JP2022168910A - Dust suppression treatment method of dust emission material - Google Patents
Dust suppression treatment method of dust emission material Download PDFInfo
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Abstract
Description
本発明は、発塵性物質の塵埃抑制処理方法に関するものであり、より詳細には、発塵性物質の塵埃を抑制する性能に優れ、再分散性にも優れた塵埃抑制処理剤組成物を用いた塵埃抑制処理方法に関する。 TECHNICAL FIELD The present invention relates to a dust suppression treatment method for dust-generating substances. More specifically, the present invention relates to a dust suppression treatment agent composition that has excellent performance in suppressing dust from dust-generating substances and is also excellent in redispersibility. It relates to the dust suppression treatment method used.
塵埃を出す物質の塵埃を抑制する技術は、健康上、安全上、環境上その他の要請から、生活のためにまた産業のために重要な技術である。
このような塵埃抑制技術としては、下記特許文献１において、ポリテトラフルオロエチレン（ＰＴＦＥ）を粉末状物質と混合し、該混合物に約２０～２００℃の温度で圧縮－剪断作用を施すことによりＰＴＦＥをフィブリル化して粉末状物質の塵埃発生を抑制する方法が提案されている。
Technology for controlling dust in dust-producing materials is an important technology for human life and industry for health, safety, environmental and other requirements.
As such a dust suppression technology, in Patent Document 1 below, polytetrafluoroethylene (PTFE) is mixed with a powdery substance, and the mixture is subjected to a compression-shearing action at a temperature of about 20 to 200 ° C. to remove PTFE. A method has been proposed for suppressing the generation of dust from powdery substances by fibrillating them.
上記特許文献１に記載されているＰＴＦＥは、組成としてはテトラフルオロエチレンのホモポリマーで形態としてはファインパウダー又はエマルジョンであるテフロン（登録商標）６又はテフロン（登録商標）３０、並びに組成としてはテトラフルオロエチレンの変性ポリマーで形態としてはファインパウダーであるテフロン（登録商標）６Ｃなどである。 The PTFE described in Patent Document 1 includes Teflon (registered trademark) 6 or Teflon (registered trademark) 30, which is a homopolymer of tetrafluoroethylene as a composition and fine powder or emulsion as a form, and tetrafluoroethylene as a composition. Teflon (registered trademark) 6C, which is a modified polymer of fluoroethylene and is in the form of fine powder.
また、下記特許文献２には、ＰＴＦＥに対して１．０質量％以上の炭化水素系アニオン界面活性剤を含有する水性エマルジョンを使用する安定性のよい塵埃抑制方法が提案されており、粉末状物質について塵埃抑制効果があることが示されている。この特許文献２によれば、ＰＴＦＥの粒子は、下記特許文献３に開示されている乳化重合法、即ちテトラフルオロエチレンを水溶性重合開始剤及びフルオロアルキル基を疎水基とするアニオン系界面活性剤（以下、含フッ素乳化剤という）を乳化剤として含む水性媒体中に圧入、重合させることにより、水性エマルジョンの形態で製造されるが、安定性を増すためにさらに乳化安定剤が添加されている。 In addition, Patent Document 2 below proposes a method for suppressing dust with good stability using an aqueous emulsion containing 1.0% by mass or more of a hydrocarbon-based anionic surfactant with respect to PTFE. Substances have been shown to have a dust-suppressing effect. According to Patent Document 2, PTFE particles are produced by the emulsion polymerization method disclosed in Patent Document 3 below, that is, an anionic surfactant having tetrafluoroethylene as a water-soluble polymerization initiator and a fluoroalkyl group as a hydrophobic group. (hereinafter referred to as a fluorine-containing emulsifier) is injected into an aqueous medium containing an emulsifier and polymerized to produce an aqueous emulsion, and an emulsion stabilizer is added to increase stability.
更に、下記特許文献４には、含フッ素乳化剤の含有率が５ ０ｐｐｍ以下である含フッ素重合体水性分散液からなる塵埃抑制処理剤組成物を用いることにより、塵埃抑制効果があって、環境への影響を懸念することなく塵埃を抑制できる方法が記載されている。 Furthermore, Patent Document 4 below discloses that the use of a dust-suppressing treatment agent composition comprising an aqueous dispersion of a fluoropolymer having a fluorine-containing emulsifier content of 50 ppm or less has a dust-suppressing effect and is environmentally friendly. describes a method that can suppress dust without worrying about the influence of
しかしながら、これらの方法に塵埃抑制処理剤組成物として用いられるＰＴＦＥは高分子量であり、その水性分散液は長期間静置された場合には沈降し易く、一度沈降したＰＴＦＥは強固に固まり再分散し難いという問題があることに加え、ＰＴＦＥ水性分散液中のＰＴＦＥ濃度の低下を引き起こすなど、使用条件によっては本来ＰＴＦＥが備えている塵埃抑制効果を十分に発揮できなくなるおそれがあった。 However, PTFE used as a dust-suppressing treatment agent composition in these methods has a high molecular weight, and its aqueous dispersion tends to settle when left standing for a long period of time. In addition to the problem that it is difficult to clean the PTFE, there is a possibility that, depending on the conditions of use, the dust-suppressing effect inherent in PTFE cannot be fully exhibited, such as a decrease in the concentration of PTFE in the aqueous PTFE dispersion.
すなわち本発明は、優れた塵埃抑制効果を有すると共に、長期間静置された後の塵埃抑制処理剤組成物中の固形分であるＰＴＦＥ粒子の再分散性にも優れ、且つ、環境性能にも優れた塵埃抑制処理剤組成物を用いた、発塵性物質の塵埃抑制処理方法を提供することを目的とする。 That is, the present invention has an excellent dust suppressing effect, is excellent in redispersibility of the PTFE particles, which are the solid content in the dust suppressing treatment agent composition after being left standing for a long time, and is also environmentally friendly. An object of the present invention is to provide a method for dust suppression treatment of dust-generating substances using an excellent dust suppression treatment agent composition.
本発明は、メチル基（－ＣＨ３）、ヒドロキシプロピル基（－ＣＨ２ＣＨＯＨＣＨ３）、およびヒドロキシエチル基（－ＣＨ２ＣＨ２ＯＨ）から選択される少なくとも１種を含有する水溶性セルロース誘導体から選択される少なくとも１種、及びポリテトラフルオロエチレン水性分散液からなる塵埃抑制処理剤組成物を、発塵性物質と混合し、該混合物に２０～２００℃の温度条件下で圧縮－剪断作用を施すことにより、ポリテトラフルオロエチレンをフィブリル化して発塵性物質の塵埃の発生を抑制することを特徴とする発塵性物質の塵埃抑制処理方法を提供する。 The present invention provides a water-soluble cellulose derivative containing at least one selected from a methyl group (--CH 3 ), a hydroxypropyl group (--CH 2 CHOHCH 3 ), and a hydroxyethyl group (--CH 2 CH 2 OH). A dust suppressing treatment agent composition comprising at least one of the selected agents and a polytetrafluoroethylene aqueous dispersion is mixed with a dust-generating substance, and the mixture is subjected to compression-shearing action at a temperature of 20 to 200°C. Provided is a method for suppressing dust from a dust-generating substance, characterized by fibrillating polytetrafluoroethylene to suppress the generation of dust from the dust-generating substance.
前記水溶性セルロース誘導体が、メチルセルロース、ヒドロキシメチルセルロース、ヒドロキシエチルセルロース、ヒドロキシプロピルセルロース、ヒドロキシエチルメチルセルロース、ヒドロキシプロピルメチルセルロース、カルボキシメチルセルロース、エチルセルロースから選択される少なくとも１種であることは、本発明の好適な態様である。 It is a preferred aspect of the present invention that the water-soluble cellulose derivative is at least one selected from methylcellulose, hydroxymethylcellulose, hydroxyethylcellulose, hydroxypropylcellulose, hydroxyethylmethylcellulose, hydroxypropylmethylcellulose, carboxymethylcellulose, and ethylcellulose. be.
