CN1451689A - Superhigh melt index polypropene and preparing process thereof - Google Patents
Superhigh melt index polypropene and preparing process thereof Download PDFInfo
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- CN1451689A CN1451689A CN 03116847 CN03116847A CN1451689A CN 1451689 A CN1451689 A CN 1451689A CN 03116847 CN03116847 CN 03116847 CN 03116847 A CN03116847 A CN 03116847A CN 1451689 A CN1451689 A CN 1451689A
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Abstract
A polypropene with ultra-high fusing index (400 g/min) is prepared from conventional polyacrylic resin (50-70%) and degradating mother particles (30-50%) through blending extruding conventional polypropene powder with organic peroxide in a screw extruder, cooling, granulating to obtain said degradating mother particles, mixing conventional polyacrylic resin with said mother particles, extruding, cooling, and granulating.
Description
Technical field
The present invention relates to a kind of acrylic resin of tool superelevation melting index, specifically, relate to melting index and reach acrylic resin that 400g/10min is above and flowing property is stable and preparation method thereof.
Background technology
Acrylic resin has advantages such as little, the easy processing of relative density, mechanical property and chemical resistance be good, cheap, thereby obtains development greatly in the more than ten years recently, is the fastest-rising kind of demand in world's general synthetic resin in recent years.Polypropylene both can be used as plastics, also can be processed into fiber, was particularly suitable as the raw material of non-woven.
What determine the polypropylene end-use is its melt flow, processing characteristics.Polyacrylic melt flowability and its molecular weight are closely related.The weight-average molecular weight of the commodity acrylic resin that is prepared by the Ziegler-Natta catalyst system of routine is generally 3 * 10
5～7 * 10
5Between.The melting index of these conventional acrylic resins is generally 2～5g/10min, the highlyest also can only reach 35～40g/10min, so its melt viscosity is big, and is mobile poor, needs the processing temperature height, and its Application Areas is restricted.
Along with the develop rapidly of chemical fibres industry and Textile Machinery Industry, nonwovens industry emerges rapidly.Polyacrylic series of advantages makes it become the preferred raw materials of non-woven.Along with the development of society, the Application Areas of non-woven is tending towards wide: aspect health care, non-woven can be isolated clothes, mouth mask, operation dress, sanitary napkin, baby diaper or the like in order to make; As building and geotechnological material, non-woven can be used for roof water-proof, road construction, hydro project aspect, or adopts spunbond, acupuncture compounding technology to produce senior roofing felt, and its work-ing life is higher 5～10 times than traditional asphalt felt; Filtering material also is one of non-woven product with fastest developing speed, can be used for gas, the liquid filtering of industries such as chemical industry, medicine, food, has and big market potential; In addition, aspect life family expenses, non-woven can be used for the manufacturing of synthetic leather, case and bag, clothing lining, bunting, cloth for wiping or dusting.Just because of the continuous development of non-woven, the requirement of its production and application is also improved constantly, as melt and spray, high-speed production, slim product etc.Therefore, to the also corresponding raising of requirement of the processing characteristics of the main raw material acrylic resin of non-woven; In addition, the production of high-speed spinning or fine denier polypropylene fibers also requires acrylic resin to have good melt flow property; Some can not more need the relatively low polypropylene of processing temperature as carrier by resistant to elevated temperatures pigment.All these superelevation melting index acrylic resin that requires processing at a lower temperature is a raw material.
Develop the polypropylene of all-purpose controllable rheology performance at present abroad, can prepare the polypropylene that melting index is 5 bit digital now, but still can not satisfy the needs of field develop rapidlys such as chemical fibres industry, Textile Machinery Industry.Therefore, development high fusion index polypropylene for improving polyacrylic processing characteristics, improves the use properties of product, and expanding polyacrylic Application Areas will play an important role.
