JPS6262710A - Manufacture of synthetic resin granule - Google Patents
Manufacture of synthetic resin granuleInfo
- Publication number
- JPS6262710A JPS6262710A JP20279285A JP20279285A JPS6262710A JP S6262710 A JPS6262710 A JP S6262710A JP 20279285 A JP20279285 A JP 20279285A JP 20279285 A JP20279285 A JP 20279285A JP S6262710 A JPS6262710 A JP S6262710A
- Authority
- JP
- Japan
- Prior art keywords
- synthetic resin
- thermoplastic synthetic
- granulation
- temperature
- low
- 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.)
- Granted
Links
Landscapes
- Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は床材等に使用される合成樹脂シートの製造に使
われる合成樹脂粒の型遣方法に関する。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a method for molding synthetic resin particles used for manufacturing synthetic resin sheets used for flooring materials and the like.
従来より貫通模様を有する合成樹脂シートは摩耗しても
常に同じ外観模様を呈することから床材の用途に多く使
用されてきた。これらの貫通模様を有する合成樹脂シー
トの製造には、合成樹脂の粉砕片、切断片等が使用され
てきたが、この粉砕片や切断片は合成樹脂をシート状ま
たは棒状に成形し、これを粉砕もしくは切断して製造し
ていたものである。したがって、これらの粉砕片や切断
片は角が尖っていたり、扁平な形状のものしか得られず
、これら粉砕片や切断片を使用して合成樹脂シートを製
造するには、基材表面に粉砕片や切断片を単層に配列移
送し、これを熱プレス等により各々熱融着させるか、配
列された各粉砕片や切断片の間隙をバインダー樹脂粉末
で充填しこれを加熱融着させる方法がとられていた。し
かしながら単層で配列移送させるのに特別な装置が必要
なことや、水玉状の模様を得るためには円形の切断片を
製造しなければならない等の手間がかかるものであった
。そこで粒状の合成樹脂を使用することが行なわれるよ
うになシ、この合成樹脂粒は合成樹脂粉を高速回転翼を
ミキサーで撹拌造粒することによって得られていた。Conventionally, synthetic resin sheets with penetrating patterns have been widely used as flooring materials because they always exhibit the same external pattern even when worn. In the production of synthetic resin sheets with these penetrating patterns, crushed or cut pieces of synthetic resin have been used. It was manufactured by crushing or cutting. Therefore, these crushed pieces and cut pieces can only be obtained with sharp corners or flat shapes, and in order to manufacture synthetic resin sheets using these crushed pieces and cut pieces, it is necessary to crush them on the surface of the base material. A method of arranging and transferring the pieces and cut pieces in a single layer and heat-sealing them using a heat press, etc., or filling the gaps between the arranged crushed pieces and cut pieces with binder resin powder and heat-sealing this. was taken. However, a special device is required to arrange and transfer the material in a single layer, and circular cut pieces must be manufactured in order to obtain a polka dot pattern, which is time-consuming. Therefore, granular synthetic resin has been used, and the synthetic resin granules have been obtained by stirring and granulating synthetic resin powder with a mixer using high-speed rotary blades.
しかしながら、従来の合成樹脂粒の製造方法においては
、単一の熱可塑性合成樹脂粉を高速回転翼型ミキサーに
投入し、これに着色剤や可塑剤等を投入して撹拌造粒を
しているが、造粒開始から造粒物が熱融着して、モチ状
の塊になる迄の時間即ち、造粒時間が短かいため造粒物
の粘度のコントロールが峻しく、さらに造粒物が出来る
と直ちに造粒物同志が熱融着し、これが極めて短時間の
内にモチ状の塊となるため、高速回転翼型ミキサーの冷
却開始時期の選択が非常に難しい等造粒作業がし難いば
かシでなく、熱可塑性合成樹脂の熔融温度より高い温度
でなければ造粒できないという問題点があった。However, in the conventional method for producing synthetic resin granules, a single thermoplastic synthetic resin powder is placed in a high-speed rotary blade mixer, and colorants, plasticizers, etc. are added to the mixer and the mixture is agitated and granulated. However, since the time from the start of granulation until the granules heat-fuse and become a sticky mass, that is, the granulation time, is short, the viscosity of the granules cannot be tightly controlled, and As soon as the granules are formed, they are thermally fused together and form a sticky mass within a very short period of time, making it difficult to select the timing to start cooling the high-speed rotary vane mixer, etc., making granulation work difficult. The problem is that granulation is not possible unless the temperature is higher than the melting temperature of the thermoplastic synthetic resin.
