JPH0762075B2 - Method for producing composite powder containing simple substance of saturated polyester resin and powder of other substances - Google Patents
Method for producing composite powder containing simple substance of saturated polyester resin and powder of other substancesInfo
- Publication number
- JPH0762075B2 JPH0762075B2 JP14058791A JP14058791A JPH0762075B2 JP H0762075 B2 JPH0762075 B2 JP H0762075B2 JP 14058791 A JP14058791 A JP 14058791A JP 14058791 A JP14058791 A JP 14058791A JP H0762075 B2 JPH0762075 B2 JP H0762075B2
- Authority
- JP
- Japan
- Prior art keywords
- powder
- polyester resin
- saturated polyester
- parts
- modified saturated
- 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 - Fee Related
Links
- 239000000843 powder Substances 0.000 title claims description 29
- 229920001225 polyester resin Polymers 0.000 title claims description 14
- 239000004645 polyester resin Substances 0.000 title claims description 14
- 229920006395 saturated elastomer Polymers 0.000 title claims description 11
- 239000000126 substance Substances 0.000 title claims description 10
- 238000004519 manufacturing process Methods 0.000 title claims description 6
- 239000002131 composite material Substances 0.000 title claims description 4
- 239000012046 mixed solvent Substances 0.000 claims description 6
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims description 3
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 3
- 238000002844 melting Methods 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- PYVHTIWHNXTVPF-UHFFFAOYSA-N F.F.F.F.C=C Chemical group F.F.F.F.C=C PYVHTIWHNXTVPF-UHFFFAOYSA-N 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 230000001590 oxidative effect Effects 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims 1
- 238000002156 mixing Methods 0.000 claims 1
- 239000002245 particle Substances 0.000 description 18
- 229920005989 resin Polymers 0.000 description 6
- 239000011347 resin Substances 0.000 description 6
- 238000000576 coating method Methods 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 229920000728 polyester Polymers 0.000 description 3
- 238000010298 pulverizing process Methods 0.000 description 3
- 239000002344 surface layer Substances 0.000 description 3
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 238000009503 electrostatic coating Methods 0.000 description 2
- 238000007610 electrostatic coating method Methods 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000011978 dissolution method Methods 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 238000009501 film coating Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Processes Of Treating Macromolecular Substances (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Description
【０００１】この発明は変性飽和ポリエステル樹脂粉末
の微粉末又は該粉末中に他物質粉末を内包させた複合粉
末の製造方法に関する。The present invention relates to a method for producing a fine powder of a modified saturated polyester resin powder or a composite powder in which the powder of another substance is included.
【０００２】[0002]
【従来の技術】金属その他の無機質材料表面に対し密着
性のよいポリエステル樹脂例えば変性飽和ポリエステル
樹脂（特開昭５４−１２９５１９号公報）粉末は流動浸
漬法による粒体塗装に利用されているが、静電塗装法に
は利用されていないのが現状である。その理由は、該樹
脂の粉末化手段が機械的粉砕法即ち冷凍粉砕に限られて
おり、粒径が３００ミクロン程度のものしか得られず静
電塗装法には適用できないからである。2. Description of the Related Art A polyester resin having good adhesion to the surface of a metal or other inorganic material, for example, a modified saturated polyester resin (Japanese Unexamined Patent Publication (Kokai) No. 54-129519) is used for granule coating by a fluidized-bed method. At present, it is not used in the electrostatic coating method. The reason is that the means for pulverizing the resin is limited to the mechanical pulverization method, that is, freeze pulverization, and only particles having a particle size of about 300 μm can be obtained, which is not applicable to the electrostatic coating method.
【０００３】[0003]
【解決しようとする課題】本発明は、静電塗装に適用で
きる約７０ミクロン以下の変性飽和ポリエステル樹脂粉
末（以下単に原料ポリエステル粉末という）及び表面層
を形成する他物質粉末を内包する同樹脂粉末を提供する
ものである。DISCLOSURE OF THE INVENTION The present invention provides a modified saturated polyester resin powder (hereinafter simply referred to as a raw material polyester powder) having a particle size of about 70 μm or less which can be applied to electrostatic coating, and a resin powder containing another substance powder forming a surface layer. Is provided.
【０００４】本発明において、変性飽和ポリエステル樹
脂とは、ポリエステル重合体１０6ｇ当り１５〜１００
当量の末端カルボキシル基を有する重合体であってその
製法及び金属に対する密着性は特開昭５４−１２９５１
９号公報に記載されているように加熱溶融によって容易
に金属表面に強力に密着するのでプライマーが不要であ
り薄膜コーティングが可能になる。更に、ポリエステル
樹脂の密着力を利用してこれより融点の高い他物質を塗
装表面層に保持させうる塗装用粉末を提供するものであ
る。In the present invention, the modified saturated polyester resin means 15 to 100 per 10 6 g of polyester polymer.