前記水溶性セルロース誘導体が、２２５～２３０℃の融点を有するヒドロキシプロピルメチルセルロースであることは、本発明の好適な態様である。 It is a preferred embodiment of the present invention that the water-soluble cellulose derivative is hydroxypropylmethylcellulose having a melting point of 225-230°C.
前記水溶性セルロース誘導体が、前記塵埃抑制処理剤組成物中に０．０１～１．００質量％の量で含有されていることは、本発明の好適な態様である。 It is a preferred embodiment of the present invention that the water-soluble cellulose derivative is contained in the dust suppressing treatment agent composition in an amount of 0.01 to 1.00% by mass.
前記ＰＴＦＥ水性分散液が、ＰＴＦＥを１～８０質量％の量で含有することは、本発明の好適な態様である。 It is a preferred aspect of the present invention that the PTFE aqueous dispersion contains 1 to 80% by mass of PTFE.
本発明の塵埃抑制処理方法は、粉末状の発塵性物質に好適に使用できる。 The dust suppression treatment method of the present invention can be suitably used for powdery dust-generating substances.
前記塵埃抑制処理剤組成物の下記式（１）で示される沈降率が１．０未満であることは、本発明の好適な態様である。
沈降率＝Ｘ１／Ｘ０＜１．０ ・・・（１）
式中、Ｘ０：前記水溶性セルロース誘導体を含まないＰＴＦＥ水性分散液１０ｇを、温度２０℃、回転速度３０００ｒｐｍにて３０分間、遠心分離機により遠心分離した際の下記式（２）で示される固形分沈降割合（％）である。
Ｘ１：前記塵埃抑制処理剤組成物１０ｇを、温度２０℃、回転速度３０００ｒｐｍにて３０分間、遠心分離機により遠心分離した際の下記式（２）で示される固形分沈降割合（％）である。
固形分沈降割合（％）＝（遠心分離後の固形分沈降量）／（遠心分離前の固形分量）×１００ ・・・（２）
It is a preferred aspect of the present invention that the dust suppressing treatment agent composition has a sedimentation rate represented by the following formula (1) of less than 1.0.
Sedimentation rate=X 1 /X 0 <1.0 (1)
In the formula, X 0 is represented by the following formula (2) when 10 g of the PTFE aqueous dispersion containing no water-soluble cellulose derivative is centrifuged at a temperature of 20 ° C. and a rotation speed of 3000 rpm for 30 minutes with a centrifuge. Solid sedimentation ratio (%).
X 1 : Solid content sedimentation ratio (%) represented by the following formula (2) when 10 g of the dust suppressing treatment agent composition is centrifuged at a temperature of 20 ° C. and a rotation speed of 3000 rpm for 30 minutes with a centrifuge. be.
Solid content sedimentation ratio (%) = (solid content sedimentation amount after centrifugation) / (solid content amount before centrifugation) x 100 (2)
本発明の塵埃抑制処理方法によれば、発塵性物質の塵埃を抑制する性能に優れ、且つ長期間静置後であっても塵埃抑制処理剤組成物中の固形分であるＰＴＦＥ粒子の再分散性に優れる塵埃抑制処理剤組成物を使用することにより、効率よくＰＴＦＥを発塵性物質の塵埃抑制処理に使用できるため、環境性能及び経済性に優れた発塵性物質の塵埃抑制処理方法が提供される。 According to the dust suppressing treatment method of the present invention, the dust suppressing performance of the dust-generating substance is excellent, and the PTFE particles, which are the solid content in the dust suppressing treatment agent composition, are recycled even after standing for a long period of time. PTFE can be efficiently used for dust control treatment of dust-generating substances by using a dust control agent composition with excellent dispersibility. is provided.
本発明の発塵性物質の塵埃抑制処理方法は、メチル基（－ＣＨ３）、ヒドロキシプロピル基（－ＣＨ２ＣＨＯＨＣＨ３）、およびヒドロキシエチル基（－ＣＨ２ＣＨ２ＯＨ）から選択される少なくとも１種を含有する水溶性セルロース誘導体、及びＰＴＦＥ水性分散液からなる塵埃抑制処理剤組成物を使用することが重要な特徴であり、この塵埃抑制処理剤組成物を発塵性物質と混合し、該混合物に約２０～２００℃の温度で圧縮－剪断作用を施すことにより、ＰＴＦＥをフィブリル化して発塵性物質の塵埃の発生を抑制することができる。
前述した通り、塵埃抑制処理剤組成物中の固形分であるＰＴＦＥ粒子は沈降し易いため、ＰＴＦＥ水性分散液が長期間静置された場合には、ＰＴＦＥ粒子が沈降し、沈降したＰＴＦＥ粒子が強固に固まり攪拌等で再分散させることが困難であるが、本発明に用いる塵埃抑制処理剤組成物においては、上記水溶性セルロース誘導体を含有することにより、沈降したＰＴＦＥ粒子が強固に固まることを抑制し、ＰＴＦＥ粒子の再分散性が顕著に向上されている。その結果、少量の塵埃抑制処理剤組成物を均一に発塵性物質と混合することができるため、発塵性物質の塵埃の発生を効率よく抑制することが可能となる。
The dust suppression treatment method for dust - generating substances of the present invention includes at least A key feature is the use of a dust control treatment composition comprising a water-soluble cellulose derivative containing one and a PTFE aqueous dispersion, wherein the dust control treatment composition is mixed with a dust-producing material, By subjecting the mixture to a compression-shearing action at a temperature of about 20 to 200° C., the PTFE can be fibrillated to suppress the generation of dust from the dust-producing substance.
As described above, the PTFE particles, which are the solid content in the dust suppressing treatment agent composition, tend to settle. It is difficult to re-disperse the dust-suppressing treatment agent composition by agitation or the like because it hardens firmly. , and the redispersibility of the PTFE particles is significantly improved. As a result, a small amount of the dust-suppressing treatment agent composition can be uniformly mixed with the dust-generating substance, so that generation of dust from the dust-generating substance can be efficiently suppressed.
本発明で用いる塵埃抑制処理剤組成物が、塵埃を抑制する性能及び再分散性に優れていることは、後述する実施例の静置沈降試験及び静置沈降再分散試験、遠心分離沈降試験、遠心分離再分散試験及び落下粉塵量試験の結果からも明らかである。
すなわち、静置沈降試験及び静置沈降再分散試験の結果を表す図１からも明らかなように、水溶性セルロース誘導体が配合された塵埃抑制処理剤組成物は、水溶性セルロース誘導体が配合されていないＰＴＦＥ水性分散液に比して沈降量が低減されている。また後述する実施例３～６に示すように、本発明に用いる塵埃抑制処理剤組成物は、塵埃抑制処理剤組成物中のＰＴＦＥ粒子の再分散性を示す、上記式（１）で示す沈降率が１．０未満、好ましくは０．９以下、好適には０．８以下であることにより、良好に再分散できることが明らかである。すなわち、上記式（１）で示される沈降率が１．０以上の場合には、沈降したＰＴＦＥ粒子が強固に固まり、再分散が困難になる。また固形分であるＰＴＦＥ粒子が沈降した結果、塵埃抑制処理剤組成物中に分散しているＰＴＦＥ粒子が減少し、沈降前と同等の塵埃を抑制する性能を維持するためには、より多くのＰＴＦＥ水性分散液が必要となる。更に強固に固まったＰＴＦＥは、塵埃抑制処理剤として利用することができないため、廃棄しなければならず、有用な資源であるＰＴＦＥの多くを無駄にしてしまうと共に、廃棄コストが発生する等、経済性の点からも好ましくない。
The fact that the dust suppressing treatment agent composition used in the present invention is excellent in dust suppressing performance and redispersibility is confirmed by the static sedimentation test, static sedimentation redispersion test, centrifugal sedimentation test, and It is also clear from the results of the centrifugal redispersion test and the falling dust amount test.
