JP3411645B2 - Method for measuring additive content in polyolefin - Google Patents
Method for measuring additive content in polyolefinInfo
- Publication number
- JP3411645B2 JP3411645B2 JP27759893A JP27759893A JP3411645B2 JP 3411645 B2 JP3411645 B2 JP 3411645B2 JP 27759893 A JP27759893 A JP 27759893A JP 27759893 A JP27759893 A JP 27759893A JP 3411645 B2 JP3411645 B2 JP 3411645B2
- Authority
- JP
- Japan
- Prior art keywords
- light
- polyolefin
- additive
- content
- measuring
- 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 - Fee Related
Links
Landscapes
- Investigating Or Analysing Materials By Optical Means (AREA)
- Extrusion Moulding Of Plastics Or The Like (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Description
【発明の詳細な説明】
【０００１】
【産業上の利用分野】本発明は、押出機から押し出され
たポリオレフィン中の添加剤の含有量を測定する方法に
係り、特に、微量添加剤成分の定量を連続的にかつ高精
度で求めることができる測定方法に関するものである。
【０００２】
【従来の技術】従来、押出機から押し出されたポリオレ
フィン中の添加剤の含有量を測定するには、例えばケー
ブル製造を例にとると、押出機に投入する樹脂ペレット
を抜き取り、ケーブル製造とは別のラインで薄いフィル
ム状に成形した後、赤外吸収スペクトルを測定すること
などで行っていた。
【０００３】
【発明が解決しようとする課題】ところが、添加剤含有
量の測定をケーブル製造とは別のラインで行ったので
は、含有量の把握が間接的となるため、実際に製造され
たケーブル中の添加剤含有量が所望通り適正な含有量で
あるか否かが正確に確定できないという問題があった。
また、赤外吸収スペクトル法では、目的とする添加剤以
外のポリオレフィンそのものの吸収強度が大きく、赤外
光を透過させる試料厚さ（パスレングス）が２ｍｍ程度
までしかとれないという問題もあった。この２ｍｍ程度
のパスレングスは、押出機の樹脂流路幅に比べて非常に
狭く、ケーブルのようなポリオレフィン流路幅の大きい
ものに対しては対応できないとい問題があった。また、
押出機の流路内に２ｍｍ程度のパスレングス測定部を設
けても、溶融粘度の高いポリオレフィンでは、周囲に比
べて測定部の通過抵抗が大きくなるため、やはりうまく
添加剤含有量が測定できないという問題があった。
【０００４】
【課題を解決するための手段】本発明は、このような従
来の実情に鑑みてなされたもので、その特徴とする点
は、ポリオレフィンが押し出される押出機に、少なくと
も投光用窓部分と受光用窓部分がガラス製の光透過材料
で構成された接続管路を直結させて透光部を設けると共
に、当該透光部の外周には加熱手段を設け、さらに前記
透光部の一方には投光用光源を設置して分光された波長
が１０００〜２５００ｎｍ未満の光を前記接続管路内の
ポリオレフィン流路中に入光させると共に、他方には受
光器を設置して前記入光の透過光を受光させる一方、前
記ポリオレフィン流路部分の透光部における温度を、当
該ポリオレフィンの融点以上に保って行うことにより、
添加剤含有量を求めることを特徴とするポリオレフィン
中の添加剤含有量測定方法にある。
【０００５】
【作用】このように押出機に接続管路を直結させて透光
部を設けることにより、押し出しポリオレフィンの全量
に対して、連続的に添加剤含有量の測定が可能となると
同時に、入光の波長を１０００〜２５００ｎｍ未満に設
定することにより、光の吸収減衰を防止し、より大きな
ポリオレフィン流路幅に対応することができる。また、
ポリオレフィン流路部分の透光部における温度を、透光
部の外周に設けた加熱手段で、ポリオレフィンの融点以
上に保つことにより、光散乱による影響を最小限に抑え
て、より高精度での測定を行うことができる。
【０００６】
【実施例】図１は、本発明に係るポリオレフィン中の添
加剤含有量測定方法を実施するための装置系の一実施例
を示した概略説明図である。図において、１は押出機
で、これには、ポリオレフィンのペレットが供給され、
その内部で加熱溶融された上記ポリオレフィンが内部ス
クリュウの回転により、図中左端から連続して押し出さ
れる。この押出機１の左端には、ポリオレフィン中の添
加剤含有量を測定するための透光部２が設けてあり、こ
の先には、ケーブル製造用のダイなどが設置される。
【０００７】上記透光部２は、接続管路３で形成され、
この接続管路３は、当該管路全体を石英ガラスなどの光
透過性部材で構成するか、あるいは少なくとも投光用窓
３ａ部分と受光用窓３ｂ部分をやはり石英ガラスなどの
光透過性部材で構成する。そして、上記投光用窓３ａ側
には、投光用光源４と回析格子５を設置して、この投光