Preparation high fusion index acrylic resin has two kinds of methods usually.The one,, reduce the molecular weight of polymkeric substance as adopting the method that improves stopper such as density of hydrogen, thereby improve melting index to control polyacrylic molecular weight and molecular weight distribution by the controlled polymerization reaction process.This method is subjected to the restriction of factors such as catalyst system, reaction conditions, and relatively difficulty is implemented in the difficult control of the stability of melting index.Melting index is reached about 40g/10min, and product is applicable to injection moulding and is unfavorable for fiberizing.Another kind method is that the polypropylene that conventional polymerization obtains is carried out control degradation, reduces its molecular weight, improves melting index.Past, high temperature degradation method commonly used reduced polyacrylic molecular weight, but the mode of this high-temperature machinery degraded has many drawbacks, as unfavorable factors such as additive loss and thermolysis, technology instabilities.Also have methods such as ultrasonic degradation in addition, but these methods often need the existence of solvent, have increased technology difficulty and cost.In recent years, the method for polypropylene chemical degradation has obtained widespread use gradually.Chemical degradation method is that polypropylene and chemical degradation agent such as organic superoxide etc. are reacted in screw extrusion press, makes polypropylene molecular chain take place to rupture and reduce its molecular weight.Compare with other degradation method, it has advantages such as degraded is complete, fluidity of molten is good, preparation technology is simple and easy to do, carries out large-scale industrial production easily.
Adopt chemical degradation method, document (" Zhang Yingzhen. the production technique of opinion polypropylene high fusion index (MFR) product. the Guangzhou chemical industry, 1999,27 (3): 56-58 ", " Zhang Baoxing, Qiao Huiping, Zhou Liangda. production of High-MIPolypropylene. petrochemical complex, 2000,29 (5): 358～360 ", " Peng Guilian, Gu Ling, Zhou Aimin, Shen Hua. the development of high-melt index PP PP Pipe Compound. modern plastics processed and applied, 1991, No.4:26～30 ", " Shen Xuegui. the research and the discussion of polypropylene exploitation high-melt index PP resin. Nanjing petrochemical complex, 1991, No.4:1～4 ") reported once that melting index MI was the preparation method of the acrylic resin of 20～80g/10min.Its product decapacitation replaces tearing film to make outside the purposes such as rope, strapping goods, woven mesh goods, can also replace cotton, fiber crops, single, be applied to sewing, weaving, spray silk, carpet backing, Nomex etc., especially for high speed spinning, non-woven and cigarette polypropylene filtering material novel product.But, melting index more than 100g/10min and flowing property stable, to be mainly used in the polyacrylic production report of superelevation melting index that slim non-woven makes also less.
Summary of the invention
One of technical issues that need to address of the present invention are to disclose a kind of superelevation melting index acrylic resin, to overcome the above-mentioned defective that prior art exists, satisfy the demand of suitability for industrialized production;
Two of the technical issues that need to address of the present invention provide the preparation method of above-mentioned superelevation melting index acrylic resin.
Technical conceive of the present invention is such: the contriver at first with behind organo-peroxide and the conventional polypropylene powder usefulness mixing machine thorough mixing, uses screw extrusion press blend granulation on the basis of existing technology again, obtains containing the degradation master batch of organic superoxide; Then conventional acrylic resin is required to mix by a certain percentage according to melting index with degradation master batch, extrude with the twin screw extruder melt blending.In these courses of processing, the free radical that organo-peroxide produces is degraded polypropylene, and polyacrylic relative molecular mass reduces.Final material can obtain the superelevation melting index acrylic resin of melting index 〉=400g/10min after cooling, granulation.
Advantage of the present invention is to use polypropylene powder and liquid degradant additive (organo-peroxide) blend granulation, makes degradation master batch and conventional acrylic resin blending reaction again, has solved the homodisperse problem of low levels additive; Organo-peroxide through for the first time with the process of polypropylene powder melt blending in, produced a large amount of free radicals, guarantee for the second time with conventional acrylic resin melt blending the time, to react completely, make its melting index stable in seasoning and use.
Superelevation melting index acrylic resin of the present invention comprises conventional acrylic resin and degradation master batch.
Wherein, by weight resin, conventional acrylic resin content is 50～70%, and degradation master batch content is 30～50%, and degradation master batch content is with the melt flow index of major decision final product.
Described degradation master batch is the part degraded blend of conventional polypropylene powder and organo-peroxide, and by master batch weight, organo-peroxide content is 0.2～1.2%, and melting index is 400g/10min～1000g/10min.