It is a polymer having an equivalent amount of terminal carboxyl groups, and its production method and adhesion to metal are described in JP-A-54-12915
As described in Japanese Patent Publication No. 9, since it strongly adheres strongly to the metal surface by heating and melting, a primer is unnecessary and thin film coating is possible. Further, the present invention provides a coating powder which can retain another substance having a higher melting point than the polyester resin on the coating surface layer by utilizing the adhesive force of the polyester resin.
【０００５】[0005]
【解決手段】本発明は前記原料樹脂を化学溶解法によっ
て粉末化するものであってこれに対する粉末化可能な溶
剤は、ジメチルアセトアミド（ＤＭＡＣ）１００容量部
と、メチルグリコール（ＭＧ）１０〜５０容量部の混合
溶剤である。According to the present invention, the raw material resin is pulverized by a chemical dissolution method, and the pulverizable solvent is 100 parts by volume of dimethylacetamide (DMAC) and 10 to 50 volumes of methyl glycol (MG). Part of a mixed solvent.
【０００６】上記範囲以外では粒子径及び形状が不整い
になる他、収率も悪くなる等の不都合がある。また溶解
させる原料樹脂量は混合溶剤１００重量部に対し３０重
量部以下とする。これ以上では粗大粒子が形成され易く
なり収率が低下する。溶解は窒素などの非酸化性気体雰
囲気下で２００℃以下の温度で行われる。粒子析出は約
１００℃から始まるが約７０℃位に低下するまでの間に
析出を完了させ、濾別作業は約４０℃以下で行なう。ま
た、他物質粉末としては平均粒径５ミクロン以下の四弗
化エチレン粒子の他、セラミックガラス粉等の無機質粉
末がある。Outside of the above range, the particle size and shape are irregular, and the yield is poor. The amount of the raw material resin to be dissolved is 30 parts by weight or less with respect to 100 parts by weight of the mixed solvent. If it is more than this, coarse particles are easily formed and the yield is lowered. The dissolution is performed at a temperature of 200 ° C. or lower in a non-oxidizing gas atmosphere such as nitrogen. The precipitation of particles starts from about 100 ° C., but is completed until the temperature drops to about 70 ° C., and the filtering operation is performed at about 40 ° C. or less. Other substance powders include tetrafluoroethylene particles having an average particle size of 5 microns or less, and inorganic powders such as ceramic glass powder.
【０００７】[0007]
【実施例１】容積１５０Ｌのジャケット付溶解槽にＤＭ
ＡＣ７０ＬとＭＧ３０Ｌを投入し、更に原料樹脂ペレッ
ト１０ｋｇを投入した後窒素ガスを導入し１ｋｇＧ／ｃ
ｍ2とした。緩速で撹拌して温度を１７０℃に保持する
と約１００分で完全溶解する。ジャケットを水冷に切換
えて８０℃まで低下させて粉末粒子を析出させた。この
後更に４０℃まで冷却しフィルタプレスによって析出粒
子と混合溶剤を濾別した。粒子を真空撹拌乾燥機に入
れ、温度８０〜９０℃、１００ｍｍＨｇ下で乾燥した。Example 1 DM in a dissolution tank with a jacket having a volume of 150 L
AC70L and MG30L are charged, and further, 10 kg of raw material resin pellets are charged, and then nitrogen gas is introduced to 1 kg G / c.
It was set to m 2 . When the temperature is maintained at 170 ° C. with slow stirring, it completely dissolves in about 100 minutes. The jacket was switched to water cooling and the temperature was lowered to 80 ° C. to precipitate powder particles. Thereafter, the mixture was further cooled to 40 ° C., and the precipitated particles and the mixed solvent were filtered off by a filter press. The particles were placed in a vacuum stirring dryer and dried at a temperature of 80 to 90 ° C. and 100 mmHg.
【０００８】得られた粒子の粒度分布を測定機：ＳＫレ
ーザーミクロンサイザーＰＲＯ−７０００Ｓ（セイシン
企業製）で測定した結果、６４ミクロン以下の粒子は８
２．１％、平均粒径は３０．７ミクロンであった。The particle size distribution of the obtained particles was measured with a measuring machine: SK laser micron sizer PRO-7000S (manufactured by Seishin Enterprise Co., Ltd.).
It was 2.1% and the average particle size was 30.7 microns.
