JP5864284B2 - Removal of selenium from chlorine bypass dust washed waste water - Google Patents
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- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 title claims description 45
- 229910052711 selenium Inorganic materials 0.000 title claims description 45
- 239000011669 selenium Substances 0.000 title claims description 45
- 239000002351 wastewater Substances 0.000 title claims description 38
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 title claims description 28
- 239000000460 chlorine Substances 0.000 title claims description 28
- 229910052801 chlorine Inorganic materials 0.000 title claims description 28
- 239000000428 dust Substances 0.000 title claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- 238000000034 method Methods 0.000 claims description 19
- -1 rare earth compound Chemical class 0.000 claims description 15
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 15
- 239000003463 adsorbent Substances 0.000 claims description 11
- 229910052684 Cerium Inorganic materials 0.000 claims description 3
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 claims description 3
- 239000011147 inorganic material Substances 0.000 claims description 3
- 229910052746 lanthanum Inorganic materials 0.000 claims description 3
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000011368 organic material Substances 0.000 claims description 3
- UZLYXNNZYFBAQO-UHFFFAOYSA-N oxygen(2-);ytterbium(3+) Chemical compound [O-2].[O-2].[O-2].[Yb+3].[Yb+3] UZLYXNNZYFBAQO-UHFFFAOYSA-N 0.000 claims description 3
- 229910003454 ytterbium oxide Inorganic materials 0.000 claims description 3
- 229940075624 ytterbium oxide Drugs 0.000 claims description 3
- 229910052727 yttrium Inorganic materials 0.000 claims description 3
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 2
- 229910010272 inorganic material Inorganic materials 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- 239000012085 test solution Substances 0.000 description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- 239000004568 cement Substances 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- UNJPQTDTZAKTFK-UHFFFAOYSA-K cerium(iii) hydroxide Chemical compound [OH-].[OH-].[OH-].[Ce+3] UNJPQTDTZAKTFK-UHFFFAOYSA-K 0.000 description 5
- 238000001179 sorption measurement Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 239000003638 chemical reducing agent Substances 0.000 description 3
- 238000006477 desulfuration reaction Methods 0.000 description 3
- 230000023556 desulfurization Effects 0.000 description 3
- 229960002089 ferrous chloride Drugs 0.000 description 3
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 2
- 239000000920 calcium hydroxide Substances 0.000 description 2
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 2
- 235000011116 calcium hydroxide Nutrition 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000010979 pH adjustment Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000001112 coagulating effect Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Description
本発明は、セメント製造設備に付設された塩素バイパスシステムにて回収した塩素バイパスダストを水洗処理した際に発生した排水からセレンを除去する方法に関する。 The present invention relates to a method for removing selenium from waste water generated when a chlorine bypass dust collected by a chlorine bypass system attached to a cement manufacturing facility is washed with water.
従来、上記塩素バイパスシステムの排水に含まれるセレンを除去するにあたって、例えば、還元剤として塩化第一鉄（ＦｅＣｌ2）を用いて凝集沈殿処理を行う方法が記載されている（例えば、特許文献１参照）。 Conventionally, for removing selenium contained in the waste water of the chlorine bypass system, for example, a method of performing coagulation precipitation using ferrous chloride (FeCl 2 ) as a reducing agent has been described (for example, Patent Document 1). reference).
また、特許文献２に記載のセレン含有水の処理方法では、ｐＨ調整等の前処理を行うことなく、希土類化合物を含む吸着剤とセレンを含有する排水とを接触させ、排水中のセレンを簡易な工程で吸着除去する方法が提案されている。 Further, in the method for treating selenium-containing water described in Patent Document 2, an adsorbent containing a rare earth compound and wastewater containing selenium are brought into contact with each other without performing pretreatment such as pH adjustment, thereby simplifying selenium in the wastewater. A method of adsorbing and removing in a simple process has been proposed.
しかし、還元剤として塩化第一鉄を用いて凝集沈殿処理を行う方法では、排水中のセレン濃度を安全とされる基準まで除去するには、還元剤としての塩化第一鉄を大量に消費し、運転コストが高騰するという問題があった。 However, in the method of coagulating and precipitating using ferrous chloride as the reducing agent, a large amount of ferrous chloride as the reducing agent is consumed to remove the selenium concentration in the wastewater to a safe level. There was a problem that the operating cost would rise.
