CN101357968A - Maleic anhydride-grafted polypropylene material and preparation method thereof - Google Patents
Maleic anhydride-grafted polypropylene material and preparation method thereof Download PDFInfo
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- CN101357968A CN101357968A CNA2008102222932A CN200810222293A CN101357968A CN 101357968 A CN101357968 A CN 101357968A CN A2008102222932 A CNA2008102222932 A CN A2008102222932A CN 200810222293 A CN200810222293 A CN 200810222293A CN 101357968 A CN101357968 A CN 101357968A
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- maleic anhydride
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Abstract
The invention discloses a maleic anhydride grafted polypropylene material and a preparation method thereof. The material is prepared with polypropylene, an initiator, maleic anhydride and a polyfunctional group monomer. In the preparation method, after the polypropylene, the initiator, the maleic anhydride and the polyfunctional group monomer are mixed uniformly, the mixture is molten and compounded, thus getting the product. The temperature for melting and compounding ranges from 150 DEG C to 250 DEG C. The mixture is molten and compounded in a double screw extruder, and the screw of the double screw extruder runs at the speed of 50 to 500 turns per minute. The ratio of length to diameter of the screw ranges from 15 to 100. In the maleic anhydride grafted polypropylene. The content of grafted maleic anhydride is more than 1.0 percent; the excellent mechanical property of the polypropylene base is kept while the polarity of the polypropylene is improved. The maleic anhydride grafted polypropylene can be used as a compatilizer for a polymer blending system to improve the surface coating performance of products.The preparation method is operated easily and simply, and is applicable for industrial production.
Description
Technical field
The present invention relates to a kind of maleic anhydride inoculated polypropylene material and preparation method thereof.
Background technology
Polypropylene (PP) is one of five big general-purpose plastics, has good mechanical property, at automobile, and household electrical appliance, many fields such as packing have a very wide range of applications.But because polyacrylic nonpolar and crystallinity, make it poor, be difficult for moisteningly, bonding that printing and coating property are poor, can not obtain the good material of performance during with the polar material blend with the consistency of most of superpolymer.Therefore need carry out modification to polypropylene, increase its polarity, widen its range of application.Modified monomer commonly used is a maleic anhydride.
Present stage has solution graft copolymerization with maleic anhydride graft to the main method on the main polymer chain, fusion-grafting, solid phase grafting and suspension grafting.
Solution graft copolymerization is that polymkeric substance is dissolved in the appropriate solvent, and graft reaction carries out in solution, and this method is not used widely owing to need to reclaim a large amount of solvents.
Chinese invention patent CN1793190A has introduced the method for utilizing solid phase method to obtain the maleic anhydride inoculated polypropylene material.This method is by introducing tensio-active agent, make graft reaction under the situation of solid phase, occur in polypropylene surface, can obtain the higher modified polypropylene material of percentage of grafting, have simple to operate simultaneously, pollute advantages such as little, but owing to graft reaction mostly occurs on the surface of polypropylene matrix, so there is the uneven shortcoming of grafting in this method.
Chinese invention patent CN1948356A has introduced the method for utilizing suspension solid phase grafting to prepare copolymer-maleic anhydride.This method uses a large amount of water to reach more than 1 hour as dispersion medium and reaction times, thereby is unfavorable for large-scale production.
The fusion-grafting method is because simple to operate, the production efficiency height, and become the most frequently used method at present.In the grafting process, the free radical that decomposition of initiator produces is captured the hydrogen on the polypropylene molecular chain and is formed macromolecular radical, but it is easy to take place the deterioration that the β chain rupture is promptly degraded and caused the low and material property of percentage of grafting, therefore how the control stabilization macromolecular radical makes reaction just become the polyacrylic key of the preparation high percentage of grafting of high-performance to the grafted direction.Chinese invention patent CN1456430A and CN1230554A have all introduced the percentage of grafting that common monomer improves maleic anhydride in polypropylene fusion graft process.In CN1230554A, adopt with vinylbenzene as the cografting monomer, but styrene monomer is easy to volatilization, harmful.In CN1456430A, application person with oleic acid for the cografting monomer can improve percentage of grafting, but and undeclared its mechanism, do not provide the information of support yet.
Summary of the invention
The purpose of this invention is to provide a kind of maleic anhydride inoculated polypropylene material and preparation method thereof.
