JP2018052779A - Production method of slag - Google Patents
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Abstract
Description
本発明は、スラグの製造方法に関するものであり、より詳しくは、Ｆｅ及びＳｉを主成分とし、Ａｓ及びＰｂを不純物として含有するスラグから、その不純物の溶出を有効に抑制したスラグを効率的に得るスラグの製造方法に関する。 The present invention relates to a method for producing slag, and more specifically, from a slag containing Fe and Si as main components and As and Pb as impurities, the slag effectively suppressing the elution of the impurities is efficiently produced. The present invention relates to a method for producing slag.
コンクリートに配合される細骨材としては、従来、海砂や川砂、砂利等が用いられてきたが、天然資源であるこれらの砂は、環境保護の観点から採取量の削減や禁止の動きが強化されてきている。 Conventionally, sand, river sand, gravel, etc. have been used as fine aggregates to be mixed with concrete, but these sands, which are natural resources, have been moving to reduce or ban their collection from the viewpoint of environmental protection. It has been strengthened.
このような背景から、非鉄金属製錬、例えば銅の乾式製錬において副生成するスラグについて、コンクリート用細骨材としての適用がＪＩＳ Ａ５０１１−３として規格化され、安定的に供給可能なことから天然資源の各種砂からの代替の動きが加速している。 From such a background, because slag by-produced in nonferrous metal smelting, for example, dry smelting of copper, is standardized as JIS A5011-3 and can be stably supplied as a fine aggregate for concrete. Movements to replace natural resources from various types of sand are accelerating.
ところが、スラグを適用するにあたっては、平成１５年環境省告示第１９号に規定される有害物質の含有量試験（ＪＩＳ Ｋ００５８−２：２００５）、及び平成３年環境庁告示第４６号に規定される有害物質の溶出量試験（ＪＩＳ Ｋ００５８−１：２００５）の結果に基づいて、土壌汚染に関する基準を満たすことが求められている。特に、平成１５年環境省告示第１９号に規定される有害物質の含有量試験（ＪＩＳ Ｋ００５８−２：２００５）に基づく基準では、その規制が強化されており、Ａｓ（砒素）、Ｐｂ（鉛）の溶出量については、可能な限り低減させることが求められている。 However, in applying slag, it is stipulated in the toxic substance content test (JIS K0058-2: 2005) stipulated in the 2003 Ministry of the Environment Notification No. 19 and the 1991 Environment Agency Notification No. 46. Based on the results of the toxic substance elution test (JIS K0058-1: 2005), it is required to satisfy the standards for soil contamination. In particular, the standards based on the content test (JIS K0058-2: 2005) for hazardous substances stipulated in the Notification No. 19 of the Ministry of the Environment in 2003 have strengthened the regulations. As (arsenic), Pb (lead ) Is required to be reduced as much as possible.
例えば、特許文献１、非特許文献１においては、上述した有害物質の含有量試験及び有害物質の溶出量試験の両方において、スラグからのＡｓ及びＰｂの溶出量を抑えたスラグを安定的に製造する技術が示されている。 For example, Patent Document 1 and Non-Patent Document 1 stably produce slag that suppresses the elution amount of As and Pb from slag in both the above-mentioned harmful substance content test and harmful substance elution amount test. Technology to do is shown.
しかしながら、これらの文献に記載の技術は、スラグを５００℃〜８００℃の温度で加熱するというものであるが、３０分以上の時間を要することが記載されており、そのため大量のスラグを処理するにあたってかなりの長時間が必要となる。 However, although the technique described in these documents is that slag is heated at a temperature of 500 ° C. to 800 ° C., it is described that it takes 30 minutes or more, and therefore a large amount of slag is processed. It takes a considerable amount of time.
銅製錬のプロセス等から生成するスラグは大量であり、大量のスラグを短時間で処理して、Ａｓ及びＰｂの溶出量を抑えたスラグを効率的に製造する技術が求められている。 There is a large amount of slag produced from a copper smelting process and the like, and there is a need for a technique for efficiently producing slag with a reduced amount of As and Pb by treating a large amount of slag in a short time.