本発明の合成樹脂粒の製造方法は、熱可塑性合成樹脂と
該熱可塑性合成樹脂より低温にて熔融する低温熔融性熱
可塑性合成樹脂とを高速回転翼型ミキサーにて撹拌造粒
することで造粒作業を大幅に改良することを目的とする
ものである。The method for producing synthetic resin particles of the present invention involves stirring and granulating a thermoplastic synthetic resin and a low-melting thermoplastic synthetic resin that melts at a lower temperature than the thermoplastic synthetic resin using a high-speed rotary blade mixer. The purpose is to significantly improve grain operation.
すなわち、熱可塑性合成樹脂と必要に応じて可塑剤、安
定剤、滑剤、充填剤、発泡剤、帯電防止剤等の通常使用
される添加剤及び低温熔融性熱可塑性合成樹脂とを高速
回転翼型ミキサーに投入し、加熱撹拌することで上記熱
可塑性合成樹脂混合物の温度の上昇に伴い、まず低温熔
融性合成樹脂が熔融゛し、この粘着力によりまだ熔融状
態にない熱可塑性合成樹脂と必要に応じて添加する添加
剤を付着せしめ粒子の成長を促進するため、造粒時間が
長くなり粘度のコントロール及び粒子の熱融着によるモ
チ状の塊の発生を抑え、これにより造粒作業を大幅に改
良することを特徴とするものである。That is, a thermoplastic synthetic resin and, if necessary, commonly used additives such as plasticizers, stabilizers, lubricants, fillers, blowing agents, antistatic agents, etc., and a low-temperature melting thermoplastic synthetic resin are mixed into a high-speed rotary blade type. When the thermoplastic synthetic resin mixture is put into a mixer and heated and stirred, the low-temperature melting synthetic resin melts first as the temperature of the thermoplastic synthetic resin mixture rises, and this adhesive force allows it to be mixed with the thermoplastic synthetic resin that is not yet in a molten state. In order to promote the growth of particles by adhering the additives added accordingly, the granulation time becomes longer, controlling the viscosity and suppressing the formation of sticky lumps due to thermal fusion of particles, thereby significantly reducing the granulation work. It is characterized by improving.
熱可塑性合成樹脂としてはポリ塩化ビニル樹脂、ポリエ
チレン、アクリル樹脂の単独重合体や共重合体環一般に
使用される熱可塑性合成樹脂であればいずれのものも使
用できる。As the thermoplastic synthetic resin, any commonly used thermoplastic synthetic resin can be used, such as a homopolymer or a copolymer ring of polyvinyl chloride resin, polyethylene, or acrylic resin.
低温熔融性熱可塑性合成樹脂としては、前記熱可塑性合
成樹脂と同様、ポリ塩化ビニル樹脂、ポリエチレン、ア
クリル樹脂の単独重合体や共重合体環一般に使用される
熱可塑性合成樹脂であればいずれのものでも良い。例え
ば、熱可塑性合成樹脂としてポリ塩化ビニル樹脂を使用
する場合、低温熔融性熱可塑性合成樹脂としては、塩化
ビニル−酢酸ビニル共重合樹脂、エチレン−酢酸ビニル
共重合樹脂、塩化ビニル−エチレン共重合樹脂、低温熔
融性ウレタン樹脂等が使用できる他、主たる熱可塑性合
成樹脂として使用するポリ塩化ビニル樹脂よりも重合度
の低いポリ塩化ビニル樹脂も低温熔融性熱可塑性合成樹
脂として使用することができる。As with the thermoplastic synthetic resins mentioned above, the low-temperature melting thermoplastic synthetic resins include any commonly used thermoplastic synthetic resins such as homopolymers and copolymers of polyvinyl chloride resin, polyethylene, and acrylic resin. But it's okay. For example, when polyvinyl chloride resin is used as the thermoplastic synthetic resin, examples of low-temperature melting thermoplastic synthetic resins include vinyl chloride-vinyl acetate copolymer resin, ethylene-vinyl acetate copolymer resin, and vinyl chloride-ethylene copolymer resin. , low-temperature-melting urethane resins, etc. can be used, and polyvinyl chloride resins having a lower degree of polymerization than the polyvinyl chloride resin used as the main thermoplastic synthetic resin can also be used as the low-temperature-melting thermoplastic synthetic resin.
