
The CD/CDI catalyst charges amount of Amoco companies is 2.0Kg/h, and triethyl aluminum inlet amount is 5.4Kg/h,
Electron donor diisobutyl methoxy silane inlet amount be 1.0Kg/h, 12 DEG C of Propylene Pre-polymerization temperature, polyase 13
Enter first reactor after minute, ethene and hydrogen add reactor together in reactor head separator, first
In reactor, ethene：The mol ratio of propylene is 0.015：1, hydrogen is 0.02 with the mol ratio of propylene：1,
In second reactor, ethene is 0.015 with the mol ratio of propylene：1, hydrogen is 0.2 with the mol ratio of propylene：1,
Reaction temperature is all 75 DEG C, and in the presence of catalyst, propylene/ethylene carries out continuous gas-phase polymerization, is obtained random
Polypropylene powder.
200t random polypropylenes are taken, adds 80Kg antioxidant 1010s, 200Kg irgasfos 168s, 80Kg to resist
Oxygen agent BHT, 200Kg calcium stearate, 100Kg erucyl amides, then by parallel dual-screw extruding machine
Extrusion, granulation, obtain final product random copolymer of propylene product.The temperature in each area of the parallel dual-screw extruding machine is：
One area：185 DEG C, 2nd area：225 DEG C, 3rd area：195 DEG C, template：195℃.
Embodiment 2
Prepare random polypropylene：Connected using two horizontal type agitated bed reactors, test load is set as 25.0t/h,
The NG/NA catalyst charges amount of Beijing Chemical Research Institute is 2.0Kg/h, and triethyl aluminum inlet amount is 5.4
Kg/h, electron donor diisobutyl methoxy silane inlet amount be 1.0Kg/h, 12 DEG C of Propylene Pre-polymerization temperature,
First reactor is entered after polyase 13 minute, ethene and hydrogen add reaction together in reactor head separator
Device, in first reactor, ethene：The mol ratio of propylene is 0.018：1, hydrogen with the mol ratio of propylene is
0.02：1, in second reactor, ethene is 0.018 with the mol ratio of propylene：1, hydrogen and propylene mole
Than for 0.2：1, reaction temperature is all 75 DEG C, in the presence of catalyst propylene/ethylene carry out continuous gas phase gather
Close, random polypropylene powder is obtained.
200t random polypropylenes are taken, adds 200Kg antioxidant 1010s, 80Kg irgasfos 168s, 80Kg to resist
Oxygen agent BHT, 300Kg zinc stearate, 100Kg oleamides, then by parallel dual-screw extruding machine
Extrusion, granulation, obtain final product random copolymer of propylene product.The temperature in each area of the parallel dual-screw extruding machine is：
One area：190 DEG C, 2nd area：230 DEG C, 3rd area：200 DEG C, template：195℃.
Embodiment 3
Prepare random polypropylene：Connected using two horizontal type agitated bed reactors, test load is set as 25.0t/h,
Beijing SAL catalyst charges amount up to catalyst Co. difficult to understand is 2.0Kg/h, and triethyl aluminum inlet amount is 5.4
Kg/h, electron donor diisobutyl methoxy silane inlet amount be 1.0Kg/h, 12 DEG C of Propylene Pre-polymerization temperature,
First reactor is entered after polyase 13 minute, ethene and hydrogen add reaction together in reactor head separator
Device, in first reactor, ethene：The mol ratio of propylene is 0.018：1, hydrogen with the mol ratio of propylene is
0.03：1, in second reactor, ethene is 0.018 with the mol ratio of propylene：1, hydrogen and propylene mole
Than for 0.3：1, reaction temperature is all 75 DEG C, in the presence of catalyst propylene/ethylene carry out continuous gas phase gather
Close, random polypropylene powder is obtained.
200t random polypropylenes are taken, 100Kg antioxidant 1010s, 200Kg irgasfos 168s, 160Kg is added
Antioxidant BHT, 300Kg zinc stearates, 100Kg oleamides, then by parallel dual-screw extruding machine
Middle extrusion, granulation, obtain final product random copolymer of propylene product.The temperature in each area of the parallel dual-screw extruding machine is：
One area：195 DEG C, 2nd area：235 DEG C, 3rd area：210 DEG C, template：200℃.
Embodiment 4
Prepare random polypropylene：Connected using two horizontal type agitated bed reactors, test load is set as 25.0t/h,
The NG/NA catalyst charges amount of Beijing Chemical Research Institute is 2.0Kg/h, and triethyl aluminum inlet amount is 5.4
Kg/h, electron donor diisobutyl methoxy silane inlet amount be 1.0Kg/h, 12 DEG C of Propylene Pre-polymerization temperature,
First reactor is entered after polyase 13 minute, ethene and hydrogen add reaction together in reactor head separator
Device, in first reactor, ethene：The mol ratio of propylene is 0.015：1, hydrogen with the mol ratio of propylene is
0.03：1, in second reactor, ethene is 0.015 with the mol ratio of propylene：1, hydrogen and propylene mole
Than for 0.3：1, reaction temperature is all 75 DEG C, in the presence of catalyst propylene/ethylene carry out continuous gas phase gather
Close, random polypropylene powder is obtained.
200t random polypropylenes are taken, adds 80Kg antioxidant 1010s, 160Kg irgasfos 168s, 60Kg to resist
Oxygen agent BHT, 200Kg zinc stearate, 100Kg oleamides, then by parallel dual-screw extruding machine
Extrusion, granulation, obtain final product random copolymer of propylene product.The temperature in each area of the parallel dual-screw extruding machine is：
One area：195 DEG C, 2nd area：230 DEG C, 3rd area：200 DEG C, template：200℃.
