JPH0456946B2 - - Google Patents
Info
- Publication number
- JPH0456946B2 JPH0456946B2 JP59204630A JP20463084A JPH0456946B2 JP H0456946 B2 JPH0456946 B2 JP H0456946B2 JP 59204630 A JP59204630 A JP 59204630A JP 20463084 A JP20463084 A JP 20463084A JP H0456946 B2 JPH0456946 B2 JP H0456946B2
- Authority
- JP
- Japan
- Prior art keywords
- liquid
- filler
- polyol blend
- rim
- supplied
- 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
- 239000007788 liquid Substances 0.000 claims description 40
- 239000000945 filler Substances 0.000 claims description 25
- 239000000203 mixture Substances 0.000 claims description 21
- 229920005862 polyol Polymers 0.000 claims description 21
- 150000003077 polyols Chemical class 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 9
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 8
- 239000003054 catalyst Substances 0.000 claims description 7
- 239000003431 cross linking reagent Substances 0.000 claims description 7
- 238000000465 moulding Methods 0.000 claims description 6
- 239000012948 isocyanate Substances 0.000 claims description 4
- 150000002513 isocyanates Chemical class 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 238000002347 injection Methods 0.000 claims description 3
- 239000007924 injection Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 2
- 239000012783 reinforcing fiber Substances 0.000 claims description 2
- 238000000926 separation method Methods 0.000 description 13
- 238000005188 flotation Methods 0.000 description 6
- 238000005259 measurement Methods 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000010107 reaction injection moulding Methods 0.000 description 1
- 210000003660 reticulum Anatomy 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/44—Resins; rubber; leather
- G01N33/442—Resins, plastics
Description
（産業上の利用分野）
本発明は、Ｒ−RIM用混合原料液の分析方法
の改良に関する。
（従来技術）
Ｒ−RIM（Reinforce−Reaction Injection
Mold）成形、つまり、補強繊維であるフイラー、
架橋剤、触媒を混合してなるポリオールブレンド
液と、イソシアネート成分液との反応射出成形に
おいては、とくにポリオールブレンド液の液管
理、とりわけ、変性の決め手となるOH基価と水
分の測定が重要である。
ところが、ポリオールブレンド液にはフイラー
が混入しており、このフイラーは、沈降性大のた
めにサンプリングの均一性が乏しくなるととも
に、自動水分測定における電気分解を妨害する。
従つて、分析前にポリオールブレンド液からフ
イラーを分離除去する必要がある。
そこで、この分離除去法としては、遠心分離法
や過法があるが、前者はOH基価に寄与する架
橋剤や触媒なども分離するので適正な分析ができ
ず、後者はポリオールブレンド液が高粘度である
こと、フイルターが目詰まりしやすいことなどか
ら迅速性に乏しいという問題があつた。
（発明の目的）
本発明は上記従来の問題点に鑑みてなされたも
ので、ポリオールブレンド液から架橋剤や触媒を
分離することなく、フイラーのみを迅速に分離除
去して、適正な分析を行なうようにすることを目
的とするものである。
（発明の構成）
このため本発明は、Ｒ−RIM成形機に供給す
べきポリオールブレンド液の一部を抜き取り、こ
れを50〜120℃に加熱したうえで下方から気泡を
供給し、フイラーを液表面に浮上させてフイラー
のみを分離除去し、ついで、この残留液を、OH
基価測定手段及び水分測定手段に供するようにし
たものである。
（発明の効果）
本発明によれば、ポリオールブレンド液を加熱
処理して粘性を下げつつ気泡を用いた浮選分離処
理するようにしたものであるから、フイラーのみ
が液表面に浮いて分離除去され、架橋剤や触媒は
分離されないので、この残留液で適正な分析が行
なえるようになる。
また、気泡によるフイラーの浮選分離プロセス
は、Ｒ−RIMプロセスと測定プロセスとの間に
組込むことができ、ポリオールブレンド液管理シ
ステムをオンライン化することが可能となる。
（実施例）
第１図に示すように、Ｒ−RIMプロセスは、
イソシアネート成分液１とポリオールブレンド液
２とをミキシングヘツド３で混合してウレタン化
反応を起こさせ、この混合液をＲ−RIM成形機
（不図示）に射出して製品（例えば自動車のボン
ネツト、フエンダーなど）を成形する。
一方、気泡によるフイラーの浮選分離プロセス
は、下部にガラスフイルター（５〜10μ孔）４
を、上部にすり合わせフランジ５を取付けた浮選
分離槽６が設けられ、該槽６の中段部分に、Ｒ−
RIM成形機に供給すべきポリオールブレンド液
２の一部を配管７で抜き取つて供給する。
該槽６内に供給されたポリオールブレンド液２
は、50〜120℃に加熱されて、粘度が200cps程度
に下げられる。
加熱温度が50℃未満では、ポリオールブレンド
液２の粘度が高く、フイラー９を浮選分離しにく
い。また、加熱温度が120℃を越えると、ポリオ
ールブレンド液２が変質するおそれがある。従つ
て、実用上は、インジエクシヨン温度が好まし
く、70〜100℃が好適である。
そして、この加熱状態下でガラスフイルター４
を通して槽６内に窒素ガス（N2）を送り込み、
窒素ガスによる多数の気泡（0.5mm以下）８を、
ポリオールブレンド液２中に懸濁しているフイラ
ー（10μφ、0.3mm）９に付着させて、気泡８の浮
力でフイラー９を液表面に浮き上がらせ、ポリオ
ールブレンド液２からフイラー９のみを迅速に分
離除去する。
この浮選分離プロセスにおいては、フイラー９
のみが分離され、架橋剤や触媒は分離されない。
フイラー９の分離のための時間は、第２図に示
すように、約４分で100％の分離が可能であつた。
次に、測定プロセスは、自動水分測定計１０と
OH基価測定フラスコ１１とが設けられ、該測定
フラスコ１１に、上記槽６の下段部分から残留液
２′を配管１２で抜き取つて計量バルブ１３で計
量した後に供給し、公知の方法で水分とOH基価
の測定を行なう。
上記各プロセスによりフイラー９を分離除去し
た後の残留液２′のOH基価と水分の測定結果を
第１表に示す。
(Industrial Application Field) The present invention relates to an improvement in a method for analyzing a mixed raw material liquid for R-RIM. (Prior art) R-RIM (Reinforce-Reaction Injection)
Mold) molding, that is, filler which is reinforcing fiber,
