JPH0733992A - Production of highly condensed thermosetting resin - Google Patents
Production of highly condensed thermosetting resinInfo
- Publication number
- JPH0733992A JPH0733992A JP18053793A JP18053793A JPH0733992A JP H0733992 A JPH0733992 A JP H0733992A JP 18053793 A JP18053793 A JP 18053793A JP 18053793 A JP18053793 A JP 18053793A JP H0733992 A JPH0733992 A JP H0733992A
- Authority
- JP
- Japan
- Prior art keywords
- thermosetting resin
- condensation
- resin
- highly condensed
- melamine resin
- 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
Landscapes
- Processes Of Treating Macromolecular Substances (AREA)
- Phenolic Resins Or Amino Resins (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、ゴム、プラスチックの
充填剤として有用である高縮合熱硬化性樹脂の製造方法
に関するもので、例えば、建築材料、塗料等に用いられ
る高縮合熱硬化性樹脂の製造方法に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a high-condensation thermosetting resin useful as a filler for rubbers and plastics, for example, a high-condensation thermosetting resin used in building materials, paints and the like. The present invention relates to a manufacturing method of.
【０００２】[0002]
【従来の技術】熱硬化性樹脂の高縮合物を得る方法とし
て、特公昭５７−２６６８６号公報では、尿素ホルムア
ルデヒド初期縮合物を濃縮し、無端ベルトに供給し固化
した後に、粉砕する方法が開示されている。しかしなが
ら、この無端ベルトで酸性溶液で固化、乾燥した場合、
メラミン樹脂等ではゲル化による固化が早すぎて全体
が、固化してしまい次工程での処理に多大な労力を要す
る。2. Description of the Related Art As a method for obtaining a highly condensate of a thermosetting resin, JP-B-57-266686 discloses a method of concentrating a urea-formaldehyde initial condensate, supplying it to an endless belt, solidifying it, and then pulverizing it. Has been done. However, when solidified and dried with an acid solution with this endless belt,
Melamine resin or the like solidifies too quickly due to gelation, and the whole solidifies, which requires a great deal of labor for treatment in the next step.
【０００３】また、従来から、熱硬化性樹脂であるメラ
ミン樹脂を高縮合する方法として、メラミン樹脂の初期
縮合物の粉末を加熱する方法が採用されている。この場
合、メラミン樹脂の初期縮合物は室温より２〜４時間で
１５０℃付近に加温される。しかし、縮合の際に、脱水
反応により生成した水が気泡となり、これが発泡し、加
熱前の体積に比較し約５０倍もの体積の嵩高な中空体と
なる。さらに、メラミン樹脂の初期縮合物の溶融が１０
０〜１５０℃で起こり、系全体が溶融し、固着して塊状
となる。塊状では取り扱いが不便なため、粉砕が必須と
なるが、この粉砕の際に、上記中空体は粘着性を有し、
粉砕に長時間を要する。Further, as a method of highly condensing a melamine resin which is a thermosetting resin, a method of heating a powder of an initial condensate of a melamine resin has been conventionally used. In this case, the initial condensate of the melamine resin is heated from room temperature to around 150 ° C in 2 to 4 hours. However, at the time of condensation, the water generated by the dehydration reaction becomes bubbles, which foam and become a bulky hollow body having a volume of about 50 times the volume before heating. Furthermore, the melting of the initial condensate of the melamine resin is 10
It occurs at 0 to 150 ° C., and the entire system melts and sticks to form a lump. Since lumpy is inconvenient to handle, crushing is essential, but at the time of this crushing, the hollow body has adhesiveness,
Milling takes a long time.
【０００４】[0004]
【発明が解決しようとする課題】本発明は上述の事実に
鑑みてなされたもので、その目的とするところは、メラ
ミン樹脂等の熱硬化性樹脂の初期縮合物を高縮合するに
際し、発泡させることなく、粉砕を必要としない高縮合
熱硬化性樹脂の製造方法を提供することにある。SUMMARY OF THE INVENTION The present invention has been made in view of the above-mentioned facts, and an object thereof is to foam an initial condensation product of a thermosetting resin such as a melamine resin during high condensation. It is to provide a method for producing a highly condensed thermosetting resin that does not require pulverization.