【０００９】上記製品粉末と冷凍粉砕粉末とのコーティ
ングを比較した結果は表１の通りであった。 テストピース：銅板 １００ｍｍ×５０ｍｍ×３ｍｍThe results of comparing the coatings of the above product powder and the frozen pulverized powder are shown in Table 1. Test piece: Copper plate 100mm x 50mm x 3mm
【００１０】[0010]
【表１】[Table 1]
【００１１】[0011]
【実施例２】同様の溶解槽に実施例１で回収した溶剤と
補充混合溶剤を投入して全量１００Ｌとし、これに原料
樹脂１０ｋｇ、平均粒径５ミクロンの四弗化エチレン粉
末１ｋｇを投入して同様の条件で溶解と析出を行った。
得られた粒子の粒度分布は実施例１とほぼ同様であっ
た。この粒子をテストピースに焼付けて表面の滑沢性を
調べたところ四弗化エチレン被膜の数値と同等であっ
た。この結果から四弗化エチレン粒子はポリエステル溶
解層の表面に露出しているものと推測される。[Example 2] Into a similar dissolution tank, the solvent recovered in Example 1 and the replenishing mixed solvent were charged to make a total amount of 100 L, and 10 kg of raw material resin and 1 kg of tetrafluoroethylene powder having an average particle size of 5 microns were charged therein. Were dissolved and precipitated under the same conditions.
The particle size distribution of the obtained particles was almost the same as in Example 1. When these particles were baked on a test piece and the lubricity of the surface was examined, it was equivalent to the numerical value of the tetrafluoroethylene film. From this result, it is assumed that the ethylene tetrafluoride particles are exposed on the surface of the polyester dissolved layer.
【００１２】[0012]
【効果】本発明によれば密着性に優れた変性飽和ポリエ
ステル樹脂を静電塗装用微粉末とすることが容易且つ経
済的に可能になり更にプライマー処理を不要にすること
ができるので塗装費用も低減できる。また、塗装の表面
層に所望する物質層を形成できる効果がある。[Effect] According to the present invention, it is possible to easily and economically make a modified saturated polyester resin having excellent adhesiveness into a fine powder for electrostatic coating, and it is possible to eliminate the need for a primer treatment. It can be reduced. Further, there is an effect that a desired material layer can be formed on the surface layer of the coating.
Claims (3)
チルグリコール１０〜５０容量部との混合溶剤１００重
量部に変性飽和ポリエステル樹脂１〜３０重量部を投入
し、非酸化性雰囲気下で１７０℃以下の温度で溶解させ
た後７０〜８０℃まで冷却して析出した粉末を濾別して
減圧乾燥することを特徴とする変性飽和ポリエステル樹
脂粉末の製造法。1. A modified saturated polyester resin (1-30 parts by weight) is added to 100 parts by weight of a mixed solvent of dimethylacetamide (100 parts by volume) and methyl glycol (10-50 parts by volume), and the temperature is 170 ° C. or lower in a non-oxidizing atmosphere. The method for producing a modified saturated polyester resin powder, which comprises dissolving the powder in 70 ° C., cooling to 70-80 ° C., filtering the precipitated powder, and drying under reduced pressure.
合溶剤中に不溶性で且つ変性飽和ポリエステル樹脂より
高融点の他物質粉末を変性飽和ポリエステル樹脂１００
重量部に対し、２０〜５重量部の範囲で混入し、前記他
物質粉末を内包する変性飽和ポリエステル樹脂複合粉末
を製造する方法。2. The powder according to claim 1, wherein another substance powder that is insoluble in the mixed solvent and has a higher melting point than the modified saturated polyester resin is modified saturated polyester resin 100.
A method for producing a modified saturated polyester resin composite powder in which the other substance powder is included by mixing in a range of 20 to 5 parts by weight with respect to parts by weight.
請求項２記載の複合粉末製造法。3. The method for producing a composite powder according to claim 2, wherein the powder of the other substance is ethylene tetrafluoride powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP14058791A JPH0762075B2 (en) | 1991-05-17 | 1991-05-17 | Method for producing composite powder containing simple substance of saturated polyester resin and powder of other substances |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP14058791A JPH0762075B2 (en) | 1991-05-17 | 1991-05-17 | Method for producing composite powder containing simple substance of saturated polyester resin and powder of other substances |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH04339828A JPH04339828A (en) | 1992-11-26 |
| JPH0762075B2 true JPH0762075B2 (en) | 1995-07-05 |
Family
ID=15272157
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP14058791A Expired - Fee Related JPH0762075B2 (en) | 1991-05-17 | 1991-05-17 | Method for producing composite powder containing simple substance of saturated polyester resin and powder of other substances |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0762075B2 (en) |
-
1991
- 1991-05-17 JP JP14058791A patent/JPH0762075B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH04339828A (en) | 1992-11-26 |
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