Performance test
Random copolymer of propylene obtained in embodiment is carried out into performance test, and with the commercially available like product (trade mark：
DP-7126-3-1000) contrasted, as a result see the table below：
By obtained in the test result of upper table can be seen that embodiments of the invention, the stretching of random copolymer of propylene is strong
Degree and bending modulus are less than commercially available prod, therefore when identical thickness silk is spun, flexibility is better than common PP products；
The normal temperature simply supported beam notch impact strength of product of the present invention apparently higher than commercially available prod, with excellent mechanical property
Energy.
Claims (9)
1. a kind of random copolymer of propylene for super soft non-woven fabrics, it is characterised in which is by following weight portion
Raw material is prepared from：1000 parts of random polypropylenes, 0.4～1.0 part of antioxidant 1010,0.4～1.0 part of antioxidant
168,0.4～0.8 part of antioxidant BHT, 0.5～1.5 part of stabilizer, 0.5～1.5 part of slipping agent；
The preparation method of the random polypropylene is as follows：By the way of two horizontal type agitated bed reactor series connection,
With Ziegler-Natta catalyst as major catalyst, triethyl aluminum is co-catalyst, diisobutyl methoxy silane
For external electron donor, propylene is raw material, enters the first horizontal type agitated bed reactor, while being passed through second after prepolymerization
Alkene and H2, random polypropylene after polymerisation, is obtained；Wherein, in the first horizontal type agitated bed reactor, ethene：
The mol ratio of propylene is 0.015～0.018：1, hydrogen is 0.02～0.03 with the mol ratio of propylene：1, second crouches
In formula agitated bed reactor, ethene is 0.015～0.018 with the mol ratio of propylene：1, hydrogen and propylene mole
Than for 0.2～0.3：1.
2. the random copolymer of propylene of super soft non-woven fabrics is used for as claimed in claim 1, it is characterised in that by
The raw material of following weight portion is prepared from：1000 parts of random polypropylenes, 0.4～0.6 part of antioxidant 1010,0.6～0.9
Part irgasfos 168,0.4～0.5 part of antioxidant BHT, 0.6～0.8 part of stabilizer, 0.5～0.8 part of slipping agent.
3. the random copolymer of propylene of super soft non-woven fabrics is used for as claimed in claim 1, it is characterised in that
The prepolymerized reaction temperature is 10～13 DEG C, and the reaction time is 1～10min.
4. the random copolymer of propylene of super soft non-woven fabrics is used for as claimed in claim 1, it is characterised in that
In first horizontal type agitated bed reactor and the second horizontal type agitated bed reactor, the temperature of polymerisation is
70～80 DEG C.
5. the random copolymer of propylene of super soft non-woven fabrics is used for as claimed in claim 1, it is characterised in that
The dosage of the Ziegler-Natta catalyst, triethyl aluminum and diisobutyl methoxy silane meets Al/Mg
(mol/mol)=10～14：1, Al/Si (mol/mol)=9:1.
6. the random copolymer of propylene of super soft non-woven fabrics is used for as claimed in claim 1, it is characterised in that described
Stabilizer is calcium stearate or zinc stearate.
7. the random copolymer of propylene of super soft non-woven fabrics is used for as claimed in claim 1, it is characterised in that described
Slipping agent is erucyl amide or oleamide.
8. the preparation of the random copolymer of propylene for super soft non-woven fabrics described in any one of claim 1 to 7
Method, it is characterised in that by random polypropylene, antioxidant 1010, irgasfos 168, antioxidant BHT,
Stabilizer, slipping agent together add extrusion, granulation in parallel dual-screw extruding machine, obtain final product.
9. the preparation method of the random copolymer of propylene of super soft non-woven fabrics is used for as claimed in claim 8, and which is special
Levy and be, the temperature in each area of the parallel dual-screw extruding machine is：One area：180～200 DEG C, 2nd area：
220～240 DEG C, 3rd area：190～210 DEG C, template：185～205 DEG C.
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| CN109233113A (en) * | 2018-08-24 | 2019-01-18 | 大连兴辉化工有限公司 | A kind of atactic copolymerized polypropene and preparation method thereof using edman degradation Edman preparation |
| 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 |
| CN110358189A (en) * | 2019-07-18 | 2019-10-22 | 广东一龙新材料科技有限公司 | A kind of non-woven fabrics softness master batch and preparation method thereof |
| US11946177B2 (en) | 2019-09-23 | 2024-04-02 | Carmel Olefins Ltd | Polypropylene compositions for soft nonwoven fabrics |
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| CN109233113A (en) * | 2018-08-24 | 2019-01-18 | 大连兴辉化工有限公司 | A kind of atactic copolymerized polypropene and preparation method thereof using edman degradation Edman preparation |
| 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 |
| CN110358189A (en) * | 2019-07-18 | 2019-10-22 | 广东一龙新材料科技有限公司 | A kind of non-woven fabrics softness master batch and preparation method thereof |
| CN110358189B (en) * | 2019-07-18 | 2022-04-12 | 广东一龙新材料科技有限公司 | Non-woven fabric soft master batch and preparation method thereof |
| US11946177B2 (en) | 2019-09-23 | 2024-04-02 | Carmel Olefins Ltd | Polypropylene compositions for soft nonwoven fabrics |
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| CN106554569B (en) | 2018-11-13 |
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