That is, as is clear from FIG. 1 showing the results of the static sedimentation test and the static sedimentation redispersion test, the dust control agent composition containing the water-soluble cellulose derivative does not contain the water-soluble cellulose derivative. The amount of sedimentation is reduced compared to the PTFE aqueous dispersion without PTFE. Further, as shown in Examples 3 to 6 to be described later, the dust suppressing treatment agent composition used in the present invention exhibits the redispersibility of PTFE particles in the dust suppressing treatment agent composition, which is represented by the above formula (1). A ratio of less than 1.0, preferably less than or equal to 0.9, preferably less than or equal to 0.8 clearly results in good redispersion. That is, when the sedimentation rate represented by the above formula (1) is 1.0 or more, the sedimented PTFE particles are firmly agglomerated, making it difficult to re-disperse them. In addition, as a result of sedimentation of the PTFE particles, which are the solid content, the number of PTFE particles dispersed in the dust suppressing treatment agent composition decreases, and in order to maintain the same dust suppressing performance as before sedimentation, more A PTFE aqueous dispersion is required. In addition, the hardened PTFE cannot be used as a dust control agent and must be discarded. It is also undesirable from a sexual point of view.
（水溶性セルロース誘導体）
本発明の塵埃抑制処理法に使用する塵埃抑制処理剤組成物に含有される水溶性セルロース誘導体は、メチル基（－ＣＨ３）、ヒドロキシプロピル基（－ＣＨ２ＣＨＯＨＣＨ３）、およびヒドロキシエチル基（－ＣＨ２ＣＨ２ＯＨ）から選択される少なくとも１種を含有する水溶性セルロース誘導体であることが好ましい。より好ましくは、メチルセルロース、ヒドロキシメチルセルロース、ヒドロキシエチルセルロース、ヒドロキシプロピルセルロース、ヒドロキシエチルメチルセルロース、ヒドロキシプロピルメチルセルロース、カルボキシメチルセルロース、エチルセルロースから選択される少なくとも１種であり、更に好ましくは、２２５～２３０℃の融点を有するヒドロキシプロピルメチルセルロースであることが望ましい。
(Water-soluble cellulose derivative)
The water-soluble cellulose derivative contained in the dust control treatment agent composition used in the dust control treatment method of the present invention has a methyl group (-CH 3 ), a hydroxypropyl group (-CH 2 CHOHCH 3 ), and a hydroxyethyl group (-CH 2 CHOHCH 3 ). —CH 2 CH 2 OH) is preferably a water-soluble cellulose derivative containing at least one selected from. More preferably, it is at least one selected from methylcellulose, hydroxymethylcellulose, hydroxyethylcellulose, hydroxypropylcellulose, hydroxyethylmethylcellulose, hydroxypropylmethylcellulose, carboxymethylcellulose, and ethylcellulose, and still more preferably has a melting point of 225 to 230°C. Preferably, it is hydroxypropyl methylcellulose.
前記水溶性セルロース誘導体は、塵埃抑制処理剤組成物中に、０．０１～１．００質量％、好ましくは０．０１～０．０５質量％、より好ましくは０．０１～０．０３質量％の量で含有されることが好ましい。水溶性セルロース誘導体の含有量が０．０１質量％未満の場合には、上記範囲にある場合に比して沈降したＰＴＦＥ粒子の再分散性が劣り、その一方１．００質量％を超える場合には、上記範囲にある場合に比してＰＴＦＥのフィブリル化を阻害し、その結果、塵埃を抑制する性能の低下を生じることに加え、塵埃抑制処理剤組成物の粘度が上昇し、著しいハンドリング性の低下も生じるおそれがある。塵埃抑制処理剤組成物の粘度の上昇は、塵埃抑制処理剤組成物を水で希釈して用いることも困難にするため好ましくない。
本発明においては、塵埃抑制処理剤組成物中の固形分であるＰＴＦＥ粒子が、輸送・保管時の静置により沈降した場合でも、水溶性セルロース誘導体を含有することにより、攪拌・転動等の作用によるＰＴＦＥ粒子の再分散が容易であることから（再分散性の向上）、塵埃抑制処理剤組成物を効率よく使用することが可能となる。
The water-soluble cellulose derivative is 0.01 to 1.00% by mass, preferably 0.01 to 0.05% by mass, more preferably 0.01 to 0.03% by mass, in the dust suppressing treatment agent composition. is preferably contained in an amount of If the content of the water-soluble cellulose derivative is less than 0.01% by mass, the redispersibility of the sedimented PTFE particles is inferior to that in the above range. inhibits the fibrillation of PTFE compared to the above range, and as a result, in addition to causing a decrease in dust suppressing performance, the viscosity of the dust suppressing treatment agent composition increases, resulting in remarkable handleability. may also cause a decrease in An increase in the viscosity of the dust suppressing treatment composition is not preferred because it also makes it difficult to dilute the dust suppressing treatment composition with water for use.
In the present invention, even if the PTFE particles, which are the solid content in the dust suppressing treatment agent composition, settle due to standing during transportation and storage, the inclusion of the water-soluble cellulose derivative prevents stirring, rolling, and the like. Since the PTFE particles can be easily redispersed by the action (improved redispersibility), the dust suppressing treatment agent composition can be used efficiently.
（ＰＴＦＥ水性分散液）
本発明に用いる塵埃抑制処理剤を構成するＰＴＦＥ水性分散液において、ＰＴＦＥは、ホモポリマーと呼ばれるテトラフルオロエチレン（ＴＦＥ）の単独重合体（ＰＴＦＥ）と、変性ポリマーと呼ばれる１％以下のコモノマーを含むテトラフルオロエチレンの共重合体（変性ＰＴＦＥ）の何れであってもよいが、ＴＦＥのホモポリマーであるＰＴＦＥであることが特に好ましい。
変性ＰＴＦＥ水性分散液からなる塵埃抑制処理剤組成物は、ＰＴＦＥ水性分散液からなる塵埃抑制処理剤組成物に比べ塵埃抑制効果が低く、同じ塵埃抑制効果を出すためにしばしば５０％以上多い量の処理剤を使用しなければならないことがある。
(PTFE aqueous dispersion)
In the PTFE aqueous dispersion that constitutes the dust control treatment agent used in the present invention, PTFE contains a homopolymer of tetrafluoroethylene (TFE) (PTFE), called homopolymer, and 1% or less of a comonomer, called modified polymer. Any copolymer of tetrafluoroethylene (modified PTFE) may be used, but PTFE, which is a homopolymer of TFE, is particularly preferred.
Dust control treatment compositions comprising modified PTFE aqueous dispersions are less effective in dust control than dust control treatment compositions comprising aqueous PTFE dispersions, often requiring 50% or more greater amounts to achieve the same dust control effect. You may have to use a processing agent.
ＰＴＦＥ水性分散液中のＰＴＦＥは、平均粒径０．１～０．５μｍ、好ましくは０．１～０．３μｍのコロイド粒子であることが望ましい。上記範囲よりも平均粒径が小さい場合には、上記範囲にある場合に比して、発塵性物質の塵埃を抑制する効果が低くなるおそれがあり、一方上記範囲よりも平均粒径が大きい場合には、上記範囲にある場合に比してコロイド粒子の分散安定性が低いおそれがある。
また、ＰＴＦＥの比重（ＳＳＧ）は２．２７以下、好ましくは２．２２以下、より好ましくは２．２０以下であることが望ましい。ＰＴＦＥの比重（ＳＳＧ）が上記範囲よりも大きい場合には、上記範囲にある場合に比して発塵性物質の塵埃を抑制する効果が劣るおそれがある。
The PTFE in the PTFE aqueous dispersion is desirably colloidal particles with an average particle size of 0.1 to 0.5 μm, preferably 0.1 to 0.3 μm. If the average particle size is smaller than the above range, the effect of the dust-generating substance to suppress dust may be lower than if it is within the above range, while the average particle size is larger than the above range. In some cases, the dispersion stability of the colloidal particles may be lower than in the above range.
Also, the specific gravity (SSG) of PTFE is desirably 2.27 or less, preferably 2.22 or less, more preferably 2.20 or less. If the specific gravity (SSG) of PTFE is greater than the above range, the effect of the dust-generating substance in suppressing dust may be inferior to that in the above range.
