CN1197086A - 预膨胀的聚烯烃珠的后发泡方法 - Google Patents
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Abstract
一种使具有高堆积密度的聚烯烃泡沫珠转变为低堆积密度的泡沫珠的方法,包括在2—25par的压力下,和在Tm-150℃至Tm-40℃的温度范围内并在1—48小时的时间内,用惰性气体填充堆积密度为20—450g/l的聚烯烃泡沫颗粒,之后将加压的泡沫颗粒连续或间断地送入产生涡流层的装置中,其中颗粒在Tm-75℃至Tm+20℃的温度范围内继续发泡。所得泡沫颗粒适于制备泡沫模塑制品。
Description
本发明涉及一种使高堆积密度的聚烯烃泡沫珠转变为低堆积密度的泡沫珠的方法。
聚烯烃泡沫颗粒物质是已知的;它们可由各种方法来制备,其共同的特征是在发泡剂存在下并在加压下加热含水的颗粒分散液,之后使热分散液通过一喷嘴排入一低压空间。在这里,颗粒进行发泡,其中膨胀速度主要依赖于颗粒的类型、发泡温度以及发泡剂的类型和用量。
与聚苯乙烯泡沫颗粒的制备方法相比,聚烯烃泡沫颗粒的制备有严重的缺点:实际上不可能在颗粒内保留发泡剂。因此可将已充满挥发性发泡剂的聚苯乙烯珠毫无困难地运输并可加工成泡沫,而聚烯烃却不能这样做。在这里首先要使后者发泡以达到最终的堆积密度,从而造成贮存和运输费用高。尽管有这种可能,即通过有目的的制备发泡的泡沫珠先制备较高堆积密度的泡沫,然后在加工前通过加压和释放压力进行加工时先发泡(DE-A-3922207;EP-A-0453836),或者在一改进方法中,在加压后将再保持在该压力下的颗粒迅速加工成低密度模制品(EP-A-0734829)。然而如此获得的体积上的减小,只有在第一步可减少贮存和运输费用。
因此本发明的目的是制备发泡的重颗粒,通过合适的后处理方法可使该颗粒再发泡成发泡的轻颗粒。
可通过下面的方法实现本发明的目的,即在2-25bar、优选在3-10bar下,和在Tm-150℃至Tm-40℃的温度下并在1-48小时,优选5-20小时的时间内,用惰性气体填充堆积密度为20-450g/l的已发泡的聚烯烃颗粒,之后将加压的泡沫颗粒连续或间断地送入有流化床的装置中,其中颗粒在Tm-75℃至Tm+20℃的温度下继续发泡。
在本发明的一个实施方式中,使加压的泡沫颗粒通过闸进入温度保持在Tm-75℃至Tm+20℃下的未加压的装置内,之后除去发泡的颗粒。这里“未加压”是指在装置内的压力大约为大气压力。
在本发明的又一实施方式中,使加压的泡沫颗粒在密闭的装置内加热到在Tm-75℃至Tm+20℃的温度,然后将颗粒释放到大气环境中。
合适的聚烯烃的例子有丙烯聚合物,如丙烯-乙烯或丙烯-丁烯无规共聚物、乙烯、丙烯和1-丁烯的三元共聚物、乙烯-丙烯的嵌段共聚物和均聚丙烯,乙烯聚合物,如低、中、高密度聚乙烯、低密度直链聚乙烯、乙烯-乙酸乙烯酯共聚物、乙烯-甲基异丁烯酸酯共聚物、离聚物,和其它聚烯烃,如1-聚丁烯。优选使用具有1-15重量%乙烯的乙烯-丙烯无规共聚物。
在预膨胀过程中,这些聚合物为单个颗粒的形式存在,且具有的平均颗粒直径优选在0.5-5mm的范围内。为了获得最终发泡效果,必要时它们可以含有起成核剂作用的填料,这与现有技术相同。
分散剂优选水,但是醇,如甲醇或乙醇也是合适的。
为防止聚集,可将磨细的分散剂和/或表面活性剂化合物加入到聚合物颗粒和分散剂的混合物中。这些例子有磷酸钙、碱式碳酸镁、碱式碳酸锌、碳酸钙、氧化铝、硫酸钡、滑石、苯磺酸烷基酯、链烷烃磺酸酯和乙氧基化物。
为了调整泡沫珠的密度,加入挥发性发泡剂也是有利的。合适的发泡剂是现有技术中已知的,例子有饱和的酯族烃,如乙烷、丙烷、正丁烷、异丁烷、戊烷或己烷,酯环烃,如环戊烷或环己烷,卤代烃,如三氯一氟甲烷、二氯二氟甲烷、二氯四氟乙烷、三氯三氟乙烷、二氯一氟甲烷、氯代甲烷、二氯甲烷和氯代乙烷,以及无机气体,如二氧化碳和氮,它们可分别单独或混合使用。
如果不加入挥发性发泡剂,那么分散剂本身作为发泡剂。尽管该方法只能达到中等的膨胀速度,但是在本发明中也可以直接使用。
在现有技术中将分散液加热然后通过膨胀喷嘴排入低压空间内,这期间颗粒发泡或具有细胞结构。
制备聚烯烃泡沫颗粒的合适方法,如公开于EP-A-0053333、EP-A-0630935和EP-A-0646619中。
在本发明的范围内,使用DSC测量方法测量晶形熔点Tm值。使一种聚烯烃试样以20℃/分钟的速率加热到210℃,然后以20℃/分钟的速率冷却到-30℃,接着再以20℃/分钟的速率进行加热。此期间所显示的最高峰值为Tm。
此外,已经知道聚烯烃泡沫珠基于后次结晶也可具有高温熔化峰值(EP-A-0123144;EP-A-0164855;EP-A-0168954)。在本发明的范围内,优选使用此类型的发泡颗粒,尤其优选在T最小值-125℃至T最小值-60℃的温度下用惰性气体加压和在T最小值-35℃至T+10℃的温度范围内进行后膨胀。这里T最小值为在DSC测量中第一个加热曲线中第一和第二峰值之间的最小值。对于具有乙烯含量大约在3.5重量%的乙烯-丙烯无规共聚物而言,T最小值大约在150℃至156℃的温度范围内。
