JPH043416B2 - - Google Patents
Info
- Publication number
- JPH043416B2 JPH043416B2 JP6963584A JP6963584A JPH043416B2 JP H043416 B2 JPH043416 B2 JP H043416B2 JP 6963584 A JP6963584 A JP 6963584A JP 6963584 A JP6963584 A JP 6963584A JP H043416 B2 JPH043416 B2 JP H043416B2
- Authority
- JP
- Japan
- Prior art keywords
- polyolefin
- ethylene
- acrylic acid
- temperature
- acid copolymer
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
- 229920000098 polyolefin Polymers 0.000 claims description 35
- 238000000034 method Methods 0.000 claims description 21
- 239000000843 powder Substances 0.000 claims description 19
- 229920006242 ethylene acrylic acid copolymer Polymers 0.000 claims description 14
- -1 polyethylene Polymers 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 238000004945 emulsification Methods 0.000 claims description 10
- 229920001577 copolymer Polymers 0.000 claims description 9
- 238000002844 melting Methods 0.000 claims description 9
- 230000008018 melting Effects 0.000 claims description 9
- 239000004698 Polyethylene Substances 0.000 claims description 7
- 239000000839 emulsion Substances 0.000 claims description 7
- 229920000573 polyethylene Polymers 0.000 claims description 7
- 238000010298 pulverizing process Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 18
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 15
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 10
- 239000002245 particle Substances 0.000 description 10
- 238000003756 stirring Methods 0.000 description 9
- 239000002994 raw material Substances 0.000 description 7
- 235000011121 sodium hydroxide Nutrition 0.000 description 6
- 229910021529 ammonia Inorganic materials 0.000 description 5
- 235000011118 potassium hydroxide Nutrition 0.000 description 5
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 4
- 238000006386 neutralization reaction Methods 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000002270 dispersing agent Substances 0.000 description 3
- 239000002609 medium Substances 0.000 description 3
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 2
- 239000005977 Ethylene Substances 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 2
- 229920006226 ethylene-acrylic acid Polymers 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 229920001155 polypropylene Polymers 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 1
- RVGRUAULSDPKGF-UHFFFAOYSA-N Poloxamer Chemical compound C1CO1.CC1CO1 RVGRUAULSDPKGF-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 239000012736 aqueous medium Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000011978 dissolution method Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 229920005648 ethylene methacrylic acid copolymer Polymers 0.000 description 1
- 239000012770 industrial material Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000000976 ink Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920001983 poloxamer Polymers 0.000 description 1
- 229920001748 polybutylene Polymers 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
Landscapes
- Processes Of Treating Macromolecular Substances (AREA)
Description
本発明はポリオレフインの微粉末化方法に関す
るものであり、更に詳しくは水を媒体とし、エチ
レンオキシド−プロピレンオキシド共重合体およ
びエチレン−アクリル酸共重合体の存在下、加熱
加圧の条件でポリオレフインを溶融撹拌して乳化
液を得、これをポリオレフインの軟化温度以下に
冷却することを特徴とするポリオレフインの数平
均粒子径５ミクロン以下の真球状微粉末を得る方
法に関する。
ポリオレフインの微粉末は、化粧品、セラミツ
ク用バインダー、印刷インキ、塗料、接着剤など
各種方面に広く用いられており、用途によつては
真球状で数平均粒子径５ミクロン以下の微粉末が
適当であり、その出現が強く要望されている。
従来、ポリオレフインの粉末化方法は大別して
機械粉砕方、溶解法、分散法の三つの方法があ
る。機械粉砕法は、高せん断微粉化装置を用い、
不規則な形をした粉末を作ることができるが、そ
の数平均粒子径は100〜300ミクロンであり、いわ
ゆる５ミクロン以下の微粉末を得ることはできな
い。溶解法はポリオレフインを溶剤に溶解し、必
要ならば非溶剤を加え、冷却により粉末を析出さ
せたり、溶剤を蒸発させたりして粉末を得る方法
である。
この場合、強力な撹拌を与えることにより細か
い粉末を得る方法がよく採用されるが、その場合
でも数平均粒子径は10〜50ミクロン程度であり、