本発明において、ＰＴＦＥ水性分散液中のＰＴＦＥ濃度は特に限定されないが、１０～８０質量％、好ましくは１５～８０質量％、より好ましくは２０～８０質量％の範囲にある。
発塵性物質へのＰＴＦＥの分散効果を高めるためには、ＰＴＦＥ濃度は低いほど好ましいが、ＰＴＦＥ濃度が高いと、ＰＴＦＥ水性分散液の分散安定性が損なわれるおそれがある。その一方、ＰＴＦＥ水性分散液を輸送する際には、その濃度が高いほど輸送コストを節約できる。従って、本発明の塵埃抑制処理法においては、塵埃抑制処理剤組成物中のＰＴＦＥ濃度が、１０質量％以上、特に２０～８０質量％の範囲にある塵埃抑制処理剤組成物を用いることが好ましく、発塵性物質へ混合する際には、ＰＴＦＥの分散効果を高めるため、ＰＴＦＥ濃度が５質量％以下となるように上記塵埃抑制処理剤組成物を水で希釈して使用することが好適である。
In the present invention, the PTFE concentration in the PTFE aqueous dispersion is not particularly limited, but is in the range of 10-80% by mass, preferably 15-80% by mass, more preferably 20-80% by mass.
In order to enhance the effect of dispersing PTFE in dust-generating substances, the lower the PTFE concentration is, the better. On the other hand, when transporting the PTFE aqueous dispersion, the higher the concentration, the more the transport cost can be saved. Therefore, in the dust suppressing treatment method of the present invention, it is preferable to use a dust suppressing treatment agent composition in which the PTFE concentration in the dust suppressing treatment agent composition is 10% by mass or more, particularly in the range of 20 to 80% by mass. When mixed with a dust-generating substance, it is preferable to dilute the dust-suppressing treatment agent composition with water so that the PTFE concentration is 5% by mass or less in order to enhance the dispersing effect of PTFE. be.
本発明に用いるＰＴＦＥ水性分散液には、乳化剤として含フッ素乳化剤（界面活性剤）が少量含有されていてもよい。含フッ素乳化剤は、重合における反応不活性の故に不可欠のものではあるが、難分解性で環境への影響が懸念されるため、その含有率は低いことが望まれており、５０ｐｐｍ以下であることが好ましい。ＰＴＦＥ水性分散液中の含フッ素乳化剤濃度は、ＰＴＦＥ水性分散液を－２０℃の冷凍庫に入れて凍らせ、ＰＴＦＥを凝集させて水と分離した後、ポリエチレン容器の中身を全てソックスレーの抽出器に移し、約８０ｍｌのメタノールで７時間抽出し、メスアップしたサンプル液を液体クロマトグラフで測定してＰＴＦＥ水性分散液中の含フッ素乳化剤濃度を算出することが出来る。 The PTFE aqueous dispersion used in the present invention may contain a small amount of a fluorine-containing emulsifier (surfactant) as an emulsifier. Fluorine-containing emulsifiers are essential because they are inert to the reaction in polymerization, but since they are difficult to decompose and have a concern about environmental impact, it is desired that their content be low, and should be 50 ppm or less. is preferred. The concentration of the fluorine-containing emulsifier in the PTFE aqueous dispersion was determined by placing the PTFE aqueous dispersion in a freezer at -20°C and freezing it to coagulate the PTFE and separate it from the water. It is transferred, extracted with about 80 ml of methanol for 7 hours, and the diluted sample liquid is measured by a liquid chromatograph to calculate the fluorine-containing emulsifier concentration in the PTFE aqueous dispersion.
含フッ素乳化剤の含有率が５０ｐｐｍ以下であるＰＴＦＥ水性分散液を調製する方法は特に制限がないが、以下の方法を例示できる。
例えば、前述した特許文献３に開示されているような乳化重合法により得られたＰＴＦＥ水性分散液、即ちＴＦＥを水溶性重合開始剤及び乳化剤としてフルオロアルキル基を疎水基とするアニオン系界面活性剤（含フッ素乳化剤）を含む水性媒体中に圧入、重合して得られる、含フッ素乳化剤（アンモニウム塩及び／又はアルカリ塩の形のパーフルオロオクタン酸）を含フッ素重合体の重量に対し約０．０２～１質量％含むＰＴＦＥ水性分散液から、例えば有効量の陰イオン交換体と接触させて分離して除去する方法（特表２００５－５０１９５６号公報及び特表２００２－５３２５８３号公報）、或いは含フッ素重合体水性分散液の限外ろ過により除去する方法（米国特許第４，３６９，２２６号）等、公知の含フッ素乳化剤の除去方法によって、含フッ素乳化剤を除去することにより得ることができる。尚、含フッ素乳化剤の除去方法は上記方法に限定されるものではない。
また含フッ素乳化剤は高価であるため、上記方法により除去された含フッ素乳化剤は回収して再利用されることが望ましい。
There are no particular restrictions on the method for preparing a PTFE aqueous dispersion containing a fluorine-containing emulsifier content of 50 ppm or less, but the following methods can be exemplified.
For example, an anionic surfactant having a fluoroalkyl group as a hydrophobic group using a PTFE aqueous dispersion obtained by an emulsion polymerization method as disclosed in the above-mentioned Patent Document 3, that is, TFE as a water-soluble polymerization initiator and emulsifier. (Fluorine-containing emulsifier) is injected into an aqueous medium containing the fluorine-containing emulsifier and polymerized. From a PTFE aqueous dispersion containing 02 to 1% by mass, for example, a method of separating and removing by contacting with an effective amount of anion exchanger (Japanese Patent Publication No. 2005-501956 and Japanese Patent Publication No. 2002-532583), or It can be obtained by removing the fluorine-containing emulsifier by a known method for removing the fluorine-containing emulsifier, such as a method of removing by ultrafiltration of a fluoropolymer aqueous dispersion (US Pat. No. 4,369,226). The method for removing the fluorine-containing emulsifier is not limited to the above method.
Further, since the fluorine-containing emulsifier is expensive, it is desirable to recover and reuse the fluorine-containing emulsifier removed by the above method.
ＰＴＦＥ水性分散液を調製する乳化重合法においては、乳化剤として上述した特許文献３に開示されている乳化剤を使用することができるが、本発明の目的のためには、特に非テロゲン性乳化剤と呼ばれることがある乳化剤を好適に使用することができる。非テロゲン性乳化剤としては、たとえば炭素数６～２０程度、好ましくは炭素数６～１２程度のＦ（ＣＦ２）ｎ（ＣＨ２）ｍＣＯＯＨ（ｍ：０または１、ｎ：６～２０）で表されるフッ素含有アルカン酸またはその塩、フッ素含有アルキルスルホン酸またはその塩などを挙げることができる。塩としては、アルカリ金属塩、アンモニウム塩、アミン塩などを挙げることができる。具体的には、パーフルオロヘプタン酸、パーフルオロオクタン酸、及びそれらの塩、２－パーフルオロヘキシルエタンスルホン酸及びその塩などを挙げることができるがこれに限られるものではない。 In the emulsion polymerization method for preparing the PTFE aqueous dispersion, the emulsifier disclosed in the above-mentioned Patent Document 3 can be used as an emulsifier, but for the purpose of the present invention, it is specifically called a non-telogenic emulsifier. Emulsifiers can be preferably used. Examples of non-telogenic emulsifiers include F(CF 2 )n(CH 2 )mCOOH (m: 0 or 1, n: 6-20) having about 6 to 20 carbon atoms, preferably about 6 to 12 carbon atoms. fluorine-containing alkanoic acid or its salt, fluorine-containing alkylsulfonic acid or its salt, and the like. Salts include alkali metal salts, ammonium salts, amine salts and the like. Specific examples include perfluoroheptanoic acid, perfluorooctanoic acid and salts thereof, 2-perfluorohexylethanesulfonic acid and salts thereof, but are not limited thereto.