In reaction injection molding of a polyol blend liquid made by mixing a crosslinking agent and catalyst with an isocyanate component liquid, it is especially important to control the polyol blend liquid, and in particular, measure the OH group value and water content, which are the deciding factors for modification. be. However, filler is mixed in the polyol blend liquid, and this filler has a high sedimentation property, leading to poor sampling uniformity and interfering with electrolysis in automatic moisture measurement. Therefore, it is necessary to separate and remove the filler from the polyol blend liquid before analysis. Therefore, there are centrifugation methods and filtration methods to separate and remove this, but the former separates crosslinking agents and catalysts that contribute to the OH group value, making it impossible to perform proper analysis, and the latter, when the polyol blend liquid has a high There was a problem of poor speed due to the high viscosity and easy clogging of the filter. (Purpose of the Invention) The present invention has been made in view of the above-mentioned conventional problems, and it is an object of the present invention to quickly separate and remove only the filler without separating the crosslinking agent or catalyst from the polyol blend liquid, and perform appropriate analysis. The purpose is to do so. (Structure of the Invention) For this reason, the present invention extracts a part of the polyol blend liquid to be supplied to the R-RIM molding machine, heats it to 50 to 120°C, and then supplies air bubbles from below to make the filler into liquid. Only the filler is separated and removed by floating it to the surface, and then this residual liquid is treated with OH
It is adapted to serve as a base value measuring means and a moisture measuring means. (Effects of the Invention) According to the present invention, since the polyol blend liquid is heated to lower its viscosity and subjected to flotation separation using air bubbles, only the filler floats on the liquid surface and is separated and removed. Since the crosslinking agent and catalyst are not separated, this residual liquid can be used for proper analysis. Additionally, a bubble-based filler flotation separation process can be incorporated between the R-RIM process and the measurement process, allowing the polyol blend liquid management system to be brought online. (Example) As shown in Figure 1, the R-RIM process is
The isocyanate component liquid 1 and the polyol blend liquid 2 are mixed in the mixing head 3 to cause a urethane reaction, and this mixed liquid is injected into an R-RIM molding machine (not shown) to form products (such as automobile bonnets and fenders). etc.). On the other hand, the flotation separation process of filler by air bubbles uses a glass filter (5~10μ holes) 4 at the bottom.
A flotation separation tank 6 is provided with a grinding flange 5 attached to the top, and in the middle part of the tank 6, R-
A part of the polyol blend liquid 2 to be supplied to the RIM molding machine is extracted through piping 7 and supplied. Polyol blend liquid 2 supplied into the tank 6
is heated to 50-120°C to reduce the viscosity to about 200 cps. If the heating temperature is less than 50°C, the viscosity of the polyol blend liquid 2 will be high, making it difficult to flotate and separate the filler 9. Moreover, if the heating temperature exceeds 120° C., there is a risk that the polyol blend liquid 2 will change in quality. Therefore, in practice, the injection temperature is preferably 70 to 100°C. Then, under this heating condition, the glass filter 4
Nitrogen gas (N 2 ) is sent into the tank 6 through the
A large number of bubbles (0.5 mm or less) 8 caused by nitrogen gas,
It is attached to the filler (10 μφ, 0.3 mm) 9 suspended in the polyol blend liquid 2, and the filler 9 is lifted to the liquid surface by the buoyancy of the bubbles 8, and only the filler 9 is quickly separated and removed from the polyol blend liquid 2. do. In this flotation separation process, filler 9
The crosslinking agent and catalyst are not separated. As shown in FIG. 2, the separation time for filler 9 was about 4 minutes, and 100% separation was possible. Next, the measurement process starts with the automatic moisture meter 10.