５ミクロン以下の微粉末は得られず、その形状も
不規則なものである。
分散法は、種々の分散剤の作用でポリオレフイ
ンの粉末を得る方法であり、ポリオレフインを溶
剤に溶解し、分散液と水とを混合することにより
分散させる方法もあるが、工業的には溶剤の回収
が不必要な水媒体のみで分散させるのが最も好ま
しく有利である。
分散法は真球状の粉末を得ることができる方法
で既に特公昭39−2395号公報、特公昭51−25371
号公報などに記載されている。この方法は、その
操作温度における原料ポリオレフインの溶融指数
が15以上となるような温度条件を選び、分散剤と
してエチレンオキシド−プロピレンオキシド共重
合体を用い、強撹拌することにより、数平均粒子
径８〜10ミクロン程度の微粉末に近いものを得て
いる。
更に、分散剤としてアルカリポリエーテル硫酸
のナトリウム塩、アルカリポリエーテルスルホン
酸のナトリムウ塩などを用いた米国特許第
4212966号明細書
エチレン−アクリル酸共重合体、エチレン−メ
タクリル酸共重合体などを用いた米国特許第
4336210号明細書
有機リン酸エステルのアルカリ金属塩を用いた
米国特許第4208528号明細書
などの記載もあるが、いずれも10ミクロン〜
160ミクロンの範囲のものしか得られておらず、
前記工業上特に要望の大きい５ミクロン以下の微
粉末を得る方法については未だ知られていない。
このような状況に鑑み、本発明者らはポリオレ
フインの微粉末化方法について鋭意検討した結
果、水を媒体とし、エチレンオキシド−プロピレ
ンオキシド共重合体およびエチレン−アクリル酸
共重合体の存在下、加熱加圧の条件でポリオレフ
インを溶融、撹拌して乳化液を得、これをポリオ
レフインの軟化温度以下に冷却することにより数
平均粒子径５ミクロン以下のポリオレフイン微粉
末を得る方法を見出し本発明に到つた。
本発明に用いるポリオレフインは２〜６個の炭
素原子からなるオレフインの重合体で、それらを
例示すればポリエチレン、ポリプロピレン、ポリ
ブチレン、ポリペンテン、ポリヘキセンなどであ
り、特に好ましいポリオレフインの種類はポリエ
チレン、ポリプロピレンであり、乳化温度におけ
る原料ポリオレフインの溶融指数が20以上、好ま
しくは50以上のものを用いる。（JISK7210記載の
方法で測定、試験荷重2.16Kg／1θ分間）
エチレンオキシド−プロピレンオキシド共重合
体とは
なる構造式を有し、Ｘ＝２〜150、Ｙ＝1θ〜90Z
＝２〜150の共重合体の総称であるが、例えば旭
電化社製：商品名プルロニツクのごとく本発明で
用いられるエチレンオキシド−プロピレンオキシ
ド共重合体はそれらの内Ｘ＝60〜130，Ｙ＝30〜
70，Ｚ＝60〜130の範囲のものが適当である。
使用量は原料ポリオレフインに対して３〜40重
量％が適当であり、更に好ましくは８〜20重量％
である。それ以下では充分な乳化を行なうことが
難かしいし、それ以上用いることは製品の徴粉末
中への混入が多くなりポリオレフインの物性を損
なうなど、工業材料として使用する場合、好まし
くない場合が多い。
エチレン−アクリル酸共重合体とは、エチレン
とアクリル酸とを例えば高圧下重合させて得られ
た重合体で
The present invention relates to a method for pulverizing polyolefin, and more specifically, it involves melting polyolefin under heating and pressure conditions in the presence of an ethylene oxide-propylene oxide copolymer and an ethylene-acrylic acid copolymer using water as a medium. The present invention relates to a method for obtaining a true spherical fine powder of polyolefin having a number average particle diameter of 5 microns or less, which comprises stirring to obtain an emulsion and cooling the emulsion to a temperature below the softening temperature of the polyolefin. Polyolefin fine powder is widely used in various fields such as cosmetics, ceramic binders, printing inks, paints, and adhesives, and depending on the application, fine powder with a true spherical shape and a number average particle size of 5 microns or less is suitable. There is a strong demand for its appearance. Conventionally, there are three methods for pulverizing polyolefins: mechanical pulverization, dissolution, and dispersion. The mechanical pulverization method uses a high shear pulverization device,
Although irregularly shaped powder can be produced, the number average particle size is 100 to 300 microns, and so-called fine powders of less than 5 microns cannot be obtained. The dissolution method is a method in which polyolefin is dissolved in a solvent, a non-solvent is added if necessary, and the powder is precipitated by cooling or the solvent is evaporated to obtain a powder. In this case, a method of obtaining fine powder by applying strong stirring is often adopted, but even in that case, the number average particle size is about 10 to 50 microns,
Fine powder of 5 microns or less cannot be obtained, and its shape is irregular. The dispersion method is a method of obtaining polyolefin powder through the action of various dispersants.There is also a method of dissolving the polyolefin in a solvent and mixing the dispersion liquid with water, but industrially it is It is most preferred and advantageous to disperse only in an aqueous medium, which does not require recovery. The dispersion method is a method by which perfectly spherical powder can be obtained and has already been disclosed in Japanese Patent Publication No. 39-2395 and Japanese Patent Publication No. 51-25371.
