JP7377658B2 - Methods for surface treatment of stainless steel, methods for producing surface-treated stainless steel, and solutions used in these methods - Google Patents
Methods for surface treatment of stainless steel, methods for producing surface-treated stainless steel, and solutions used in these methods Download PDFInfo
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- JP7377658B2 JP7377658B2 JP2019176685A JP2019176685A JP7377658B2 JP 7377658 B2 JP7377658 B2 JP 7377658B2 JP 2019176685 A JP2019176685 A JP 2019176685A JP 2019176685 A JP2019176685 A JP 2019176685A JP 7377658 B2 JP7377658 B2 JP 7377658B2
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- stainless steel
- acid
- component
- salts
- surface treatment
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- 229910001220 stainless steel Inorganic materials 0.000 title claims description 88
- 239000010935 stainless steel Substances 0.000 title claims description 87
- 238000000034 method Methods 0.000 title claims description 55
- 238000004381 surface treatment Methods 0.000 title claims description 21
- 235000011007 phosphoric acid Nutrition 0.000 claims description 45
- 150000003016 phosphoric acids Chemical class 0.000 claims description 38
- 150000003839 salts Chemical class 0.000 claims description 32
- 238000004140 cleaning Methods 0.000 claims description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical class [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 claims description 15
- 150000001875 compounds Chemical class 0.000 claims description 13
- 239000006185 dispersion Chemical class 0.000 claims description 13
- 229910019142 PO4 Inorganic materials 0.000 claims description 12
- 235000021317 phosphate Nutrition 0.000 claims description 12
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 9
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 7
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- 238000004519 manufacturing process Methods 0.000 claims description 5
- 150000003013 phosphoric acid derivatives Chemical class 0.000 claims description 5
- DOOTYTYQINUNNV-UHFFFAOYSA-N Triethyl citrate Chemical compound CCOC(=O)CC(O)(C(=O)OCC)CC(=O)OCC DOOTYTYQINUNNV-UHFFFAOYSA-N 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
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- 235000013769 triethyl citrate Nutrition 0.000 claims description 4
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- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 14
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- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 4
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- 125000000217 alkyl group Chemical group 0.000 description 3
- 235000001014 amino acid Nutrition 0.000 description 3
- 229910021529 ammonia Inorganic materials 0.000 description 3
- BTANRVKWQNVYAZ-UHFFFAOYSA-N butan-2-ol Chemical compound CCC(C)O BTANRVKWQNVYAZ-UHFFFAOYSA-N 0.000 description 3
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- RUPBZQFQVRMKDG-UHFFFAOYSA-M Didecyldimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCC[N+](C)(C)CCCCCCCCCC RUPBZQFQVRMKDG-UHFFFAOYSA-M 0.000 description 2
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- WBHHMMIMDMUBKC-QJWNTBNXSA-M ricinoleate Chemical compound CCCCCC[C@@H](O)C\C=C/CCCCCCCC([O-])=O WBHHMMIMDMUBKC-QJWNTBNXSA-M 0.000 description 1
- 229940066675 ricinoleate Drugs 0.000 description 1
- 229960004889 salicylic acid Drugs 0.000 description 1
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 235000010413 sodium alginate Nutrition 0.000 description 1
- 239000000661 sodium alginate Substances 0.000 description 1
- 229940005550 sodium alginate Drugs 0.000 description 1
- 229940077386 sodium benzenesulfonate Drugs 0.000 description 1
- UKLNMMHNWFDKNT-UHFFFAOYSA-M sodium chlorite Chemical compound [Na+].[O-]Cl=O UKLNMMHNWFDKNT-UHFFFAOYSA-M 0.000 description 1
- 229960002218 sodium chlorite Drugs 0.000 description 1
- BTURAGWYSMTVOW-UHFFFAOYSA-M sodium dodecanoate Chemical compound [Na+].CCCCCCCCCCCC([O-])=O BTURAGWYSMTVOW-UHFFFAOYSA-M 0.000 description 1
