JPH0693108A - Method of sphering thermoplastic synthetic resin - Google Patents

Method of sphering thermoplastic synthetic resin

Info

Publication number
JPH0693108A
JPH0693108A JP3887392A JP3887392A JPH0693108A JP H0693108 A JPH0693108 A JP H0693108A JP 3887392 A JP3887392 A JP 3887392A JP 3887392 A JP3887392 A JP 3887392A JP H0693108 A JPH0693108 A JP H0693108A
Authority
JP
Japan
Prior art keywords
synthetic resin
polymer
particles
thermoplastic synthetic
organopolysiloxane
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.)
Pending
Application number
JP3887392A
Other languages
Japanese (ja)
Inventor
Takehiko Kobayashi
武彦 小林
Yasuo Kogure
保夫 木暮
Kiyomine Taniguchi
清峰 谷口
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
NIKKO KAGAKU KENKYUSHO KK
Nittetsu Mining Co Ltd
Original Assignee
NIKKO KAGAKU KENKYUSHO KK
Nittetsu Mining Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by NIKKO KAGAKU KENKYUSHO KK, Nittetsu Mining Co Ltd filed Critical NIKKO KAGAKU KENKYUSHO KK
Priority to JP3887392A priority Critical patent/JPH0693108A/en
Publication of JPH0693108A publication Critical patent/JPH0693108A/en
Pending legal-status Critical Current

Links

Landscapes

  • Processes Of Treating Macromolecular Substances (AREA)

Abstract

PURPOSE:To form a thermoplastic synthetic resin or elastomer into true spheres by dispersing particles of the resin or elastomer with diameters of 5-3,000mum into a medium and melting the particles while preventing the particles from fusing to one another. CONSTITUTION:A thermoplastic synthetic resin or elastomer (A) is dispersed into an organopolysiloxane (B) having a structure represented by the formula. The dispersion is gradually heated to a temp. higher than the melting point of the polymer (A) when it is noncrystalline, or to a temp. higher than the glass transition temp. of the polymer (A) when it is crystalline. The polymer (A) is thus melted in the medium (B), while the dispersion is being stirred. Because the solubility parameter of the polymer (A) and that of the medium (B) differ to such an extent that the two are incompatible or immiscible with each other, the particles of the polymer (A) do not swell during melting and dispersion. The molten particles become truly spherical during stirring due to interfacial tension.

Description

【発明の詳細な説明】Detailed Description of the Invention

【0001】[0001]

【化2】 の一般式に示されるポリアルキル又はフェニルポリシロ
キサンを 用いて熱可塑性合成樹脂を球状化する技術
に関するものである。
[Chemical 2] The present invention relates to a technique for spheroidizing a thermoplastic synthetic resin by using a polyalkyl or phenyl polysiloxane represented by the general formula (1).

【化2】 [Chemical 2]

【化2】 において、n=1以上であり、R=Rは、水素、メ
チル基、フェニル基、フロロ基を含むオルガノポリシロ
キサンである。
[Chemical 2] In, n is 1 or more and R 1 = R 2 is an organopolysiloxane containing hydrogen, a methyl group, a phenyl group, and a fluoro group.

【産業上の利用分野】[Industrial applications]

【0002】本発明は、粒径が5〜3,000μmの範
囲で、粒径の揃った球状の合成樹脂の粉末を容易に形成
する技術を提供するものである。
The present invention provides a technique for easily forming a spherical synthetic resin powder having a uniform particle size in the range of 5 to 3,000 μm.

【従来の技術】[Prior art]

【0003】従来より、熱可塑性合成樹脂を球状化する
方法としては、球状化技術の先行文献によれば、溶融空
中飛散冷却法、溶融転動造粒法、水中懸濁分散重合法等
の方法がある。
Conventionally, as a method for spheroidizing a thermoplastic synthetic resin, according to prior art documents on spheroidizing technology, a method such as a melt-in-air flying cooling method, a melt tumbling granulation method, and a water suspension dispersion polymerization method. There is.

【発明が解決しようとする課題】[Problems to be Solved by the Invention]

【0004】溶融空中飛散冷却法は必ずといえるほどお
たまじゃくしの尻尾のような髭ができる欠点があり、こ
の髭を無くするためには、再度熱処理する必要がある。
また、溶融転動造粒法は、かなり良好な球形を形成する
が、一度に球状化する量を多くすると、粒子同士が融着
し、徐々に大きな粒子に成長する好ましくない状況を生
じる。水中懸濁分散重合法は、重合単量体(モノマー)
を所望の粒径に懸濁・分散するのが困難であり、且つ、
高温・高圧重合には適さず、更には、球状化出来る合成
樹脂の種類が限定されることになる。本発明は、溶解パ
ラメーターの差を応用して、ポリシロキサン中にて球状
化するという画期的な方法である。
The melting airborne cooling method has a drawback that a beard such as the tail of a tadpole can always be produced. To eliminate the beard, it is necessary to perform heat treatment again.
Further, the melt tumbling granulation method forms a very good spherical shape, but if the amount of spheroidization at one time is increased, the particles are fused to each other and gradually grow into large particles, which is not preferable. The suspension dispersion polymerization method in water is a polymerization monomer (monomer).
Is difficult to suspend and disperse into a desired particle size, and
It is not suitable for high temperature / high pressure polymerization, and further limits the types of synthetic resins that can be spheroidized. The present invention is an epoch-making method of applying spheroidization in polysiloxane by applying the difference in solubility parameter.

