JPH0658877A - Method for evaluating gel amount in cellulose acetate - Google Patents
Method for evaluating gel amount in cellulose acetateInfo
- Publication number
- JPH0658877A JPH0658877A JP21412992A JP21412992A JPH0658877A JP H0658877 A JPH0658877 A JP H0658877A JP 21412992 A JP21412992 A JP 21412992A JP 21412992 A JP21412992 A JP 21412992A JP H0658877 A JPH0658877 A JP H0658877A
- Authority
- JP
- Japan
- Prior art keywords
- cellulose acetate
- gel
- light intensity
- amount
- scattering light
- 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.)
- Pending
Links
Landscapes
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は酢酸セルロース中のゲル
量の評価方法に関する。更に詳しくは、酢酸セルロース
の物性に大きな影響を与える酢酸セルロース中のゲル量
を簡便且つ精度よく評価する方法に関する。TECHNICAL FIELD The present invention relates to a method for evaluating the amount of gel in cellulose acetate. More specifically, it relates to a method for easily and accurately evaluating the amount of gel in cellulose acetate, which has a great influence on the physical properties of cellulose acetate.
【０００２】[0002]
【従来の技術】酢酸セルロースはタバコのフィルタート
ウの原料として用いられている。タバコのフィルタート
ウは酢酸セルロースのアセトンドープを紡糸することに
より得られるものであるが、このアセトンドープにはゲ
ル、即ちアセトン不溶物が存在している。かかる不溶物
は紡糸する際、ドープフィルターの目詰まり、紡糸ノズ
ルの目詰まり、糸切れ等の問題を引き起こし、酢酸セル
ロースの物性に大きな影響を与えている。そのため、工
程上、ゲルの量を正確に評価して対応するためにゲル量
評価方法の必要性は大きい。従来の酢酸セルロース溶液
中のゲル量評価方法は、酢酸セルロースのアセトン溶液
を遠心分離にかけ、アセトン不溶物としてゲルを分取
し、その重量を測定する方法であった。BACKGROUND OF THE INVENTION Cellulose acetate is used as a raw material for tobacco filter tow. The tobacco filter tow is obtained by spinning an acetone dope of cellulose acetate, and a gel, that is, an acetone insoluble substance is present in this acetone dope. Such insoluble matter causes problems such as clogging of the dope filter, clogging of the spinning nozzle, and yarn breakage during spinning, and has a great influence on the physical properties of cellulose acetate. Therefore, there is a great need for a gel amount evaluation method in order to accurately evaluate and respond to the amount of gel in the process. The conventional method for evaluating the amount of gel in a cellulose acetate solution is a method in which an acetone solution of cellulose acetate is centrifuged to separate the gel as an acetone insoluble matter, and the weight is measured.
【０００３】[0003]
【発明が解決しようとする課題】しかしながら、上記の
ゲル量評価方法は非常に手間と時間がかかり、また多く
の試料を必要とするという問題があった。However, the above-mentioned gel amount evaluation method has problems that it takes a lot of time and labor and that many samples are required.
【０００４】[0004]
【課題を解決するための手段】本発明者らは酢酸セルロ
ース中のゲル量の評価方法として、簡便で且つ少量の試
料で評価が可能で、しかも精度の良い方法を提供すべく
鋭意研究した結果、ゲル量が光散乱法により求められる
散乱光強度とほぼ正比例するという相関関係があり、こ
れを利用して酢酸セルロース溶液中のゲル量が評価でき
ることを見出し、本発明をなすに至った。As a method for evaluating the amount of gel in cellulose acetate, the present inventors have earnestly studied to provide a method that is simple and can be evaluated with a small amount of sample, and that is highly accurate. The inventors have found that there is a correlation that the amount of gel is almost directly proportional to the intensity of scattered light obtained by the light scattering method, and that the amount of gel in a cellulose acetate solution can be evaluated by utilizing this, and the present invention has been completed.
【０００５】即ち本発明は、酢酸セルロース試料のアセ
トン溶液の散乱光強度を測定し、これを既知濃度のゲル
を含む酢酸セルロースのアセトン溶液の散乱光強度とゲ
ル量との関係を示す検量線と比較して前記酢酸セルロー
ス中のゲルの量を定量することを特徴とする酢酸セルロ
ース中のゲル量の評価方法を提供するものである。That is, the present invention measures the scattered light intensity of an acetone solution of a cellulose acetate sample, and uses this as a calibration curve showing the relationship between the scattered light intensity of an acetone solution of cellulose acetate containing a gel of known concentration and the gel amount. A method for evaluating the amount of gel in cellulose acetate is provided by quantifying the amount of gel in the cellulose acetate for comparison.