一方、特許文献２に記載のセレン含有水の処理方法では、ｐＨ調整等の前処理が不要で簡易な工程で処理できるという利点があるものの、種々の製造設備等で発生する具体的な個々の排水について適用可能かどうかは不明であり、個々の排水について、例えばｐＨ調整によってセレンの除去率が異なることも考えられた。 On the other hand, in the method for treating selenium-containing water described in Patent Document 2, there is an advantage that pretreatment such as pH adjustment is unnecessary and treatment can be performed in a simple process, but specific individual items generated in various production facilities and the like are available. It is unclear whether it can be applied to wastewater, and it has been considered that the removal rate of selenium varies depending on the pH of each wastewater, for example.
そこで、本発明は、上記の点に鑑みてなされたものであって、運転コストを低く抑えながら、排水から４価及び６価のセレンを高率で除去することを目的とする。 Then, this invention is made | formed in view of said point, Comprising: It aims at removing tetravalent and hexavalent selenium from waste water at a high rate, keeping operating cost low.
上記目的を達成するため、本発明は、塩素バイパスダストを水洗処理した際に発生した排水からのセレン除去方法であって、塩素バイパスダストを水洗処理した際に発生した排水をｐＨ３．０以上７．０未満に調整し、希土類化合物を含む吸着剤と接触させることを特徴とする。 In order to achieve the above object, the present invention is a method for removing selenium from wastewater generated when chlorine bypass dust is washed with water, and the wastewater generated when chlorine bypass dust is washed with water has a pH of 3.0 or more and 7 It is characterized by being adjusted to less than 0.0 and contacting with an adsorbent containing a rare earth compound.
ここで、塩素バイパスダストとは、セメントキルンの窯尻から最下段サイクロンに至るまでのキルン排ガス流路より、燃焼ガスの一部を抽気して塩素を除去する塩素バイパス設備から排出された、塩素等の揮発性成分を固形化させたダストをいい、塩素バイパスダストを水洗処理した際に発生した排水とは、このダストに水を加えてスラリー化した後、固液分離して得られるろ液等をいう。 Here, chlorine bypass dust refers to chlorine discharged from a chlorine bypass facility that extracts chlorine from a kiln exhaust gas passage from the bottom of the kiln of the cement kiln to the bottom cyclone to remove chlorine. The waste water generated when the chlorine bypass dust is washed with water is slurried by adding water to the dust, and then the liquid obtained by solid-liquid separation. Etc.
そして、本発明によれば、ｐＨを３．０以上７．０未満に調整してセレンを希土類化合物を含む吸着剤に吸着させることで、４価のセレンも６価のセレンも共に除去することが可能で、高いセレン除去率を達成することができ、運転コストを低く抑えながら、排水からセレンを高率で除去することができる。 According to the present invention, both tetravalent selenium and hexavalent selenium are removed by adjusting the pH to 3.0 or more and less than 7.0 and adsorbing selenium on an adsorbent containing a rare earth compound. And a high selenium removal rate can be achieved, and selenium can be removed from the waste water at a high rate while keeping operating costs low.
上記排水からのセレン除去方法において、前記希土類化合物は、イットリウム、ランタン、セリウム、イッテルビウムの酸化物、又は水酸化物の中から選ばれる１種類又は２種類以上の希土類化合物の混合物を含むことができる。 In the method for removing selenium from the waste water, the rare earth compound may include one or a mixture of two or more rare earth compounds selected from yttrium, lanthanum, cerium, ytterbium oxide, or hydroxide. .
また、上記排水からのセレン除去方法において、前記希土類化合物を多孔質の無機材料又は有機材料に担持させたものを前記吸着剤として使用することができ、セレンの吸着に供する表面積を増大させ、さらに効率よくセレンを吸着除去することができる。 Further, in the method for removing selenium from the waste water, a material in which the rare earth compound is supported on a porous inorganic material or organic material can be used as the adsorbent, and the surface area used for adsorption of selenium is increased. Selenium can be efficiently removed by adsorption.
以上のように、本発明によれば、 運転コストを低く抑えながら、塩素バイパスダストを水洗処理した際に発生した排水から４価及び６価のセレンを高率で除去することができる。 As described above, according to the present invention, tetravalent and hexavalent selenium can be removed at a high rate from the wastewater generated when the chlorine bypass dust is washed with water while keeping the operating cost low.