用光源４からの光を回析格子５により分光させ、その波
長を１０００〜２５００ｎｍ未満の光として、上記接続
管路３中を流れるポリオレフィン流路Ｐ中に入光させる
と共に、上記受光用窓３ｂ側には、分光スペクトル装置
側の受光器６を設置して、上記ポリオレフィン流路Ｐ中
に入光された光の透過光を受光する。この受光量の変化
により、ポリオレフィン中に含まれる添加剤含有量を求
めることができる。
【０００８】上記入光の波長を１０００〜２５００ｎｍ
未満とするのは、測定光を赤外光（波長約２５００〜２
５０００ｎｍ程度）により短くして、光の吸収減衰をな
るべく小さくするためである。
【０００９】さらに、上記分光スペクトルの測定時、透
光部２に電熱ヒーターなどの加熱手段７を設け、この透
光部２におけるポリオレフィンの温度を、当該ポリオレ
フィンの融点以上、例えばポリエチレンでは１１０℃以
上、ポリプロピレンでは１６０℃以上に保って行うと、
結晶部の融解によるポリマーの均一化などの理由によ
り、光散乱の影響が受けにくくなり、より良好な光の透
過率が得られる。このため、より高精度での添加剤含有
量が求められる。
【００１０】因に、表１に示した試料（ポリエチレン）
について、本発明に係る測定方法による実施例１〜４の
場合と、本発明条件を欠く方法による比較例１の場合と
を比べると、同表の如き添加剤（老化防止剤）の測定値
が得られた。
【００１１】
【表１】【００１２】この表１から、ポリエチレンにおいて、波
長が１０００〜２５００ｎｍ未満で、透光部のポリエチ
レン流路温度を当該ポリエチレンの融点（１１０℃）以
上である１２０℃とした場合（実施例１〜３）、極めて
精度の高い添加剤含有量の値が得られることが判る。ま
た、波長が１０００〜２５００ｎｍ未満であっても、透
光部のポリエチレン流路温度を当該ポリエチレンの融点
以下である１００℃とした場合（実施例４）、実用可能
な値が得られるものの、測定精度が少々低下することが
判る。これに対して、波長が＞２５００（注、２５００
を越える大きさ）〜１４０００ｎｍで、本発明の設定値
より長い場合（比較例１）には、ポリエチレン流路幅が
上記各実施例１〜４の半分の値（２５ｍｍ）で、かつ流
路温度が１２０℃であっても、添加剤含有量が測定不能
であることが判る。
【００１３】
【発明の効果】以上の説明から明らかなように本発明に
係るポリオレフィン中の添加剤含有量測定方法によれ
ば、次のような優れた効果が得られる。
（１）先ず、透光部が押出機に少なくとも投光用窓部分
と受光用窓部分がガラス製の光透過材料で構成された接
続管路として直結されて設けてあるため、押し出しポリ
オレフィンの全量、すなわちケーブルにあってはケーブ
ルの全長にわたって、連続的にかつ直接的に添加剤含有
量を測定することができる。
（２）また、入光の波長を１０００〜２５００ｎｍ未満
に設定してあるため、光の吸収減衰が小さく、より大き
なポリオレフィン流路幅、例えばケーブル製造時のポリ
オレフィン絶縁層に十分対応することができる。
（３）さらに、ポリオレフィン流路部分の透光部におけ
る温度を、透光部の外周に設けた加熱手段で、ポリオレ
フィンの融点以上に保てば、光散乱による影響を最小限
に抑えることができるため、より高精度での測定を行う
ことができる。Description: BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for measuring the content of an additive in a polyolefin extruded from an extruder, and more particularly, to the determination of a trace amount of an additive component. And a measurement method capable of continuously and highly accurately obtaining the same. [0002] Conventionally, in order to measure the content of additives in polyolefin extruded from an extruder, for example, in the case of manufacturing a cable, resin pellets to be put into the extruder are extracted and the After forming into a thin film on a separate line from the production, the infrared absorption spectrum is measured and the like. [0003] However, if the measurement of the additive content is performed on a separate line from the cable production, the content of the additive is indirectly grasped. There was a problem that it was not possible to accurately determine whether the additive content in the cable was an appropriate content as desired.
