KR940001516B1 - Dispersion of tio2 particle - Google Patents
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- KR940001516B1 KR940001516B1 KR1019910005122A KR910005122A KR940001516B1 KR 940001516 B1 KR940001516 B1 KR 940001516B1 KR 1019910005122 A KR1019910005122 A KR 1019910005122A KR 910005122 A KR910005122 A KR 910005122A KR 940001516 B1 KR940001516 B1 KR 940001516B1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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Abstract
Description
제1도는 종래의 이산화티타늄의 분산장치를 도시한 것이다.1 shows a conventional dispersing device of titanium dioxide.
제2도는 본 발명의 이산화티타늄의 분산장치를 도시한 것이다.2 shows a dispersing device of titanium dioxide of the present invention.
본 발명의 이산화티타늄의 입자의 분산방법에 관한 것이다. 근래의 들어서 폴리에스테르는 그 자체의 우수한 물성때문에 산업용, 의류용등에 널리 사용되고 있다. 그러나 폴리에스테르가 가지고 있는 합성섬유 자체의 빛에 대한 반사, 표면의 평활성등에 의하여 의류용으로 사용시 많은 문제점을 노출시키고 있는 것도 또한 사실이다. 그러므로 최근에 와서는 이러한 문제점을 해결하고자 폴리에스테르의 중합시에 에틸렌글리콜 용액에 이산화티타늄(TiO2)입자를 첨가시켜 슬러리를 제조한후 이를 중합, 방사, 알칼리감량가공의 방법에 의해 표면의 미세요철을 부여하고 또한 덜(Dull)한 특성을 부여하는 방법이 알려지고 있다.The present invention relates to a method for dispersing particles of titanium dioxide of the present invention. In recent years, polyester has been widely used in industrial and clothing applications because of its excellent physical properties. However, it is also true that the synthetic fiber itself has a lot of problems when used for clothing due to the reflection of light and the smoothness of the surface. Therefore, in recent years, in order to solve these problems, a slurry is prepared by adding titanium dioxide (TiO 2 ) particles to an ethylene glycol solution during the polymerization of polyester, and then the surface fines are polymerized, spun, and reduced by alkali. It is known how to impart irregularities and to impart less properties.
그러나 이산화티타늄입자의 분산이 원활하지 않을 경우에는 폴리에스테르 중합과정시 필터(Filter) 압력상승의 요인이 되고 방사과정에서 필라멘트에 분산이 덜된 미립자 덩어리가 포함되면 절사의 요인이 되기도 하였다. 종래의 알려진 이산화 티타늄을 에틸렌글리콜 용액에 첨가하여 분산이 잘 되도록 하기 위한 방법으로는 프리믹싱 용기(Premixing vessel) 및 교반기(Agitator)로 에틸렌글리콜 용액에 이산화티타늄을 젖게(Wetting)한후 샌드 그라인더(Sand grinder)에서 이산화티타늄 덩어리를 분쇄해준후 원심분리기(Decantor)에서 분산액중의 조대입자를 제거해주는 방법이 알려지고 있다. 그러나 상기와 같은 방법에서는 통상으로 첨가하는 이산화티타늄 입자 자체가 크기가 직경 0.2-0.5㎛ 정도로 매우 적고 또한 이들은 서로 엉켜져 있으며 특히 에틸렌글리콜과 이산화티타늄의 친화성을 돕기위하여 이산화티타늄을 유기화합물로 코팅한 경우 이들 입자는 더욱 엉켜져 있기 때문에 입자의 덩어리가 큰경우(덩어리 직경이 50㎛ 이상인 경우) 분쇄효과가 크지만 분쇄된 덩어리의 크기가 작아질수록 분쇄효과가 급격히 저하된다.However, when the dispersion of the titanium dioxide particles is not smooth, it is a factor of the filter pressure rise during the polyester polymerization process, and the filament contains less dispersed particles in the spinning process. Conventionally known methods of adding titanium dioxide to ethylene glycol solution to ensure good dispersion include sand mixing after wetting titanium dioxide in ethylene glycol solution with a premixing vessel and an agitator. It is known to remove coarse particles in the dispersion in a decantor after crushing the titanium dioxide mass in a grinder. However, in such a method, the titanium dioxide particles which are usually added are very small in size of 0.2-0.5 μm in diameter, and they are entangled with each other, and in particular, titanium dioxide is coated with an organic compound to help the affinity of ethylene glycol and titanium dioxide. In this case, since these particles are more entangled, when the mass of the particles is large (larger diameter of 50 µm or more), the grinding effect is large, but the grinding effect decreases rapidly as the size of the grinding mass becomes smaller.