本発明に係る塩素バイパスダストを水洗処理した際に発生した排水（以下、適宜「排水」と略称する）からのセレン除去方法は、該排水をｐＨ３．０以上７．０未満に調整し、希土類化合物を含む吸着剤と接触させることを特徴とする。希土類化合物、特にイットリウム、ランタン、セリウム、イッテルビウムの酸化物、又は水酸化物の中から選ばれる１種類又は２種類以上の希土類化合物の混合物等は、４価及び６価のセレンを効果的に吸着除去することができ、排水中に４価のセレンと６価のセレンが共存する場合でも、排水のｐＨを３．０以上７．０未満に調整するだけでセレン除去が可能となる。尚、吸着剤として使用する希土類化合物は、上記列挙したものが好ましいが、これらに限定されるものではない。 The method for removing selenium from wastewater generated when the chlorine bypass dust according to the present invention is washed with water (hereinafter, abbreviated as “drainage” where appropriate) adjusts the wastewater to pH 3.0 or more and less than 7.0. It is characterized by contacting with an adsorbent containing a compound. Rare earth compounds, especially yttrium, lanthanum, cerium, ytterbium oxide, or a mixture of one or more rare earth compounds selected from hydroxides effectively adsorb tetravalent and hexavalent selenium. Even when tetravalent selenium and hexavalent selenium coexist in the wastewater, the selenium can be removed only by adjusting the pH of the wastewater to 3.0 or more and less than 7.0. The rare earth compounds used as the adsorbent are preferably those listed above, but are not limited thereto.
上記希土類化合物を粉末状にして直接排水に投入し、撹拌してセレンを吸着してもよいが、上記希土類化合物を多孔質の無機材料又は有機材料に担持させ、セレンの吸着に供する表面積を増大させたものを吸着剤として使用する方が、セレン除去率をさらに高めることができて好ましい。 The rare earth compound may be powdered and put directly into the wastewater, and stirred to adsorb selenium, but the rare earth compound is supported on a porous inorganic or organic material to increase the surface area for selenium adsorption. It is preferable to use the adsorbent as an adsorbent because the selenium removal rate can be further increased.
尚、塩素バイパスダストを水洗処理した際に発生した排水とは、セメント製造設備に付設された塩素バイパスシステムにて回収した塩素バイパスダストを水洗処理した際に発生した排水そのものだけでなく、該排水に重金属を除去する目的でＮａＳＨ溶液と、塩酸と、消石灰とを順次添加して得られた排水を含むものとする。 The wastewater generated when the chlorine bypass dust was washed with water was not only the wastewater itself generated when the chlorine bypass dust collected by the chlorine bypass system attached to the cement manufacturing facility was washed with water, but also the wastewater. In addition, wastewater obtained by sequentially adding a NaSH solution, hydrochloric acid, and slaked lime for the purpose of removing heavy metals is included.
また、塩素バイパスダストを水洗処理した際に発生した排水の他の例として、塩素バイパスダストに含まれるカルシウム分を用いた湿式排ガス脱硫処理排水が挙げられる。この脱硫処理は湿式処理であるため、排ガス中に含まれるＨＣｌガスも処理されている。 Another example of the wastewater generated when the chlorine bypass dust is washed with water is wet exhaust gas desulfurization treatment wastewater using calcium contained in the chlorine bypass dust. Since this desulfurization process is a wet process, HCl gas contained in the exhaust gas is also processed.
セメント製造設備に付設された塩素バイパスシステムにて回収した塩素バイパスダストを水洗処理した際に発生した排水を供試液とした。この供試液は、セレンを１．２ｐｐｍ含有しており、そのｐＨは１２．７であった。尚、本法におけるｐＨは、１２．０〜１３．５の数値範囲を取り得る。 Drainage generated when the chlorine bypass dust collected by the chlorine bypass system attached to the cement production facility was washed was used as a test solution. This test solution contained 1.2 ppm of selenium, and its pH was 12.7. In addition, pH in this method can take the numerical range of 12.0-13.5.