Maleic anhydride inoculated polypropylene material provided by the invention is made by polypropylene, initiator, maleic anhydride and polyfunctional monomer;
Wherein, initiator is a di-isopropylbenzene hydroperoxide, 2,5-dimethyl-2,5-bis(t-butylperoxy) hexane, dicumyl peroxide, di-t-butyl peroxide or peroxidized t-butyl perbenzoate; Preferred di-isopropylbenzene hydroperoxide, 2,5-dimethyl-2,5-bis(t-butylperoxy) hexane, dicumyl peroxide;
Polyfunctional monomer is a tripropylene glycol diacrylate, propylene glycol diacrylate, 1, the 6-hexanediyl ester, 1,4 butanediol diacrylate, neopentylglycol diacrylate, ethoxylated neopentylglycol diacrylate, PDDA, ethoxylated bisphenol a diacrylate, Viscoat 295, ethoxylated trimethylolpropane triacrylate, the propoxylation Viscoat 295, trimethylolpropane trimethacrylate, glycerol propoxylate triacrylate or pentaerythritol triacrylate; Preferred pentaerythritol triacrylate, Viscoat 295, trimethylolpropane trimethacrylate or ethoxylated neopentylglycol diacrylate;
Polypropylene is homopolymer polypropylene and/or polypropylene copolymer.
In the above-mentioned maleic anhydride inoculated polypropylene material, polyacrylic mass fraction is 100, and the mass fraction of initiator is 0.005-4, preferred 0.05-1, more preferably 0.075-0.3; The mass fraction of maleic anhydride is 1-10, preferred 1-5, more preferably 1.5-3; The mass fraction of polyfunctional monomer is 0.05-5, preferred 0.5-3, more preferably 0.75-2.25.
The method of the above-mentioned maleic anhydride inoculated polypropylene material of preparation provided by the invention is that fusion behind polypropylene, initiator, maleic anhydride and the polyfunctional monomer mixing is compound, obtains the maleic anhydride inoculated polypropylene material;
Wherein, used initiator and polyfunctional monomer are all as mentioned above.
In this method, polyacrylic mass fraction is 100, and the mass fraction of initiator is 0.005-4, preferred 0.05-1, more preferably 0.075-0.3; The mass fraction of maleic anhydride is 1-10, preferred 1-5, more preferably 1.5-3; The mass fraction of polyfunctional monomer is 0.05-5, preferred 0.5-3, more preferably 0.75-2.25.
Fusion compound temperature is 150-250 ℃, preferred 150-200 ℃, and more preferably 170-195 ℃.This fusion composite steps can be carried out in twin screw extruder, and screw speed is 50-500 rev/min, and length-to-diameter ratio is 15-100.
The preparating mechanism of this method is that initiator at high temperature decomposes the generation free radical, slough hydrogen atom from polypropylene backbone, form macromolecular radical, polyfunctional monomer can combine with macromolecular radical, form more stable free radical and branched structure, effectively suppressed polyacrylic DeR; Polyfunctional monomer and maleic anhydride have copolymerization performance preferably simultaneously, can improve the transformation efficiency of maleic anhydride, make the maleic anhydride inoculated polypropylene material with high percentage of grafting.
The maleic anhydride inoculated polypropylene of the present invention's preparation, the grafted maleic anhydride content is more than 1.0%, also keep polypropylene base-material excellent mechanical property simultaneously at raising polypropylene polar, can be used for the compatilizer of Polymer Blending System, improved the surface daub on a wall performance of goods.Preparation method provided by the invention is easy and simple to handle, is easy to suitability for industrialized production.
Description of drawings
Fig. 1 is the infrared spectrogram of the maleic anhydride inoculated polypropylene material of the embodiment of the invention 1 and Comparative Examples 1 preparation.
Fig. 2 is the infrared spectrogram of the maleic anhydride inoculated polypropylene material of embodiment of the invention 2-5 preparation.
Embodiment
The invention will be further described below in conjunction with specific embodiment, but the present invention is not limited to following examples.
Embodiment 1, preparation maleic anhydride inoculated polypropylene material
Feed composition (pressing mass fraction, down together): 100 parts of homo-polypropylene, Daqing petrochemical company production, the trade mark is T30S, all adopts this homo-polypropylene among the following embodiment; 0.05 part of dicumyl peroxide; 1.5 parts of maleic anhydrides; 1.5 parts of pentaerythritol triacrylates.