本発明は、このような実情に鑑みて提案されたものであり、Ａｓ及びＰｂを不純物として含有するスラグにおいて、その不純物の溶出の少ないスラグを短時間の処理で効率的に製造することができる方法を提供することを目的とする。 The present invention has been proposed in view of such a situation, and in a slag containing As and Pb as impurities, a slag with less elution of the impurities can be efficiently produced in a short process. It aims to provide a method.
本発明者らは、上述した課題を解決するために鋭意検討を重ねた。その結果、スラグに対して、大気圧雰囲気下で、９００℃以上の温度、２０秒以上３０分未満の時間で熱処理を施すことで、効率的な操作で、Ａｓ及びＰｂの溶出量を有効に抑制したスラグを製造できることを見出し、本発明を完成するに至った。 The inventors of the present invention have made extensive studies in order to solve the above-described problems. As a result, the amount of As and Pb eluted can be effectively controlled by applying heat treatment to the slag in an atmospheric pressure atmosphere at a temperature of 900 ° C. or higher and for a time of 20 seconds to less than 30 minutes. The present inventors have found that a suppressed slag can be produced and have completed the present invention.
（１）本発明の第１の発明は、Ｆｅ及びＳｉを主成分とし、Ａｓ及びＰｂを不純物として含有するスラグを、大気圧雰囲気下で、９００℃以上の温度、２０秒以上３０分未満の時間で熱処理する工程を含み、前記熱処理後に得られるスラグは、ＪＩＳＫ００５８−２に準じて測定されるＡｓ及びＰｂの溶出量が１５０ｍｇ／ｋｇ未満である、スラグの製造方法である。 (1) In the first invention of the present invention, a slag containing Fe and Si as main components and As and Pb as impurities is at a temperature of 900 ° C. or higher and 20 seconds or longer and less than 30 minutes in an atmospheric pressure atmosphere. The slag obtained after the heat treatment, which includes a step of heat treatment with time, is a method for producing slag in which the elution amounts of As and Pb measured according to JISK0058-2 are less than 150 mg / kg.
（２）本発明の第２の発明は、第１の発明において、前記スラグは、Ｐｂを０．０１質量％以上０．２質量％以下、Ａｓを０．０１質量％以上０．２質量％以下の割合で含有する、スラグの製造方法である。 (2) According to a second aspect of the present invention, in the first aspect, the slag includes 0.01 mass% to 0.2 mass% of Pb and 0.01 mass% to 0.2 mass% of As. It is the manufacturing method of slag contained in the following ratios.
（３）本発明の第３の発明は、第１又は第２の発明において、前記スラグは、Ｆｅを３５質量％以上４５質量％以下の割合で含有する、スラグの製造方法である。 (3) 3rd invention of this invention is a manufacturing method of slag in said 1st or 2nd invention, The said slag contains Fe in the ratio of 35 mass% or more and 45 mass% or less.
（４）本発明の第４の発明は、第１乃至第３のいずれかの発明において、前記スラグは、さらにＣａＯを１．０質量％以上６．０質量％以下の割合で含む、スラグの製造方法である。 (4) A fourth invention of the present invention is the slag according to any one of the first to third inventions, wherein the slag further contains CaO at a ratio of 1.0 mass% to 6.0 mass%. It is a manufacturing method.
（５）本発明の第５の発明は、第１乃至第４のいずれかの発明において、前記スラグは、水砕されたものである、スラグの製造方法である。 (5) The fifth invention of the present invention is the slag manufacturing method according to any one of the first to fourth inventions, wherein the slag is water-ground.
本発明によれば、Ａｓ及びＰｂを不純物として含有するスラグにおいて、その不純物の溶出の少ないスラグを短時間の処理で効率的に製造することができる。 ADVANTAGE OF THE INVENTION According to this invention, in the slag containing As and Pb as impurities, the slag with little elution of the impurities can be efficiently produced in a short time.
