JP3951146B2 - Process for producing colorant composition for polyvinyl butyral interlayer film - Google Patents
Process for producing colorant composition for polyvinyl butyral interlayer film Download PDFInfo
- Publication number
- JP3951146B2 JP3951146B2 JP35479895A JP35479895A JP3951146B2 JP 3951146 B2 JP3951146 B2 JP 3951146B2 JP 35479895 A JP35479895 A JP 35479895A JP 35479895 A JP35479895 A JP 35479895A JP 3951146 B2 JP3951146 B2 JP 3951146B2
- Authority
- JP
- Japan
- Prior art keywords
- polyvinyl butyral
- parts
- interlayer film
- plasticizer
- colorant composition
- 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
Landscapes
- Joining Of Glass To Other Materials (AREA)
Description
【０００１】
【産業上の利用分野】
本発明はポリビニルブチラール中間膜用着色剤組成物の製造方法に関する。
【０００２】
【従来の技術】
従来より、２枚のガラス板の中間層として透明なポリビニルブチラールからなる中間膜をはさんだガラス板が、建物の窓ガラスや自動車のフロントガラス等に多用されている。この用途に使用されるポリビニルブチラール中間膜は、その全面または一部が油溶性染料や顔料で着色される場合が多いが、油溶性染料は耐候性が不十分で、且つガラス板の中間層に入る前の着色ポリビニルブチラール中間膜シート保存中に油溶性染料が表面に移行し、表面を汚染するといった欠点がある。一方、顔料は一部の顔料を除き、耐光性良好で、且つ顔料が表面に移行することもなく、油溶性染料が透明性で良好でヘーズ値が低いのに対し、顔料を用いて着色したポリビニルブチラール中間膜は透明性が悪くヘーズ値が高いという欠点がある
【０００３】
【発明が解決しようとする課題】
一般的に、ポリビニルブチラール中間膜の着色は、ポリビニルブチラール用可塑剤にあらかじめ顔料を分散し、その可塑剤をポリビニルブチラールに添加する方法により製造される。
本発明は、顔料をポリビニルブチラール用可塑剤にあらかじめ分散加工する過程での条件を限定することにより、ヘーズ値の低い透明性の勝れたポリビニルブチラール中間膜用着色剤組成物の製造方法を提供するものである。
【０００４】
【課題を解決するための手段】
本発明者らは上記の課題を解決すべく鋭意検討を重ねた結果、あらかじめ顔料とロジン変性マレイン酸樹脂を加熱・混練し、これをポリビニルブチラール用可塑剤に溶解したのち、ポリビニルブチラール樹脂に着色することによりヘーズ値の低い透明性の勝れた着色ポリビニルブチラール中間膜が出来ることを見出し、この発明を完成するに至った。
以下、本発明を詳細に説明する。
【０００５】
本発明に使用されるロジン変性マレイン酸樹脂は、ポリエステル樹脂の一種でロジンと無水マレイン酸からなり、多価アルコールでエステル化したものである。 本発明において使用される顔料は粒子径が０．１μｍ以下と粒子径が小さい、ヘーズ値の低い顔料の使用が望ましい。また、本発明において使用されるポリビニルブチラール用可塑剤としては、ジカルボン酸エステル類、ポリエーテルエステル類又は、それ等の混合物が挙げられる。
【０００６】
本発明のポリビニルブチラール中間膜用着色剤の製造方法としては、以下の方法が例示される。
ロジン変性マレイン酸樹脂１００重量部に対し、顔料１０〜２００重量部、好ましくは４０〜１００重量部をあらかじめタンブラー等で予備ブレンド後、９０〜１３０℃、好ましは１００〜１１０℃に加熱された三本ロール等で混練し、顔料を分散加工する。分散加工終了後冷却し、ハンマーミル等で粉砕したのちポリビニルブチラール用可塑剤を加えディスパー等でよく攪拌し溶解させる。
【０００７】
尚、顔料をあらかじめロジン変性マレイン酸樹脂で分散加工処理したものと、ポリビニルブチラール用可塑剤との比率は１００重量部：１００重量部から１００重量部：１０００重量部より好ましくは１００重量部：４００重量部から１００重量部：８００重量部が溶解速度や濃度の点で使用が容易である。
尚、可塑剤への溶解工程においてディスパー攪拌で溶解が不充分な場合は、更に、三本ロールまたはビーズミル等で分散加工すると容易に溶解することができる。
【０００８】
【発明の効果】
本発明の方法により、製造された組成物を用いてポリビニルブチラール樹脂を着色することによりヘーズ値の低い透明性の勝れたポリビニルブチラール中間膜フィルムが出来る。
【０００９】
【実施例】
以下、実施例により本発明を説明する。
但し、例中、 部とあるのは重量部を表す。
【実施例１】
銅フタロシアニンビルー４０部とロジン変性マレイン酸樹脂（マルキード＃２、荒川化学（株）製）６０部をタンブラーで２０分間予備ブレンドしたのち、１００〜１１０℃に加熱された三本ロールで混練分散させる。混練分散加工終了後、冷却したのちハンマーミルで粉砕し、この粉砕品１００部にポリビニルブチラール用可塑剤トリエチレングリコールジー（２−エチル）ブチレート（ポリエーテルエステル類）を７００部を加え、ディスパーにて３０分間攪拌溶解させる。若干未溶解物が残るため、密閉連続式のビーズミルに通すことにより完全溶解した銅フタロシアニンブルー５重量％の分散溶解液を得た。
【００１０】
【実施例２】
縮合多環系エロー、クロモフタールエロー２ＲＬＴ（チバガイギー（株）製）３０部とロジン変性マレイン酸樹脂（マルキード＃２、荒川化学（株）製）７０部をタンブラーで２０分間予備ブレンドしたのち、１００〜１１０℃に加熱された三本ロールで混練分散させる。混練分散加工終了後、冷却したのちハンマーミルで粉砕し、この粉砕品１００部にポリビニルブチラール用可塑剤トリエチレングリコールジー（２−エチル）ブチレート（ポリエーテルエステル類）５００部を加えディスパーにて３０分間攪拌溶解させる。若干未溶解物が残るため、三本ロールに通すことにより完全溶解したクロモフタールエロー２ＲＬＴ５重量％の分散溶解液を得た。