Term " blend of partly degrading " refers to the product that the conventional polypropylene powder in the degradation master batch is obtained by organo-peroxide part chemical degradation in the blend process.
The structure of described organo-peroxide is:
R-O-O-R
Wherein R is an alkyl, preferably comprises 2,5-dimethyl 2,5 dual-tert-butyl peroxidation hexanes, two-2-t-tutyl cumyl peroxide, 2, a kind of in 5-dimethyl-2,5 dual-tert-butyl peroxidation-3-hexene or the di-t-butyl peroxide etc.They can be to select according to their transformation period length under processing temperature, and most preferred is di-t-butyl peroxide, and its transformation period is about 1min under 193 ℃.
The acrylic resin without granulation of described polypropylene powder for obtaining by conventional suspension polymerization, as the trade mark of raising sub-petrochemical industry is the polypropylene powder of F401, its relative molecular mass is about 38～400,000, the melting index scope is 2～5g/10min.
The preparation method of superelevation melting index acrylic resin of the present invention comprises the steps:
(1) be about 0.5～1.5% with conventional polypropylene powder and weight fraction, organo-peroxide, after preferred liquid di-t-butyl peroxide thorough mixing is even, in screw extrusion press, extrude in 180～190 ℃ of following blend, according to screw diameter and length-to-diameter ratio, the control rotating speed makes residence time of material≤1min, and product obtains degradation master batch through cooling, granulation;
(2) conventional acrylic resin and (1) are set by step obtained contain di-t-butyl peroxide be 0.2～1.2% degradation master batch by a certain percentage thorough mixing evenly after, in twin screw extruder, extrude in 190～220 ℃ of following blend, according to screw diameter and length-to-diameter ratio, it is 0.5～4min that the control rotating speed makes residence time of material, product obtains superelevation melting index acrylic resin through cooling, granulation.With this understanding, if the weight fraction of di-t-butyl peroxide is 0.5% in the degradation master batch, the weight fraction of degradation master batch is 30%, and the melting index of the superelevation melting index acrylic resin that finally obtains is about 400g/10min; Strengthening the consumption of degradation master batch, can obtain higher melting index, is 50% o'clock at the weight fraction of degradation master batch, and melting index can reach about 1000g/10min.
The mensuration ordinary method of melting index is: making material is the kapillary of 1.18mm at 230 ℃ of temperature, the load diameter of flowing through under the 21.17cN, and the outflow quality in 10min is the numerical value of melting index.Because acrylic resin melt fluidity of the present invention is very good, take-off rate is very fast, can't be by the 10min timing measuring.The method that the present invention adopts is that (measuring method of limiting viscosity is: dissolve acrylic resin with perhydronaphthalene according to the melting index of acrylic resin and the linear relationship of its limiting viscosity under log-log coordinates, be mixed with the solution of 0.1g/dL, with capillary diameter is that the Ubbelohde viscometer of 0.4～0.5mm is measured its limiting viscosity), measure the less and limiting viscosity known acrylic resin of its numerical value of a series of melting index and obtain working curve, the relation of determining by working curve can obtain melting index by limiting viscosity.
Measure with aforesaid method that the present invention contains degradation master batch 30% (containing 0.5% di-t-butyl peroxide) and 70% conventional polyacrylic degraded product, Borealis's nominal melting index are that 400g/10min acrylic resin and spulon nominal melting index are the 400g/10min acrylic resin, its melting index is respectively 403,389,278g/10min.
The judgment basis of melting index stability: degraded product is used the twin screw extruder extruding pelletization more under the same conditions, measure the melting index of extruding product for twice respectively, the polyacrylic melting index deviation of superelevation melting index of the present invention is in ± 5%.
By above-mentioned disclosed technical scheme as seen, preparation method of the present invention, operating process is very easy, is the above superelevation melting index acrylic resin of 100g/10min but can obtain melting index, thereby can satisfies the demand of suitability for industrialized production.
Embodiment
Embodiment 1
Through metered charge, the F401 polypropylene powder that with weight ratio is 99: 1 mixes in the GH200 high-speed mixer with di-t-butyl peroxide, the mixing machine rotating speed is 10rpm, mix 4min, again mixture is used φ 65mm, extrude in 195 ℃ under 60～80rpm rotating speed in the single screw extrusion machine of L/D=20, cooling, granulation obtain degradation master batch.