【課題を解決するための手段】[Means for Solving the Problems]

【0005】前述したように、従来より行われた球状化
の方法は、多くの欠点を有するものであるが、溶解パラ
メーター値が、球状化を目的とした合成樹脂のそれと比
較して、1.0以上の差を持っているときは、該合成樹
脂とポリシロキサンが相溶または相混和することがない
ことが判り、オルガノポリシロキサン中で溶融分散法に
て球状化できる方法を提供するものである。
As described above, the conventional spheroidizing method has many drawbacks, but the solubility parameter value is 1. When the difference is 0 or more, it is understood that the synthetic resin and the polysiloxane do not become compatible or miscible with each other, and a method capable of spheroidizing in the organopolysiloxane by the melt dispersion method is provided. is there.

【作 用】[Work]

【0006】本願発明において使用できる熱可塑性合成
樹脂
Thermoplastic synthetic resin usable in the present invention

【表1】 及びオルガノポリシロキサンの例を[Table 1] And examples of organopolysiloxanes

【表2】 に列記するが、これに限定されるものではなく、特許請
求の範囲に述べた条件を満たすのものであれば、使用可
能である。
[Table 2] However, the present invention is not limited to this, and may be used as long as it satisfies the conditions described in the claims.

【表1】 [Table 1]

【表2】 [Table 2]

【0007】[0007]

【化1】 の一般式に示されるオルガノポリシロキサンであって、
粘度は好ましくは50〜1,000csの範囲が良い球
状化の結果をもたらす。
[Chemical 1] An organopolysiloxane represented by the general formula:
The viscosity is preferably in the range of 50 to 1,000 cs to give good spheronization results.

【化1】 [Chemical 1]

【化1】 において、ここでR=Rはメチル基であり、R
は、水素、メチル基、フェニル基である。xの値
は、0〜2,200の範囲内であって、球状化に適する
粘度になる数とする。yの数は1以上であって、x+y
は、2,200を超えることはない。従ってジメチルポ
リシロキサン、メチルフェニルポリシロキサン等であ
る。これらオルガノポリシロキサンの溶解パラメーター
値は7.3〜7.8である。更には、オルガノポリシロ
キサンの温度は、該合成樹脂が非結晶の場合はその融
点、結晶性の場合はガラス転移点より10℃以上高いこ
とが好ましい。
[Chemical 1] In which R 1 = R 2 is a methyl group and R 3 =
R 4 is hydrogen, a methyl group or a phenyl group. The value of x is in the range of 0 to 2,200 and is a number that provides a viscosity suitable for spheroidization. The number of y is 1 or more, and x + y
Does not exceed 2,200. Therefore, it is dimethylpolysiloxane, methylphenylpolysiloxane or the like. The solubility parameter value of these organopolysiloxanes is 7.3 to 7.8. Further, the temperature of the organopolysiloxane is preferably 10 ° C. or more higher than the melting point of the synthetic resin when it is amorphous and the glass transition point when it is crystalline.

【0008】本発明は、熱可塑性合成樹脂と相溶性もし
くは相混和性を持たない溶解パラメーター値をもつオル
ガノポリシロキサン中で溶融分散球状化を行う方法であ
る。
The present invention is a method of performing melt dispersion spheroidization in an organopolysiloxane having a solubility parameter value that is not compatible or miscible with a thermoplastic synthetic resin.

【実施例】【Example】

【0009】(1) 1,000mlのステンレス製ビ
ーカーに、オルガノポリシロキサン100gを入れ、平
均粒径150メッシュ(104μm)に粉砕した合成樹
脂50gを分散し、毎分450回転で撹拌しながらオル
ガノポリシロキサンを所定温度に加熱し、その温度を保
ちながら3時間撹拌した。次いで加熱を停止し、オルガ
ノポリシロキサンの温度が50℃になるまで冷却を行
い、これを遠心分離機にかけ、樹脂とオルガノポリシロ
キサンに分別した。分別した樹脂は、更に、四塩化炭素
で3回洗浄し、樹脂に付着しているオルガノポリシロキ
サンを完全に除去後、50〜60℃の温風で樹脂を乾燥
した。この乾燥した樹脂の粒子について真球度と平均球
径を測定した。 (2) オルガノポリシロキサンのかわりに、
(1) 100 g of organopolysiloxane was placed in a 1,000 ml beaker made of stainless steel, 50 g of crushed synthetic resin having an average particle size of 150 mesh (104 μm) was dispersed, and organopolysiloxane was stirred at 450 rpm. The siloxane was heated to a predetermined temperature and stirred at that temperature for 3 hours. Then, the heating was stopped, the organopolysiloxane was cooled until the temperature reached 50 ° C., and this was centrifuged to separate the resin and the organopolysiloxane. The separated resin was further washed with carbon tetrachloride three times to completely remove the organopolysiloxane adhering to the resin, and then dried with hot air at 50 to 60 ° C. The sphericity and the average spherical diameter of the dried resin particles were measured. (2) Instead of organopolysiloxane,