以下、本発明の具体的な実施形態（以下、「本実施の形態」という）について詳細に説明する。なお、本発明は、以下の実施形態に限定されるものではなく、本発明の要旨を変更しない範囲で種々の変更が可能である。また、本明細書において、「Ｘ〜Ｙ」（Ｘ、Ｙは任意の数値）との表記は、「Ｘ以上Ｙ以下」の意味である。 Hereinafter, a specific embodiment of the present invention (hereinafter referred to as “the present embodiment”) will be described in detail. In addition, this invention is not limited to the following embodiment, A various change is possible in the range which does not change the summary of this invention. In this specification, the notation “X to Y” (X and Y are arbitrary numerical values) means “X or more and Y or less”.
本実施の形態に係るスラグの製造方法は、銅の乾式製錬等の非鉄金属製錬のプロセスにて副産物として生成されるスラグであって、Ｆｅ及びＳｉを主成分とし、さらにＡｓ及びＰｂを不純物として含有するスラグから、それらＡｓ及びＰｂの溶出量を抑制したスラグを製造する方法である。 The method for producing slag according to the present embodiment is slag produced as a by-product in a non-ferrous metal smelting process such as dry smelting of copper, and mainly contains Fe and Si, and further contains As and Pb. This is a method for producing slag from which leaching amounts of As and Pb are suppressed from slag contained as impurities.
主成分とは、スラグ中の含有割合が５１質量％以上のものをいう。Ｆｅ及びＳｉを主成分とするスラグでは、主成分の含有割合とは、Ｆｅ及びＳｉの合計含有割合をいう。 A main component means that whose content rate in slag is 51 mass% or more. In the slag mainly composed of Fe and Si, the content ratio of the main component refers to the total content ratio of Fe and Si.
具体的に、このスラグの製造方法は、Ｆｅ及びＳｉを主成分とし、かつＡｓ及びＰｂを不純物として含有するスラグに対して、大気圧雰囲気下で、９００℃以上の温度、２０秒以上３０分未満の時間で熱処理する工程を含むことを特徴としている。このような方法により得られる熱処理後のスラグにおいては、ＪＩＳＫ００５８−２に準じて測定されるＡｓ及びＰｂの溶出量が１５０ｍｇ／ｋｇ未満となる。このように、本実施の形態に係るスラグの製造方法によれば、３０分未満の極めて短い時間で、Ａｓ及びＰｂの溶出量を抑制したスラグを安定的に製造することができる。 Specifically, this method for producing slag has a temperature of 900 ° C. or higher and 20 seconds or longer and 30 minutes under atmospheric pressure with respect to slag containing Fe and Si as main components and As and Pb as impurities. It is characterized by including a step of heat-treating in less time. In the slag after heat treatment obtained by such a method, the elution amounts of As and Pb measured according to JISK0058-2 are less than 150 mg / kg. As described above, according to the slag manufacturing method according to the present embodiment, it is possible to stably manufacture slag in which the elution amounts of As and Pb are suppressed in an extremely short time of less than 30 minutes.
（原料のスラグ）
原料のスラグは、上述せいたように、Ｆｅ及びＳｉを主成分とし、さらにＡｓ及びＰｂを含むスラグである。例えば、原料スラグの組成としては、Ｆｅの含有量が３５質量％〜４５質量％であり、ＳｉＯ２の含有量が２５質量％〜４０質量％であり、不純物成分としてＰｂを０．０１質量％〜０．２質量％、Ａｓを０．０１質量％〜０．２質量％の割合で含む。また、この原料スラグにおいては、Ｃｕを０．５質量％〜３．０質量％、ＣａＯを１．０質量％〜６．０質量％、及びその他の不純物として例えばＡｌ２Ｏ３（アルミナ）、ＭｇＯ（マグネシア）等を含んでいてもよい。
(Raw slag)
As described above, the raw material slag is a slag containing Fe and Si as main components and further containing As and Pb. For example, as the composition of the raw material slag, the Fe content is 35 mass% to 45 mass%, the SiO 2 content is 25 mass% to 40 mass%, and Pb is 0.01 mass% as an impurity component. -0.2 mass%, As is contained in the ratio of 0.01 mass%-0.2 mass%. Further, in this raw slag, the Cu 0.5 wt% to 3.0 wt%, the CaO 1.0 wt% to 6.0 wt%, and as other impurities as Al 2 O 3 (alumina), MgO (magnesia) etc. may be included.