It is stated in the issue bulletin etc. In this method, temperature conditions are selected such that the melting index of the raw material polyolefin is 15 or more at the operating temperature, ethylene oxide-propylene oxide copolymer is used as a dispersant, and by strong stirring, the number average particle size is 8 to 8. We have obtained something close to a fine powder of about 10 microns. Furthermore, U.S. Patent No.
No. 4212966 U.S. patent using ethylene-acrylic acid copolymer, ethylene-methacrylic acid copolymer, etc.
There are also descriptions such as US Patent No. 4336210 and US Patent No. 4208528 using an alkali metal salt of an organic phosphate ester, but all of them are 10 microns to
Only those in the 160 micron range have been obtained,
A method for obtaining fine powder of 5 microns or less, which is particularly desired in the industry, is not yet known. In view of this situation, the present inventors conducted intensive studies on a method for pulverizing polyolefins, and found that they were heated and heated in the presence of an ethylene oxide-propylene oxide copolymer and an ethylene-acrylic acid copolymer using water as a medium. The inventors have discovered a method of obtaining a fine polyolefin powder having a number average particle size of 5 microns or less by melting and stirring polyolefin under pressure conditions to obtain an emulsion and cooling this to a temperature below the softening temperature of the polyolefin, and have arrived at the present invention. The polyolefin used in the present invention is a polymer of olefin consisting of 2 to 6 carbon atoms, and examples thereof include polyethylene, polypropylene, polybutylene, polypentene, and polyhexene. Particularly preferred types of polyolefin are polyethylene and polypropylene. The melting index of the raw polyolefin at the emulsification temperature is 20 or more, preferably 50 or more. (Measured using the method described in JISK7210, test load 2.16Kg/1θ minutes) What is ethylene oxide-propylene oxide copolymer? It has the structural formula, X = 2 ~ 150, Y = 1θ ~ 90Z
= 2 to 150, for example, the ethylene oxide-propylene oxide copolymer used in the present invention, such as the product name Pluronic manufactured by Asahi Denka Co., Ltd., has X = 60 to 130 and Y = 30. ~
70, Z=60 to 130 is suitable. The appropriate amount to use is 3 to 40% by weight, more preferably 8 to 20% by weight based on the raw material polyolefin.
It is. If it is less than that, it is difficult to achieve sufficient emulsification, and if it is used more than that, it is often mixed into the powder of the product and impairs the physical properties of the polyolefin, which is often undesirable when used as an industrial material. Ethylene-acrylic acid copolymer is a polymer obtained by polymerizing ethylene and acrylic acid under high pressure.