Further, in the infrared absorption spectrum method, there is also a problem that the absorption intensity of the polyolefin itself other than the target additive is large, and the sample thickness (pass length) for transmitting infrared light can be only up to about 2 mm. The pass length of about 2 mm is very narrow as compared with the resin flow path width of the extruder, and there is a problem that it cannot cope with a large polyolefin flow path width such as a cable. Also,
Even if a pass length measuring section of about 2 mm is provided in the flow path of the extruder, the passivation resistance of the measuring section is higher than that of the surroundings in the case of polyolefin having a high melt viscosity, so that the additive content cannot be measured properly. There was a problem. SUMMARY OF THE INVENTION The present invention has been made in view of such conventional circumstances, and is characterized in that an extruder from which polyolefin is extruded is at least provided with an extruder.
Light-transmitting material made of glass for the light-emitting window and light-receiving window
When the light transmitting part is provided by directly connecting the connecting
In addition, a heating means is provided on the outer periphery of the light-transmitting portion, and a light source for projection is installed on one of the light-transmitting portions, and light having a wavelength of less than 1000 to 2500 nm is dispersed in the connection conduit. <br/> While allowing light to enter the polyolefin flow path, a light receiver is installed on the other side to receive the transmitted light of the incoming light, and
The temperature in the light-transmitting part of the polyolefin flow path
By performing at a temperature higher than the melting point of the polyolefin ,
A method for measuring the content of an additive in a polyolefin, comprising determining the content of the additive. [0005] By providing a light transmitting portion by directly connecting the connecting pipe line to the extruder, it is possible to continuously measure the additive content with respect to the total amount of extruded polyolefin. By setting the wavelength of incoming light to less than 1000 to 2500 nm, light absorption and attenuation can be prevented, and a larger polyolefin flow path width can be accommodated. Also,
The temperature in the light- transmitting part of the polyolefin flow path
By maintaining the temperature at or above the melting point of the polyolefin by the heating means provided on the outer periphery of the portion, the influence of light scattering can be minimized, and the measurement can be performed with higher accuracy. FIG. 1 is a schematic explanatory view showing one embodiment of an apparatus system for carrying out a method for measuring the content of an additive in a polyolefin according to the present invention. In the figure, 1 is an extruder, which is supplied with polyolefin pellets,
The polyolefin heated and melted therein is continuously extruded from the left end in the figure by rotation of the internal screw. At the left end of the extruder 1, a light transmitting section 2 for measuring the additive content in the polyolefin is provided, and a die or the like for manufacturing a cable is provided ahead of the light transmitting section 2. The light transmitting portion 2 is formed by a connecting conduit 3.
In the connection pipe 3, the entire pipe is made of a light transmitting member such as quartz glass, or at least the light projecting window 3a and the light receiving window 3b are made of a light transmitting member such as quartz glass. Constitute. On the side of the light projecting window 3a, a light projecting light source 4 and a diffraction grating 5 are installed, and the light from the light projecting light source 4 is split by the diffraction grating 5, and its wavelength is 1000 to 1000. Light having a wavelength of less than 2500 nm enters the polyolefin flow path P flowing through the connection conduit 3, and a light-receiving device 6 on the side of the spectral spectrum device is installed on the light-receiving window 3b side. The transmitted light of the light incident on the path P is received. From the change in the amount of received light, the content of the additive contained in the polyolefin can be determined. The wavelength of the incident light is 1000 to 2500 nm.