【００１１】
【比較例１】
実施例１と同じ銅フタロシアニンブルー４０部とポリビニルブチラール用可塑剤トリエチレングリコールジー（２−エチル）ブチレート（ポリエーテルエステル類）７６０部を加え、あらかじめディスパーにて３０分間攪拌したのち、密閉連続式のビーズミルを通し、銅フタロシアニンブルー５重量％の分散溶解液を得た。
【００１２】
【比較例２】
実施例２と同じ縮合多環系エロー，クロモフタールエロー２ＲＬＴ ３０部とポリビニルブチラール用可塑剤トリエチレングリコールジー（２−エチル）ブチレート（ポリエーテルエステル類）７０部をディスパーで２０分間予備ブレンドしたのち、三本ロールで混練分散させる。混練分散加工終了後、更にトリエチレングリコールジー（２−エチル）ブチレート（ポリエーテルエステル類）５００部を加え、希釈したのち再び三本ロールを通し、クロモフタールエロー２ＲＬＴ５重量％の分散溶解液を得た。
【００１３】
上記実施例１〜２，比較例１〜２で得られたポリビニルブチラール樹脂用顔料分散液を下記配合でラボプラストミル（東洋精機製）で混練後、０．５ｍｍシートに加圧プレスし、全自動ヘーズメーター（東京電色（株）製）にてヘーズ値を
測定した結果【表−１】の如くであった。
【００１４】
【表−１】
[Industrial application fields]
The present invention relates to a method for producing a colorant composition for a polyvinyl butyral interlayer film.
[0002]
[Prior art]
2. Description of the Related Art Conventionally, a glass plate sandwiching an intermediate film made of transparent polyvinyl butyral as an intermediate layer between two glass plates has been frequently used for building window glass, automobile windshields, and the like. The polyvinyl butyral interlayer used for this purpose is often colored entirely or partly with an oil-soluble dye or pigment, but the oil-soluble dye has insufficient weather resistance and is used as an intermediate layer of a glass plate. There is a drawback that the oil-soluble dye migrates to the surface during the storage of the colored polyvinyl butyral interlayer film sheet before entering and contaminates the surface. On the other hand, except for some pigments, the pigments were colored with the pigments, while the light resistance was good and the pigments did not migrate to the surface, and the oil-soluble dyes were transparent and good and had a low haze value. Polyvinyl butyral interlayers have the disadvantage of poor transparency and high haze values.
[Problems to be solved by the invention]
In general, the polyvinyl butyral interlayer is colored by a method in which a pigment is dispersed in advance in a plasticizer for polyvinyl butyral and the plasticizer is added to polyvinyl butyral.
The present invention provides a method for producing a colorant composition for a polyvinyl butyral interlayer film having a low haze value and excellent transparency by limiting the conditions in the process of dispersing the pigment in the plasticizer for polyvinyl butyral in advance. To do.
[0004]
[Means for Solving the Problems]
As a result of intensive studies to solve the above-mentioned problems, the present inventors previously heated and kneaded the pigment and rosin-modified maleic resin, dissolved this in a plasticizer for polyvinyl butyral, and then colored the polyvinyl butyral resin. As a result, it was found that a colored polyvinyl butyral interlayer having a low haze value and excellent transparency could be produced, and the present invention was completed.
Hereinafter, the present invention will be described in detail.
