JPH0458809B2 - - Google Patents
Info
- Publication number
- JPH0458809B2 JPH0458809B2 JP17107187A JP17107187A JPH0458809B2 JP H0458809 B2 JPH0458809 B2 JP H0458809B2 JP 17107187 A JP17107187 A JP 17107187A JP 17107187 A JP17107187 A JP 17107187A JP H0458809 B2 JPH0458809 B2 JP H0458809B2
- Authority
- JP
- Japan
- Prior art keywords
- polyolefin resin
- particles
- parts
- heating
- particle size
- 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
- 239000012046 mixed solvent Substances 0.000 claims description 6
- 229920005672 polyolefin resin Polymers 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- BFSVOASYOCHEOV-UHFFFAOYSA-N 2-diethylaminoethanol Chemical compound CCN(CC)CCO BFSVOASYOCHEOV-UHFFFAOYSA-N 0.000 claims description 3
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000008096 xylene Substances 0.000 claims description 3
- 230000001590 oxidative effect Effects 0.000 claims description 2
- 230000001376 precipitating effect Effects 0.000 claims 1
- 239000002245 particle Substances 0.000 description 17
- 239000002904 solvent Substances 0.000 description 5
- -1 polyethylene Polymers 0.000 description 4
- 229920005989 resin Polymers 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000004698 Polyethylene Substances 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 229920001155 polypropylene Polymers 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 150000001414 amino alcohols Chemical class 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000011978 dissolution method Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
Landscapes
- Processes Of Treating Macromolecular Substances (AREA)
Description
この発明は、ポリオレフイン樹脂の微粉末を低
コストで製造する方法に関する。
(従来技術)
ポリエチレン、ポリプロピレン等の粉末は、塗
装材料などとして広く使用されており最も需要の
多い粒度範囲は10μ〜60μである。
従つて溶解法の改良は、これらの粒度範囲にお
ける形状粒子を効率よく製造することに主眼があ
り溶剤回収工程も含めて生産効率のよい溶剤の発
見が望まれていたのである。
(発明の目的)
本発明の目的は、上記粒度範囲のポリオレフイ
ン樹脂の球状粒子を収率よく製造し、溶剤回収が
容易で生成粒子の水洗を不要にできる製造法を提
供することである。
(解決手段及び本発明の特長)
本発明者はこれらの目的を達成しうるものとし
て各種の水溶性低沸点溶剤について研究した結
果、ジエチルエタノールアミン(日本乳化剤製ア
ミノアルコール2A)とキシレンの混合溶剤が効
果的であることを発見した。
この溶剤は回収も容易でしかも製品粒子を水洗
する必要がない利点がある。
(発明の構成)
本発明における混合溶剤は、ジエチルンエタノ
ールアミン6〜8容量部とキシレン4〜2容量部
の混合溶剤である。
特に7:3の混合割合が最も効率がよい。
この混合溶剤100容量部に、ポリオレフイン樹
脂40重量部を超えない範囲で投入し、非酸化性雰
囲気下で約140℃に加熱しつつ攪拌溶解させてか
ら、攪拌を停止して除冷しこの除冷過程で微粒子
を析出させる。
この生成粒子を濾別して真空乾燥(70°〜90℃、
5〜40mmHg)し、分級して製品とするものであ
る。
実施例 1
加圧溶解槽に混合溶剤30と1.5Kgのポリプロ
ピレン樹脂を投入し窒素ガスを封入して圧力1
Kg/cm2とし、攪拌しながら140℃まで加熱した。
約2時間後完全溶解したので加熱及び攪拌を停
止し、水冷却を行つた。
約70℃で粒子が析出し更に40℃まで冷却した。
その後再び20分間撹拌し、フイルタープレスで
粒子を濾別した。
回収粒子を真空度10mmHg、80℃の加熱真空乾
燥機に入れて乾燥し製品を得た。
製品粒子の粒度分布は表の如くであつた。
実施例 2
ポリエチレン1.5Kgを実施例1と同様の条件で
溶解させ冷却した。
この場合は約80℃で粒子が析出した。
その後同様にして製品を得た。
この粒度分布は表の如くであつた。
The present invention relates to a method for producing fine powder of polyolefin resin at low cost. (Prior Art) Powders of polyethylene, polypropylene, etc. are widely used as coating materials, and the particle size range most in demand is 10μ to 60μ. Therefore, improvements in the dissolution method are aimed at efficiently producing shaped particles within these particle size ranges, and there has been a desire to discover a solvent with good production efficiency, including the solvent recovery process. (Objective of the Invention) An object of the present invention is to provide a method for producing spherical particles of a polyolefin resin having a particle size within the above-mentioned particle size range with good yield, easy solvent recovery, and no need for washing the produced particles with water. (Solution Means and Features of the Present Invention) As a result of researching various water-soluble low-boiling point solvents that can achieve these objectives, the present inventor developed a mixed solvent of diethylethanolamine (Amino Alcohol 2A manufactured by Nippon Nyukazai