Used twin screw extruder is for rotating the cord wood twin screw extruder in the same way, and screw diameter is 30mm, and length-to-diameter ratio is 40, and seven sections heating temperature controls are adopted in speed control by frequency variation.Below all select this twin screw extruder for use among each embodiment.
Said components is mixed with high-speed mixer, in twin screw extruder, melt extrude granulation then, promptly obtain maleic anhydride inoculated polypropylene material provided by the invention.Wherein, the forcing machine rotating speed is 150 rev/mins, and twin screw each section temperature from the spout to the head is: 170 ℃, 180 ℃, 190 ℃, 195 ℃, 195 ℃, 190 ℃, 185 ℃.
Place cable-styled extractor with acetone extracting 12 hours product, place dimethylbenzene fully to dissolve the product after the extracting then, utilize acid base titration to measure percentage of grafting, the product after the extracting simultaneously is pressed into the film infrared analysis.
Embodiment 2, preparation maleic anhydride inoculated polypropylene material
Feed composition: 100 parts of homo-polypropylene; 2,5-dimethyl-2,0.075 part of 5-bis(t-butylperoxy) hexane; 1.5 parts of maleic anhydrides; 0.75 part of pentaerythritol triacrylate.
Said components is mixed with high-speed mixer, in twin screw extruder, melt extrude granulation then, promptly obtain maleic anhydride inoculated polypropylene material provided by the invention.Wherein, the forcing machine rotating speed is 150 rev/mins, and twin screw each section temperature from the spout to the head is: 170 ℃, 180 ℃, 190 ℃, 195 ℃, 195 ℃, 190 ℃, 185 ℃.
Place cable-styled extractor to use acetone extracting 12 hours product, the product after the extracting is pressed into the film infrared analysis.
Embodiment 3, preparation maleic anhydride inoculated polypropylene material
Adopt and embodiment 2 identical preparation conditions, only with raw material and corresponding mass fraction thereof according to change as follows: 100 parts of homo-polypropylene; 0.10 part of dicumyl peroxide; 2.0 parts of maleic anhydrides; 2.25 parts of pentaerythritol triacrylates.
Place cable-styled extractor to use acetone extracting 12 hours products therefrom, the product after the extracting is pressed into the film infrared analysis.
Embodiment 4, preparation maleic anhydride inoculated polypropylene material
Adopt and embodiment 2 identical preparation conditions, only with raw material and corresponding mass fraction thereof according to change as follows: 100 parts of homo-polypropylene; 0.15 part of dicumyl peroxide; 2.5 parts of maleic anhydrides; 3 parts of pentaerythritol triacrylates.
Place cable-styled extractor to use acetone extracting 12 hours products therefrom, the product after the extracting is pressed into the film infrared analysis.
Embodiment 5, preparation maleic anhydride inoculated polypropylene material
Adopt and embodiment 2 identical preparation conditions, only with raw material and corresponding mass fraction thereof according to change as follows: 100 parts of homo-polypropylene; 0.3 part of dicumyl peroxide; 3.0 parts of maleic anhydrides; 3 parts of Viscoat 295s.
Place cable-styled extractor to use acetone extracting 12 hours products therefrom, the product after the extracting is pressed into the film infrared analysis.
The percentage of grafting of the maleic anhydride inoculated polypropylene material that the foregoing description 2-5 prepares characterizes and sees Table 1.Fig. 2 is the infared spectrum of the maleic anhydride inoculated polypropylene of embodiment 2-5 gained.Wherein, 2721cm
-1The absorption peak at place is polyacrylic charateristic avsorption band, 1784cm
-1And 1860cm
-1The absorption peak at place is the charateristic avsorption band of maleic anhydride.1784cm
-1The integral area and the 2721cm of the absorption peak at place
-1Locate the ratio of integral area, can react the percentage of grafting size of maleic anhydride in the polypropylene, the big more then percentage of grafting of ratio is high more.By table 1 as seen, percentage of grafting improves along with the increase of polyfunctional monomer consumption, and the mechanical property of the maleic anhydride inoculated polypropylene material that embodiment 2-5 prepares is identical with embodiment 1.
The percentage of grafting of the maleic anhydride inoculated polypropylene material that table 1 embodiment 2-5 prepares
Comparative Examples 1
Remove and do not add pentaerythritol triacrylate, other component and preparation condition embodiment 1 are identical, obtain the maleic anhydride inoculated polypropylene material.