【０００５】[0005]
【課題を解決するための手段】本発明の高縮合熱硬化性
樹脂の製造方法は、熱硬化性樹脂の初期縮合物の粉末を
加熱して、高縮合熱硬化性樹脂を製造するにあたり、上
記熱硬化性樹脂の軟化点以下温度で、且つ、加熱速度が
２５℃／ｈｒ以下で加熱することを特徴とする。The method for producing a high-condensation thermosetting resin of the present invention comprises the steps of heating the powder of the initial condensation product of the thermosetting resin to produce a high-condensation thermosetting resin. It is characterized by heating at a temperature not higher than the softening point of the thermosetting resin and at a heating rate of 25 ° C./hr or lower.
【０００６】[0006]
【作用】本発明の製造方法では、熱硬化性樹脂の初期縮
合物の粉末に加熱する際に、熱硬化性樹脂の軟化点以下
温度で加熱速度が２５℃／ｈｒ以下で温度上昇させるの
で、粉末状態のままで高縮合が起こり、発泡したり、全
体が溶融、融着固化して塊となることを防止できる。In the production method of the present invention, when the powder of the precondensate of the thermosetting resin is heated, the temperature is raised below the softening point of the thermosetting resin at a heating rate of 25 ° C./hr or less. It is possible to prevent high condensation from occurring in a powder state, foaming, and melting and fusion solidification of the whole to form a lump.
【０００７】以下、本発明を詳細に説明する。本発明の
対象となる熱硬化性樹脂は、例えば、メラミン樹脂、グ
アナミン、フェノール樹脂、ユリア樹脂等の単独、変性
物が挙げられる。上記熱硬化性樹脂の初期縮合物の粉末
は、スプレードライヤー等を用いて作製される。The present invention will be described in detail below. Examples of the thermosetting resin which is a target of the present invention include melamine resins, guanamines, phenol resins, urea resins and the like, which are independent or modified products. The powder of the initial condensate of the thermosetting resin is produced by using a spray dryer or the like.
【０００８】本発明においては、上記熱硬化性樹脂の初
期縮合物の粉末を加熱する際に、上記熱硬化性樹脂の軟
化点以下の温度から、加熱速度が２５℃／ｈｒ以下で加
熱される。この加熱温度は、３〜２５℃／ｈｒが好まし
く、５〜２０℃／ｈｒがより好ましい。上記加熱速度が
２５℃／ｈｒを越える速さで加熱されると、同時に縮合
反応も生じ、この縮合による脱水した水の蒸発で著しい
発泡が起きる。上記加熱速度を２５℃／ｈｒ以下で行う
と、溶融状態を経ずに縮合により生じた水分が系外に放
出されて、不溶不融の高縮合熱硬化性樹脂が、発泡する
ことなく、粉のままで得られる。この加熱法としては、
限定はされず、例えば、熱風箱型乾燥機を用いる乾燥法
が挙げられる。In the present invention, when the powder of the precondensate of the thermosetting resin is heated, it is heated at a heating rate of 25 ° C./hr or less from a temperature below the softening point of the thermosetting resin. . The heating temperature is preferably 3 to 25 ° C / hr, more preferably 5 to 20 ° C / hr. When the heating rate is higher than 25 ° C./hr, a condensation reaction also occurs, and dehydration of water caused by this condensation causes remarkable foaming. When the heating rate is 25 ° C./hr or less, the water generated by the condensation is released to the outside of the system without passing through the molten state, and the insoluble and infusible highly condensed thermosetting resin does not foam and is powdered. It can be obtained as is. For this heating method,
The method is not limited, and examples thereof include a drying method using a hot air box dryer.
【０００９】例えば、熱硬化性樹脂がメラミン樹脂の場
合、当量比でメラミン１に対しホルムアルデヒドを１〜
３の比率で配合したメラミン樹脂の初期縮合物の粉末
は、１００℃付近で縮合が開始し出し、１５０℃まで加
熱すると縮合が終了する。この高縮合メラミン樹脂は、
メラミン樹脂の初期縮合物と比べ、加熱の際の重量減を
殆ど生じない粉末として得られる。For example, when the thermosetting resin is a melamine resin, formaldehyde is added in an amount of 1 to 1 of melamine in an equivalent ratio.
