JPS6228194B2 - - Google Patents
Info
- Publication number
- JPS6228194B2 JPS6228194B2 JP15560682A JP15560682A JPS6228194B2 JP S6228194 B2 JPS6228194 B2 JP S6228194B2 JP 15560682 A JP15560682 A JP 15560682A JP 15560682 A JP15560682 A JP 15560682A JP S6228194 B2 JPS6228194 B2 JP S6228194B2
- Authority
- JP
- Japan
- Prior art keywords
- parts
- weight
- epoxy resin
- silica
- coating
- 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
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 52
- 238000000576 coating method Methods 0.000 claims description 30
- 239000000843 powder Substances 0.000 claims description 25
- 239000011248 coating agent Substances 0.000 claims description 23
- 239000000377 silicon dioxide Substances 0.000 claims description 21
- 239000003822 epoxy resin Substances 0.000 claims description 13
- 229920000647 polyepoxide Polymers 0.000 claims description 13
- 239000011256 inorganic filler Substances 0.000 claims description 12
- 229910003475 inorganic filler Inorganic materials 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 239000004606 Fillers/Extenders Substances 0.000 claims description 4
- 239000000049 pigment Substances 0.000 claims description 4
- 239000004593 Epoxy Substances 0.000 claims description 3
- 239000003086 colorant Substances 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 239000008199 coating composition Substances 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- 239000004576 sand Substances 0.000 description 9
- 239000003973 paint Substances 0.000 description 6
- 238000009835 boiling Methods 0.000 description 5
- 238000004898 kneading Methods 0.000 description 5
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 229910001018 Cast iron Inorganic materials 0.000 description 3
- 238000005299 abrasion Methods 0.000 description 3
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical class C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 3
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000004952 Polyamide Substances 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 2
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 description 2
- 239000006229 carbon black Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 150000002170 ethers Chemical class 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229920002647 polyamide Polymers 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- QTWJRLJHJPIABL-UHFFFAOYSA-N 2-methylphenol;3-methylphenol;4-methylphenol Chemical compound CC1=CC=C(O)C=C1.CC1=CC=CC(O)=C1.CC1=CC=CC=C1O QTWJRLJHJPIABL-UHFFFAOYSA-N 0.000 description 1
- VEORPZCZECFIRK-UHFFFAOYSA-N 3,3',5,5'-tetrabromobisphenol A Chemical compound C=1C(Br)=C(O)C(Br)=CC=1C(C)(C)C1=CC(Br)=C(O)C(Br)=C1 VEORPZCZECFIRK-UHFFFAOYSA-N 0.000 description 1
- UMHJEEQLYBKSAN-UHFFFAOYSA-N Adipaldehyde Chemical compound O=CCCCCC=O UMHJEEQLYBKSAN-UHFFFAOYSA-N 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000008064 anhydrides Chemical class 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 229930003836 cresol Natural products 0.000 description 1
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 description 1
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical class C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 150000002460 imidazoles Chemical class 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 229920003986 novolac Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 150000007519 polyprotic acids Polymers 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
Description
本発明は、耐衝撃性、耐摩耗性、平滑性、耐水
性及び耐沸とう水性等の塗膜性能に優れるととも
に安価なコストのエポキシ樹脂系粉体塗料に関す
るものである。
一般に、塗膜に耐衝撃性、耐摩耗性などの性能
を向上させるとともに、塗料コストの引き下げに
効果のある材料としてシリカ系の無機質充てん材
が知られている。
エポキシ樹脂系粉体塗料においても、上記のよ
うな塗膜性能の向上と塗料コストの引き下げにシ
リカ系無機質充てん材を配合することは有効であ
る。
本発明者らは、エポキシ樹脂系粉体塗料の耐衝
撃性、耐摩耗性、耐水性及び耐沸とう水性を向上
させるとともに、塗料コストを大巾に引き下げる
ために前記(A)の100重量部に対して130〜400重量
部のシリカ系無機質充てん材の配合が有効である
という知見を得たので、該塗料の効果的な製造方
法について検討した。
一般に粉体塗料の製造方法、特に各原料の混合
の形態としては、溶融混練法と単に混合する方法
