JPS63248875A - Production of fine saturated polyester resin powder - Google Patents
Production of fine saturated polyester resin powderInfo
- Publication number
- JPS63248875A JPS63248875A JP7981087A JP7981087A JPS63248875A JP S63248875 A JPS63248875 A JP S63248875A JP 7981087 A JP7981087 A JP 7981087A JP 7981087 A JP7981087 A JP 7981087A JP S63248875 A JPS63248875 A JP S63248875A
- Authority
- JP
- Japan
- Prior art keywords
- polyester resin
- saturated polyester
- particles
- fine
- dimethylacetamide
- 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
- 229920001225 polyester resin Polymers 0.000 title claims abstract description 8
- 239000004645 polyester resin Substances 0.000 title claims abstract description 8
- 229920006395 saturated elastomer Polymers 0.000 title claims abstract description 6
- 239000000843 powder Substances 0.000 title claims description 8
- 238000004519 manufacturing process Methods 0.000 title claims description 4
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229920005989 resin Polymers 0.000 claims abstract description 9
- 239000011347 resin Substances 0.000 claims abstract description 9
- 239000002904 solvent Substances 0.000 claims abstract description 9
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000010419 fine particle Substances 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 239000008188 pellet Substances 0.000 claims abstract 4
- 238000001816 cooling Methods 0.000 claims abstract 3
- 238000000034 method Methods 0.000 claims description 4
- 230000001590 oxidative effect Effects 0.000 claims description 2
- 230000001376 precipitating effect Effects 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 21
- 238000010583 slow cooling Methods 0.000 abstract description 4
- 239000012798 spherical particle Substances 0.000 abstract description 4
- 238000000151 deposition Methods 0.000 abstract 1
- 238000009826 distribution Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 229920001707 polybutylene terephthalate Polymers 0.000 description 3
- 229920000139 polyethylene terephthalate Polymers 0.000 description 3
- 239000005020 polyethylene terephthalate Substances 0.000 description 3
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- -1 polyethylene terephthalate Polymers 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009503 electrostatic coating Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
Landscapes
- Paints Or Removers (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Polyesters Or Polycarbonates (AREA)
Abstract
Description
【発明の詳細な説明】
この発明は、溶解法によってポリエチレンテレフタレー
ト又はポリブチレンテレフタレート樹脂の微粉末を低コ
ストで製造する方法に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing fine powder of polyethylene terephthalate or polybutylene terephthalate resin at low cost by a melting method.
（従来技術）
飽和ポリエステル樹脂粉末は、静電塗装用材料として需
要があるが、この種用途に供しうる球状粒子特に１０〜
５０μＯ１の粒子を多量に含む粉末を低価格で生産する
ことは困難であった。(Prior Art) Saturated polyester resin powder is in demand as a material for electrostatic coating.
It has been difficult to produce powder containing a large amount of 50 μO1 particles at a low cost.
（発明の目的）
本発明の目的は、粒径１０〜６０μｍの球状粒子を高収
率で生産しうる製造法を提供することである。(Objective of the Invention) An object of the present invention is to provide a manufacturing method capable of producing spherical particles having a particle size of 10 to 60 μm at a high yield.
（解決手段）
本発明者は各種の溶剤について研究した結果、ジメチル
ホルムアミド又はジメチルアセトアミドを溶剤として選
択することによって、平均粒度１５〜３０μｍの球状粒
子を５０％以上含む３粉末を高効率で生産できることを
発見した。(Solution Means) As a result of research on various solvents, the present inventor found that by selecting dimethylformamide or dimethylacetamide as the solvent, three powders containing 50% or more of spherical particles with an average particle size of 15 to 30 μm can be produced with high efficiency. discovered.
更にこの溶剤に対する樹脂の溶解量は溶剤１００ｐに対
して５０ｋｇまで可能であり溶解量によって粒子径及び
粒度分布を変化させることができることが確認された。Furthermore, it was confirmed that the amount of resin dissolved in this solvent can be up to 50 kg per 100 parts of the solvent, and that the particle size and particle size distribution can be changed depending on the amount dissolved.