なお、このようなスラグとしては、例えば、非鉄製錬スラグ、廃棄物溶融スラグ等が挙げられ、より具体的には、銅の製錬プロセスにて副産物として生成する銅スラグ（例えば、自溶炉スラグ、錬かん炉スラグ）が挙げられる。 Examples of such slag include non-ferrous smelting slag, waste melting slag, etc. More specifically, copper slag (for example, flash furnace) produced as a by-product in the copper smelting process Slag, smelting furnace slag).
加熱処理に対象となる原料スラグとしては、水砕されたものであることが好ましい。なお、水砕されたスラグを「水砕スラグ」という。加熱処理の対象となるスラグは、重金属溶出性を抑えるために、加熱処理による表面の酸化被膜の種類や膜厚を調整し、あるいは結晶化度を調整する観点から、予め水砕された水砕スラグを用いることが好ましい。スラグを水砕する方法としては、例えば、加圧水を噴射して粒状化する方法や、スラグを水槽に注入して急冷させることで粒状化する方法等が挙げられる。 The raw material slag to be subjected to the heat treatment is preferably water-crushed. The slag that has been crushed is referred to as “granulated slag”. In order to suppress heavy metal elution, the slag that is the subject of the heat treatment is a granulated water granulated in advance from the viewpoint of adjusting the type and thickness of the oxide film on the surface by the heat treatment or adjusting the crystallinity. It is preferable to use slag. Examples of the method of granulating slag include a method of spraying pressurized water to granulate and a method of granulating by injecting slag into a water tank and quenching.
通常、スラグは、非鉄製錬等の副産物として得られるものであり、水砕することにより、副産物であるスラグに対する冷却処理を兼ねることができ、大気中で徐冷するのに比べると冷却に要する時間を短くすることができる。また、水砕して急冷させることにより、スラグ組成をより均一にすることができる。このように、例えば製錬プロセスにて炉から取り出したスラグを使用する場合には、得られたスラグを水砕することによって、効率的に冷却し、加熱処理前のスラグを短時間で製品用途に適切な組成とすることができる。また、水砕することで、運搬しやすい粒度に効率的に調整することができる。 Usually, slag is obtained as a by-product such as non-ferrous smelting, and by water granulation, it can also serve as a cooling treatment for slag, which is a by-product, and requires cooling compared to slow cooling in the air Time can be shortened. Moreover, a slag composition can be made more uniform by carrying out water granulation and making it cool rapidly. Thus, for example, when using slag taken out of a furnace in a smelting process, the obtained slag is efficiently cooled by water granulation, and the slag before heat treatment is used in a product in a short time. It can be set as a suitable composition. Moreover, it can adjust efficiently to the particle size which is easy to convey by carrying out water granulation.
（Ａｓ及びＰｂの溶出抑制処理）
本実施の形態に係るスラグの製造方法においては、上述した原料のスラグに対して、９００℃以上の温度、２０秒以上３０分未満の時間の条件で熱処理する。
(As and Pb elution suppression treatment)
In the slag manufacturing method according to the present embodiment, the above-described raw material slag is heat-treated under conditions of a temperature of 900 ° C. or higher and a time of 20 seconds or longer and less than 30 minutes.
ここで、Ｆｅ及びＳｉを主成分とするスラグにおいて、微量含まれている不純物のＡｓやＰｂの溶出を抑制したスラグを得る方法として、結晶化を促進する方法がある。ところが、原料として水砕スラグを用いる場合には、この水砕処理により結晶化を促進させることは難しく、加熱及び冷却の工程が必要となる。また、スラグの表層をマグネタイトで覆うことによって溶出をバリアする層を形成する方法として、大気圧雰囲気下で５００℃程度の温度に加熱する方法が知られているが、処理に長時間を要する。 Here, in a slag mainly composed of Fe and Si, there is a method of promoting crystallization as a method of obtaining a slag in which trace amounts of impurities such as As and Pb are prevented from being eluted. However, when granulated slag is used as a raw material, it is difficult to promote crystallization by this granulation treatment, and heating and cooling steps are required. Further, as a method of forming a layer that blocks elution by covering the surface layer of slag with magnetite, a method of heating to a temperature of about 500 ° C. in an atmospheric pressure atmosphere is known, but the processing takes a long time.
