JPH0585573B2 - - Google Patents
Info
- Publication number
- JPH0585573B2 JPH0585573B2 JP101788A JP101788A JPH0585573B2 JP H0585573 B2 JPH0585573 B2 JP H0585573B2 JP 101788 A JP101788 A JP 101788A JP 101788 A JP101788 A JP 101788A JP H0585573 B2 JPH0585573 B2 JP H0585573B2
- Authority
- JP
- Japan
- Prior art keywords
- powder
- solvent
- pressure
- pes
- fine powder
- 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 - Lifetime
Links
- 239000000843 powder Substances 0.000 claims description 30
- 239000002904 solvent Substances 0.000 claims description 16
- YNAVUWVOSKDBBP-UHFFFAOYSA-N Morpholine Chemical compound C1COCCN1 YNAVUWVOSKDBBP-UHFFFAOYSA-N 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 6
- 229920005989 resin Polymers 0.000 claims description 5
- 239000011347 resin Substances 0.000 claims description 5
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 claims description 4
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 4
- 229920000570 polyether Polymers 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 238000011084 recovery Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims 1
- 230000001590 oxidative effect Effects 0.000 claims 1
- 238000011978 dissolution method Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000004809 Teflon Substances 0.000 description 3
- 229920006362 Teflon® Polymers 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- MHABMANUFPZXEB-UHFFFAOYSA-N O-demethyl-aloesaponarin I Natural products O=C1C2=CC=CC(O)=C2C(=O)C2=C1C=C(O)C(C(O)=O)=C2C MHABMANUFPZXEB-UHFFFAOYSA-N 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 230000002542 deteriorative effect Effects 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
- 238000001914 filtration Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
Landscapes
- Polymers With Sulfur, Phosphorus Or Metals In The Main Chain (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Description
【発明の詳細な説明】
この発明はポリエーテルスルホン酸樹脂（以下
PESという）を溶解法によつて粉末を製造する方
法に関するものである。[Detailed Description of the Invention] This invention relates to polyether sulfonic acid resin (hereinafter referred to as polyether sulfonic acid resin).
This invention relates to a method for producing powder from PES (PES) by a dissolution method.
（従来技術）
PESは耐熱性及び機械的強度等に優れているこ
とは周知であつて現在も高性能耐熱液体塗料とし
て市販されている。(Prior Art) It is well known that PES has excellent heat resistance and mechanical strength, and is currently on the market as a high-performance heat-resistant liquid paint.
しかしながらこの液体塗料は一回塗装による膜
厚が薄く何回も重ね塗りをしなければならず従つ
てその都度乾燥する必要がある。 However, this liquid paint has a thin film thickness when applied once, so it must be reapplied many times and must be dried each time.
その上、乾燥時間に長時間を要する他、溶剤蒸
気によつて作業環境を悪化させる欠点があるため
粉体塗料用PES粉末の開発が望まれていた。 Furthermore, it takes a long time to dry and has the drawbacks of deteriorating the working environment due to solvent vapor, so the development of PES powder for powder coatings has been desired.
PESは硬度が高いため機械粉砕は不能であつて
仮令可能であつても機械粉砕法によつて任意の着
色粉末は製造できないこと明らかである。 It is clear that mechanical pulverization of PES is impossible due to its high hardness, and even if it were possible, any colored powder could not be produced by mechanical pulverization.
従つて着色粉末を製造するには化学溶解法に依
らざるを得ないが粉末を有効に生成する溶剤が見
当らなかつたため、敢えて高価なテフロン粉末が
用いられていたのである。 Therefore, in order to produce colored powder, a chemical dissolution method must be used, but since no solvent was found that would effectively produce powder, expensive Teflon powder was intentionally used.
塗装用として使用されるテフロン粉末はテフロ
ン製造元のみが供給できるもので高価であり、更
に着色不能であるという欠点がある。 Teflon powder used for painting is expensive because it can only be supplied by Teflon manufacturers, and it also has the disadvantage that it cannot be colored.
（本発明の解決課題及び特長）
本発明は静電塗装焼付塗膜に供する40μm以下
のPES微粉末を製造するものである。(Problems to be solved and features of the present invention) The present invention is to produce PES fine powder of 40 μm or less for use in electrostatic coating baking coatings.
一般に合成樹脂粉末又はその着色粉末を製造す
る手段として溶解法が有効であることは知られて
いるが、溶解法における溶剤は単に樹脂を溶解さ
せるだけでは不充分であつて生成粉末を容易に分
離できる他、所望の微粉末を得るには二次凝集等
の不都合を起し難いものであることが必要であ
る。 It is generally known that the dissolution method is effective as a means of producing synthetic resin powder or its colored powder, but the solvent used in the dissolution method is not sufficient to simply dissolve the resin, and the resulting powder can be easily separated. In addition, in order to obtain the desired fine powder, it is necessary that it is resistant to problems such as secondary aggregation.
本発明者は、種々の溶剤について研究した結果
モルホリンが最も有効であることを確認した。 As a result of research on various solvents, the present inventor confirmed that morpholine is the most effective.
因にPESはDMACその他の溶剤にもよく溶解
するが、その後の粉末生成は不可能である。 Incidentally, although PES dissolves well in DMAC and other solvents, subsequent powder formation is impossible.