【表3】 に示す耐熱性オイルを使用して上記(1)と同様の実験
を行ったところ、合成樹脂は膨潤し、融着して球状化が
困難であり、オルガノポリシロキサンのみ合成樹脂の球
状化に有効であることを確認した。
[Table 3] When the same experiment as in (1) above was performed using the heat resistant oil shown in (1), the synthetic resin swelled and was fused and difficult to be spheroidized, and only organopolysiloxane was effective in spheroidizing the synthetic resin. Was confirmed.

【表3】 [Table 3]

【0010】(1),(2)の測定結果を、The measurement results of (1) and (2) are

【表4】 に示す。[Table 4] Shown in.

【表4】 [Table 4]

───────────────────────────────────────────────────── フロントページの続き (72)発明者 谷口 清峰 東京都三鷹市下連雀8丁目10番16号 日鉄 鉱業株式会社内 ─────────────────────────────────────────────────── ─── Continued Front Page (72) Inventor Kiyomine Taniguchi 8-10-16 Shimorenjaku, Mitaka City, Tokyo Nittetsu Mining Co., Ltd.

Claims (2)

【特許請求の範囲】[Claims] 【請求項1】 【化1】 に示す一般式の化学構造を有するオルガノポリシロキサ
ン中で、合 成樹脂を溶融分散することを特徴とする熱
可塑性合成樹脂の球状化方法。 【化1】
Claims: A method for spheroidizing a thermoplastic synthetic resin, comprising melting and dispersing a synthetic resin in an organopolysiloxane having a chemical structure represented by the general formula: [Chemical 1]
【請求項2】オルガノポリシロキサンの溶解パラメータ
ーと合成樹脂の溶解パラメーターとの差が、1.0以上
であることを特徴とする熱可塑性合成樹脂の球状化方
法。
2. A method of spheroidizing a thermoplastic synthetic resin, wherein the difference between the solubility parameter of the organopolysiloxane and the solubility parameter of the synthetic resin is 1.0 or more.
JP3887392A 1992-01-10 1992-01-10 Method of sphering thermoplastic synthetic resin Pending JPH0693108A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP3887392A JPH0693108A (en) 1992-01-10 1992-01-10 Method of sphering thermoplastic synthetic resin

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP3887392A JPH0693108A (en) 1992-01-10 1992-01-10 Method of sphering thermoplastic synthetic resin

Publications (1)

Publication Number Publication Date
JPH0693108A true JPH0693108A (en) 1994-04-05

Family

ID=12537333

Family Applications (1)

Application Number Title Priority Date Filing Date
JP3887392A Pending JPH0693108A (en) 1992-01-10 1992-01-10 Method of sphering thermoplastic synthetic resin

Country Status (1)

Country Link
JP (1) JPH0693108A (en)

Similar Documents

Publication Publication Date Title
Kuczynski et al. Study of sintering of poly (methyl methacrylate)
Fleming et al. Nanosphere− microsphere assembly: methods for core− shell materials preparation
KR0177491B1 (en) Process for making dry microspheres and microsphere product
JP4846425B2 (en) Microsphere used in powder sintering additive manufacturing method, manufacturing method thereof, powder sintering additive manufacturing method, and manufacturing method thereof
JP2688438B2 (en) Method for producing polymer particles
JPH10501454A (en) Method of forming microparticles in an electric field cage and apparatus therefor
JP2591612B2 (en) Method for producing spherical particles
US4107071A (en) Method of producing microcapsules and resulting product
JP2656808B2 (en) Method for producing hollow glass microspheres with high silica content
US4599294A (en) Particles obtained by atomization while applying voltage
CN106751906B (en) Preparation method with controllable multiple dimensioned pore structure silicon rubber foam
EP1219348A2 (en) Encapsulation process
TW324726B (en) Process for producing thermosetting resin particles
JP3921262B2 (en) Silicone resin hollow body and method for producing the same
Ives Rate theories
CN109988323A (en) The method of monodisperse polyvinyl alcohol microparticles is quickly prepared under a kind of room temperature
US4610944A (en) Production of toner
JPH0693108A (en) Method of sphering thermoplastic synthetic resin
JPS63202658A (en) Production of granular silicone rubber
CN109985588A (en) A kind of micro passage reaction
JPH04506087A (en) Dispersion system of spherical inorganic particles
JP2004059802A (en) Preparation method of solid fine particulate and its apparatus
US4923649A (en) Pelletizing polymers
JPS63108030A (en) Production of thermoplastic resin microparticle
JPH11172007A (en) Production of polymer particle