【式】の
構造を有し、エチレンにアクリル酸が不規則に結
合したものであり、アクリル酸を３〜20重量％含
むものである。（ダウケミカル社製：商品名
EAA）
本発明に用いエチレン−アクリル酸共重合体は
苛性ソーダー、苛性カリ、アンモニアなどを用い
る部分的に中和したものも使用できる。中和度は
０〜20％まで可能であるが好ましくは０〜15％の
範囲である。中和度がそれ以上になるとエチレン
−アクリル酸共重合体が水に溶解し、乳化剤とし
ての機能を失なうので好ましくない。中和のため
苛性ソーダー、苛性カリ、アンモニアなどの添加
はあらかじめ別の容器で行なうこともできるし、
エチレン−アクリル酸共重合体を仕込んだ耐圧オ
ートクレーブ内で、必要量だけ苛性ソーダー、苛
性カリ、アンモニアなどを添加することにより使
用することもできる。工業的には後者の方が簡便
であり、有利である場合が多い。乳化時に使用す
るエチレン−アクリル酸共重合体は、原料ポリオ
レフインに対し0.5〜20％の範囲、好ましくは１
〜10％の範囲である。0.5％以下の使用量では５
ミクロン以下の微粉末を得ることができず、20％
以上使用すると乳化がうまく行なえない。乳化時
媒体として使用する水は原料ポリオレフイン１重
量部に対して0.5〜10の範囲、好ましくは１〜５
の範囲である。
水の使用量がそれ以下では所望の粒子径のポリ
オレフインを安定に得ることが難しく、粗大粒子
径のポリオレフインが生成する場合もあり好まし
くなく、水の使用量がそれ以上になると反応器容
積に対する微粉末の取得の効率が悪くなり、工業
上不利である。乳化方法は必要ならばN2など不
活性ガスにより置換した耐圧オートクレーブにま
ず水、あるいは蒸気を入れ、次いで原料ポリオレ
フイン、エチレンオキシド−プロピレンオキシド
共重合体、エチレン−アクリル酸共重合体を入
れ、必要ならば苛性ソーダ、苛性カリ、アンモニ
アなどの塩基性物質を上記記載の適当量添加し、
系内を密閉し、所定の温度まで昇温する。
通常はジヤケツトへ油、スチームなどを送入す
ることにより加熱し、必要ならば撹拌を行なつて
溶融を促進する。
別法として水および蒸気を所定の温度まで昇温
した耐圧オートクレーブ中に圧送などの方法で原
料ポリオレフイン、エチレンオキシド−プロピレ
ンオキシド共重合体、エチレン−アクリル酸共重
合体、苛性ソーダ−、苛性カリ、アンモニアなど
の塩基性物質を添加する方法も採用できる。
温度、圧力条件は使用するポリオレフインの種
類により異なるが、一般的にはより高温、高圧の
方が目的に合致した微粉末が得られる場合が多
い。しかし、ポリオレフインの分解や分散剤の分
解などを考慮すれば、温度100〜300℃、圧力１〜
85Kg／cm2の条件が好ましい。通常、加熱は原料ポ
リオレフインのその乳化温度における溶融指数が
20以上になる温度にまで行なう。そのときの系内
圧力はおおむねその温度に対応する水の蒸気圧を
示す。昇温後の内容物の撹拌はオートクレーぶの
大きさ、仕込量などによつて異なるが通常２分〜
２時間、撹拌翼先端速度は１〜５ｍ／秒で充分で
あり、特に強力な撹拌は必要としない。以下実施
例を示す。
実施例 １
径250mmのプロペラ型撹拌羽根を備えた内径500
mm、高さ1100mmのジヤケツト付き内容積200の
耐圧オートクレーブに純水26.2Kgポリエチレン
（住友化学社製商品名スミカセンG807，190℃で
の溶融指数75）12Kgエチレンオキシド−プロピレ
ンオキシド共重合体（分子式HO
ｘ＝126，ｙ＝54，ｚ＝126（旭電化社製；商品名
プルロニツクＦ−108）1.2Kgとエチレン−アクリ
ル酸共重合体（ダウケミカル社製；商品名EAA
XO−2375−33）0.6Kg、苛性ソーダ−6.6ｇを仕
込み密閉する。エチレン−アクリル酸共重合体の
アクリル酸の中和度は10％である。次にジヤケツ
ト部に加熱油を循環させることにより、オートク
レーブ内部の温度を上昇させる。約１時間後に内
部の温度が200℃になつた。（その温度における原
料ポリエチレンの溶融指数81であつた。）圧力は
ゲージ圧で17Kg／cm2を示した。
撹拌機を始動させ、毎分230回転で60分撹拌し
た。撹拌半翼先端速度は３ｍ／秒である。次いで
冷却を行ない内温が90℃になつたところで内容物
をオートクレーブより取り出した。
内容物は乳化液状態であり、これを過乾燥し
て得られた微粉末ポリエチレンの数平均粒子径は
3.2ミクロンであり、真球状であつた。
比較例 １
エチレン−アクリル酸共重合体を使用しない以
外は実施例１と同様に乳化を行ない、冷却後内容
物を取り出した。内容物は乳化液状態であつたが
得られた粉末ポリエチレンの数平均粒子径は8.4
ミクロンであつた。
実施例 ２〜４
各種の原料ポリオレフインを用い第１表に示す
乳化温度および圧力下において、実施例１と同様
の操作を行ない、第１表の結果を得た。It has the structure of [Formula], in which acrylic acid is randomly bonded to ethylene, and contains 3 to 20% by weight of acrylic acid. (Manufactured by Dow Chemical Company: Product name
EAA) The ethylene-acrylic acid copolymer used in the present invention may be partially neutralized using caustic soda, caustic potash, ammonia, or the like. The degree of neutralization can range from 0 to 20%, but is preferably from 0 to 15%. If the degree of neutralization is higher than that, the ethylene-acrylic acid copolymer will dissolve in water and lose its function as an emulsifier, which is not preferable. Caustic soda, caustic potash, ammonia, etc. can be added in advance in a separate container for neutralization, or