低温熔融性熱可塑性合成樹脂としては、主たる熱可塑性
合成樹脂より高化式フローテスター(ノズル:1%$x
1oX)での圧力150 b/all、粘度10 po
ise の際の流動温度が10℃以上低いものが好まし
い。流動温度が10℃以上低くないと実質的な効果がな
い。For low-temperature melting thermoplastic synthetic resins, Koka type flow tester (nozzle: 1%
Pressure 150 b/all at 1oX), viscosity 10 po
It is preferable that the flow temperature during rise is 10°C or more lower. There is no substantial effect unless the flow temperature is lower by 10° C. or more.
熱可塑性合成樹脂に対する低温熔融性熱可塑性合成樹脂
の使用量は熱可塑性合成樹脂100重量部に対し、低温
熔融性熱可塑性合成樹脂5重量部〜300重量部である
。低温熔融性熱可塑性合成樹脂の使用景氷5重量部未満
の場合には実質的に効果がなく、また300重量部を越
えると低温熔融性熱可塑性合成樹脂の粘着により撹拌造
粒時に熱可塑性合成樹脂組成物の流動性が著しく低下し
大きな塊を発生し易いという欠点がある。The amount of the low-temperature melting thermoplastic synthetic resin used is 5 parts by weight to 300 parts by weight of the low-temperature melting thermoplastic synthetic resin per 100 parts by weight of the thermoplastic synthetic resin. Usage of low-temperature melting thermoplastic synthetic resin If the amount is less than 5 parts by weight, there is virtually no effect, and if it exceeds 300 parts by weight, thermoplastic synthesis may occur during stirring and granulation due to adhesion of the low-temperature melting thermoplastic synthetic resin. The disadvantage is that the fluidity of the resin composition is significantly reduced and large lumps are likely to occur.
また、必要に応じて前記熱可塑性合成樹脂に可塑剤、安
定剤、滑剤、充填剤、着色剤、発泡剤、帯電防止剤、防
カビ剤等通常使用される添加剤が添加される。Further, if necessary, commonly used additives such as plasticizers, stabilizers, lubricants, fillers, colorants, foaming agents, antistatic agents, and fungicides are added to the thermoplastic synthetic resin.
可塑剤としては、ジオクチルフタレート、ジブチル7タ
レート、ブチルベンジルフタレート、ジオクチルアジペ
ート、トリクレジルフォスフェート等の汎用可塑剤の池
、DAP、アクリル系モノマー、アクリル系オリゴマー
等の反応性可塑剤、トリプトキシエチル7オスフエート
、ブチルジグリコールアジペート、サンソサイザー〇−
1100(新日本理化層)等の帯電防止性可塑剤、ドデ
シルベンゼン誘導体等の二次可塑剤等が挙げられる。Examples of plasticizers include general-purpose plasticizers such as dioctyl phthalate, dibutyl 7-thalate, butylbenzyl phthalate, dioctyl adipate, and tricresyl phosphate, reactive plasticizers such as DAP, acrylic monomers, and acrylic oligomers, and tryptoxy. Ethyl 7 phosphate, butyl diglycol adipate, Sansocizer〇-
Examples include antistatic plasticizers such as 1100 (Shin Nippon Rikagyoku), secondary plasticizers such as dodecylbenzene derivatives, and the like.
可塑剤の添加量は樹脂100重量部に対し10〜100
重量部が好ましい。The amount of plasticizer added is 10 to 100 parts by weight per 100 parts by weight of resin.