【０００６】本発明の酢酸セルロースのゲル量評価方法
は、まず種々のゲル量既知の酢酸セルロースについて散
乱光強度を求め、それを指標とし、それとゲル量未知の
酢酸セルロースについて求めた散乱光強度を比較すれば
ゲル量未知の酢酸セルロース中のゲル量を評価すること
ができる。本発明の酢酸セルロースのゲル量評価方法は
二酢酸セルロースに適応できる。In the method for evaluating the amount of gel of cellulose acetate of the present invention, first, the scattered light intensity is obtained for various cellulose acetates having known gel amounts, and it is used as an index to determine the scattered light intensity obtained for cellulose acetate of unknown gel amount. By comparison, the amount of gel in cellulose acetate with an unknown amount of gel can be evaluated. The gel amount evaluation method for cellulose acetate of the present invention can be applied to cellulose diacetate.
【０００７】散乱光強度測定用のサンプルはポアサイズ
10μm のフィルターで濾過を行うのが好ましい。濾過を
行う理由は散乱光強度測定を行う際、ゴミの影響を除く
ためである。また、フィルターとしてポアサイズ10μm
のものが望ましい理由は、10μm 以下のゲルが紡糸の際
問題になっていることが明らかになっているからであ
る。散乱光強度の測定角度はサンプル中に混ざっている
ゴミの散乱の影響が最も少ない角度が選択される。ま
た、散乱光強度の測定は通常常温で行われる。測定回数
は精度確認のためにも１サンプルにつき最低３回、でき
れば５回以上が望ましい。The sample for measuring scattered light intensity has a pore size
It is preferable to perform filtration with a 10 μm filter. The reason for filtering is to eliminate the influence of dust when measuring the scattered light intensity. Also, as a filter, pore size 10 μm
The reason why the gel of 10 μm or less is desirable is that gels of 10 μm or less have been found to be a problem during spinning. The angle at which the scattered light intensity is measured is selected to have the least influence of scattering of dust mixed in the sample. The scattered light intensity is usually measured at room temperature. It is desirable that the number of measurements be at least 3 times, preferably 5 times or more, for each sample for accuracy confirmation.
【０００８】本発明において、酢酸セルロース溶液とは
酢酸セルロースをアセトン等の溶剤に溶解したものであ
り、溶液中の酢酸セルロース濃度は 0.1〜30重量％、好
ましくは１〜10重量％である。In the present invention, the cellulose acetate solution is a solution of cellulose acetate in a solvent such as acetone, and the concentration of cellulose acetate in the solution is 0.1 to 30% by weight, preferably 1 to 10% by weight.
【０００９】尚、酢酸セルロースとしては高温酢化法と
高温熟成法によって得られたものが好ましく、それらの
条件は、例えば酢化時の反応温度61〜63℃、反応時間は
70〜80分、熟成時の反応温度150 ℃、反応時間は120 分
である。As the cellulose acetate, those obtained by the high temperature acetylation method and the high temperature aging method are preferable, and those conditions are, for example, a reaction temperature of 61 to 63 ° C. and a reaction time of acetylation.
70-80 minutes, the reaction temperature during aging is 150 ° C, and the reaction time is 120 minutes.
【００１０】[0010]
【実施例】以下実施例にて本発明を説明するが、本発明
はこれらの実施例に限定されるものではない。EXAMPLES The present invention will be described below with reference to examples, but the present invention is not limited to these examples.
【００１１】参考例＜検量線の作成＞ 酢酸セルロース５重量％アセトン溶液を調製し、50000r
pm、３時間遠心分離を行い、アセトン可溶物（ゲルを含
まない酢酸セルロース）とアセトン不溶物（ゲル＋少量
の酢酸セルロース）に分離する。更にゲルのみを分取す
るためアセトン不溶物をアセトンに24時間以上分散さ
せ、再度50000rpm、３時間遠心分離を行いゲルを得る。
このゲルを24時間真空乾燥し、重量測定を行うことによ
りゲルの定量を行う。また、上記で用いた酢酸セルロー
スの散乱光強度を測定した。酢酸セルロース５％アセト
ン溶液を調製し、ポアサイズ10μm のフィルターを用い
て濾過を行った。このフィルターで濾過したサンプルを
測定用セルに注入し、光散乱測定装置（DLS-700 ；大塚
電子社製，波長633 nm）で散乱光強度を固定角90°で測
定した。測定温度は25±0.2 ℃、測定回数は１サンプル
につき５回とし、平均値をデータとした。以上の定量結
果と散乱光強度を表１に示す。この結果を図に示すと図
１の検量線が得られる。Reference Example <Preparation of Calibration Curve> A 5% by weight acetone solution of cellulose acetate was prepared, and 50,000 r
The mixture is centrifuged at pm for 3 hours to separate into an acetone-soluble material (gel-free cellulose acetate) and an acetone-insoluble material (gel + a small amount of cellulose acetate). Further, in order to collect only the gel, the acetone insoluble matter is dispersed in acetone for 24 hours or more, and the gel is obtained by centrifuging again at 50,000 rpm for 3 hours.