（発明の構成）
本発明は、ジメチルアセトアミド又はジメチルホルムア
ミド１００容量部に対してポリエステル樹脂を５０重量
部を超えない範囲で非酸化性雰囲気の加圧下において熱
溶解させる工程と、撹拌を減速して除冷しこの除冷過程
で微粒子を析出させる工程と、この生成粒子と溶剤を分
離する工程とからなり、溶剤分離手段としては濾別又は
減圧回。(Structure of the Invention) The present invention comprises a step of thermally dissolving polyester resin in an amount not exceeding 50 parts by weight in 100 parts by volume of dimethylacetamide or dimethylformamide under pressure in a non-oxidizing atmosphere, and decelerating stirring. It consists of a step of slow cooling, and a step of precipitating fine particles during this slow cooling process, and a step of separating the generated particles from the solvent, and the solvent separation means is filtration or depressurization.
収のいずれも可能であるが濾別によるほうが経済的であ
る。Both methods of collection are possible, but separation by filtration is more economical.
本発明においてポリエステル樹脂の最大溶解量は溶剤１
００容量部に対して５０重量部であって溶解量が多い程
、生成粒子の平均粒径は大きい方に移行する。従って所
望する粒度に応じて溶解量を選定することが好ましい。In the present invention, the maximum amount of polyester resin dissolved is 1
The larger the dissolved amount (50 parts by weight to 00 parts by volume), the larger the average particle size of the produced particles becomes. Therefore, it is preferable to select the amount to be dissolved depending on the desired particle size.
（実施例１）
容積１５０Ｊの溶解槽に、ジメチルアセトアミド１００
ｐとＰＢＴ樹脂（三菱化成＞１０ｋｇを投入し、窒素ガ
スを充填して１６０°Ｃに加熱して槽内圧力１０ｋｇ／
ｃｎｆ、 撹拌翼の回転速度を２００ ｒｐｍとした。(Example 1) 100 g of dimethylacetamide was placed in a dissolution tank with a volume of 150 J.
P and PBT resin (Mitsubishi Kasei > 10 kg were charged, filled with nitrogen gas, heated to 160°C, and the pressure inside the tank was 10 kg/
cnf, the rotational speed of the stirring blade was 200 rpm.
約１時間後に完全溶解したので、撹拌速度を１００ ｒ
ｐｍとして加熱を停止して除冷した。After about 1 hour, it was completely dissolved, so the stirring speed was increased to 100 r.
pm, heating was stopped and the mixture was slowly cooled.
約１００’″Ｃにおいて液が白濁してＰＥＴ微粒子が析
出したことが確認された。At about 100'''C, the liquid became cloudy and it was confirmed that PET fine particles were precipitated.
その後液温が約７０°Ｃになったとき液をフィルタープ
レスに導入して溶剤と析出粒子を分離し生成粒子を真空
乾燥した。Thereafter, when the liquid temperature reached approximately 70°C, the liquid was introduced into a filter press to separate the solvent and precipitated particles, and the resulting particles were vacuum-dried.
得られた粒子の粒径と粒度分布は以下のようで・あった
。The particle size and particle size distribution of the obtained particles were as follows.
粒径μｍ 容量％
１０．１〜１２．７ ５．８５４１２．７〜１
６．０ １６．３１５１６．０〜２０，２
３０．０３８２０．２〜２５．４ １９．２９
０２５．４〜３２．０ ７．７７４３２．０〜
４０．３ ３’、９３５４０．３〜５０．８
３．７４３５０．８〜６４．０ ３．
５５１６４．０〜８０．６ ３．３５９８０．
６〜 ６．１４２（実施例２）
ＰＢＴ樹脂をＰＥＴ樹脂（ユニチカ）に替え、溶解温度
を１８０＠Ｃとした以外は実施例１と同様の条件で行っ
た。Particle size μm Volume % 10.1-12.7 5.85412.7-1
6.0 16.31516.0~20,2
30.03820.2-25.4 19.29
025.4~32.0 7.77432.0~
40.3 3', 93540.3-50.8
3.74350.8~64.0 3.