Parts by weight are preferred.
また、必要に応じて安定剤、滑剤、充填剤、発泡剤、帯
電防止剤、防カビ剤など通常使用される添加剤が使用さ
れる。Further, commonly used additives such as stabilizers, lubricants, fillers, foaming agents, antistatic agents, and fungicides are used as necessary.
特に充填剤は高速回転翼型ミキサーでの撹拌時の熱可塑
性合成樹脂組成物の粘着による流動性低下を改良し、粗
大粒子の発生を抑える効果があシ支障のない範囲で添加
することが好ましい。また、このような目的以外に、コ
ストダウン、軽量化等の目的で炭酸カルシウム、クレー
、シリカ、シラスバルーン、ガラスバルーン、木粉、コ
ルク粉等の軽量充填剤、導電性や帯電防止性付与の目的
でカーボン粉末、炭素繊維や銀、鋼、ニッケル、アルミ
ニウム、ステンレス、鉄等の金属よりなる粉末や短繊維
などの導電性粉末充填剤や導電性短繊維、耐摩耗性や防
滑性付与の目的で珪砂粒、珪酸化合物粒子、ガラス粉末
、陶磁器粉砕粒、カーボランダム、アランダムなどの硬
質粉粒体、寸法安定性付与の目的でガラス短繊維、チタ
ン酸カリウムの短繊維、MOS(カルシウムメタシリケ
ート)短繊維などの無機物短繊維等が使用できる。In particular, the filler is effective in improving fluidity reduction due to adhesion of the thermoplastic synthetic resin composition during stirring with a high-speed rotary blade mixer and suppressing the generation of coarse particles, and is preferably added within a range that does not cause any problems. . In addition to these purposes, lightweight fillers such as calcium carbonate, clay, silica, shirasu balloons, glass balloons, wood flour, and cork powder, as well as materials that impart conductivity and antistatic properties, are also used for purposes such as cost reduction and weight reduction. Conductive powder fillers and conductive short fibers such as carbon powder, carbon fiber, powders and short fibers made of metals such as silver, steel, nickel, aluminum, stainless steel, and iron, for the purpose of imparting wear resistance and anti-slip properties silica sand grains, silicate compound particles, glass powder, crushed ceramic grains, hard powders such as carborundum and alundum, short glass fibers, short fibers of potassium titanate, and MOS (calcium metasilicate) for the purpose of imparting dimensional stability. ) Inorganic short fibers such as short fibers can be used.
導電性粉末充填剤は粒径が0.5〜1000μが好まし
く導電性短繊維は径が4μ〜600μで長さが0.5〜
2o■の範囲が好ましい。添加量は目的とする抵抗値に
より適宜設定する必要があるが、導電性粉末充填剤の場
合で約2重量%以上、導電性短繊維の場合で約lt量チ
以上の添加が必要である。硬質粉粒体は径が10μ〜1
000μが好ましく、添加量は5重量%以上の添加が好
ましい。The conductive powder filler preferably has a particle size of 0.5 to 1000μ, and the conductive short fibers have a diameter of 4μ to 600μ and a length of 0.5 to 1000μ.
A range of 2o■ is preferred. The amount added needs to be set appropriately depending on the desired resistance value, but in the case of a conductive powder filler, it is necessary to add about 2% by weight or more, and in the case of conductive short fibers, it is necessary to add about 100% by weight or more. Hard powder particles have a diameter of 10μ to 1
The amount of addition is preferably 5% by weight or more.
他の添加剤、充填剤等は使用目的により適当1添加使用
する。Other additives, fillers, etc. may be added as appropriate depending on the purpose of use.
これらの添加剤は単独で使用しても良いし、2種以上を
混合使用しても何らさしつかえないものである。These additives may be used alone or in combination of two or more.
低温熔融性熱可塑性合成樹脂を高速回転翼型ミキサーに
投入する時期は、熱可塑性合成樹脂と同時に投入しても
良いし、熱可塑性合成樹脂をヘンシェルミキサーに投入
し撹拌を開始した後でも良いが、投入時期は早い方が好
ましい。The low-melting thermoplastic synthetic resin may be introduced into the high-speed rotary blade mixer at the same time as the thermoplastic synthetic resin, or after the thermoplastic synthetic resin has been introduced into the Henschel mixer and stirring has started. , the earlier the introduction time, the better.