用作加压的惰性气体的例子为氮气、空气或CO2。
适于进行后膨胀的装置为那些其中通过机械或气动方式操作的涡流层。对于机械操作的涡流层而言,例如可使用搅拌容器、浆式干燥器或转鼓干燥器;对于用气动方式操作的流化床而言,可使用管道式流动干燥器或类似的装置。
在一个实施例中,用于后膨胀的装置为密封装置,借此加热加压的、发泡的颗粒,如使用饱和蒸气。依靠温度发泡颗粒的停留时间在30至300秒的范围内,蒸气压力在1.7至5.5bar的范围内。在这段时间之后,使发泡加热的颗粒进入大气压的气氛中。
使人吃惊地是,通过本发明的方法可使发泡颗粒进一步发泡以形成低堆积密度的泡沫颗粒,从而可使重颗粒具有很宽的堆积密度范围。此外,为了使堆积密度进一步减小,必要时可重复后处理步骤。这种做法在使用具有堆积密度高于350g/l的发泡的颗粒时尤其有用。
按照本发明制备的泡沫珠的特征在于具有平的光滑表面。此外,在使用圆柱形颗粒时可得到基本上为球形的泡沫颗粒。用任何现有技术中的方法可使泡沫珠加工成模塑制品。
通过下述实施例详细描述本发明。在所有实施例中,在所有实施例中所使用的发泡颗粒是按现有技术来制备的原始颗粒。
实施例1
将Tm=147℃和T最小值=153℃且堆积密度为21g/l的乙烯-丙烯无规共聚物的发泡颗粒在30℃并在4.6bar的压力下进行处理20小时。然后释放压力容器内的压力,再加压,使部分发泡的颗粒转入具有空气温度为140℃的涡流层上。如此调节空气的体积流以使其产生强烈的涡流。后发泡的、较轻的泡沫珠堆积在装置的顶部,由于它们较大的体积使它们具有较大的浮力,然后它们经过溢流口流出涡流层装置并冷却。最终的堆积密度为14g/l,见表1。
实施例2
与实施例1相同,只是发泡颗粒的堆积密度为53g/l。工艺参数和结果示于表1中。
实施例3
与实施例1相同,只是发泡颗粒的堆积密度为83g/l。工艺参数和结果示于表1中。
实施例4
将堆积密度为210g/l的发泡颗粒保持在压力为6bar、温度为80℃的密闭反应器内10小时,在此期间使内含物充分混合。在该时间后释放反应器内的压力并引入饱和蒸气。在5.1bar蒸气压和153℃的相应温度下保持4分钟,之后释放反应器内的压力和排出后膨胀的泡沫颗粒。
表1:过程参数和结果
实施例 | 堆积密度(g/l) | 后处理 | 后发泡 | ||||
T(℃) | P(bar) | t(h) | T(℃) | t(min) | 堆积密度(g/l) | ||
1 | 21 | 30 | 4.6 | 20 | 140 | 1 | 14 |
2 | 53 | 30 | 4.6 | 20 | 145 | 1 | 25 |
3 | 83 | 50 | 5.8 | 12 | 160 | 3 | 24 |
4 | 210 | 80 | 6 | 10 | 153 | 4 | 63 |
Claims (7)
1.一种使发泡的聚烯烃颗粒后发泡的方法,其中在2-25bar的压力下,和在Tm-150℃至Tm-40℃的温度下并在1-48小时的时间内,用惰性气体填充堆积密度为20-450g/l的聚烯烃发泡颗粒,之后将加压的泡沫颗粒连续或间断地送入产生涡流层的装置中,其中颗粒在Tm-75℃至Tm+20℃的温度下继续发泡。
2.根据权利要求1的方法,其特征在于使加压的发泡颗粒通过一闸门进入温度保持在Tm-75℃至Tm+20℃的未加压装置内,之后取出发泡颗粒。
3.根据权利要求1的方法,其特征在于使加压的发泡颗粒在一密闭的装置内加热,使温度从Tm-75℃至Tm+20℃,然后使颗粒进入大气压的气氛中。
4.根据上述任何一个权利要求所述的方法,其特征在于在3-10bar的压力下的输入惰性气体的时间为5至20小时。
5.根据上述任何一个权利要求所述的方法,其特征在于聚烯烃为含有1-15重量%乙烯的一种乙烯-丙烯无规共聚物。
6.根据上述任何一个权利要求所述的方法,其特征在于聚烯烃泡沫珠具有高温熔化峰值。
7.根据权利要求6所述的方法,其特征在于在T最小值-125℃至T最小值-60℃的温度范围内输入惰性气体并在T最小值-35℃至T最小值+10℃的温度范围内再进行发泡。其中T最小值为在DSC测量中第一个加热曲线中第一和第二峰值之间的最小值。
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DE19706884.7 | 1997-02-21 | ||
DE19706884A DE19706884A1 (de) | 1997-02-21 | 1997-02-21 | Verfahren zum Nachschäumen von preexpandierten polyolefinischen Partikeln |
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US (1) | US5830922A (zh) |
EP (1) | EP0860262B1 (zh) |
JP (1) | JPH10237212A (zh) |