The powder of the initial condensate of the melamine resin blended in the ratio of 3 starts the condensation at around 100 ° C, and the condensation ends when heated to 150 ° C. This highly condensed melamine resin is
It is obtained as a powder which hardly causes a weight loss upon heating as compared with the initial condensate of melamine resin.
【００１０】[0010]
実施例１ メラミン２５．２ｋｇ、４０％のホルムアルデヒド３０
ｋｇ、水１２．４ｋｇ、及び４％のＮａＯＨ水溶液２０
ｇを６０リットルの反応槽で９５℃、２時間反応させた
後に、スプレードライヤーで乾燥し、メラミン樹脂の初
期縮合物の粉末を得た。この粉末の粒径は５０〜８０ミ
クロンであった。Example 1 Melamine 25.2 kg, 40% formaldehyde 30
kg, 12.4 kg of water, and 4% NaOH aqueous solution 20
After reacting g in a 60-liter reaction tank at 95 ° C. for 2 hours, it was dried with a spray dryer to obtain a powder of an initial condensate of a melamine resin. The particle size of this powder was 50-80 microns.
【００１１】このメラミン樹脂の初期縮合物の粉末１ｋ
ｇを５０×４０ｃｍ、深さ４ｃｍのステンレス製バット
に入れ、箱型熱風乾燥機に入れた。この箱型熱風乾燥機
の温度上昇を２０℃から１５０℃まで２４時間かけて直
線的に加温し、高縮合メラミン樹脂を得た。この際の、
加温速度は５．４℃／ｈｒであった。１００℃付近から
縮合が起こり、１５０℃で縮合は終了していた。得られ
た高縮合メラミン樹脂は、発泡がなく、白色の粉末であ
った。粒径を測定したところ、５０〜８０ミクロンで、
初期縮合物と同一でり、嵩比重は０．７であった。Powder 1k of the precondensate of this melamine resin
g was placed in a stainless steel vat having a size of 50 × 40 cm and a depth of 4 cm, and placed in a box-type hot air dryer. The temperature of the box-type hot air dryer was linearly heated from 20 ° C to 150 ° C over 24 hours to obtain a highly condensed melamine resin. At this time,
The heating rate was 5.4 ° C./hr. Condensation occurred from around 100 ° C, and the condensation was completed at 150 ° C. The obtained highly condensed melamine resin was a white powder without foaming. When the particle size was measured, it was 50-80 microns,
It was the same as the initial condensate and had a bulk specific gravity of 0.7.
【００１２】上記得られた高縮合メラミン樹脂は、１２
０℃、３時間加熱して後の、加熱減量は１％以下であ
り、原料として用いたメラミン樹脂の初期縮合物の粉末
の加熱減量は１２％であり、縮合が完結していることが
確認できた。The highly condensed melamine resin obtained above is 12
After heating at 0 ° C. for 3 hours, the heating loss was 1% or less, and the heating loss of the powder of the initial condensate of the melamine resin used as the raw material was 12%, confirming that the condensation was completed. did it.
【００１３】実施例２ 実施例１の温度上昇を２０℃から１５０℃まで１３時間
かけ、加温速度を１０℃／ｈｒとした以外は実施例１と
同様にして高縮合メラミン樹脂を得た。得られた高縮合
メラミン樹脂は実施例１同様、発泡がなく、白色の粉末
であった。粒径を測定したところ、５０〜８０ミクロン
であった。この高縮合メラミン樹脂は、１２０℃、３時
間加熱して後の、加熱減量は１％以下であった。Example 2 A highly condensed melamine resin was obtained in the same manner as in Example 1 except that the temperature rise in Example 1 was increased from 20 ° C. to 150 ° C. for 13 hours and the heating rate was 10 ° C./hr. The obtained highly condensed melamine resin was a white powder without foaming as in Example 1. The particle size was measured and found to be 50-80 microns. This highly condensed melamine resin had a heating loss of 1% or less after heating at 120 ° C. for 3 hours.