It can also be used by adding necessary amounts of caustic soda, caustic potash, ammonia, etc. in a pressure-resistant autoclave containing the ethylene-acrylic acid copolymer. Industrially, the latter is simpler and often more advantageous. The ethylene-acrylic acid copolymer used during emulsification is in the range of 0.5 to 20%, preferably 1% to the raw material polyolefin.
In the range of ~10%. 5 for usage below 0.5%
Unable to obtain fine powder below micron, 20%
If you use more than that, emulsification will not work properly. The amount of water used as a medium during emulsification is in the range of 0.5 to 10, preferably 1 to 5, per 1 part by weight of the raw material polyolefin.
is within the range of If the amount of water used is less than that, it will be difficult to stably obtain polyolefin with the desired particle size, and polyolefin with a coarse particle size may be produced, which is undesirable. The efficiency of obtaining the powder becomes poor, which is disadvantageous industrially. The emulsification method is to first put water or steam into a pressure-resistant autoclave which has been purged with an inert gas such as N 2 if necessary, then put the raw material polyolefin, ethylene oxide-propylene oxide copolymer, and ethylene-acrylic acid copolymer, and if necessary, Add basic substances such as caustic soda, caustic potash, and ammonia in appropriate amounts as described above,
The inside of the system is sealed and the temperature is raised to a predetermined temperature. The jacket is usually heated by introducing oil, steam, etc. into the jacket, and if necessary stirred to promote melting. Alternatively, raw materials such as polyolefin, ethylene oxide-propylene oxide copolymer, ethylene-acrylic acid copolymer, caustic soda, caustic potash, ammonia, etc. are prepared by pumping water and steam into a pressure-resistant autoclave heated to a predetermined temperature. A method of adding a basic substance can also be adopted. Temperature and pressure conditions vary depending on the type of polyolefin used, but generally a fine powder that meets the purpose can often be obtained at higher temperatures and pressures. However, if we take into account the decomposition of polyolefin and dispersant, the temperature is 100 to 300℃ and the pressure is 1 to 100℃.
A condition of 85 Kg/cm 2 is preferred. Usually, heating is performed to increase the melting index of the raw polyolefin at its emulsification temperature.
Continue until the temperature reaches 20 or higher. The pressure within the system at that time roughly indicates the vapor pressure of water corresponding to that temperature. Stirring of the contents after raising the temperature varies depending on the size of the autoclave, the amount of preparation, etc., but it usually takes 2 minutes or more.