KR (1) | KR19980071531A (zh) |
CN (1) | CN1197086A (zh) |
AT (1) | ATE207403T1 (zh) |
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JP3950557B2 (ja) * | 1998-07-30 | 2007-08-01 | 株式会社カネカ | ポリプロピレン系樹脂予備発泡粒子およびそれからの型内発泡成形体の製造方法 |
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AT3797U1 (de) * | 1999-07-13 | 2000-08-25 | Hirsch Maschinenbau Gmbh & Co | Verfahren und vorrichtung zum mehrfachen schäumen von expandierbaren kunststoffen |
CN1311013C (zh) | 1999-12-28 | 2007-04-18 | 钟渊化学工业株式会社 | 可发泡的聚苯乙烯树脂粒子和由其生产的泡沫制品 |
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WO2022050375A1 (ja) | 2020-09-04 | 2022-03-10 | 株式会社カネカ | 押出発泡粒子およびその製造方法 |
EP4279539A1 (en) | 2021-01-15 | 2023-11-22 | Kaneka Corporation | Polypropylene resin extruded foam particles, method for producing same, and foam molded body |
WO2022163627A1 (ja) | 2021-01-26 | 2022-08-04 | 株式会社カネカ | 分岐構造を有するポリプロピレン系樹脂の製造方法、押出発泡粒子の製造方法、および、発泡成形体の製造方法 |
WO2022181762A1 (ja) | 2021-02-25 | 2022-09-01 | 株式会社カネカ | ポリプロピレン系樹脂押出発泡粒子およびポリプロピレン系樹脂発泡成形体 |
EP4317274A1 (en) | 2021-03-25 | 2024-02-07 | Kaneka Corporation | Polypropylene resin extruded foam particles, method for producing same, and foam molded body |
JPWO2022210645A1 (zh) | 2021-03-29 | 2022-10-06 |
Family Cites Families (15)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3821342A (en) * | 1970-12-29 | 1974-06-28 | Motch Merryweather Machinery | Method for expanding synthetic plastic beads in a fluid bed |
GB1560768A (en) * | 1976-08-02 | 1980-02-06 | Lezier G | Prefoaming process for expansible materials |
JPS5923731B2 (ja) * | 1980-11-22 | 1984-06-04 | 日本スチレンペ−パ−株式会社 | ポリプロピレン系樹脂予備発泡粒子 |
FR2497814B1 (fr) * | 1981-01-13 | 1986-08-08 | Gerard Aye | Billes creuses obtenues a partir de matieres plastiques expansibles et procede d'obtention |
EP0123144B1 (en) * | 1983-03-25 | 1987-10-07 | Japan Styrene Paper Corporation | Polypropylene resin prefoamed particles |
US4704239A (en) * | 1984-04-28 | 1987-11-03 | Japan Styrene Paper Corp. | Process for the production of expanded particles of a polymeric material |
US4676939A (en) * | 1984-06-14 | 1987-06-30 | Japan Styrene Paper Corporation | Process for the production of expanded particles of a polypropylene resin |