Co., Ltd.) and xylene. was found to be effective. This solvent has the advantage that it is easy to recover and does not require washing the product particles with water. (Structure of the Invention) The mixed solvent in the present invention is a mixed solvent of 6 to 8 parts by volume of diethylethanolamine and 4 to 2 parts by volume of xylene. In particular, a mixing ratio of 7:3 is the most efficient. Add not more than 40 parts by weight of the polyolefin resin to 100 parts by volume of this mixed solvent, stir and dissolve while heating to approximately 140°C in a non-oxidizing atmosphere, then stop stirring and slowly cool the resin. Fine particles are precipitated during the cooling process. The generated particles are filtered and dried under vacuum (70° to 90°C,
5 to 40 mmHg) and then classified into products. Example 1 Put 30 kg of mixed solvent and 1.5 kg of polypropylene resin into a pressurized dissolution tank, fill it with nitrogen gas, and raise the pressure to 1.
Kg/cm 2 and heated to 140° C. with stirring. After about 2 hours, the solution was completely dissolved, so heating and stirring were stopped, and water cooling was performed. Particles precipitated at about 70°C, and the mixture was further cooled to 40°C. Thereafter, the mixture was stirred again for 20 minutes and the particles were filtered off using a filter press. The recovered particles were placed in a heated vacuum dryer at 80° C. with a degree of vacuum of 10 mmHg and dried to obtain a product. The particle size distribution of the product particles was as shown in the table. Example 2 1.5 kg of polyethylene was melted and cooled under the same conditions as in Example 1. In this case, particles precipitated at about 80°C. Thereafter, a product was obtained in the same manner. The particle size distribution was as shown in the table.
【表】【table】
【表】
なお上記実施例における樹脂濃度は約5%であ
るが、この濃度を高くすることによつて平均粒径
が大きくなるからこの性質を利用して粒度調整が
可能である。[Table] Note that the resin concentration in the above examples is about 5%, but by increasing this concentration, the average particle size becomes larger, so it is possible to adjust the particle size using this property.
Claims (1)
ポリオレフイン樹脂1〜40重量部をジエチルエタ
ノールアミンとキシレンとの混合溶剤100容量部
に非酸化性雰囲気下において加圧加熱溶解させた
後、加熱攪拌を停止して除冷し、この除冷過程で
ポリオレフイン樹脂微粉末を析出させることを特
徴とするポリオレフイン樹脂微粉末の製造法。1 In a container equipped with a stirring and heating device,
After dissolving 1 to 40 parts by weight of a polyolefin resin in 100 parts by volume of a mixed solvent of diethylethanolamine and xylene under pressure and heating in a non-oxidizing atmosphere, heating and stirring were stopped and the mixture was gradually cooled. A method for producing fine polyolefin resin powder, which comprises precipitating fine polyolefin resin powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP17107187A JPS6416841A (en) | 1987-07-10 | 1987-07-10 | Production of polyolefin resin fine powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP17107187A JPS6416841A (en) | 1987-07-10 | 1987-07-10 | Production of polyolefin resin fine powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6416841A JPS6416841A (en) | 1989-01-20 |
| JPH0458809B2 true JPH0458809B2 (en) | 1992-09-18 |
Family
ID=15916491
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP17107187A Granted JPS6416841A (en) | 1987-07-10 | 1987-07-10 | Production of polyolefin resin fine powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6416841A (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5477632B2 (en) * | 2010-01-12 | 2014-04-23 | Dic株式会社 | Method for producing polypropylene wax dispersion |
-
1987
- 1987-07-10 JP JP17107187A patent/JPS6416841A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6416841A (en) | 1989-01-20 |
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