本発明において使用される高速回転翼型ミキサーは従来
から一般に使用されているものが使用でき、例えばヘン
シェルミキサ−(三井三池化工機製)、スーパーミキサ
ー(用田製作所製)、ニューグラマシン(大和化工機製
)等が使用可能である。尚、高速回転翼型ミキサーで合
成樹脂組成物を撹拌造粒する場合、ミキサーの機種、容
積等により造粒条件が多少異なるので、それぞれに合せ
て造粒条件を調整する必要がある。As the high-speed rotary vane type mixer used in the present invention, those commonly used can be used, such as the Henschel mixer (manufactured by Mitsui Miike Kakoki), the super mixer (manufactured by Yoda Seisakusho), and the New Gram Machine (manufactured by Daiwa Kakoki). ) etc. can be used. In addition, when agitating and granulating a synthetic resin composition using a high-speed rotary blade mixer, the granulation conditions differ somewhat depending on the mixer model, volume, etc., so it is necessary to adjust the granulation conditions accordingly.
以下本発明をさらに詳しく説明するために実施例を掲げ
るが、本発明は実施例に限定されるものではなか。Examples are given below to explain the present invention in more detail, but the present invention is not limited to the examples.
実施例1
下記表に示す組成で白色熱可塑性合成樹脂粒を製造した
。Example 1 White thermoplastic synthetic resin particles were produced with the composition shown in the table below.
ヘンシェルミキサーFIM10B(三井三池化工機M)
に配合(υの樹脂、炭酸カルシウム、白色着色剤を投入
し高速撹拌しつつ可塑剤、エポキシ化大豆油、安定剤の
液状成分を投入する。投入し終わった後ヘンシェルミキ
サーのジャケットに2.5Kf/−の蒸気を通し上記樹
脂組成物の温度が120℃になった時点で蒸気を停止し
、その後、撹拌による摩擦熱により上記樹脂組成物の温
度が132℃になった時点で回転翼を低速にし、更に粒
が成長した時点でジャケットを水冷し、樹脂組成物の温
度が40℃になった時点でヘンシールミキサーより排出
し、0.5〜3mの粒径を有する白色熱可塑性合成樹脂
粒を得た。Henschel mixer FIM10B (Mitsui Miike Kakoki M)
Add the resin, calcium carbonate, and white coloring agent (υ), and add the liquid components of plasticizer, epoxidized soybean oil, and stabilizer while stirring at high speed.After adding, add 2.5Kf to the jacket of Henschel mixer. When the temperature of the resin composition reaches 120°C, the steam is stopped, and when the temperature of the resin composition reaches 132°C due to frictional heat caused by stirring, the rotor is rotated at low speed. When the particles have grown, the jacket is cooled with water, and when the temperature of the resin composition reaches 40°C, it is discharged from the Henshil mixer to form white thermoplastic synthetic resin particles with a particle size of 0.5 to 3 m. I got it.
比較例1
実施例1の低温熔融性の塩化ビニル/酢酸ビニル共重合
樹脂(Goon400X150ML、酢酸ビニル含有量
15チ、流48度152℃)を使用せず、塩化ビニル/
酢酸ビニル共重合樹脂(Geon103IF−85,酢
酸ビニル含有量5 ’I’ を流動温度1マロ℃)を1
00重量部使用する以外は実施例1と同じ組成の樹脂組
成物を実施例1と同様の操作で加熱撹拌した。Comparative Example 1 The low-temperature melting vinyl chloride/vinyl acetate copolymer resin of Example 1 (Goon 400 x 150 ML, vinyl acetate content 15 inches, flow rate 48 degrees and 152 degrees Celsius) was not used, and vinyl chloride/vinyl acetate copolymer resin was used.
Vinyl acetate copolymer resin (Geon103IF-85, vinyl acetate content 5 'I', flow temperature 1 malo ℃)
A resin composition having the same composition as in Example 1 except that 0.00 parts by weight was used was heated and stirred in the same manner as in Example 1.