【００１４】実施例３ 実施例１の温度上昇を２０℃から１５０℃まで８時間か
け、加温速度を１６℃／ｈｒとした以外は実施例１と同
様にして高縮合メラミン樹脂を得た。得られた高縮合メ
ラミン樹脂は実施例１同様、発泡がなく、白色の粉末で
あった。粒径を測定したところ、５０〜８０ミクロンで
あった。この高縮合メラミン樹脂は、１２０℃、３時間
加熱して後の、加熱減量は１％以下であった。Example 3 A highly condensed melamine resin was obtained in the same manner as in Example 1 except that the temperature rise in Example 1 was increased from 20 ° C. to 150 ° C. for 8 hours and the heating rate was 16 ° C./hr. The obtained highly condensed melamine resin was a white powder without foaming as in Example 1. The particle size was measured and found to be 50-80 microns. This highly condensed melamine resin had a heating loss of 1% or less after heating at 120 ° C. for 3 hours.
【００１５】比較例１ 温度上昇を２０℃から１５０℃まで４時間かけ、加温速
度を３２．５℃／ｈｒとした以外は実施例１と同様にし
て縮合を行ったところ、約１２０℃付近から急激に発泡
し、バット上部よりあふれ出てしまった。この発泡物の
嵩比重は約０．０２であった。ハンマーミルを用いて粉
砕を試みたが、粘着性があり、１００ミクロン以下の粉
砕はできなかった。Comparative Example 1 Condensation was carried out in the same manner as in Example 1 except that the temperature was raised from 20 ° C. to 150 ° C. for 4 hours and the heating rate was 32.5 ° C./hr. Foamed rapidly from the top and overflowed from the top of the bat. The bulk specific gravity of this foam was about 0.02. An attempt was made to grind using a hammer mill, but it was sticky and could not be ground to less than 100 microns.
【００１６】[0016]
【発明の効果】本発明の製造方法によって、メラミン樹
脂等の熱硬化性樹脂の初期縮合物の粉末を、発泡させる
ことなく高縮合熱硬化性樹脂を得ることができる。得ら
れた高縮合熱硬化性樹脂の粒径が、熱硬化性樹脂の初期
縮合物とほぼ同一であるから粉砕を必要としない。According to the production method of the present invention, a highly condensed thermosetting resin can be obtained without foaming the powder of the initial condensation product of the thermosetting resin such as melamine resin. Since the particle size of the obtained high-condensation thermosetting resin is almost the same as that of the initial condensation product of the thermosetting resin, pulverization is not necessary.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 古屋 裕子 富山県婦負郡婦中町笹倉636 日産化学工 業株式会社富山工場内 (72)発明者 土田 美喜夫 富山県婦負郡婦中町笹倉636 日産化学工 業株式会社富山工場内 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Yuko Furuya 636 Sasara, Menaka-cho, Women-in-gun, Toyama Prefecture Nissan Chemical Industry Co., Ltd.Toyama Plant (72) Inventor Mikio Tsucha 636 Sasakura, Menaka-cho, Women-in-gun, Toyama Prefecture Nissan Chemical Industry Co., Ltd. Toyama Factory Co., Ltd.
Claims (2)
して、高縮合熱硬化性樹脂を製造するにあたり、上記熱
硬化性樹脂の軟化点以下温度で、且つ、加熱速度が２５
℃／ｈｒ以下で加熱することを特徴とする高縮合熱硬化
性樹脂の製造方法。1. When a powder of an initial condensate of a thermosetting resin is heated to produce a highly condensed thermosetting resin, the temperature is not higher than the softening point of the thermosetting resin and the heating rate is 25.
A method for producing a high-condensation thermosetting resin, which comprises heating at a temperature of not more than ° C / hr.
ことを特徴とする請求項１記載の高縮合熱硬化性樹脂の
製造方法。2. The method for producing a highly condensed thermosetting resin according to claim 1, wherein the thermosetting resin is a melamine resin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP05180537A JP3126267B2 (en) | 1993-07-22 | 1993-07-22 | Method for producing highly condensed melamine resin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP05180537A JP3126267B2 (en) | 1993-07-22 | 1993-07-22 | Method for producing highly condensed melamine resin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0733992A true JPH0733992A (en) | 1995-02-03 |
| JP3126267B2 JP3126267B2 (en) | 2001-01-22 |
Family
ID=16085006
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP05180537A Expired - Lifetime JP3126267B2 (en) | 1993-07-22 | 1993-07-22 | Method for producing highly condensed melamine resin |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3126267B2 (en) |
-
1993
- 1993-07-22 JP JP05180537A patent/JP3126267B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JP3126267B2 (en) | 2001-01-22 |
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