[0005]
The rosin-modified maleic resin used in the present invention is a kind of polyester resin, which is composed of rosin and maleic anhydride and esterified with a polyhydric alcohol. The pigment used in the present invention is preferably a pigment having a particle size of 0.1 μm or less and a small particle size and a low haze value. In addition, examples of the plasticizer for polyvinyl butyral used in the present invention include dicarboxylic acid esters, polyether esters, and mixtures thereof.
[0006]
The following method is illustrated as a manufacturing method of the coloring agent for polyvinyl butyral interlayer films of the present invention.
10 to 200 parts by weight, preferably 40 to 100 parts by weight of the pigment was preliminarily blended with a tumbler or the like, and heated to 90 to 130 ° C., preferably 100 to 110 ° C., with respect to 100 parts by weight of the rosin-modified maleic resin. The pigment is dispersed by kneading with three rolls. After the dispersion processing is completed, the mixture is cooled, pulverized with a hammer mill or the like, and then added with a plasticizer for polyvinyl butyral.
[0007]
In addition, the ratio of the pigment previously dispersed with rosin-modified maleic resin and the plasticizer for polyvinyl butyral is 100 parts by weight: 100 parts by weight to 100 parts by weight: more preferably 100 parts by weight: 400 parts by weight. From 100 parts by weight to 800 parts by weight is easy to use in terms of dissolution rate and concentration.
In the step of dissolving in a plasticizer, if the dissolution is insufficient by stirring with a disper, it can be easily dissolved by further dispersing with a three-roll or bead mill.
[0008]
【The invention's effect】
According to the method of the present invention, a polyvinyl butyral interlayer film having a low haze value and excellent transparency can be obtained by coloring the polyvinyl butyral resin using the produced composition.
[0009]
【Example】
Hereinafter, the present invention will be described by way of examples.
However, in the examples, “part” means part by weight.
[Example 1]
40 parts of copper phthalocyanine building and 60 parts of rosin-modified maleic resin (Marquide # 2, manufactured by Arakawa Chemical Co., Ltd.) are pre-blended for 20 minutes with a tumbler, and then kneaded and dispersed with three rolls heated to 100 to 110 ° C. . After completion of the kneading and dispersing process, the mixture is cooled and then pulverized with a hammer mill. To 100 parts of this pulverized product, 700 parts of a polyvinyl butyral plasticizer triethylene glycol di (2-ethyl) butyrate (polyetheresters) is added, and the disperser is added. And dissolve for 30 minutes. Since some undissolved material remained, a dispersion solution of 5% by weight of copper phthalocyanine blue completely dissolved was obtained by passing through a closed continuous bead mill.
[0010]
[Example 2]
After pre-blending 20 parts of condensed polycyclic yellow and chromoftal yellow 2RLT (manufactured by Ciba Geigy Co., Ltd.) and 70 parts of rosin-modified maleic resin (Marquide # 2, Arakawa Chemical Co., Ltd.) with a tumbler, The mixture is kneaded and dispersed with three rolls heated to 100 to 110 ° C. After completion of the kneading and dispersing process, the mixture is cooled and then pulverized by a hammer mill. To 100 parts of this pulverized product, 500 parts of a plasticizer for polyvinyl butyral, triethylene glycol di (2-ethyl) butyrate (polyetheresters) is added, and 30 parts are added using a disper. Dissolve with stirring for minutes. Since some undissolved material remained, a dispersion solution of 5% by weight of chromoftal yellow 2RLT completely dissolved by passing through a three roll was obtained.
[0011]
[Comparative Example 1]
40 parts of the same copper phthalocyanine blue as in Example 1 and 760 parts of a plasticizer for polyethylene butyral triethylene glycol di (2-ethyl) butyrate (polyetheresters) were added, and the mixture was stirred in advance with a disper for 30 minutes. The dispersion solution of copper phthalocyanine blue 5% by weight was obtained.
[0012]
[Comparative Example 2]
30 parts of the same condensed polycyclic yellow, chromofal yellow 2RLT as in Example 2 and 70 parts of a plasticizer for polyvinyl butyral triethylene glycol di (2-ethyl) butyrate (polyetheresters) were pre-blended with a disper for 20 minutes. After that, it is kneaded and dispersed with three rolls. After completion of the kneading and dispersing process, 500 parts of triethylene glycol di (2-ethyl) butyrate (polyetherester) is further added, diluted, and then passed through three rolls again to obtain a dispersion solution of 5% by weight of chromophal yellow 2RLT. Obtained.
[0013]
The polyvinyl butyral resin pigment dispersions obtained in Examples 1 and 2 and Comparative Examples 1 and 2 were kneaded with the Labo Plast Mill (manufactured by Toyo Seiki Co., Ltd.) with the following composition, and then press-pressed into 0.5 mm sheets. Table 1 shows the result of measuring the haze value with an automatic haze meter (manufactured by Tokyo Denshoku Co., Ltd.).