供試液を９００ｇ採取し、ＨＣｌ、ＮａＯＨ水溶液を添加し、所定のｐＨに調整した。そこに水酸化セリウム試薬６．８ｇを担持した樹脂を添加し、３０分間撹拌した。処理水に含まれるセレン濃度を測定したところ、図１に示す結果が得られた。ｐＨ＝１．０〜３．０での処理水は、ｐＨを上げるほど処理水に含まれるセレン濃度は低下した。ｐＨ＝３．０〜７．０での処理水に含まれるセレン濃度には、大きな変化がなく、０．１８〜０．２９ｐｐｍと低い数値であった。一方、ｐＨ＝１２．７での処理水に含まれるセレン濃度はこの範囲よりも高く、０．４５ｐｐｍであった。図２は、図１に示した処理水に含まれるセレン濃度からセレン除去率を算出したものであり、ｐＨ３．０〜７．０において高い除去率であった。 900 g of the test solution was collected, and HCl and NaOH aqueous solution were added to adjust to a predetermined pH. A resin carrying 6.8 g of cerium hydroxide reagent was added thereto and stirred for 30 minutes. When the selenium concentration contained in the treated water was measured, the results shown in FIG. 1 were obtained. In the treated water at pH = 1.0 to 3.0, the concentration of selenium contained in the treated water decreased as the pH was raised. The selenium concentration contained in the treated water at pH = 3.0 to 7.0 did not change greatly and was a low value of 0.18 to 0.29 ppm. On the other hand, the selenium concentration contained in the treated water at pH = 12.7 was higher than this range and was 0.45 ppm. FIG. 2 shows the selenium removal rate calculated from the selenium concentration contained in the treated water shown in FIG. 1, and the removal rate was high at pH 3.0 to 7.0.
セメント製造設備に付設された塩素バイパスシステムにて回収した塩素バイパスダストを水洗処理した際に発生した排水に、ＮａＳＨ溶液と塩酸と消石灰を順次添加して得られた排水を供試液とした。この供試液は、セレンを０．２４ｐｐｍ含有しており、そのｐＨは６．５であった。尚、本法におけるｐＨは、６．５〜８．５の数値範囲を取り得る。 The wastewater obtained by sequentially adding NaSH solution, hydrochloric acid and slaked lime to the wastewater generated when the chlorine bypass dust collected by the chlorine bypass system attached to the cement production facility was washed with water was used as a test solution. This test solution contained 0.24 ppm of selenium, and its pH was 6.5. In addition, pH in this method can take the numerical range of 6.5-8.5.
供試液を９００ｇ採取し、そこに水酸化セリウム試薬６．８ｇを担持した樹脂を添加し、３０分間撹拌した。処理水に含まれるセレン濃度を測定したところ、０．０９６ｐｐｍであり、除去率は６０％であった。 900 g of a test solution was collected, and a resin carrying 6.8 g of a cerium hydroxide reagent was added thereto, followed by stirring for 30 minutes. When the concentration of selenium contained in the treated water was measured, it was 0.096 ppm and the removal rate was 60%.
セメント製造設備に付設された塩素バイパスシステムにて回収した塩素バイパスダストに含まれるカルシウム分を用いた湿式排ガス脱硫処理排水を供試液とした。この供試液は、セレンを１．１ｐｐｍ含有しており、そのｐＨは５．０であった。尚、本法におけるｐＨは、４．０〜７．０の数値範囲を取り得る。 Wet exhaust gas desulfurization treatment wastewater using calcium contained in chlorine bypass dust collected by a chlorine bypass system attached to a cement production facility was used as a test solution. This test solution contained 1.1 ppm of selenium, and its pH was 5.0. In addition, pH in this method can take the numerical range of 4.0-7.0.
供試液を９００ｇ採取し、そこに水酸化セリウム試薬６．８ｇを担持した樹脂を添加し、３０分間撹拌した。処理水に含まれるセレン濃度を測定したところ、０．２０ｐｐｍであり、除去率は８２％であった。 900 g of a test solution was collected, and a resin carrying 6.8 g of a cerium hydroxide reagent was added thereto, followed by stirring for 30 minutes. When the concentration of selenium contained in the treated water was measured, it was 0.20 ppm and the removal rate was 82%.
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| JP5206453B2 (en) * | 2009-02-03 | 2013-06-12 | 宇部興産株式会社 | Cement kiln extraction dust processing method |
| JP5191058B2 (en) * | 2009-04-07 | 2013-04-24 | 太平洋セメント株式会社 | Wastewater treatment method |
| EP2435372A1 (en) * | 2009-05-27 | 2012-04-04 | Conocophillips Company | Operations of selenium removal sorbent beds |
| US8974676B2 (en) * | 2010-02-25 | 2015-03-10 | Phillips 66 Company | Treatment stages for selenium removal |
| JP5468945B2 (en) * | 2010-03-16 | 2014-04-09 | 太平洋セメント株式会社 | How to remove selenium |
| JP5003786B2 (en) * | 2010-03-31 | 2012-08-15 | 住友大阪セメント株式会社 | Method and apparatus for treating chlorine-containing waste as a raw material for cement |
| US20110290666A1 (en) * | 2010-05-25 | 2011-12-01 | Eric Vogler | Method and apparatus for removing selenium from water |
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