상기와 같이 초미립자의 용액중분산이 불량할 경우 폴리에스테르 중합과정의 필터(Filter)압력상승의 요인이되고 방사과정에서 필라멘트에 분쇄가 충분하지 못한 미립자 덩어리가 포함되면 절사의 요인이 된다. 따라서 본 발명자는 종래의 문제점을 해결하고자 초음파 분쇄방법을 사용하였다.As described above, poor dispersion of the ultrafine particles in the solution may cause a filter pressure increase during the polyester polymerization process, and may cause a cut if the filament contains fine particles that are not sufficiently pulverized in the spinning process. Therefore, the present inventors used the ultrasonic grinding method to solve the conventional problems.
그러므로 본 발명의 목적은 초음파분쇄방법을 사용하여 이산화티타늄을 에틸렌글리콜 슬러리상에 양호하게 분산시키는 방법을 제공하는데 그 목적이 있다.It is therefore an object of the present invention to provide a method for dispersing titanium dioxide onto an ethylene glycol slurry using an ultrasonic grinding method.
이하 본 발명을 상세히 설명하면 다음과 같다. 통상적으로 알려진 이산화티타늄 분산방법에서 샌드그라인더 통과직후 또는 원심분리기 통과직후에 이산화티타늄이 포함된 에틸렌글리콜 슬러리의 온도를 80℃ 내지 180℃로 유지하면서 진동수가 초당 2만 내지 100만인 초음파를 2 내지 5시간 가한다. (제2도는 본 발명의 한 예시를 나타낸 것이다). 이때 슬러리의 온도가 80℃ 미만인 경우 이산화티타늄과 에틸렌글리콜의 혼합이 잘되지않으며 에틸렌글리콜 자체의 특성상 180℃가 넘는 온도에서는 반응기 조절이 곤란하다.Hereinafter, the present invention will be described in detail. In the known titanium dioxide dispersing method, ultrasonic waves having a frequency of 20,000 to 1 million per second while maintaining the temperature of the titanium dioxide-containing ethylene glycol slurry at 80 ° C. to 180 ° C. immediately after passing through the sand grinder or after passing through the centrifuge are 2 to 5 Add time. (Figure 2 shows an example of the present invention). In this case, when the temperature of the slurry is less than 80 ° C., the mixing of titanium dioxide and ethylene glycol is not easy, and it is difficult to control the reactor at a temperature of more than 180 ° C. due to the nature of ethylene glycol itself.
또한 초음파의 진동수가 초당 2만미만과 처리시간이 2시간미만인 경우 그 효과가가 미비하며, 진동수가 초당 100만이 넘는 경우와 처리시간을 5시간 이상으로 한 경우는 그 효과의 증가가 미비하므로 그 이상 사용시 비용상승의 문제가 있으므로 좋지않다. 본 발명의 초음파처리는 샌드 그라인더통과직후 또는 원심분리기통과직후 모두 가능하다. 샌드 그라인더통과직후 초음파처리를 행하는 경우 원심분리과정에 보다 분쇄가 잘된 슬러리를 공급하여 원심분리효과가 양호하나 그라인딩과 초음파처리에도 불구하고 분쇄되지 못한 덩어리가 원심분리과정에서 충분히 제거되지 못하면 중합공정중에 투입되어 필터의 압력상승과 절사의 원인이 된다. 또한 원심분리직후 초음파처리를 행할 경우 이산화티타튬 입자는 그라인더를 통과함으로서 분쇄되고 여기서 미분된 덩어리는 원심분리기에서 제거된다. 그러나 원심분리기능에도 한계가 있으므로 50㎛이하의 덩어리가 다소 존재할 것이며 이러한 덩어리를 초음파 처리하여 분쇄하여줌으로써 슬러리중의 입자 분산상태를 극대화 할 수 있다. 따라서 본 발명의 초음파처리는 원심분리직후 행하는 것이 본 발명의 효과를 극대화할 수 있다. 이렇게 처리한 것은 이산화티타늄의 분산이 잘 이루어져 중합공정의 필터 압력 상승방지와 방사공정에서의 절사방지 및 이로인한 원사품질향상, 그리고 수지전체에 대해 강도가 균일하게 유지되는 효과가 있다.In addition, if the frequency of the ultrasonic wave is less than 20,000 per second and the processing time is less than 2 hours, the effect is insignificant. If the frequency is more than 1 million per second and the processing time is 5 hours or more, the effect is insufficient. It is not good because there is a problem of cost increase when using it over The sonication of the present invention is possible either immediately after passing through a sand grinder or immediately after passing through a centrifuge. In case of performing the ultrasonic treatment immediately after passing through the sand grinder, the finely ground slurry is supplied during the centrifugation process, so the centrifugation effect is good. Doing so may cause a rise in pressure and cut off of the filter. In addition, when sonication is performed immediately after centrifugation, the titanium dioxide particles are pulverized by passing through a grinder, where the finely divided mass is removed in a centrifuge. However, since there is a limit in the centrifugal separation function, there may be some lumps of 50 μm or less, and by pulverizing these lumps by ultrasonication, the state of particle dispersion in the slurry can be maximized. Therefore, the ultrasonic treatment of the present invention may be performed immediately after centrifugation to maximize the effect of the present invention. This treatment is effective in dispersing titanium dioxide, preventing filter pressure rise in the polymerization process, cutting off in the spinning process, thereby improving yarn quality, and maintaining strength uniformly over the entire resin.