本発明者らは、９００℃以上の温度条件で、かつ、２０秒以上３０分未満の短時間で熱処理することによって、スラグの表層のマグネタイト化と結晶性化の促進との、両方の作用を効率的に実現することができ、不純物であるＡｓ及びＰｂの溶出を有効に抑えることができることを見出した。 The inventors of the present invention have both the effects of magnetizing the surface layer of slag and promoting crystallization by heat-treating at a temperature of 900 ° C. or higher and in a short time of 20 seconds to less than 30 minutes. It has been found that it can be efficiently realized and elution of impurities As and Pb can be effectively suppressed.
熱処理における温度条件について、９００℃未満であると、処理に長時間を要してしまうとともに、スラグ表層のマグネタイト化を有効に促進させることができない。なお、温度の上限値としては、特に限定されないが、１５００℃以下であることが好ましい。熱処理温度が１５００℃を超えても、それ以上に効果の向上は期待されず、熱エネルギーが増大して効率的な処理を行うことができない。 When the temperature condition in the heat treatment is less than 900 ° C., the treatment takes a long time and the slag surface layer cannot be effectively magnetized. The upper limit of the temperature is not particularly limited, but is preferably 1500 ° C. or lower. Even if the heat treatment temperature exceeds 1500 ° C., no further improvement in the effect is expected, and the heat energy increases, so that efficient treatment cannot be performed.
また、熱処理の時間条件について、２０秒未満であると、熱処理が不十分となってＡｓ及びＰｂの溶出を効果的に抑えることができない。一方で、３０分を超えると、処理時間が長くなって非効率となるとともに、結晶化が有効に促進されず、十分に溶出を抑えることができない可能性がある。 Further, if the heat treatment time condition is less than 20 seconds, the heat treatment is insufficient and the elution of As and Pb cannot be effectively suppressed. On the other hand, if it exceeds 30 minutes, the treatment time becomes long and inefficient, and the crystallization is not effectively promoted, and the elution may not be sufficiently suppressed.
熱処理における加熱方法としては、特に限定されず、例えば、キルンのようなもので加熱することができ、また、バーナー等を使用して加熱してもよい。 It does not specifically limit as a heating method in heat processing, For example, it can heat with things like a kiln and may also heat using a burner etc.
以下、本発明の実施例を示してより具体的に説明するが、本発明は以下の実施例に何ら限定されるものではない。 EXAMPLES Hereinafter, the present invention will be described in more detail with reference to examples, but the present invention is not limited to the following examples.
＜原料スラグの調製＞
表１に示したような組成のスラグを原料スラグとして用いた。このスラグは、銅の溶融製錬（自溶炉）によって銅を製造するときに生成した副産物の溶融スラグを、水冷却によって水砕産物（水砕スラグ）とした。なお、スラグを適切に水砕するのに必要な水量は、スラグ１ｔ当たり１０ｍ３〜２０ｍ３であった。そして、水砕後のスラグに対して、篩い分けや破砕等の処理によって粒度調整加工を行い、粒径２ｍｍ以下に整粒した試験サンプルのスラグを調製した。
<Preparation of raw material slag>
Slag having a composition as shown in Table 1 was used as raw material slag. As for this slag, by-product molten slag produced when copper was produced by melting and smelting copper (self-smelting furnace) was converted into a granulated product (granulated slag) by water cooling. Incidentally, the amount of water needed to properly granulated slag was slag 1t per 10 m 3 to 20 m 3. And the particle size adjustment process was performed with respect to the slag after water granulation by processes, such as sieving and crushing, and the slag of the test sample which adjusted the particle size to 2 mm or less was prepared.
＜加熱処理＞
次に、試験サンプルのスラグを、アルミナ製の坩堝に装入し、下記表２の条件に基づいて加熱処理を施した。
<Heat treatment>
Next, the slag of the test sample was charged into an alumina crucible and subjected to heat treatment based on the conditions shown in Table 2 below.