With the F401 acrylic resin is matrix, adds the above-mentioned degradation master batch of 30% weight fraction, after mixing, in φ 35mm * 2, melt extrudes granulation on the twin screw extruder of L/D=25 under 190～200 ℃, screw speed 60～75rpm.Extrudate obtains final product after cooling, granulation, its melting index is 403g/10min.
Embodiment 2
Through metered charge, the F401 polypropylene powder that with weight ratio is 99: 1 mixes in the GH200 high-speed mixer with di-t-butyl peroxide, the mixing machine rotating speed is 10rpm, mix 4min, again mixture is used φ 65mm, extrude in 190 ℃ under 60～80rpm rotating speed in the single screw extrusion machine of L/D=20, cooling, granulation obtain degradation master batch.
With the F401 acrylic resin is matrix, adds the above-mentioned degradation master batch of 40% weight fraction, after mixing, in φ 35mm * 2, melt extrudes granulation on the twin screw extruder of L/D=25 under 190～200 ℃, screw speed 60～75rpm.Extrudate obtains final product after cooling, granulation, its melting index is 750g/10min.
Embodiment 3
Through metered charge, the F401 polypropylene powder that with weight ratio is 99: 1 mixes in the GH200 high-speed mixer with di-t-butyl peroxide, the mixing machine rotating speed is 10rpm, mix 4min, again mixture is used φ 65mm, extrude in 1200 ℃ under 60～80rpm rotating speed in the single screw extrusion machine of L/D=20, cooling, granulation obtain degradation master batch.
With the F401 acrylic resin is matrix, adds the above-mentioned degradation master batch of 35% weight fraction, after mixing, in φ 72mm * 2, melt extrudes granulation on the twin screw extruder of L/D=35 under 190～200 ℃, screw speed 60～70rpm.Extrudate obtains final product after cooling, granulation, its melting index is 580g/10min.
Embodiment 4
Through metered charge, the F401 polypropylene powder that with weight ratio is 99: 1 mixes in the GH200 high-speed mixer with di-t-butyl peroxide, the mixing machine rotating speed is 10rpm, mix 4min, again mixture is used φ 65mm, extrude in 195 ℃ under 60～80rpm rotating speed in the single screw extrusion machine of L/D=20, cooling, granulation obtain degradation master batch.With the F401 acrylic resin is matrix, adds the above-mentioned degradation master batch of 50% weight fraction, after mixing, in φ 72mm * 2, melt extrudes granulation on the twin screw extruder of L/D=35 under 190～200 ℃, screw speed 60～70rpm.Extrudate obtains final product after cooling, granulation, its melting index is 1011g/10min.
Claims (10)
1. a superelevation melting index polypropylene is characterized in that, comprises conventional acrylic resin and degradation master batch, and wherein, by weight resin, conventional acrylic resin content is 50～70%, and degradation master batch content is 30～50%;
Described degradation master batch is the part degraded blend of conventional polypropylene powder and organo-peroxide, and by master batch weight, organo-peroxide content is 0.2～1.2%.
2. polypropylene according to claim 1 is characterized in that, its melting index is 400g/10min～1000g/10min.
3. polypropylene according to claim 2 is characterized in that organo-peroxide comprises 2,5-dimethyl-2,5 dual-tert-butyl peroxidation hexanes, two-2-t-tutyl cumyl peroxide, 2, a kind of in 5-dimethyl-2,5 dual-tert-butyl peroxidation-3-hexene or the di-t-butyl peroxide.
4. polypropylene according to claim 3 is characterized in that, organo-peroxide is a di-t-butyl peroxide.
5. according to each described polypropylene of claim 1～4, it is characterized in that the acrylic resin without granulation of described polypropylene powder for obtaining by conventional suspension polymerization.
6. according to each described polypropylene of claim 1～4, it is characterized in that the polypropylene powder relative molecular mass is 38～400,000, the melting index scope is 2～5g/10min.