とが代表的である。勿論、最終的に粉体塗料とな
し得るためには、これに粉砕及び必要に応じて分
級の工程が加わることが必要である。
本発明者らは、上記のシリカ系無機質充てん材
を多量に配合せるエポキシ樹脂系粉体塗料の場
合、上記した塗膜の平滑性並びに耐水性、耐沸と
う水性の向上には溶融混練法が有効であるが、シ
リカ系無機質充てん材の配合量が一定量に達する
と、上記の向上程度が小さくなり飽和してしまう
ことを知つた。かゝる一定量以上のシリカ系無機
質充てん材の溶融混練のもとでは、シリカ系無機
質充てん材の配合量増大のために混練物の硬度が
増加し、粉末塗料化のための混練物の粉柁上、粉
砕機の早期摩損など不利である。
そこで、本発明者らは、この点について鋭意検
討した結果、(A)軟化点が60〜150℃、エポキシ当
量が400〜2000の固形エポキシ樹脂、(B)硬化剤、
(C)上記(A)の100重量部に対して、130〜400重量部
のシリカ系無機質充てん材、(D)必要に応じて着色
材及び／又は体質顔料とからなるエポキシ樹脂系
粉体塗料組成物において、(C)の50〜120重量部を
(A)、(B)並びに(D)と混合、溶融混練、粉砕、分級し
たものに(C)の残部を混合したことを特徴とするエ
ポキシ樹脂系粉体塗料の製造方法が極めて効果的
であることを見いだした。
本発明者らの実験によると、溶融混練に供する
シリカ系無機質充てん材の量は、上記(A)の100重
量部に対して50〜120重量部とするのが有効であ
ることが判明している。即ち、50重量部未満の場
合は塗膜の平滑性が不十分となる。又、120重量
部を越えて溶融混練してもそれによつて塗膜の平
滑性などの性能が更に大きく変化することはな
く、従つて、溶融混練するシリカ系無機質充てん
材の量は最大120重量部で充分である。
本発明に適した前記固形のエポキシ樹脂(A)とし
ては、ビスフエノールＡ、ビスフエノールＦある
いはテトラブロモ・ビスフエノールＡなどのジグ
リシジルエーテル、フエノールあるいはクレゾー
ル・ノボラツクのポリグリシジルエーテル及びこ
れらの変性エポキシ樹脂、さらには多価アルコー
ルのポリグリシジルエーテル、多塩基酸のポリグ
リシジルエステル及びこれらの変性エポキシ樹脂
などとして知られる慣用のエポキシ樹脂があげら
れる。
他方、本発明に適した前記硬化剤(B)としては、
アミン及びアミン・アダクト、ポリアミド、ポリ
アミド・アダクト、酸基含有ポリエステル、多価
カルボン酸又は無水物及びそれらの変性物、ジシ
アンジアミド及びその変性物、イミダゾール類な
ど、公知慣用の硬化剤から選ばれるものである。
さらに、前記シリカ系無機質充てん材(C)として
は、石英粉とかケイ砂などの名称で一般に呼ばれ
ているものが適用可能である。着色材及び／又は
体質顔料(D)としては、酸化チタン、カーボンブラ
ツク、沈降性硫酸バリウム、タルク、その他一般
に公知の着色顔料、染料、及び体質顔料を用いる
ことができる。
そのほか、塗膜の表面状態、たとえばオレンジ
ピール、レベリング性などを改良するために、必
要に応じて流れ調整剤を加えても良い。
該塗料の塗装方法としては、吹付塗装、静電粉
体塗装、流動浸漬塗装など鋳鉄管、鋳鉄異形管及
び鋳鉄バルブに実施されているいずれの粉体塗装
方法も適用が可能である。
以下、実施例によつて具体的に説明する。尚、
「部」は「重量部」をもつて示す。
実施例 １
軟化点が95℃、エポキシ当量が900のビスフエ
ノールＡ型エポキシ樹脂（商品名：エポトート
YD−014・東都化成(株)製）100部、アジピン酸ジ
ヒドラド３部、イミダゾール３部、酸化チタン10
部、カーボンブラツク0.2部、モダフロー（流動
調整剤：米国モンサント社製）0.5部、ケイ砂微
粉（粒度100μ以下、平均粒径40μ）100部を予備
混合したのち、ブス・コニーダーPR−46（スイ
ス国ブス社製）を用いて加熱溶融混練し、粉砕、
分級して平均粒径40μの粉末を調整した。これに
ケイ砂微粉100部を混合して粉体塗料とした。
実施例 ２
実施例１において、最終混合時のケイ砂微粉の
量を200部とした以外は全く同様にして粉体塗料
を調整した。
実施例 ３
実施例１において、最終混合時のケイ砂微粉の
量を300部とした以外は全く同様にして粉体塗料
を調整した。
比較例
実施例１において、ケイ砂微粉の全量を単に混
合した以外は全く同様にして粉体塗料を調整し
た。
上記実施例１〜３及び比較例によつて調整した
粉体塗料を250℃に予熱した鋼板に静電塗装し、
その後放冷して500〜800μの膜厚の試験片とな
し、塗膜性能を調べた結果を表−１に示す。
尚、上記の各実施例に対し、塗料全体としての
ケイ砂微粉の添加量は同一であるが、加熱溶融混
練するケイ砂微粉量を50部以下としたところ、各
実施例に較べて塗膜の平滑性、耐水性、耐沸とう
水性が共に低下した。一方、加熱溶融混練するケ
イ砂微粉量を上記の50部以下に代え120部以上と
したところ、上記塗膜の平滑性、耐水性、耐沸と
う水性は120部のものとほとんど異なるところが
なく、これら特性の向上は飽和状態となつた。
The present invention relates to an epoxy resin powder coating that is inexpensive and has excellent coating film performance such as impact resistance, abrasion resistance, smoothness, water resistance, and boiling water resistance. In general, silica-based inorganic fillers are known as materials that improve performance such as impact resistance and abrasion resistance of paint films, and are effective in reducing paint costs. Also in epoxy resin powder coatings, it is effective to incorporate silica-based inorganic fillers to improve coating film performance and reduce coating costs as described above. In order to improve the impact resistance, abrasion resistance, water resistance, and boiling water resistance of epoxy resin powder coatings, and to significantly reduce the coating cost, the present inventors added 100 parts by weight of the above (A). Since we found that it is effective to mix 130 to 400 parts by weight of a silica-based inorganic filler to the paint, we investigated an effective method for producing the paint. In general, typical methods for producing powder coatings, particularly methods for mixing raw materials, include a melt-kneading method and a simple mixing method. Of course, in order to finally obtain a powder coating, it is necessary to add a process of pulverization and, if necessary, classification. The present inventors have found that in the case of epoxy resin powder coatings containing a large amount of the above-mentioned silica-based inorganic filler, the melt-kneading method can be used to improve the smoothness, water resistance, and boiling water resistance of the above-mentioned coating films. Although it is effective, it has been found that when the amount of silica-based inorganic