이하 본 발명을 실시예에 의해 설명한다.Hereinafter, the present invention will be described by way of examples.
[실시예 1]Example 1
프리믹싱 용기(Premixing vessel)에 에틸렌글리콜 850㎏과 이산화티타늄 300㎏을 첨가한다. 이를 공지의 방법에 의해 교반기(Agitator)로 교반하고 샌드 그라인더를 통과후 원심분리기에 넣어 이산화티타늄을 분쇄한다. 그후 세립조에서 에틸렌글리콜 슬러리의 온도를 100℃로 유지하면서 초당 5만의 진동수를 가지는 초음파를 3시간 처리한후 에틸렌글리콜내의 이산화티타늄의 입도분포를 컬터 카운터(Culter counter)로 측정하였다.850 kg of ethylene glycol and 300 kg of titanium dioxide are added to a premixing vessel. This is stirred by an agitator by a known method, passed through a sand grinder, and then put into a centrifuge to grind titanium dioxide. Thereafter, while maintaining the temperature of the ethylene glycol slurry at 100 ° C., the ultrasonic wave having 50,000 frequencies per second was treated for 3 hours, and then the particle size distribution of titanium dioxide in the ethylene glycol was measured by a Culter counter.
[실시예 2-4 및 비교예 1]Example 2-4 and Comparative Example 1
실시예 1과 동일한 조건으로 하되 에틸렌글리콜 슬러리의 온도, 초음파처리시간 및 진동수를 표 1과 같이 하여 실험을 행하였다.The experiment was carried out under the same conditions as in Example 1, but with the temperature, the sonication time, and the frequency of the ethylene glycol slurry as shown in Table 1.
[실시예 5]Example 5
초음파처리조건은 실시예 1과 동일하게 초음파처리를 그라인더 통과직후 행하였다.Sonication conditions were performed immediately after passing the grinder in the same manner as in Example 1.
[비교예 2-3]Comparative Example 2-3
실시예 1과 동일한 방법으로 행하되 비교예 2는 초음파처리조건중 초음파진동수를 초당 110만으로, 비교예 3은 초음파처리조건중 초음파처리시간을 6시간으로 했으나 효과가 본 발명의 실시예보다 그리 뛰어나지 않았으며 반면 처리시간 및 처리조건의 과다로 인한 에너지의 손실이 컸다.In the same manner as in Example 1, Comparative Example 2, the ultrasonic frequency in the ultrasonic treatment conditions of 1.1 million per second, Comparative Example 3 in the ultrasonic treatment conditions of the ultrasonic treatment time 6 hours, but the effect was not much better than the embodiment of the present invention On the other hand, energy loss was large due to excessive treatment time and treatment conditions.
[비교예 4][Comparative Example 4]
종래의 방법에 의한 예로서 초음파처리를 행하지 않았다.As an example by the conventional method, ultrasonication was not performed.
그 결과는 다음 표 1과 같다.The results are shown in Table 1 below.
[표 1]TABLE 1
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| Application Number | Priority Date | Filing Date | Title |
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| KR1019910005122A KR940001516B1 (en) | 1991-03-30 | 1991-03-30 | Dispersion of tio2 particle |
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| KR1019910005122A KR940001516B1 (en) | 1991-03-30 | 1991-03-30 | Dispersion of tio2 particle |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CZ301279B6 (en) * | 1998-09-02 | 2009-12-30 | Sachtleben Chemie Gmbh | Process for preparing processing aid and processing aid prepared in such a manner |
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| KR100385301B1 (en) * | 2000-11-28 | 2003-05-23 | 한국화학연구원 | Novel titania photocatalyst and its manufacturing method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CZ301279B6 (en) * | 1998-09-02 | 2009-12-30 | Sachtleben Chemie Gmbh | Process for preparing processing aid and processing aid prepared in such a manner |
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