7. according to each described polyacrylic preparation method of claim 1～6, it is characterized in that, comprise the steps:
(1) with conventional polypropylene powder and weight fraction is 0.5～1.5% organo-peroxide, after the mixing, extrude in 180～190 ℃ of following blend in screw extrusion press, the control rotating speed makes residence time of material≤1min, product obtains degradation master batch through cooling, granulation;
(2) after the degradation master batch that conventional acrylic resin and (1) are set by step obtained mixed, blend was extruded in twin screw extruder, and product obtains superelevation melting index acrylic resin through cooling, granulation.
8. polyacrylic preparation method according to claim 7 is characterized in that, organo-peroxide is liquid di-t-butyl peroxide.
9. polyacrylic preparation method according to claim 7, it is characterized in that, it with conventional polypropylene powder and weight fraction 0.5～1.5% organo-peroxide, behind the thorough mixing, extrude in 180～190 ℃ of following blend in screw extrusion press, the control rotating speed makes residence time of material≤1min.
10. polyacrylic preparation method according to claim 7; it is characterized in that; after the degradation master batch that conventional acrylic resin and (1) are set by step obtained mixes; in twin screw extruder, extrude in 190～220 ℃ of following blend; it is 0.5～4min that the control rotating speed makes residence time of material; product obtains superelevation melting index acrylic resin through cooling, granulation.
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| CN1314745C (en) * | 2005-01-11 | 2007-05-09 | 武汉化工学院 | Manufacturing method of high fluidity polypropylene |
| CN100461043C (en) * | 2006-12-22 | 2009-02-11 | 浙江大学 | Melt index detection fault diagnosis system and method for industial polypropylene production |
| CN100461044C (en) * | 2006-12-22 | 2009-02-11 | 浙江大学 | Melt index detection fault diagnozing system and method in propylene polymerization production |
| CN101429308B (en) * | 2007-11-08 | 2011-04-20 | 中国石油天然气股份有限公司 | Method for manufacturing polypropylene degradation master batch |
| CN102146185B (en) * | 2010-02-04 | 2012-12-19 | 中国石油化工股份有限公司 | Controllable-rheological toughened transparent polypropylene and preparation method thereof |
| CN103483682A (en) * | 2013-08-27 | 2014-01-01 | 陕西省轻工业研究设计院 | Method for preparing polypropylene coating by modifying T30S granules |
| CN104231432A (en) * | 2014-09-15 | 2014-12-24 | 陕西延长石油（集团）有限责任公司 | Method for preparing high-melt-flow-rate polypropylene by virtue of polypropylene T30s aggregate modification |
| CN105733093A (en) * | 2016-03-28 | 2016-07-06 | 中国石油化工股份有限公司 | Special high-flowability resin for polypropylene fibers and preparation method thereof |
| CN108003488A (en) * | 2017-12-15 | 2018-05-08 | 大连工业大学 | A kind of controllable PB Polybutene-1 material of melt index and preparation method |
| CN109054186A (en) * | 2018-08-24 | 2018-12-21 | 大连兴辉化工有限公司 | A kind of Functional Polyolefine solid degradation agent |
| CN110117395A (en) * | 2019-06-06 | 2019-08-13 | 东莞市恒彩塑胶颜料有限公司 | A kind of PP flow master batch |
| CN111423660A (en) * | 2020-04-28 | 2020-07-17 | 青岛中孚科力橡塑有限公司 | Expanded and fused electret antibacterial master batch, processing technology and application |
| CN111499970A (en) * | 2020-04-21 | 2020-08-07 | 广州市聚赛龙工程塑料股份有限公司 | Electret modified polypropylene material special for melt-blown non-woven fabric applicable to mask and preparation method thereof |
| CN111533994A (en) * | 2020-05-09 | 2020-08-14 | 东华能源(张家港)新材料有限公司 | High-cracking-rate high-melt-index polypropylene material and preparation method and application 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 |
| CN112092234A (en) * | 2020-08-25 | 2020-12-18 | 万华化学集团股份有限公司 | Starting method for polypropylene granulation and granulation method |