55164.0-80.6 3.35980.
6 to 6.142 (Example 2) The same conditions as in Example 1 were conducted except that the PBT resin was replaced with a PET resin (Unitika) and the melting temperature was set to 180@C.
この場合の粒度分布は実施例１と略同様であった。The particle size distribution in this case was approximately the same as in Example 1.
（効果）
上記実施例によって明らかな如く本発明によって得られ
るポリエステル微粉末は４０μｍ以下の粒子が殆どであ
ってしかも１０μｍ以下の粒子を含まないから下限の分
級が不要であり、４０μｍ以上の粒子をカットするだけ
で塗装用粉末として使用できるから従来の製品に比して
低価格で提供できるのである。(Effects) As is clear from the above examples, the polyester fine powder obtained by the present invention contains most particles of 40 μm or less and does not contain any particles of 10 μm or less, so there is no need to classify the lower limit, and particles of 40 μm or more are excluded. Because it can be used as a coating powder just by cutting it, it can be provided at a lower price than conventional products.
特′許出願人 村 山 茂Patent applicant Shigeru Murayama
Claims (1)
ステル樹脂ペレット１〜５０重量部をジメチルアセトア
ミド又はジメチルホルムアミド１００容量部に非酸化性
雰囲気の加圧下において加熱溶解させた後、撹拌を減速
して除冷し、この除冷過程で前記樹脂微粒子を析出させ
、その後更に温度を低下させてから溶剤と析出微粒子を
濾別することを特徴とする飽和ポリエステル樹脂微粉末
の製造法。In a container equipped with a stirring and heating device, 1 to 50 parts by weight of saturated polyester resin pellets are heated and dissolved in 100 parts by volume of dimethylacetamide or dimethylformamide under pressure in a non-oxidizing atmosphere, and then the stirring is slowed down and removed. A method for producing a saturated polyester resin fine powder, which comprises cooling, precipitating the resin fine particles during this gradual cooling process, and then further lowering the temperature, and then filtering out the solvent and the precipitated fine particles.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7981087A JPS63248875A (en) | 1987-04-02 | 1987-04-02 | Production of fine saturated polyester resin powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7981087A JPS63248875A (en) | 1987-04-02 | 1987-04-02 | Production of fine saturated polyester resin powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63248875A true JPS63248875A (en) | 1988-10-17 |
| JPH0513974B2 JPH0513974B2 (en) | 1993-02-23 |
Family
ID=13700565
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP7981087A Granted JPS63248875A (en) | 1987-04-02 | 1987-04-02 | Production of fine saturated polyester resin powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63248875A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20180022633A (en) | 2015-06-29 | 2018-03-06 | 도레이 카부시키가이샤 | Polyester resin powder mixture |
| WO2018096964A1 (en) * | 2016-11-25 | 2018-05-31 | 東レ株式会社 | Method for producing polybutylene terephthalate resin particles, and polybutylene terephthalate resin particles |
| US11001046B2 (en) | 2015-06-29 | 2021-05-11 | Toray Industries, Inc. | Polybutylene terephthalate resin powder mixture |
-
1987
- 1987-04-02 JP JP7981087A patent/JPS63248875A/en active Granted
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20180022633A (en) | 2015-06-29 | 2018-03-06 | 도레이 카부시키가이샤 | Polyester resin powder mixture |
| US11001046B2 (en) | 2015-06-29 | 2021-05-11 | Toray Industries, Inc. | Polybutylene terephthalate resin powder mixture |
| WO2018096964A1 (en) * | 2016-11-25 | 2018-05-31 | 東レ株式会社 | Method for producing polybutylene terephthalate resin particles, and polybutylene terephthalate resin particles |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0513974B2 (en) | 1993-02-23 |
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