更に該溶剤において微粉末を生成させる溶剤回
収条件は高温であつてはならず60℃以下において
行なわなければならないことも確認した。 Furthermore, it was confirmed that the solvent recovery conditions for producing fine powder in the solvent should not be at high temperatures, but should be carried out at 60°C or lower.
本発明は、溶解から粉末生成までの所要時間が
比較的長くかかり一見不経済のようにみえるが、
粉末生成後の濾別工程が不要で且つ溶液濃度を約
30％以上にすることも可能であるため溶剤使用量
が少なくて済むなど全体としての効率はよいもの
である。 The present invention requires a relatively long time from melting to powder production, which may seem uneconomical at first glance;
Eliminates the need for a filtration process after powder generation, and reduces solution concentration to approx.
Since it is possible to increase the amount to 30% or more, the overall efficiency is good, as the amount of solvent used can be reduced.
（構成）
PESをモルホリンの沸点以下で溶解させた高濃
度溶液を攪拌を継続しつつ60℃以下まで除冷し、
溶剤を減圧回収する。(Structure) A highly concentrated solution in which PES is dissolved below the boiling point of morpholine is slowly cooled to below 60°C while stirring.
Collect the solvent under reduced pressure.
この回収過程で生成した粉末を溶剤残存率10％
以下にしてから真空攪拌乾燥機に移しPES微粉末
を得る。 The powder generated in this recovery process has a solvent residual rate of 10%.
After the following conditions, transfer to a vacuum stirring dryer to obtain PES fine powder.
本発明における溶液濃度は粉体塗装用粉末の場
合約30％またはそれ以下であることが好ましい。 The solution concentration in the present invention is preferably about 30% or less for powder coating powders.
（実施例）
容積50のニーダー中にPES3Kg、モルホリン
10を投入してから窒素ガス２Kg／cm2を封入し攪
拌しつつ約120℃で90分加熱すると完全溶解した。(Example) PES3Kg, morpholine in a kneader with a volume of 50
10 was added, 2 kg/cm 2 of nitrogen gas was filled in, and the mixture was heated at about 120° C. for 90 minutes with stirring to completely dissolve it.
攪拌を継続して加熱を停止し液温が50℃になつ
たとき窒素ガスを放出させ溶剤を減圧回収（40mm
Hg）する。 Continue stirring, stop heating, and when the liquid temperature reaches 50℃, release nitrogen gas and recover the solvent under reduced pressure (40mm
Hg).
約4.5時間後溶剤７が回収されPESの微粉末
が生成された。 After about 4.5 hours, solvent 7 was recovered and a fine powder of PES was produced.
液温40℃になつたとき20mmHgに減圧し、更に
溶剤２を回収した。 When the liquid temperature reached 40°C, the pressure was reduced to 20 mmHg, and solvent 2 was further recovered.
この時点でニーダー中の生成粉末を取り出し真
空攪拌乾燥機に移して一部の二次凝集粉末を分離
し、溶剤残存率１％以下として平均20μmPES粉
末を得た。 At this point, the powder produced in the kneader was taken out and transferred to a vacuum stirring dryer to separate some secondary agglomerated powder, yielding PES powder with an average diameter of 20 μm and a solvent residual rate of 1% or less.
全所要時間は14時間であつた。 The total time required was 14 hours.
（効果）
上記の粉末は風乾により溶剤が完全気散するの
でそのまま製品として使用できる。(Effects) The above powder can be used as a product as it is because the solvent is completely diffused by air drying.
また溶解工程で任意の耐熱性顔料を混入させる
ことによつて所望の着色粉末が得られる。 In addition, a desired colored powder can be obtained by mixing an arbitrary heat-resistant pigment in the dissolution step.
Claims (1)
脂を非酸化性雰囲気においてモルホリンに加熱加
圧溶解させ、その後溶液を60℃以下に除冷してか
ら除圧し、更に減圧下で溶剤回収し、この溶剤回
収過程で生成した粉末を攪拌乾燥して微粉末を得
ることを特徴とするポリエーテルスルホン酸樹脂
微粉末の製造法。1 Dissolve polyether sulfonic acid resin in morpholine under heat and pressure in a non-oxidizing atmosphere using a heat-pressure stirrer, then slowly cool the solution to 60°C or less, remove the pressure, and recover the solvent under reduced pressure. A method for producing polyether sulfonic acid resin fine powder, which comprises stirring and drying the powder produced in the recovery process to obtain fine powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP101788A JPH01178525A (en) | 1988-01-06 | 1988-01-06 | Production of fine polyether sulfonic acid powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP101788A JPH01178525A (en) | 1988-01-06 | 1988-01-06 | Production of fine polyether sulfonic acid powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH01178525A JPH01178525A (en) | 1989-07-14 |
| JPH0585573B2 true JPH0585573B2 (en) | 1993-12-08 |
Family
ID=11489801
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP101788A Granted JPH01178525A (en) | 1988-01-06 | 1988-01-06 | Production of fine polyether sulfonic acid powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01178525A (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0810544Y2 (en) * | 1990-11-26 | 1996-03-29 | 株式会社村上開明堂 | Automatic anti-glare water drop removal door mirror |
| JPH0480748U (en) * | 1990-11-26 | 1992-07-14 |
-
1988
- 1988-01-06 JP JP101788A patent/JPH01178525A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPH01178525A (en) | 1989-07-14 |
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