その結果、樹脂組成物の温度が160℃になってもほと
んど粒子の成長が認められず、さらに加熱撹拌を続けた
ところ、樹脂組成物の温度が170℃となったころから
目立った粒子の成長が始まったが、その直後には急激な
粒子の成長が起こυ、部分的にモチ状の大きな塊を生じ
、所望の粒径の合成樹脂粒子を得ることができなかった
。As a result, almost no particle growth was observed even when the temperature of the resin composition reached 160°C, and when heating and stirring were continued, noticeable particle growth was observed when the temperature of the resin composition reached 170°C. Immediately after that, rapid particle growth occurred, resulting in partially sticky large lumps, making it impossible to obtain synthetic resin particles with the desired particle size.
本発明においては熱可塑性合成樹脂に低温熔融性熱可塑
性合成樹脂を併用して撹拌造粒しているので、熱可塑性
合成樹脂単独で撹拌造粒する場合よりも低温で造粒する
ことができるばかりでなく、造粒作業、特に粒径のコン
トロールのための冷却時期の選択が容易となる効果があ
る。In the present invention, since the thermoplastic synthetic resin and the low-melting thermoplastic synthetic resin are used together for stirring and granulation, the granulation can be performed at a lower temperature than when stirring and granulating the thermoplastic synthetic resin alone. In addition, it has the effect of making it easier to select the cooling time for granulation work, especially for controlling particle size.
Claims (1)
融する低温熔融性熱可塑性合成樹脂とを高速回転翼型ミ
キサーにて撹拌造粒することを特徴とする合成樹脂粒の
製造方法。A method for producing synthetic resin particles, which comprises stirring and granulating a thermoplastic synthetic resin and a low-melting thermoplastic synthetic resin that melts at a lower temperature than the thermoplastic synthetic resin using a high-speed rotary blade mixer.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP20279285A JPS6262710A (en) | 1985-09-13 | 1985-09-13 | Manufacture of synthetic resin granule |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP20279285A JPS6262710A (en) | 1985-09-13 | 1985-09-13 | Manufacture of synthetic resin granule |
Publications (2)
Publication Number | Publication Date |
---|---|
JPS6262710A true JPS6262710A (en) | 1987-03-19 |
JPH0553605B2 JPH0553605B2 (en) | 1993-08-10 |
Family
ID=16463268
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP20279285A Granted JPS6262710A (en) | 1985-09-13 | 1985-09-13 | Manufacture of synthetic resin granule |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPS6262710A (en) |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP6968479B1 (en) * | 2021-07-12 | 2021-11-17 | マルイチ エアリアル エンジニア株式会社 | Evaluation system |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS5116359A (en) * | 1974-07-31 | 1976-02-09 | Asahi Chemical Ind | CHAKUSHOKUSENJOHORIESUTERUPERETSUTONO SEIZOHOHO |
JPS56159116A (en) * | 1980-05-13 | 1981-12-08 | Asahi Chem Ind Co Ltd | Method of coarse granulation of crystalline polyolefin powder and coarse granules |
JPS6223716A (en) * | 1985-07-24 | 1987-01-31 | Achilles Corp | Preparation of multi-color synthetic resin particle |
-
1985
- 1985-09-13 JP JP20279285A patent/JPS6262710A/en active Granted
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS5116359A (en) * | 1974-07-31 | 1976-02-09 | Asahi Chemical Ind | CHAKUSHOKUSENJOHORIESUTERUPERETSUTONO SEIZOHOHO |
JPS56159116A (en) * | 1980-05-13 | 1981-12-08 | Asahi Chem Ind Co Ltd | Method of coarse granulation of crystalline polyolefin powder and coarse granules |
JPS6223716A (en) * | 1985-07-24 | 1987-01-31 | Achilles Corp | Preparation of multi-color synthetic resin particle |
Also Published As
Publication number | Publication date |
---|---|
JPH0553605B2 (en) | 1993-08-10 |
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Legal Events
Date | Code | Title | Description |
---|---|---|---|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
LAPS | Cancellation because of no payment of annual fees |