Performances such as the maleic anhydride inoculated polypropylene material that embodiment 1 and this Comparative Examples 1 are prepared and the bending of polypropylene matrix, stretching are tested, the gained data are as shown in table 2, show that the relative polypropylene matrix melting index with the graft polypropylene of gained in the Comparative Examples 1 of embodiment 1 increases to some extent, but that the graft polypropylene melting index of embodiment 1 gained is compared the polypropylene matrix increasing degree is very little.The graft polypropylene mechanical property of embodiment 1 gained is better than polypropylene matrix, and the graft polypropylene mechanical property of Comparative Examples 1 gained is then than polypropylene matrix difference.The percentage of grafting of the graft polypropylene of embodiment 1 gained will be far above the graft polypropylene of Comparative Examples 1 gained.MFI (melting index) and mechanical property are all according to the ASTM standard test, and percentage of grafting is measured by acid base titration
The infared spectrum of embodiment 1 and Comparative Examples 1 as shown in Figure 1,2721cm wherein
-1The absorption peak at place is polyacrylic charateristic avsorption band, 1784cm
-1And 1860cm
-1The absorption peak at place is the charateristic avsorption band of maleic anhydride, 1735cm
-1The absorption peak at place is the charateristic avsorption band of acrylate.1784cm
-1The integral area and the 2721cm of the absorption peak at place
-1Locate the ratio of integral area, can react the percentage of grafting size of maleic anhydride in the polypropylene, the big more then percentage of grafting of ratio is high more.As seen from Figure 1, this ratio of embodiment 1 is significantly higher than comparative example 1, this with table 2 in the result of the maleic anhydride grafting ratio directly measured be consistent.
The polypropylene material that table 2 embodiment 1, Comparative Examples 1 prepare and the performance data of polypropylene matrix
Claims (10)
1, a kind of maleic anhydride inoculated polypropylene material is made by polypropylene, initiator, maleic anhydride and polyfunctional monomer;
Wherein, described initiator is a di-isopropylbenzene hydroperoxide, 2,5-dimethyl-2,5-bis(t-butylperoxy) hexane, dicumyl peroxide, di-t-butyl peroxide or peroxidized t-butyl perbenzoate;
Described polyfunctional monomer is a tripropylene glycol diacrylate, propylene glycol diacrylate, 1, the 6-hexanediyl ester, 1,4 butanediol diacrylate, neopentylglycol diacrylate, ethoxylated neopentylglycol diacrylate, PDDA, ethoxylated bisphenol a diacrylate, Viscoat 295, ethoxylated trimethylolpropane triacrylate, the propoxylation Viscoat 295, trimethylolpropane trimethacrylate, glycerol propoxylate triacrylate or pentaerythritol triacrylate.
2, maleic anhydride inoculated polypropylene material according to claim 1 is characterized in that: described initiator is a di-isopropylbenzene hydroperoxide, 2,5-dimethyl-2,5-bis(t-butylperoxy) hexane or dicumyl peroxide; Described polyfunctional monomer is pentaerythritol triacrylate, Viscoat 295, trimethylolpropane trimethacrylate or ethoxylated neopentylglycol diacrylate.
3, maleic anhydride inoculated polypropylene material according to claim 1 and 2 is characterized in that: the ratio of quality and the number of copies of described polypropylene and initiator, maleic anhydride and polyfunctional monomer is 100: 0.005-4: 1-10: 0.05-5.
4, maleic anhydride inoculated polypropylene material according to claim 3 is characterized in that: the mass fraction of described initiator is 0.05-1, preferred 0.075-0.3;
The mass fraction of described maleic anhydride is 1-5, preferred 1.5-3;
The mass fraction of described polyfunctional monomer is 0.5-3, preferred 0.75-2.25.
5, a kind of method for preparing the arbitrary described maleic anhydride inoculated polypropylene material of claim 1-4 is that fusion behind polypropylene, initiator, maleic anhydride and the polyfunctional monomer mixing is compound, obtains described maleic anhydride inoculated polypropylene material;
Described initiator is a di-isopropylbenzene hydroperoxide, 2,5-dimethyl-2,5-bis(t-butylperoxy) hexane, dicumyl peroxide, di-t-butyl peroxide or peroxidized t-butyl perbenzoate;
Described polyfunctional monomer is a tripropylene glycol diacrylate, propylene glycol diacrylate, 1, the 6-hexanediyl ester, 1,4 butanediol diacrylate, neopentylglycol diacrylate, ethoxylated neopentylglycol diacrylate, PDDA, ethoxylated bisphenol a diacrylate, Viscoat 295, ethoxylated trimethylolpropane triacrylate, the propoxylation Viscoat 295, trimethylolpropane trimethacrylate, glycerol propoxylate triacrylate or pentaerythritol triacrylate.