更にＰＴＦＥ水性分散液は、ＰＴＦＥ水性分散液の安定性を高めるため乳化安定剤を含んでいてもよい。乳化安定剤としては、炭化水素系アニオン系界面活性剤が好ましい。この界面活性剤は本質的に土中成分であるカルシウム、アルミニウム及び鉄分と水に不溶性又は難溶性の塩を形成するため、界面活性剤に起因する河川、湖沼及び地下水汚染を回避することが出来る。 Furthermore, the PTFE aqueous dispersion may contain an emulsion stabilizer to enhance the stability of the PTFE aqueous dispersion. Hydrocarbon anionic surfactants are preferred as emulsion stabilizers. Since this surfactant essentially forms a water-insoluble or sparingly soluble salt with calcium, aluminum and iron, which are soil components, pollution of rivers, lakes and groundwater caused by surfactants can be avoided. .
このような炭化水素系アニオン系界面活性剤としては、高級脂肪酸塩類、高級アルコール硫酸エステル塩類、液体脂肪油硫酸エステル塩類、脂肪族アルコールリン酸エステル塩類、二塩基性脂肪酸エステルスルホン酸塩類、アルキルアリルスルホン酸塩類などがあるが、特にポリオキシエチレンアルキルフェニルエーテルエチレンスルホン酸（ポリオキシエチレンのｎは１～６、アルキルの炭素数は８～１１）、アルキルベンゼンスルホン酸（アルキルの炭素数は１０～１２）、ジアルキルスルホコハク酸エステル（アルキルの炭素数は８～１０）などのＮａ，Ｋ，Ｌｉ及びＮＨ４ 塩は、ＰＴＦＥ水性分散液に高い機械的安定性を付与可能であり、高速攪拌等によりＰＴＦＥ粒子が凝集すること等が防止されるため、好ましいものとして例示することができる。 Examples of such hydrocarbon-based anionic surfactants include higher fatty acid salts, higher alcohol sulfate salts, liquid fatty oil sulfate salts, fatty alcohol phosphate salts, dibasic fatty acid ester sulfonates, alkylaryl There are sulfonates and the like, especially polyoxyethylene alkylphenyl ether ethylene sulfonic acid (n of polyoxyethylene is 1 to 6, alkyl has 8 to 11 carbon atoms), alkylbenzene sulfonic acid (alkyl has 10 to 10 carbon atoms), 12), Na, K, Li and NH4 salts such as dialkyl sulfosuccinates (alkyl has 8 to 10 carbon atoms) can impart high mechanical stability to PTFE aqueous dispersions, and high-speed agitation can Since aggregation of PTFE particles is prevented, it can be exemplified as a preferable one.
（塵埃抑制処理方法）
本発明の塵埃抑制処理方法は、上述した塵埃抑制処理剤組成物を発塵性物質と混合し、該混合物に２０～２００℃、好ましくは５０～１５０℃の温度で圧縮－剪断作用を施し該組成物中のＰＴＦＥをフィブリル化することにより、発塵性物質の塵埃の発生を抑制することができる。
すなわち、特定のＰＴＦＥは、上記したような適度な条件下で圧縮－剪断作用を施すとフィブリル化したクモの巣状に超微細繊維化するため、本発明の方法により処理された塵埃抑制処理物は、発塵性物質がクモの巣状の微細繊維に捕捉凝集されて塵埃抑制されていると考えられる。
(Dust suppression treatment method)
In the dust control treatment method of the present invention, the dust control agent composition described above is mixed with a dust-generating substance, and the mixture is subjected to a compression-shearing action at a temperature of 20 to 200°C, preferably 50 to 150°C. By fibrillating the PTFE in the composition, it is possible to suppress the generation of dust from dust-generating substances.
That is, when the specific PTFE is subjected to compression-shearing action under moderate conditions as described above, it becomes fibrillated spider web-like ultrafine fibers, so the dust-suppressing treated material treated by the method of the present invention is It is considered that dust-generating substances are trapped and aggregated by spider web-like fine fibers to suppress dust.
本発明の塵埃抑制処理法により処理される発塵性物質は、無機及び／または有機の発塵性物質であって、物質、形状などには特に限定はない。本発明は、発塵性物質として発塵性粉末状物質にも効果的に適用できる。特に好適に処理可能な発塵性物質としては、例えば、ポルトランドセメント、アルミナセメントなどのセメント類、消石灰、生石灰粉末、炭酸カルシウム、ドロマイト、マグネサイト、タルク、珪石、蛍石などの鉱産物粉末、カオリン、ベントナイト等の粘土鉱物粉、鉄鋼等の金属、非鉄金属の製造工程で副生されるスラグ粉末、石炭、ゴミ等の燃焼灰粉末、石膏粉末、粉末状金属、カーボンブラック、活性炭粉、金属酸化物等のセラミックス粉、顔料等が挙げられ、すなわち固体粒子状物質が空気中に飛散し浮遊し、塵埃を発生する全ての発塵性物質が挙げられる。 The dust-generating substances treated by the dust-suppressing treatment method of the present invention are inorganic and/or organic dust-generating substances, and there are no particular restrictions on the substance, shape, and the like. The present invention can also be effectively applied to dust-generating powdery substances as dust-generating substances. Dust-producing substances that can be particularly preferably treated include, for example, cements such as Portland cement and alumina cement, slaked lime, quicklime powder, mineral powders such as calcium carbonate, dolomite, magnesite, talc, silica, and fluorite, Clay mineral powder such as kaolin and bentonite, metals such as iron and steel, slag powder by-produced in the manufacturing process of non-ferrous metals, coal, combustion ash powder such as garbage, gypsum powder, powdered metals, carbon black, activated carbon powder, metals Examples include ceramic powder such as oxides, pigments, and the like, that is, all dust-generating substances that generate dust when solid particulate matter scatters and floats in the air.
本発明において、塵埃抑制処理剤組成物の発塵性物質への添加量は、発塵性物質の種類、粒度分布、比重（真比重、見掛け比重）、塵埃抑制処理温度、施す圧縮－剪断作用の度合い、得られる塵埃抑制処理物の塵埃抑制の程度等によって適宜設定することができる。
なお、添加量の目安としては、例えば、発塵性粉末状物質に対して塵埃抑制処理剤組成物をＰＴＦＥ樹脂固形分換算で０．００１～１．０質量％、好ましくは０．００５～０．５質量％の範囲で添加することにより、発塵性粉末状物質から発生する塵埃を抑制することができる。
In the present invention, the amount of the dust suppressing agent composition to be added to the dust-generating substance depends on the type of the dust-generating substance, particle size distribution, specific gravity (true specific gravity, apparent specific gravity), dust suppressing treatment temperature, compression-shearing action to be applied. It can be appropriately set depending on the degree of dust suppression, the degree of dust suppression of the obtained dust-suppressed product, and the like.
As a guideline for the amount to be added, for example, the dust suppressing treatment composition is 0.001 to 1.0% by mass, preferably 0.005 to 0.0%, in terms of PTFE resin solid content, relative to the dust-generating powdery substance. By adding in the range of 0.5% by mass, dust generated from the dust-generating powdery substance can be suppressed.
以下に本発明を、実施例および比較例を挙げてさらに具体的に説明するが、この説明が本発明を限定するものではない。
本発明において各物性の測定は、下記の方法によって行った。
EXAMPLES The present invention will be described in more detail below with reference to Examples and Comparative Examples, but the description does not limit the present invention.
In the present invention, each physical property was measured by the following methods.
（１）ＰＴＦＥ粒子の平均粒子径
ＰＴＦＥ粒子の平均粒径は、マイクロトラックＵＰＡ１５０ Ｍｏｄｅｌ Ｎｏ．９３４０（日機装社製）を用いて測定した。
（２）発塵性粉体の粒子径
（株）堀場製作所製レーザー回折／散乱式粒度分布測定器にて、エタノールを分散媒として測定した。
(1) Average Particle Diameter of PTFE Particles 9340 (manufactured by Nikkiso Co., Ltd.) was used for the measurement.