filler blended reaches a certain amount, the above-mentioned improvement becomes smaller and becomes saturated. When melt-kneading more than a certain amount of silica-based inorganic filler, the hardness of the kneaded product increases due to the increased amount of silica-based inorganic filler, and the powder of the kneaded material for making powder coating increases. Moreover, there are disadvantages such as early wear and tear of the crusher. Therefore, as a result of intensive study on this point, the present inventors found that (A) a solid epoxy resin with a softening point of 60 to 150°C and an epoxy equivalent of 400 to 2000, (B) a curing agent,
(C) An epoxy resin powder coating consisting of 130 to 400 parts by weight of a silica-based inorganic filler per 100 parts by weight of (A) above, and (D) a coloring agent and/or extender pigment as necessary. In the composition, 50 to 120 parts by weight of (C)
A method for producing an epoxy resin powder coating characterized by mixing (A), (B), and (D), mixing, melt-kneading, crushing, and classifying the mixture with the remainder of (C) is extremely effective. I discovered something. According to experiments conducted by the present inventors, it has been found that it is effective to set the amount of silica-based inorganic filler used for melt-kneading to 50 to 120 parts by weight per 100 parts by weight of (A) above. There is. That is, if the amount is less than 50 parts by weight, the smoothness of the coating film will be insufficient. Furthermore, even if the amount of silica-based inorganic filler is melt-kneaded in excess of 120 parts by weight, the performance such as the smoothness of the coating film will not change significantly. part is sufficient. The solid epoxy resin (A) suitable for the present invention includes diglycidyl ethers such as bisphenol A, bisphenol F or tetrabromo bisphenol A, polyglycidyl ethers of phenol or cresol novolak, and modified epoxy resins thereof. Furthermore, conventional epoxy resins known as polyglycidyl ethers of polyhydric alcohols, polyglycidyl esters of polybasic acids, and modified epoxy resins thereof can be mentioned. On the other hand, the curing agent (B) suitable for the present invention includes:
A curing agent selected from known and commonly used curing agents such as amines and amine adducts, polyamides, polyamide adducts, acid group-containing polyesters, polyhydric carboxylic acids or anhydrides and modified products thereof, dicyandiamide and modified products thereof, imidazoles, etc. be. Further, as the silica-based inorganic filler (C), those commonly called quartz powder, silica sand, etc. can be used. As the colorant and/or extender (D), titanium oxide, carbon black, precipitated barium sulfate, talc, and other generally known color pigments, dyes, and extender pigments can be used. In addition, a flow control agent may be added as necessary to improve the surface condition of the coating film, such as orange peel and leveling properties. As a coating method for the paint, any powder coating method used for cast iron pipes, cast iron irregular shaped pipes, and cast iron valves can be applied, such as spray coating, electrostatic powder coating, and fluidized dipping coating. Hereinafter, the present invention will be specifically explained using examples. still,
"Parts" are expressed as "parts by weight." Example 1 Bisphenol A type epoxy resin with a softening point of 95°C and an epoxy equivalent of 900 (product name: Epotote)
YD-014 (manufactured by Toto Kasei Co., Ltd.) 100 parts, adipic acid dihydride 3 parts, imidazole 3 parts, titanium oxide 10 parts
After premixing 0.2 parts of Carbon Black, 0.5 parts of Modaflow (flow control agent: manufactured by Monsanto, USA), and 100 parts of silica sand fine powder (particle size of 100 μ or less, average particle size of 40 μ), Buss Co Kneader PR-46 (Switzerland) (manufactured by Kunibusu Co., Ltd.), heat, melt and knead, crush,