| CN112606257A (en) * | 2020-10-29 | 2021-04-06 | 杭州聚丰新材料有限公司 | Low-odor and narrow-molecular-weight-distribution high-melt-index polypropylene and preparation method thereof |
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| CN115505168A (en) * | 2021-06-23 | 2022-12-23 | 松山湖材料实验室 | Production of high-fluidity polypropylene by chemical degradation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1314745C (en) * | 2005-01-11 | 2007-05-09 | 武汉化工学院 | Manufacturing method of high fluidity polypropylene |
| CN100461043C (en) * | 2006-12-22 | 2009-02-11 | 浙江大学 | Melt index detection fault diagnosis system and method for industial polypropylene production |
| CN100461044C (en) * | 2006-12-22 | 2009-02-11 | 浙江大学 | Melt index detection fault diagnozing system and method in propylene polymerization production |
| CN101429308B (en) * | 2007-11-08 | 2011-04-20 | 中国石油天然气股份有限公司 | Method for manufacturing polypropylene degradation master batch |
| CN102146185B (en) * | 2010-02-04 | 2012-12-19 | 中国石油化工股份有限公司 | Controllable-rheological toughened transparent polypropylene and preparation method thereof |
| CN103483682A (en) * | 2013-08-27 | 2014-01-01 | 陕西省轻工业研究设计院 | Method for preparing polypropylene coating by modifying T30S granules |
| CN104231432A (en) * | 2014-09-15 | 2014-12-24 | 陕西延长石油（集团）有限责任公司 | Method for preparing high-melt-flow-rate polypropylene by virtue of polypropylene T30s aggregate modification |
| CN105733093A (en) * | 2016-03-28 | 2016-07-06 | 中国石油化工股份有限公司 | Special high-flowability resin for polypropylene fibers and preparation method thereof |
| CN108003488A (en) * | 2017-12-15 | 2018-05-08 | 大连工业大学 | A kind of controllable PB Polybutene-1 material of melt index and preparation method |
| CN109054186B (en) * | 2018-08-24 | 2021-09-14 | 任国辉 | Functional polyolefin solid degradation agent |
| CN109054186A (en) * | 2018-08-24 | 2018-12-21 | 大连兴辉化工有限公司 | A kind of Functional Polyolefine solid degradation agent |
| CN110117395A (en) * | 2019-06-06 | 2019-08-13 | 东莞市恒彩塑胶颜料有限公司 | A kind of PP flow master batch |
| CN113388188A (en) * | 2020-03-11 | 2021-09-14 | 广东奇德新材料股份有限公司 | Ultrahigh-fluidity antibacterial PP material and preparation method thereof |
| CN111499970A (en) * | 2020-04-21 | 2020-08-07 | 广州市聚赛龙工程塑料股份有限公司 | Electret modified polypropylene material special for melt-blown non-woven fabric applicable to mask and preparation method thereof |
| CN111423660A (en) * | 2020-04-28 | 2020-07-17 | 青岛中孚科力橡塑有限公司 | Expanded and fused electret antibacterial master batch, processing technology and application |
| CN111533994A (en) * | 2020-05-09 | 2020-08-14 | 东华能源(张家港)新材料有限公司 | High-cracking-rate high-melt-index polypropylene material and preparation method and application 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 |
| CN112092234A (en) * | 2020-08-25 | 2020-12-18 | 万华化学集团股份有限公司 | Starting method for polypropylene granulation and granulation method |
| CN112606257A (en) * | 2020-10-29 | 2021-04-06 | 杭州聚丰新材料有限公司 | Low-odor and narrow-molecular-weight-distribution high-melt-index polypropylene and preparation method thereof |
| CN112812445A (en) * | 2021-01-18 | 2021-05-18 | 侯会春 | Stone-plastic box modified master batch, preparation method thereof and obtained product |
| CN115505168A (en) * | 2021-06-23 | 2022-12-23 | 松山湖材料实验室 | Production of high-fluidity polypropylene by chemical degradation method |
| CN115505168B (en) * | 2021-06-23 | 2024-03-08 | 松山湖材料实验室 | Production of high fluidity polypropylene by chemical degradation method |
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Assignee: Zhongshan Konky Health-care Products Co., Ltd. Assignor: Donghua University Contract fulfillment period: 2007.11.26 to 2012.11.25 contract change Contract record no.: 2008440000449 Denomination of invention: Superhigh melt index polypropene and preparing process thereof Granted publication date: 20050907 License type: Exclusive license Record date: 20081128 |
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