(2) Particle size of dust-generating powder Measured with a laser diffraction/scattering particle size distribution analyzer manufactured by HORIBA, Ltd. using ethanol as a dispersion medium.
（３）ＰＴＦＥの標準比重（ＳＳＧ）
ＡＳＴＭ Ｄ－４８９４により測定した。
乳化重合により得られるＰＴＦＥ水性分散体を、純水を用いて１５質量％濃度に調整する。その後ポリエチレン容器（１０００ｍｌ容量）に約７５０ｍｌ入れ手で激しく振蕩して重合体を凝集させる。水から分離した重合体のパウダーを１５０℃で１６時間乾燥する。乾燥した樹脂粉末１２．０ｇを直径２．８５ｃｍの円筒形型中に入れてならし、３０秒後に最終圧力が３５０ｋｇ／ｃｍ２となるよう圧力を次第に増加し、３５０ｋｇ／ｃｍ２の最終圧力で２分間保持する。このようにして得られた予備成形体を３０分間３８０℃の空気炉中で焼成した後、１分間１℃の割合で２９４℃まで冷却し、２９４℃で１分間保持した後、空気炉中から取り出し室温（２３±１℃）で冷却して標準試料とする。室温（２３℃±１℃）における同体積の水の重量に対する標準試料の重量比を標準比重とする。
この標準比重は平均分子量の目安となり、一般に標準比重が低い程分子量は大きい。
(3) Standard specific gravity of PTFE (SSG)
Measured according to ASTM D-4894.
A PTFE aqueous dispersion obtained by emulsion polymerization is adjusted to a concentration of 15% by mass using pure water. After that, the polymer is agglomerated by shaking vigorously with about 750 ml of a polyethylene container (1000 ml capacity) with a hand. The polymer powder separated from the water is dried at 150° C. for 16 hours. 12.0 g of dried resin powder was placed in a cylindrical mold with a diameter of 2.85 cm and leveled, and after 30 seconds the pressure was gradually increased to a final pressure of 350 kg/cm 2 , and the final pressure was 350 kg/cm 2 . Hold for 2 minutes. The preform thus obtained was fired in an air furnace at 380°C for 30 minutes, then cooled to 294°C at a rate of 1°C per minute, held at 294°C for 1 minute, and then removed from the air furnace. Take out and cool at room temperature (23±1°C) to use as a standard sample. The standard specific gravity is the weight ratio of the standard sample to the weight of the same volume of water at room temperature (23°C ± 1°C).
This standard specific gravity serves as a measure of the average molecular weight, and generally, the lower the standard specific gravity, the larger the molecular weight.
（４）静置沈降性試験
表１に示すように、１８．０ｇの塵埃抑制処理剤組成物またはＰＴＦＥ水性分散液を試験管に入れ、パラフィルムで試験管の口を閉じた後に、上下反転を２０回繰り返して混合した。その後、３０日間及び６０日間、各々室温にて静置した。３０日間または６０日間静置後、パラフィルムを取り、沈降している固形分以外（液部分：上澄み及び塵埃抑制処理剤組成物）を除去し、その重量（試験管の重量と試験管の底に沈降した固形分量の合計）を測定し、静置後の固形分量を算出した。
(4) Static sedimentation test As shown in Table 1, put 18.0 g of the dust control agent composition or PTFE aqueous dispersion in a test tube, close the mouth of the test tube with parafilm, and turn it upside down. was repeated 20 times to mix. After that, it was allowed to stand at room temperature for 30 days and 60 days. After standing still for 30 days or 60 days, remove the parafilm, remove the sedimented solid content (liquid part: supernatant and dust control agent composition), weigh the weight (weight of the test tube and the bottom of the test tube The total amount of solids sedimented to the bottom) was measured, and the amount of solids after standing was calculated.
（５）静置沈降再分散試験
上記（４）において静置した試験管の重量を測定し、該試験管に１０ｇの純水を加え、パラフィルムで試験管の口を閉じた後に、上下反転を２０回繰り返して混合した。その後、試験管の底に沈降している固形分以外（液部分：上澄み及び塵埃抑制処理剤組成物）を除去し、その重量（試験管の重量と試験管の底に沈降した固形分量の合計）を測定し、再分散後の固形分量を算出した。
(5) Static sedimentation redispersion test Measure the weight of the test tube left still in (4) above, add 10 g of pure water to the test tube, close the mouth of the test tube with parafilm, and then turn it upside down. was repeated 20 times to mix. After that, remove the solid content other than the solid content that has settled at the bottom of the test tube (liquid part: supernatant and dust control agent composition), and remove its weight (the total weight of the test tube and the amount of solid content that has settled at the bottom of the test tube ) was measured, and the solid content after redispersion was calculated.
（６）遠心分離沈降試験
表２に示す組成の塵埃抑制処理剤組成物またはＰＴＦＥ水性分散液１０ｇを、遠沈管（コーニング株式会社製、１５ｍｌ遠沈管）に入れ、遠心分離機（クボタ株式会社製、テーブルトップ冷却遠心機５５００、アングルローター ＲＡ５０８）を用い、温度２０℃、回転数３０００ｒｐｍにて３０分間遠心分離を行った。遠心分離後の遠沈管から遠沈管の底に沈降した固形分以外（液部分：上澄み及び塵埃抑制処理剤組成物）を除去し、遠沈管を逆さの状態で３０分間静置し液部分を更に除去して、その重量（遠沈管の重量と遠沈管の底に沈降した固形分量の合計）を測定し、上述した式（２）から固形分沈降割合、及び上述した式（１）から沈降率を算出した。
(6) Centrifugal sedimentation test 10 g of the dust control agent composition or PTFE aqueous dispersion having the composition shown in Table 2 is placed in a centrifuge tube (manufactured by Corning, 15 ml centrifuge tube) and centrifuged (manufactured by Kubota Corporation). , table top refrigerated centrifuge 5500, angle rotor RA508), and centrifuged at a temperature of 20° C. and a rotation speed of 3000 rpm for 30 minutes. From the centrifuge tube after centrifugation, remove the solid content other than the solids that have settled at the bottom of the centrifuge tube (liquid portion: supernatant and dust-inhibiting treatment composition), leave the centrifuge tube upside down for 30 minutes, and remove the liquid portion. Removed and measured the weight (the weight of the centrifuge tube and the total amount of solid content that settled at the bottom of the centrifuge tube), the solid content sedimentation ratio from the above equation (2), and the sedimentation rate from the above equation (1) was calculated.
（７）遠心分離再分散試験
上記（６）において液部分を除去した遠沈管の重量を測定し、該遠沈管に１０ｇの純水を加え、遠沈管の底に沈降した固形分を、３８ｋＨｚにて１分間超音波分散した後、遠沈管の底に沈降した固形分以外（液部分）を除去し、遠沈管を逆さの状態で３０分間静置し液部分を更に除去して、その重量（遠沈管の重量と遠沈管の底に沈降した固形分量の合計）を測定し、下記式（４）から再分散固形分沈降割合、及び下記式（３）から再分散沈降率を算出した。
(7) Centrifugal redispersion test The weight of the centrifuge tube from which the liquid portion was removed in (6) above was measured, 10 g of pure water was added to the centrifuge tube, and the solid content that settled at the bottom of the centrifuge tube was adjusted to 38 kHz. After ultrasonic dispersion for 1 minute, remove the solid content (liquid portion) other than the solid content that has settled at the bottom of the centrifuge tube, leave the centrifuge tube upside down for 30 minutes, remove the liquid portion, and remove the weight ( The total weight of the centrifuge tube and the amount of solid content that settled at the bottom of the centrifuge tube) was measured, and the redispersed solid content sedimentation ratio was calculated from the following equation (4), and the redispersion sedimentation ratio was calculated from the following equation (3).