6, method according to claim 5 is characterized in that: described initiator is a di-isopropylbenzene hydroperoxide, 2,5-dimethyl-2,5-bis(t-butylperoxy) hexane or dicumyl peroxide;
Described polyfunctional monomer is pentaerythritol triacrylate, Viscoat 295, trimethylolpropane trimethacrylate or ethoxylated neopentylglycol diacrylate.
7, according to claim 5 or 6 described methods, it is characterized in that: the ratio of quality and the number of copies of described polypropylene, initiator, maleic anhydride and polyfunctional monomer is 100: 0.005-4: 1-10: 0.05-5.
8, method according to claim 7 is characterized in that: the mass fraction of described initiator is 0.05-1, preferred 0.075-0.3;
The mass fraction of described maleic anhydride is 1-5, preferred 1.5-3;
The mass fraction of described polyfunctional monomer is 0.5-3, preferred 0.75-2.25.
9, according to claim 5 or 6 described methods, it is characterized in that: described fusion compound temperature is 150-250 ℃.
10, according to the arbitrary described method of claim 5-9, it is characterized in that: described fusion composite steps is carried out in twin screw extruder, and the screw speed of described twin screw extruder is 50-500 rev/min, and length-to-diameter ratio is 15-100.
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| CN103772612A (en) * | 2012-10-25 | 2014-05-07 | 合肥杰事杰新材料股份有限公司 | Preparation method for maleic anhydride-grafted polypropylene |
| CN104804143A (en) * | 2015-05-14 | 2015-07-29 | 华东理工大学 | Preparation method of maleic anhydride grafted polypropylene |
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| CN103772612A (en) * | 2012-10-25 | 2014-05-07 | 合肥杰事杰新材料股份有限公司 | Preparation method for maleic anhydride-grafted polypropylene |
| CN104804143A (en) * | 2015-05-14 | 2015-07-29 | 华东理工大学 | Preparation method of maleic anhydride grafted polypropylene |
| CN105153683A (en) * | 2015-07-28 | 2015-12-16 | 苏州科淼新材料有限公司 | Method for preparing toughened resin composition |
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| CN106188405A (en) * | 2016-08-19 | 2016-12-07 | 中国科学院化学研究所 | Graft modification super high molecular weight micronized polyethylene and solid phase grafting method thereof |
| CN106188405B (en) * | 2016-08-19 | 2019-02-15 | 中国科学院化学研究所 | Graft modification super high molecular weight micronized polyethylene and its solid phase grafting method |
| CN110441253A (en) * | 2019-07-22 | 2019-11-12 | 杭州华聚复合材料有限公司 | A kind of method of quick detection PP-g-MAH grafting rate |
| CN111040363A (en) * | 2019-12-27 | 2020-04-21 | 无锡邰某人材料科技有限公司 | Low-density polyethylene film material for printing and preparation method thereof |
| CN111440271A (en) * | 2020-04-13 | 2020-07-24 | 广州鹿山新材料股份有限公司 | Maleic anhydride grafted polyolefin wax, hot-melt pressure-sensitive adhesive modified by using same, and preparation method and application of hot-melt pressure-sensitive adhesive |
| CN111548682A (en) * | 2020-04-28 | 2020-08-18 | 金旸（厦门）新材料科技有限公司 | Anticorrosive polypropylene powder coating and preparation method thereof |
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| CN111795942A (en) * | 2020-07-08 | 2020-10-20 | 上海叶心材料科技有限公司 | Method for detecting grafting rate of polyolefin maleic anhydride |
| CN113231044A (en) * | 2021-05-20 | 2021-08-10 | 南京工业大学 | High-efficiency environment-friendly adsorption fiber for removing indigo in wastewater and preparation method thereof |
| CN115648764A (en) * | 2022-10-26 | 2023-01-31 | 江苏利特尔绿色包装股份有限公司 | Composite membrane, preparation method of microwave heating exhaust bag and microwave heating exhaust bag |
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