[0014]
[Table-1]
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP35479895A JP3951146B2 (en) | 1995-12-27 | 1995-12-27 | Process for producing colorant composition for polyvinyl butyral interlayer film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP35479895A JP3951146B2 (en) | 1995-12-27 | 1995-12-27 | Process for producing colorant composition for polyvinyl butyral interlayer film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH09183638A JPH09183638A (en) | 1997-07-15 |
| JP3951146B2 true JP3951146B2 (en) | 2007-08-01 |
Family
ID=18439981
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP35479895A Expired - Lifetime JP3951146B2 (en) | 1995-12-27 | 1995-12-27 | Process for producing colorant composition for polyvinyl butyral interlayer film |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3951146B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20200007207A (en) | 2018-07-12 | 2020-01-22 | 에스케이씨 주식회사 | Film for laminating glasses, laminated glasses comprising of the same and vehicle comprising of the same |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| MX2019011438A (en) * | 2017-03-31 | 2019-12-16 | Sekisui Chemical Co Ltd | Thermoplastic resin film and glass plate-containing laminate. |
-
1995
- 1995-12-27 JP JP35479895A patent/JP3951146B2/en not_active Expired - Lifetime
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20200007207A (en) | 2018-07-12 | 2020-01-22 | 에스케이씨 주식회사 | Film for laminating glasses, laminated glasses comprising of the same and vehicle comprising of the same |
| US11498313B2 (en) | 2018-07-12 | 2022-11-15 | Skc Co., Ltd. | Film for glass lamination, laminated glass comprising same, and transportation vehicle comprising laminated glass |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH09183638A (en) | 1997-07-15 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| TWI386462B (en) | Black enamel pigment | |
| CN101668812B (en) | Composition for producing heat-ray shielding vinyl chloride film, method for producing same, and heat-ray shielding vinyl chloride film | |
| JPH02199403A (en) | Color filter and its production | |
| JP2003522268A (en) | Color-stable colored polymer film | |
| CN101790462A (en) | Light-to-heat conversion layer incorporating modified pigments | |
| DE69736169T2 (en) | LIQUID CRYSTAL DISPLAY ELEMENT AND SPACER FOR THIS | |
| KR101582818B1 (en) | Pigment dispersion | |
| JP2619288B2 (en) | Manufacturing method of colored laminated glass | |
| JP3951146B2 (en) | Process for producing colorant composition for polyvinyl butyral interlayer film | |
| CN112004895A (en) | Alcohol-soluble printing ink composition | |
| DE69907980T2 (en) | Colored film | |
| CN1352597A (en) | Colored polyvinyl butyral interlayer with improved haze properties | |
| DE69719159T2 (en) | Brittle film made of acrylic resin | |
| JPH0584738A (en) | Production of colored intermediate film for safety glass and production of safety glass | |
| WO2000078873A1 (en) | Process for preparing green pigment composition containing no halogen | |
| WO2001042158A1 (en) | Dispersion composition of fine inorganic particles, composition for interlayer for laminated glass, interlayer, and laminated glass | |
| JPH03221571A (en) | Production of pigment ink | |
| JP3879444B2 (en) | Aqueous shading coating composition for display device and insulating shading film | |
| JPH0819366B2 (en) | Color chip manufacturing method | |
| JP2505285B2 (en) | Electrodeposition coating composition | |
| JP3861882B2 (en) | Coating composition | |
| TW200936704A (en) | Pigment dispersion | |
| CN110776778A (en) | Surface printing composite universal ink for plastic film and preparation method thereof | |
| JP3861881B2 (en) | Display coating composition | |
| JP2009144037A (en) | Tungsten oxide fine particle dispersion for resin addition, tungsten oxide fine particle dispersed vinyl chloride resin molded body, and method for producing tungsten oxide fine particle dispersed vinyl chloride resin molded body |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A977 | Report on retrieval |
Free format text: JAPANESE INTERMEDIATE CODE: A971007 Effective date: 20051118 |
|
| A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20060523 |
|
| A521 | Written amendment |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20060831 |
|
| TRDD | Decision of grant or rejection written | ||
| A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 Effective date: 20070320 |
|
| A61 | First payment of annual fees (during grant procedure) |
Free format text: JAPANESE INTERMEDIATE CODE: A61 Effective date: 20070411 |
|
| R150 | Certificate of patent or registration of utility model |
Free format text: JAPANESE INTERMEDIATE CODE: R150 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20110511 Year of fee payment: 4 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20120511 Year of fee payment: 5 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20120511 Year of fee payment: 5 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20130511 Year of fee payment: 6 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20130511 Year of fee payment: 6 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20140511 Year of fee payment: 7 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| EXPY | Cancellation because of completion of term |