再分散沈降率＝Ｘ３／Ｘ２ ・・・（３）
式中、
Ｘ２：前記水溶性セルロース誘導体を含まないＰＴＦＥ水性分散液１０ｇを、温度２０℃、回転速度３０００ｒｐｍにて３０分間、遠心分離機により遠心分離した後、再分散させた際の下記式（４）で示される固形分沈降割合（％）である。
Ｘ３：前記塵埃抑制処理剤組成物１０ｇを、温度２０℃、回転速度３０００ｒｐｍにて３０分間、遠心分離機により遠心分離した後、再分散させた際の下記式（４）で示される固形分沈降割合（％）である。
再分散後の固形分沈降割合（％）
＝（再分散後の固形分沈降量）／（遠心分離前の固形分量）×１００ ・・・（４）
Redispersion sedimentation rate = X 3 /X 2 (3)
During the ceremony,
X 2 : The following formula (4) when 10 g of the PTFE aqueous dispersion containing no water-soluble cellulose derivative is centrifuged at a temperature of 20° C. and a rotation speed of 3000 rpm for 30 minutes with a centrifuge, and then redispersed. is the solid content sedimentation ratio (%) shown.
X 3 : Solid content represented by the following formula (4) when 10 g of the dust suppressing treatment agent composition is centrifuged at a temperature of 20°C and a rotation speed of 3000 rpm for 30 minutes with a centrifuge, and then redispersed. Sedimentation rate (%).
Solid sedimentation ratio after redispersion (%)
= (Amount of sedimentation of solid content after redispersion) / (Amount of solid content before centrifugation) x 100 (4)
（８）落下粉塵量
内径３９ｃｍ、高さ５９ｃｍの円筒容器の頂部投入口より試料（塵埃処理物）２００ｇを自然落下させ、底面より高さ４５ｃｍの位置の容器内の浮遊粉塵量（相対濃度（ＣＰＭ：Ｃｏｕｎｔ ｐｅｒ Ｍｉｎｕｔｅ）を散乱光式デジタル粉塵計により測定する。浮遊粉塵量の測定は、試料投入後１分間計測を連続し５回行い、試料投入前の測定値（ダークカウント）を差し引いた値の幾何平均値を当該試料の「落下粉塵量」とする。幾何平均値ｘは下記式（５）により求める。
(8) Falling dust amount Let 200 g of the sample (dust-treated material) fall naturally from the top inlet of a cylindrical container with an inner diameter of 39 cm and a height of 59 cm, and the amount of floating dust in the container at a height of 45 cm from the bottom (relative concentration ( CPM (Counts per Minute) is measured by a scattered light digital dust meter.The amount of suspended dust is measured five times continuously for 1 minute after the sample is added, and the measured value (dark count) before the sample is subtracted. The geometric mean value of the values is defined as the “falling dust amount.” The geometric mean value x is obtained by the following formula (5).
Ｌｏｇ ｘ＝１／５×Σｌｏｇ（ｘｉ‐ｄ） ・・・（５）
式中、ｘｉ：個々の浮遊粉塵量、ｄ：ダークカウントである。
Log x=1/5×Σlog(xi−d) (5)
In the formula, xi: individual airborne dust amount, d: dark count.
（実施例１及び２）
乳化重合法により得られた樹脂固形分濃度３０質量％のＰＴＦＥ水性分散液（平均粒径０．２μｍ、含フッ素乳化剤含有量２１ｐｐｍ、比重（ＳＳＧ）２．１９、アニオン系界面活性剤をＰＴＦＥの重量に対して３．０質量％含む）、及びヒドロキシプロピルメチルセルロース（ＨＰＭＣ）（信越化学工業社製 メトローズ（登録商標）６５ＳＨ）を表１に記載した量で用い、塵埃抑制処理剤組成物を調製した。
得られた塵埃抑制処理剤組成物について、静置沈降性試験、静置沈降再分散試験を行った。結果を表１及び図１に示す。
(Examples 1 and 2)
PTFE aqueous dispersion with a resin solid content concentration of 30% by mass obtained by emulsion polymerization (average particle size 0.2 μm, fluorine-containing emulsifier content 21 ppm, specific gravity (SSG) 2.19, anionic surfactant added to PTFE) 3.0% by mass based on the weight) and hydroxypropyl methylcellulose (HPMC) (manufactured by Shin-Etsu Chemical Co., Ltd. Metolose (registered trademark) 65SH) in the amounts shown in Table 1 to prepare a dust suppressing treatment composition. did.
A static sedimentation test and a static sedimentation redispersion test were carried out on the obtained dust control agent composition. The results are shown in Table 1 and FIG.
（比較例１）
実施例１で用いた樹脂固形分濃度３０質量％のＰＴＦＥ水性分散液を用い、実施例１と同様にして静置沈降性試験、静置沈降再分散試験を行った。結果を表１及び図１に示す。
(Comparative example 1)
A stationary settling test and a stationary settling redispersion test were conducted in the same manner as in Example 1 using the PTFE aqueous dispersion having a resin solid content concentration of 30 mass % used in Example 1. The results are shown in Table 1 and FIG.
（実施例３～５）
実施例１で用いた樹脂固形分濃度３０質量％のＰＴＦＥ水性分散液及びＨＰＭＣを用い、表２に示す組成の塵埃抑制処理剤組成物を調製した。得られた塵埃抑制処理剤組成物について、遠心分離沈降性試験、遠心分離再分散試験を行った。結果を表２に示す。
(Examples 3-5)
Using the PTFE aqueous dispersion having a resin solid content concentration of 30% by mass and HPMC used in Example 1, a dust suppressing treatment agent composition having the composition shown in Table 2 was prepared. A centrifugal sedimentation test and a centrifugal redispersion test were carried out on the obtained dust control agent composition. Table 2 shows the results.
（比較例２）
実施例１で用いた樹脂固形分濃度３０質量％のＰＴＦＥ水性分散液を用い、実施例３と同様にして遠心分離沈降性試験、遠心分離再分散試験を行った。結果を表２に示す。
(Comparative example 2)
A centrifugal sedimentation test and a centrifugal redispersion test were conducted in the same manner as in Example 3 using the PTFE aqueous dispersion having a resin solid content concentration of 30 mass % used in Example 1. Table 2 shows the results.
（実施例６）
実施例１で用いた樹脂固形分濃度３０質量％のＰＴＦＥ水性分散液２００ｇを、冷蔵庫（１～３℃）で４０時間静置し、樹脂相と上澄み相に分離させた後、上澄み相を回収し、樹脂固形分濃度６６．６質量％、界面活性剤濃度２．６質量％のＰＴＦＥ水性分散液を得た。得られたＰＴＦＥ水性分散液に回収した上澄み相を添加し、樹脂固形分濃度６０．０質量％に調整した。この樹脂固形分濃度６０．０質量％のＰＴＦＥ水性分散液、及び実施例１で用いたＨＰＭＣを用い、表２に示すように、ＨＰＭＣが０．１８質量％、総重量が１５．０ｇの塵埃抑制処理剤組成物を調製した。得られた塵埃抑制処理剤組成物について、遠心分離沈降性試験、遠心分離再分散試験を行った。結果を表２に示す。
(Example 6)
200 g of the PTFE aqueous dispersion with a resin solid content concentration of 30% by mass used in Example 1 was allowed to stand in a refrigerator (1 to 3 ° C.) for 40 hours to separate the resin phase and the supernatant phase, and then the supernatant phase was recovered. Then, a PTFE aqueous dispersion having a resin solid content concentration of 66.6% by mass and a surfactant concentration of 2.6% by mass was obtained. The recovered supernatant phase was added to the obtained PTFE aqueous dispersion to adjust the resin solid content concentration to 60.0% by mass. Using this PTFE aqueous dispersion with a resin solid content concentration of 60.0% by mass and the HPMC used in Example 1, as shown in Table 2, HPMC is 0.18% by mass and dust with a total weight of 15.0 g An inhibitory treatment composition was prepared. A centrifugal sedimentation test and a centrifugal redispersion test were carried out on the obtained dust control agent composition. Table 2 shows the results.