The reason for making the measurement light less than that is that the measurement light is infrared light (wavelength of about 2500 to 2
(About 5000 nm) in order to minimize light absorption attenuation. Further, at the time of measuring the above-mentioned spectral spectrum, a heating means 7 such as an electric heater is provided in the light transmitting section 2 so that the temperature of the polyolefin in the light transmitting section 2 is higher than the melting point of the polyolefin, for example, 110 ° C. or higher in the case of polyethylene. , For polypropylene, if it is kept above 160 ° C,
Due to the homogenization of the polymer due to the melting of the crystal part, it is hardly affected by light scattering, and a better light transmittance can be obtained. For this reason, a more precise additive content is required. [0010] The samples shown in Table 1 (polyethylene)
About the case of Examples 1 to 4 by the measuring method according to the present invention and the case of Comparative Example 1 by the method lacking the conditions of the present invention, the measured values of the additives (antiaging agents) as shown in the table are Obtained. [Table 1] From Table 1, it can be seen that, in the case of polyethylene, the wavelength is less than 1000 to 2500 nm and the temperature of the polyethylene channel in the light transmitting portion is 120 ° C., which is higher than the melting point (110 ° C.) of the polyethylene (Examples 1 to 3). ), It can be seen that an extremely accurate value of the additive content can be obtained. In addition, even when the wavelength is less than 1000 to 2500 nm, when the temperature of the polyethylene channel in the light transmitting portion is set to 100 ° C. which is equal to or lower than the melting point of the polyethylene (Example 4), a practical value is obtained, but the measurement is performed. It can be seen that the accuracy is slightly reduced. In contrast, wavelengths> 2500 (note 2500
In the case where the width is larger than the set value of the present invention (Comparative Example 1), the width of the polyethylene channel is half (25 mm) of each of Examples 1 to 4 and the channel temperature is Is 120 ° C., the additive content cannot be measured. As apparent from the above description, the following excellent effects can be obtained by the method for measuring the content of an additive in a polyolefin according to the present invention. (1) First, the light- transmitting part should be at least a light- transmitting window part in the extruder.
The light receiving window is made of glass light transmitting material.
Since it is provided directly as a continuous line, the total amount of extruded polyolefin, that is, in the case of a cable, the additive content can be continuously and directly measured over the entire length of the cable. (2) In addition, since the wavelength of incident light is set to be less than 1000 to 2500 nm, light absorption attenuation is small, and it can sufficiently cope with a larger polyolefin channel width, for example, a polyolefin insulating layer at the time of manufacturing a cable. can do. (3) Further, if the temperature of the light transmitting portion of the polyolefin flow path portion is maintained at a temperature equal to or higher than the melting point of the polyolefin by the heating means provided on the outer periphery of the light transmitting portion, the influence of light scattering can be minimized. Therefore, the measurement can be performed with higher accuracy.