For 2 hours, a stirring blade tip speed of 1 to 5 m/sec is sufficient, and particularly strong stirring is not required. Examples are shown below. Example 1 Inner diameter 500 with propeller-type stirring blades 250 mm in diameter
In a pressure autoclave with an internal volume of 200 mm and a height of 1100 mm, 26.2 kg of pure water polyethylene (product name Sumikasen G807 manufactured by Sumitomo Chemical Co., Ltd., melting index at 190°C 75) and 12 kg of ethylene oxide-propylene oxide copolymer (molecular formula HO x = 126, y = 54, z = 126 (manufactured by Asahi Denka Co., Ltd.; trade name Pluronic F-108) 1.2 kg and ethylene-acrylic acid copolymer (manufactured by Dow Chemical Company; trade name EAA)
XO-2375-33) Charge 0.6 kg and 6.6 g of caustic soda and seal. The degree of neutralization of acrylic acid in the ethylene-acrylic acid copolymer is 10%. Next, by circulating heated oil through the jacket, the temperature inside the autoclave is raised. After about an hour, the internal temperature reached 200℃. (The melting index of the raw polyethylene at that temperature was 81.) The pressure was 17 kg/cm 2 in gauge pressure. The stirrer was started and stirred at 230 revolutions per minute for 60 minutes. The stirring half-blade tip speed is 3 m/sec. Next, the autoclave was cooled, and when the internal temperature reached 90°C, the contents were taken out from the autoclave. The contents are in the form of an emulsion, and the number average particle size of the finely powdered polyethylene obtained by over-drying this is:
It was 3.2 microns and perfectly spherical. Comparative Example 1 Emulsification was carried out in the same manner as in Example 1 except that the ethylene-acrylic acid copolymer was not used, and the contents were taken out after cooling. Although the contents were in the form of an emulsion, the number average particle size of the powdered polyethylene obtained was 8.4.
It was micron. Examples 2 to 4 The same operations as in Example 1 were carried out using various raw material polyolefins at the emulsification temperatures and pressures shown in Table 1, and the results shown in Table 1 were obtained.
【表】
いずれも数平均粒子径５ミクロン以下であつ
た。[Table] All had a number average particle diameter of 5 microns or less.
Claims (1)
媒体とし、エチレンオキシド−プロピレンオキシ
ド共重合体およびエチレン−アクリル酸共重合体
の存在下、加熱、加圧下にポリオレフインを溶
融、撹拌して乳化液を得、これをポリオレフイン
の軟化温度以下に冷却することを特徴とするポリ
オレフインの微粉末化方法。 ２ 加熱乳化時のポリオレフインの溶融指数が20
以上である特許請求の範囲第１記載の方法。 ３ ポリオレフインがポリエチレンである特許請
求の範囲第１記載の方法。[Scope of Claims] 1. To finely powder a polyolefin, the polyolefin is melted and stirred under heat and pressure in the presence of an ethylene oxide-propylene oxide copolymer and an ethylene-acrylic acid copolymer using water as a medium. A method for pulverizing a polyolefin, which comprises obtaining an emulsion and cooling the emulsion to a temperature below the softening temperature of the polyolefin. 2 The melting index of polyolefin during heat emulsification is 20
The method according to claim 1, which is the above. 3. The method according to claim 1, wherein the polyolefin is polyethylene.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6963584A JPS60212430A (en) | 1984-04-06 | 1984-04-06 | Pulverization of polyolefin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6963584A JPS60212430A (en) | 1984-04-06 | 1984-04-06 | Pulverization of polyolefin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS60212430A JPS60212430A (en) | 1985-10-24 |
| JPH043416B2 true JPH043416B2 (en) | 1992-01-23 |
Family
ID=13408514
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP6963584A Granted JPS60212430A (en) | 1984-04-06 | 1984-04-06 | Pulverization of polyolefin |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS60212430A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022075637A1 (en) | 2020-10-08 | 2022-04-14 | 주식회사 엘지에너지솔루션 | Electrode assembly stacking fault detection method, electrode assembly including insulating member, and battery cell including same |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4606806B2 (en) * | 2004-08-03 | 2011-01-05 | 住友精化株式会社 | Method for producing polyolefin resin particles |
| CN102498160B (en) * | 2009-09-04 | 2013-11-27 | 住友精化株式会社 | Polyolefin-based composite resin spherical particles, coating composition and coated object |
-
1984
- 1984-04-06 JP JP6963584A patent/JPS60212430A/en active Granted
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022075637A1 (en) | 2020-10-08 | 2022-04-14 | 주식회사 엘지에너지솔루션 | Electrode assembly stacking fault detection method, electrode assembly including insulating member, and battery cell including same |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS60212430A (en) | 1985-10-24 |
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