（実施例７）
ＣａＯを９２．３％及びＭｇＯを１．１％含有する粉末生石灰（２．０ｍｍの標準網フルイを全通、６００μｍの標準網フルイ残分６．６９％、３００μｍの標準網フルイ残分２３．０７％、１５０μｍの標準網フルイ残分２０．００％、１５０μｍの標準網フルイ通過分５０．２４％の粉末生石灰）１，０００ｇを容積５リットルの小型ソイルミキサーに投入し、回転数１４０ｒ．ｐ．ｍ．で攪拌しながら、実施例５で調製した塵埃抑制処理剤組成物をＰＴＦＥが樹脂固形分換算で０．１ｇ（生石灰に対しＰＴＦＥ樹脂固形分で０．０１質量％）に相当する質量を秤量し、塵埃抑制処理剤組成物に含まれる水分と清水との合計が１００ｇになるように清水で希釈して、該組成物を分散させた分散液を徐々に投入した。
投入開始より約１分後には生石灰の水和反応熱による水蒸気を発生し始め、その後約２分で水分のすべてが生石灰の水和による消石灰の生成のため使用され尽くし、水蒸気の発生が無くなった。攪拌開始より３分後にミキサーの攪拌を止めた。このときの温度を温度計で計測すると１１６℃であった。この塵埃抑制処理された生石灰は、水和反応により新たに生成した消石灰約３０％を含む生石灰と消石灰の混合物であった。得られた塵埃抑制処理物の落下粉塵量を測定した。結果を表３に示す。
(Example 7)
Powdered quicklime containing 92.3% CaO and 1.1% MgO (through a 2.0 mm standard mesh sieve, 600 μm standard mesh sieve residue 6.69%, 300 μm standard mesh sieve residue 23.69%). 07%, 150 μm standard mesh sieve residue 20.00%, 150 μm standard mesh sieve passing content 50.24%) 1,000 g of powdered quicklime) was put into a small soil mixer with a volume of 5 liters, and the rotation speed was 140 r.p.m. p. m. While stirring, the dust suppressing treatment agent composition prepared in Example 5 was weighed in a mass corresponding to 0.1 g of PTFE in terms of resin solid content (0.01% by mass of PTFE resin solid content with respect to quicklime). , the dust-suppressing treatment agent composition was diluted with fresh water so that the total amount of water and fresh water contained in the composition was 100 g, and a dispersion containing the composition was gradually added.
About 1 minute after the start of feeding, steam started to be generated due to the heat of hydration reaction of quicklime, and in about 2 minutes after that, all of the water was exhausted for the production of slaked lime by hydration of quicklime, and the generation of steam stopped. . Stirring of the mixer was stopped 3 minutes after the start of stirring. When the temperature at this time was measured with a thermometer, it was 116°C. This dust-suppressing quicklime was a mixture of quicklime and slaked lime containing about 30% of slaked lime newly formed by hydration reaction. The amount of falling dust of the obtained dust-suppressing treated material was measured. Table 3 shows the results.
（実施例８、比較例３）
実施例６、比較例１で調製した塵埃抑制処理剤組成物を用いて、実施例７と同様にして塵埃抑制処理された生石灰と消石灰の混合物を得た。得られた塵埃抑制処理物の落下粉塵量を測定した。結果を表３に示す。
(Example 8, Comparative Example 3)
A mixture of quicklime and slaked lime treated for dust suppression was obtained in the same manner as in Example 7 using the dust suppression treatment composition prepared in Example 6 and Comparative Example 1. The amount of falling dust of the obtained dust-suppressing treated material was measured. Table 3 shows the results.
（実施例９）
実施例５で調製した塵埃抑制処理剤組成物を、ＰＴＦＥが樹脂固形分換算で０．２ｇ（生石灰に対しＰＴＦＥ樹脂固形分で０．０２質量％）に相当する質量を秤量し、塵埃抑制処理剤組成物に含まれる水分と清水との合計が１００ｇになるように清水で希釈して、該組成物を分散させた分散液を使用した以外は、実施例７と同様にして塵埃抑制処理された生石灰と消石灰の混合物を得た。得られた塵埃抑制処理物の落下粉塵量を測定した。結果を表３に示す。
(Example 9)
The dust suppressing treatment agent composition prepared in Example 5 was weighed in a mass equivalent to 0.2 g of PTFE in terms of resin solid content (0.02% by mass of PTFE resin solid content relative to quicklime), and dust suppressing treatment was performed. The dust suppression treatment was carried out in the same manner as in Example 7, except that the composition was diluted with fresh water so that the total amount of water and fresh water contained in the agent composition was 100 g, and the composition was dispersed. A mixture of quicklime and slaked lime was obtained. The amount of falling dust of the obtained dust-suppressing treated material was measured. Table 3 shows the results.
（実施例１０、比較例４）
実施例６、比較例１で用いた塵埃抑制処理剤組成物について、実施例９と同様にして塵埃抑制処理された生石灰と消石灰の混合物を得た。得られた塵埃抑制処理物の落下粉塵量を測定した。結果を表３に示す。
(Example 10, Comparative Example 4)
A mixture of quicklime and slaked lime was obtained in the same manner as in Example 9 with respect to the dust-inhibiting treatment composition used in Example 6 and Comparative Example 1. The amount of falling dust of the obtained dust-suppressing treated material was measured. Table 3 shows the results.
（比較例５）
塵埃抑制処理剤組成物を使用せず清水１００ｇを用いた以外は、実施例７と同様にして得られた生石灰と消石灰の混合物の落下粉塵量を測定した。結果を表３に示す。
(Comparative Example 5)
A mixture of quicklime and slaked lime was obtained in the same manner as in Example 7 except that 100 g of fresh water was used without using the dust-suppressing treatment agent composition, and the amount of falling dust was measured. Table 3 shows the results.
本発明の塵埃抑制処理剤組成物を用いた塵埃抑制処理方法は、建材分野、土壌安定材分野、固化材分野、肥料分野、焼却灰又は有害物質の埋立処分分野、防爆分野、化粧品分野、各種プラスチックス類への充填材分野等において、発塵性物質を塵埃抑制処理して発塵性物質の塵埃抑制処理物を得るのに好適に用いられる。 The dust suppression treatment method using the dust suppression treatment agent composition of the present invention can be used in various fields such as the field of building materials, the field of soil stabilizers, the field of solidifying materials, the field of fertilizers, the field of landfill disposal of incineration ash or hazardous substances, the field of explosion protection, and the field of cosmetics. In the field of fillers for plastics, etc., it is suitably used to obtain a dust-inhibiting treated product of a dust-producing substance by subjecting it to dust-inhibiting treatment.
Claims (7)
沈降率＝Ｘ１／Ｘ０＜１．０
式中、
Ｘ０：前記水溶性セルロース誘導体を含まないポリテトラフルオロエチレン水性分散液１０ｇを、温度２０℃、回転速度３０００ｒｐｍにて３０分間、遠心分離機により遠心分離した際の下記式で示される固形分沈降割合（％）
Ｘ１：前記塵埃抑制処理剤組成物１０ｇを、温度２０℃、回転速度３０００ｒｐｍにて３０分間、遠心分離機により遠心分離した際の下記式で示される固形分沈降割合（％）
固形分沈降割合（％）＝（遠心分離後の固形分沈降量）／（遠心分離前の固形分量）×１００ 7. The dust suppressing treatment method according to any one of claims 1 to 6, wherein the dust suppressing treatment agent composition has a sedimentation ratio of less than 1.0 as represented by the following formula.
Sedimentation rate = X 1 /X 0 <1.0
During the ceremony,
X 0 : Solid sedimentation represented by the following formula when 10 g of the polytetrafluoroethylene aqueous dispersion containing no water-soluble cellulose derivative is centrifuged at a temperature of 20° C. and a rotation speed of 3000 rpm for 30 minutes with a centrifuge. ratio(%)
X 1 : Solid sedimentation ratio (%) represented by the following formula when 10 g of the dust suppressing treatment agent composition is centrifuged at a temperature of 20°C and a rotation speed of 3000 rpm for 30 minutes with a centrifuge.
Solid content sedimentation ratio (%) = (solid content sedimentation amount after centrifugation) / (solid content amount before centrifugation) x 100
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