【図面の簡単な説明】
【図１】本発明に係るポリオレフィン中の添加剤含有量
測定方法を実施するための装置系を示した部分縦断概略
説明図である。
【符号の説明】
１ 押出機
２ 透光部
３ 接続管路
３ａ 投光用窓
３ｂ 受光用窓
４ 投光用光源
５ 回析格子
６ 受光器
７ 加熱手段
Ｐ ポリオレフィン流路BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a schematic partial longitudinal sectional view showing an apparatus system for carrying out a method for measuring an additive content in a polyolefin according to the present invention. [Description of Signs] 1 Extruder 2 Light-transmitting part 3 Connection conduit 3a Light-emitting window 3b Light-receiving window 4 Light-emitting source 5 Diffraction grating 6 Light-receiving device 7 Heating means P Polyolefin flow path
───────────────────────────────────────────────────── フロントページの続き (72)発明者 長谷川 正一 東京都江東区木場１丁目５番１号 株式 会社フジクラ内 (56)参考文献 特開 平１−265140（ＪＰ，Ａ) Ａｎａｌｕｓｉｓ，フランス，1982 年，Ｖｏｌ．10，Ｎｏ．４，ｐｐ．166 −171 Ａｎａｌｕｓｉｓ，フランス，1990 年，Ｖｏｌ．18，Ｎｏ．５，ｐｐ．310 −312 (58)調査した分野(Int.Cl.7，ＤＢ名) G01N 21/00 - 21/01 G01N 21/17 - 21/61 ＪＩＣＳＴファイル（ＪＯＩＳ) 実用ファイル（ＰＡＴＯＬＩＳ) 特許ファイル（ＰＡＴＯＬＩＳ)────────────────────────────────────────────────── ─── Continuation of front page (72) Inventor Shoichi Hasegawa 1-5-1, Kiba, Koto-ku, Tokyo Inside Fujikura Co., Ltd. (56) References JP-A-1-265140 (JP, A) Analusis, France, 1982, Vol. 10, No. 4, pp. 166-171 Analussis, France, 1990, Vol. 18, No. 5, pp. 310-312 (58) Fields investigated (Int. Cl. 7 , DB name) G01N 21/00-21/01 G01N 21/17-21/61 JICST file (JOIS) Practical file (PATOLIS) Patent file (PATOLIS)
Claims (1)
に、少なくとも投光用窓部分と受光用窓部分がガラス製
の光透過材料で構成された接続管路を直結させて透光部
を設けると共に、当該透光部の外周には加熱手段を設
け、さらに前記透光部の一方には投光用光源を設置して
分光された波長が１０００〜２５００ｎｍ未満の光を前
記接続管路内のポリオレフィン流路中に入光させると共
に、他方には受光器を設置して前記入光の透過光を受光
させる一方、前記ポリオレフィン流路部分の透光部にお
ける温度を、当該ポリオレフィンの融点以上に保って行
うことにより、添加剤含有量を求めることを特徴とする
ポリオレフィン中の添加剤含有量測定方法。(57) [Claims] [Claim 1] Extruder from which polyolefin is extruded
In addition, at least the light emitting window and the light receiving window are made of glass.
The light transmission part is directly connected to the connection pipe made of the light transmission material.
And a heating means on the outer periphery of the light transmitting portion.
In addition, a light source for light projection is installed on one of the light-transmitting portions to allow light having a wavelength of less than 1000 to 2500 nm to enter the polyolefin flow channel in the connection conduit , and Install a receiver to receive the transmitted light
On the other hand, the light-transmitting portion of the
The temperature of the polyolefin at or above the melting point of the polyolefin.
A method for measuring the content of an additive in a polyolefin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP27759893A JP3411645B2 (en) | 1993-10-09 | 1993-10-09 | Method for measuring additive content in polyolefin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP27759893A JP3411645B2 (en) | 1993-10-09 | 1993-10-09 | Method for measuring additive content in polyolefin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH07110295A JPH07110295A (en) | 1995-04-25 |
| JP3411645B2 true JP3411645B2 (en) | 2003-06-03 |
Family
ID=17585676
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP27759893A Expired - Fee Related JP3411645B2 (en) | 1993-10-09 | 1993-10-09 | Method for measuring additive content in polyolefin |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3411645B2 (en) |
-
1993
- 1993-10-09 JP JP27759893A patent/JP3411645B2/en not_active Expired - Fee Related
Non-Patent Citations (2)
| Title |
|---|
| Ａｎａｌｕｓｉｓ，フランス，１９８２年，Ｖｏｌ．１０，Ｎｏ．４，ｐｐ．１６６−１７１ |
| Ａｎａｌｕｓｉｓ，フランス，１９９０年，Ｖｏｌ．１８，Ｎｏ．５，ｐｐ．３１０−３１２ |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH07110295A (en) | 1995-04-25 |
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