This gel is vacuum dried for 24 hours, and the weight of the gel is measured to quantify the gel. Further, the scattered light intensity of the cellulose acetate used above was measured. A 5% acetone solution of cellulose acetate was prepared and filtered using a filter having a pore size of 10 μm. The sample filtered with this filter was injected into a measurement cell, and the scattered light intensity was measured at a fixed angle of 90 ° with a light scattering measurement device (DLS-700; manufactured by Otsuka Electronics Co., Ltd., wavelength 633 nm). The measurement temperature was 25 ± 0.2 ° C., the number of measurements was 5 times per sample, and the average value was used as the data. Table 1 shows the above quantitative results and scattered light intensity. When this result is shown in the figure, the calibration curve of FIG. 1 is obtained.
【００１２】[0012]
【表１】 [Table 1]
【００１３】実施例１ ゲル量未知の高温酢化、高温熟成の酢酸セルロースの8.
5 ％アセトン溶液を調製し、ポアサイズ10μm のフィル
ターを用いて濾過を行った。このフィルターで濾過した
サンプルを測定用セルに注入し、光散乱測定装置（DLS-
700 ；大塚電子社製，波長633 nm）で散乱光強度を固定
角90°で測定した。測定温度は25±0.2℃、測定回数は
５回で実施したところ、その測定平均値は10672 であっ
た。図１の検量線から求めたゲル量は0.75重量％であっ
た。なお、同じ試料を用いてゲル量を従来の遠心分離法
で測定したところ、0.74重量％であった。Example 1 High temperature acetylated and high temperature aged cellulose acetate of unknown gel amount 8.
A 5% acetone solution was prepared and filtered using a filter having a pore size of 10 μm. The sample filtered with this filter is injected into the measurement cell, and the light scattering measurement device (DLS-
700; Otsuka Electronics Co., Ltd., wavelength 633 nm) and the scattered light intensity was measured at a fixed angle of 90 °. When the measurement temperature was 25 ± 0.2 ° C. and the measurement was performed 5 times, the average value of the measurement was 10672. The gel amount obtained from the calibration curve in FIG. 1 was 0.75% by weight. When the gel amount was measured by the conventional centrifugation method using the same sample, it was 0.74% by weight.
【００１４】[0014]
【発明の効果】本発明により、酢酸セルロース溶液中の
ゲル量評価が短時間で簡便且つ正確に行なえるようにな
り、更に少量のサンプルでゲル量の評価が可能となっ
た。従って、工場工程での検査工程でのチェックが容易
になり、他の工程への迅速なアクションが容易になる。According to the present invention, the gel amount in a cellulose acetate solution can be evaluated easily and accurately in a short time, and the gel amount can be evaluated with a small amount of sample. Therefore, it becomes easy to check in the inspection process in the factory process, and quick action to other processes becomes easy.
【図１】ゲル量と散乱光強度との関係を示す検量線であ
る。FIG. 1 is a calibration curve showing the relationship between gel amount and scattered light intensity.
Claims (2)
乱光強度を測定し、これを既知濃度のゲルを含む酢酸セ
ルロースのアセトン溶液の散乱光強度とゲル量との関係
を示す検量線と比較して前記酢酸セルロース中のゲルの
量を定量することを特徴とする酢酸セルロース中のゲル
量の評価方法。1. The scattered light intensity of an acetone solution of a cellulose acetate sample is measured and compared with a calibration curve showing the relationship between the scattered light intensity of an acetone solution of cellulose acetate containing a gel of known concentration and the gel amount. A method for evaluating the amount of gel in cellulose acetate, which comprises quantifying the amount of gel in the cellulose acetate.
法で得られたものである請求項１記載の酢酸セルロース
中のゲル量の評価方法。2. The method for evaluating the amount of gel in cellulose acetate according to claim 1, wherein the cellulose acetate is obtained by a high temperature acetylation method and a high temperature aging method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP21412992A JPH0658877A (en) | 1992-08-11 | 1992-08-11 | Method for evaluating gel amount in cellulose acetate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP21412992A JPH0658877A (en) | 1992-08-11 | 1992-08-11 | Method for evaluating gel amount in cellulose acetate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0658877A true JPH0658877A (en) | 1994-03-04 |
Family
ID=16650707
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP21412992A Pending JPH0658877A (en) | 1992-08-11 | 1992-08-11 | Method for evaluating gel amount in cellulose acetate |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0658877A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011526622A (en) * | 2008-07-01 | 2011-10-13 | ルピン・リミテッド | Sustained release pharmaceutical composition containing quetiapine |
| JP2020085467A (en) * | 2018-11-15 | 2020-06-04 | アンリツ株式会社 | Physical property inspection device |
-
1992
- 1992-08-11 JP JP21412992A patent/JPH0658877A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011526622A (en) * | 2008-07-01 | 2011-10-13 | ルピン・リミテッド | Sustained release pharmaceutical composition containing quetiapine |
| JP2014196334A (en) * | 2008-07-01 | 2014-10-16 | ルピン・リミテッドＬｕｐｉｎ Ｌｉｍｉｔｅｄ | Sustained release pharmaceutical composition containing quetiapine |
| JP2020085467A (en) * | 2018-11-15 | 2020-06-04 | アンリツ株式会社 | Physical property inspection device |
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