＜加熱処理後に得られたスラグの評価＞
（平成１５年環境省告示第１９号（含有量試験））
ＪＩＳ Ｋ００５８−２に準じ、得られたスラグを粉砕して試料を得たのち、当該試料を用いて「六価クロム化合物及びシアン化合物以外の物質についての検液の調製」の項に従って検液を調製した。そして、得られた検液を用いて、ＪＩＳ Ｋ０１０２：２００８に従い、ＩＣＰ−ＡＥＳ（発光分光分析）法によりＰｂ、Ａｓの濃度を測定した。下記表２に測定結果を示す。
<Evaluation of slag obtained after heat treatment>
(2003 Ministry of the Environment Notification No. 19 (Content Test))
According to JIS K0058-2, the obtained slag is pulverized to obtain a sample, and then the sample is used according to the section “Preparation of a test solution for substances other than hexavalent chromium compounds and cyanide compounds”. Prepared. And the density | concentration of Pb and As was measured by ICP-AES (luminescence spectroscopy analysis) according to JISK0102: 2008 using the obtained test solution. The measurement results are shown in Table 2 below.
表２の結果に示すように、大気雰囲気下、９００℃以上の温度で２０秒以上３０分未満の熱処理を施した実施例１〜４では、ＪＩＳ Ｋ００５８−２に準じて測定されるＡｓ、Ｐｂの溶出量が、規格値の１５０ｍｇ／ｋｇ未満となり、有効に溶出を抑制できた。 As shown in the results of Table 2, As and Pb measured according to JIS K0058-2 in Examples 1 to 4 where heat treatment was performed at a temperature of 900 ° C. or higher for 20 seconds to less than 30 minutes in an air atmosphere. Elution amount was less than the standard value of 150 mg / kg, and the elution could be effectively suppressed.
一方、比較例１〜４では、熱処理温度が低いか、あるいは熱処理時間が短かったため、Ａｓ、Ｐｂの溶出量は、規格値の１５０ｍｇ／ｋｇを超える値となった。 On the other hand, in Comparative Examples 1 to 4, since the heat treatment temperature was low or the heat treatment time was short, the elution amounts of As and Pb exceeded the standard value of 150 mg / kg.
なお、従来例１では、熱処理温度８００℃で、１時間の熱処理を行った。その結果、Ａｓ、Ｐｂの溶出量は、規格値の１５０ｍｇ／ｋｇ未満となったものの、スラグを処理するに当たり長時間を要するという問題が生じた。 In Conventional Example 1, heat treatment was performed at a heat treatment temperature of 800 ° C. for 1 hour. As a result, the elution amounts of As and Pb were less than the standard value of 150 mg / kg, but there was a problem that it took a long time to process the slag.
Claims (5)
前記熱処理後に得られるスラグは、ＪＩＳＫ００５８−２に準じて測定されるＡｓ及びＰｂの溶出量が１５０ｍｇ／ｋｇ未満である
スラグの製造方法。 Including a step of heat-treating a slag containing Fe and Si as main components and As and Pb as impurities under an atmospheric pressure atmosphere at a temperature of 900 ° C. or higher and for a time of 20 seconds or longer and less than 30 minutes,
The slag obtained after the heat treatment is a slag manufacturing method in which the elution amounts of As and Pb measured in accordance with JISK0058-2 are less than 150 mg / kg.
請求項１に記載のスラグの製造方法。 The slag manufacturing method according to claim 1, wherein the slag contains Pb in a proportion of 0.01% by mass to 0.2% by mass and As in a proportion of 0.01% by mass to 0.2% by mass.
請求項１又は２に記載のスラグの製造方法。 The slag manufacturing method according to claim 1 or 2, wherein the slag contains Fe in a proportion of 35 mass% to 45 mass%.
請求項１乃至３のいずれか１項に記載のスラグの製造方法。 The slag manufacturing method according to any one of claims 1 to 3, wherein the slag further includes CaO at a ratio of 1.0 mass% to 6.0 mass%.
請求項１乃至４のいずれか１項に記載のスラグの製造方法。 The slag manufacturing method according to any one of claims 1 to 4, wherein the slag is water-ground.
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