A residual liquid 2' is extracted from the lower part of the tank 6 through a pipe 12, and after being measured with a measuring valve 13, the residual liquid 2' is supplied to the measuring flask 11 by a known method. and measure the OH value. Table 1 shows the measurement results of the OH group value and water content of the residual liquid 2' after the filler 9 was separated and removed by each of the above processes.
【表】
分離時間が０分では、フイラー９が一部沈降し
ているので、OH基価は高くでている。
分離時間が１〜３分では、フイラー９が分離さ
れたものとして分析しているのでOH基価は少な
くでている。
比較のために、遠心分離法によりフイラー９を
分離除去した場合のOH基価と水分の測定結果を
第２表に示す。[Table] When the separation time is 0 minutes, the filler 9 has partially settled, so the OH value appears high. When the separation time is 1 to 3 minutes, the OH group value is small because the filler 9 is analyzed as being separated. For comparison, Table 2 shows the measurement results of the OH group value and water content when the filler 9 was separated and removed by centrifugation.
【表】【table】
【表】
分離時間が長くなるほど、OH基価に寄与する
架橋剤や触媒が著しく分離されることが明らかで
ある。[Table] It is clear that the longer the separation time, the more the crosslinking agent and catalyst that contribute to the OH group value are separated.
第１図はポリオールブレンド液の管理システム
図、第２図は分離時間とフイラー分離率との関係
を示すグラフである。
１……イソシアネート成分液、２……ポリオー
ルブレンド液、２′……残留液、６……浮選分離
槽、９……フイラー、１０……自動水分測定計、
１１……OH基価測定フラスコ。
FIG. 1 is a diagram of a management system for a polyol blend liquid, and FIG. 2 is a graph showing the relationship between separation time and filler separation rate. 1... Isocyanate component liquid, 2... Polyol blend liquid, 2'... Residual liquid, 6... Flotation separation tank, 9... Filler, 10... Automatic moisture meter,
11...OH group measurement flask.
Claims (1)
合してなるポリオールブレンド液と、イソシアネ
ート成分液とを反応射出成形するＲ−RIM成形
に用いる前記ポリオールブレンド液の分析方法で
あつて、 Ｒ−RIM成形機に供給すべき前記ポリオール
ブレンド液の一部を抜き取り、 これを50〜120℃に加熱したうえで下方から気
泡を供給し、フイラーを液表面に浮上させてフイ
ラーのみを分離除去し、 ついで、この残留液を、OH基価測定手段及び
水分測定手段に供するようにしたことを特徴とす
るＲ−RIM用混合原料液の分析方法。[Scope of Claims] 1. A method for analyzing the polyol blend liquid used in R-RIM molding in which a polyol blend liquid formed by mixing a filler that is a reinforcing fiber, a crosslinking agent, and a catalyst and an isocyanate component liquid are reaction injection molded. A portion of the polyol blend liquid to be supplied to the R-RIM molding machine is extracted, heated to 50 to 120°C, and bubbles are supplied from below to float the filler to the liquid surface, leaving only the filler alone. 1. A method for analyzing a mixed raw material liquid for R-RIM, characterized in that: the residual liquid is separated and removed, and then this residual liquid is subjected to an OH group value measuring means and a moisture measuring means.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP20463084A JPS6182164A (en) | 1984-09-28 | 1984-09-28 | Analysis for mixed raw material liquid for r-rim |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP20463084A JPS6182164A (en) | 1984-09-28 | 1984-09-28 | Analysis for mixed raw material liquid for r-rim |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6182164A JPS6182164A (en) | 1986-04-25 |
| JPH0456946B2 true JPH0456946B2 (en) | 1992-09-10 |
Family
ID=16493651
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP20463084A Granted JPS6182164A (en) | 1984-09-28 | 1984-09-28 | Analysis for mixed raw material liquid for r-rim |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6182164A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5756004A (en) * | 1980-09-24 | 1982-04-03 | Hitachi Ltd | Bubble separator |
| JPS59142261A (en) * | 1983-02-02 | 1984-08-15 | Hitachi Chem Co Ltd | Room-temperature curable traffic paint |
| JPS59145145A (en) * | 1983-02-09 | 1984-08-20 | 株式会社リコー | Mat film |
-
1984
- 1984-09-28 JP JP20463084A patent/JPS6182164A/en active Granted
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5756004A (en) * | 1980-09-24 | 1982-04-03 | Hitachi Ltd | Bubble separator |
| JPS59142261A (en) * | 1983-02-02 | 1984-08-15 | Hitachi Chem Co Ltd | Room-temperature curable traffic paint |
| JPS59145145A (en) * | 1983-02-09 | 1984-08-20 | 株式会社リコー | Mat film |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6182164A (en) | 1986-04-25 |
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