It was classified to prepare a powder with an average particle size of 40μ. This was mixed with 100 parts of fine silica sand to form a powder coating. Example 2 A powder coating material was prepared in exactly the same manner as in Example 1, except that the amount of fine silica sand was changed to 200 parts in the final mixing. Example 3 A powder coating was prepared in exactly the same manner as in Example 1, except that the amount of fine silica sand was changed to 300 parts in the final mixing. Comparative Example A powder coating was prepared in exactly the same manner as in Example 1, except that the entire amount of fine silica sand was simply mixed. The powder coatings prepared according to Examples 1 to 3 and Comparative Examples above were electrostatically applied to a steel plate preheated to 250°C.
Thereafter, it was left to cool to form a test piece with a film thickness of 500 to 800 μm, and the coating film performance was investigated. The results are shown in Table 1. In addition, for each of the above examples, the amount of silica sand fine powder added to the entire paint was the same, but when the amount of silica sand fine powder to be heated and melted and kneaded was 50 parts or less, the coating film was The smoothness, water resistance, and boiling water resistance were all reduced. On the other hand, when the amount of silica sand fine powder to be heat-melted and kneaded was changed to 120 parts or more instead of the above 50 parts or less, the smoothness, water resistance, and boiling water resistance of the coating film were almost the same as those of 120 parts. Improvements in these properties reached a saturated state.
【表】【table】
Claims (1)
2000の固形エポキシ樹脂、(B)硬化剤、(C)上記(A)の
100重量部に対して、130〜400重量部のシリカ系
無機質充てん材、(D)必要に応じて着色材及び／又
は体質顔料とからなるエポキシ樹脂系粉体塗料組
成物において、(C)の50〜120重量部を(A)、(B)並び
に(D)と混合、溶融混練、粉砕、分級したものに(C)
の残部を混合したことを特徴とするエポキシ樹脂
系粉体塗料。1 (A) Softening point is 60~150℃, epoxy equivalent is 400~
2000 solid epoxy resin, (B) hardening agent, (C) above (A)
In an epoxy resin powder coating composition consisting of 130 to 400 parts by weight of a silica-based inorganic filler, (D) a coloring agent and/or an extender pigment as necessary, based on 100 parts by weight, (C) 50 to 120 parts by weight of (A), (B), and (D) are mixed, melt-kneaded, crushed, and classified (C)
An epoxy resin powder coating characterized by mixing the remainder of.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP15560682A JPS5945366A (en) | 1982-09-06 | 1982-09-06 | Epoxy resin powder paint |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP15560682A JPS5945366A (en) | 1982-09-06 | 1982-09-06 | Epoxy resin powder paint |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5945366A JPS5945366A (en) | 1984-03-14 |
| JPS6228194B2 true JPS6228194B2 (en) | 1987-06-18 |
Family
ID=15609696
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP15560682A Granted JPS5945366A (en) | 1982-09-06 | 1982-09-06 | Epoxy resin powder paint |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5945366A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09226214A (en) * | 1996-02-27 | 1997-09-02 | Hokuriku Nippon Denki Software Kk | Informing system for printer information |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60226567A (en) * | 1984-04-26 | 1985-11-11 | Nippon Paint Co Ltd | Preparation of powder coating compound |
| US8258225B2 (en) * | 2000-12-08 | 2012-09-04 | Ppg Industries Ohio, Inc | Coating compositions providing improved mar and scratch resistance and methods of using the same |
-
1982
- 1982-09-06 JP JP15560682A patent/JPS5945366A/en active Granted
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09226214A (en) * | 1996-02-27 | 1997-09-02 | Hokuriku Nippon Denki Software Kk | Informing system for printer information |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5945366A (en) | 1984-03-14 |
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