JPH0788432B2 (ja) * | 1988-08-31 | 1995-09-27 | 鐘淵化学工業株式会社 | ポリオレフィン系樹脂予備発泡粒子の製造方法 |
DE3922207A1 (de) * | 1989-07-06 | 1991-01-17 | Basf Ag | Verfahren zum expandieren von geschrumpften schaumstoffpartikeln aus propylenpolymeren |
DE4012239A1 (de) * | 1990-04-14 | 1991-10-17 | Basf Ag | Schaumstoffe auf basis eines olefincopolymeren |
DE4211972A1 (de) * | 1992-04-09 | 1993-10-14 | Huels Chemische Werke Ag | Verfahren zur Herstellung von Schaumperlen |
DE4319587A1 (de) * | 1993-06-14 | 1994-12-15 | Huels Chemische Werke Ag | Verfahren zur Herstellung vorgeschäumter Polyolefin-Partikel |
DE4332724A1 (de) * | 1993-09-25 | 1995-03-30 | Huels Chemische Werke Ag | Verfahren zur Herstellung von Schaumperlen |
DE4429844A1 (de) * | 1994-08-23 | 1996-02-29 | Basf Ag | Verfahren zur Herstellung von expandierten Polyolefin-Partikeln |
DE19512059A1 (de) * | 1995-03-31 | 1996-10-02 | Huels Chemische Werke Ag | Verfahren zur Herstellung von Formkörpern aus geschäumten Polyolefinen |
-
1997
- 1997-02-21 DE DE19706884A patent/DE19706884A1/de not_active Withdrawn
-
1998
- 1998-01-12 AT AT98100384T patent/ATE207403T1/de not_active IP Right Cessation
- 1998-01-12 DE DE59801829T patent/DE59801829D1/de not_active Expired - Lifetime
- 1998-01-12 EP EP98100384A patent/EP0860262B1/de not_active Expired - Lifetime
- 1998-02-19 BR BR9800716-5A patent/BR9800716A/pt not_active Application Discontinuation
- 1998-02-20 US US09/026,535 patent/US5830922A/en not_active Expired - Lifetime
- 1998-02-20 JP JP10038792A patent/JPH10237212A/ja active Pending
- 1998-02-20 CN CN98107069A patent/CN1197086A/zh active Pending
- 1998-02-20 KR KR1019980005255A patent/KR19980071531A/ko not_active Application Discontinuation
Also Published As
Publication number | Publication date |
---|---|
US5830922A (en) | 1998-11-03 |
EP0860262B1 (de) | 2001-10-24 |
ATE207403T1 (de) | 2001-11-15 |
EP0860262A1 (de) | 1998-08-26 |
JPH10237212A (ja) | 1998-09-08 |
BR9800716A (pt) | 2000-01-18 |
DE59801829D1 (de) | 2001-11-29 |
KR19980071531A (ko) | 1998-10-26 |
DE19706884A1 (de) | 1998-08-27 |
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