- 229940082004 sodium laurate Drugs 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- MZSDGDXXBZSFTG-UHFFFAOYSA-M sodium;benzenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C1=CC=CC=C1 MZSDGDXXBZSFTG-UHFFFAOYSA-M 0.000 description 1
- 229940035044 sorbitan monolaurate Drugs 0.000 description 1
- 239000001593 sorbitan monooleate Substances 0.000 description 1
- 235000011069 sorbitan monooleate Nutrition 0.000 description 1
- 229940035049 sorbitan monooleate Drugs 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
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- 239000010959 steel Substances 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- XOAAWQZATWQOTB-UHFFFAOYSA-N taurine Chemical class NCCS(O)(=O)=O XOAAWQZATWQOTB-UHFFFAOYSA-N 0.000 description 1
- UJJLJRQIPMGXEZ-UHFFFAOYSA-N tetrahydro-2-furoic acid Chemical compound OC(=O)C1CCCO1 UJJLJRQIPMGXEZ-UHFFFAOYSA-N 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- UAXOELSVPTZZQG-UHFFFAOYSA-N tiglic acid Natural products CC(C)=C(C)C(O)=O UAXOELSVPTZZQG-UHFFFAOYSA-N 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- 229940117013 triethanolamine oleate Drugs 0.000 description 1
- UNXRWKVEANCORM-UHFFFAOYSA-N triphosphoric acid Chemical compound OP(O)(=O)OP(O)(=O)OP(O)(O)=O UNXRWKVEANCORM-UHFFFAOYSA-N 0.000 description 1
- 229940048102 triphosphoric acid Drugs 0.000 description 1
- 229960004418 trolamine Drugs 0.000 description 1
- 229940005605 valeric acid Drugs 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000000230 xanthan gum Substances 0.000 description 1
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- 229940082509 xanthan gum Drugs 0.000 description 1
- UHVMMEOXYDMDKI-JKYCWFKZSA-L zinc;1-(5-cyanopyridin-2-yl)-3-[(1s,2s)-2-(6-fluoro-2-hydroxy-3-propanoylphenyl)cyclopropyl]urea;diacetate Chemical compound [Zn+2].CC([O-])=O.CC([O-])=O.CCC(=O)C1=CC=C(F)C([C@H]2[C@H](C2)NC(=O)NC=2N=CC(=CC=2)C#N)=C1O UHVMMEOXYDMDKI-JKYCWFKZSA-L 0.000 description 1
Description
本発明は、ステンレス鋼の表面処理方法に関する。 The present invention relates to a method for surface treatment of stainless steel.
ステンレス鋼は建築、家電、厨房、輸送、産業等の様々な分野で利用されており、耐食性、耐熱性、強度、成形性等が必要とされる場面で用いられている。その中で化学・食品産業の設備や配管では、過酷な使用条件での腐食や金属片（異物）を防ぐため、ステンレス鋼の中でも特に耐食性に優れたＳＵＳ３１６が用いられる場合がある。 Stainless steel is used in various fields such as architecture, home appliances, kitchens, transportation, and industry, and is used in situations where corrosion resistance, heat resistance, strength, formability, etc. are required. Among these, SUS316, which has particularly excellent corrosion resistance among stainless steels, is sometimes used in equipment and piping in the chemical and food industries to prevent corrosion and metal fragments (foreign objects) under harsh usage conditions.
ステンレス鋼は鉄を主成分とし、種類によりニッケル、クロム等を含む合金である。ステンレス鋼の表面には鉄やクロムの酸化物、若しくはそれらの金属の水酸化物が存在しており、これらが不動態被膜として機能し耐食性に寄与するが、より耐食性を向上させるために硝酸を用いてステンレス鋼表面に酸化被膜を形成させる方法が知られている（例えば、特許文献１など）。この方法では、クロム濃度の高い不動態被膜を形成できることから、耐食性の高いステンレス鋼を得ることができる。一方で、この方法は、取り扱いが難しい硝酸を使用し、その廃液処理も煩雑であることから、作業者の負担が大きいという課題があった。 Stainless steel is an alloy whose main component is iron and may contain nickel, chromium, etc. depending on the type. Oxides of iron and chromium, or hydroxides of these metals exist on the surface of stainless steel, and these function as a passive film and contribute to corrosion resistance. A method is known in which an oxide film is formed on the surface of stainless steel using a method of forming an oxide film on the surface of stainless steel (for example, Patent Document 1). With this method, a passive film with a high chromium concentration can be formed, so stainless steel with high corrosion resistance can be obtained. On the other hand, this method uses nitric acid, which is difficult to handle, and its waste liquid treatment is also complicated, which poses a problem in that it places a heavy burden on the operator.
硝酸等の強酸を用いないステンレス鋼の表面処理方法としては、亜塩素酸ナトリウム溶液のような酸化剤を含む溶液を用いる方法が知られている（例えば、特許文献２など）。この方法では、耐食性に優れたステンレス鋼を得ることができるが、このステンレス鋼を用いた機材を、食品衛生分野に使用される過酸化水素水の貯蔵に用いた場合、過酸化水素水の安定度が低下してしまうという課題があった。 As a surface treatment method for stainless steel that does not use a strong acid such as nitric acid, a method using a solution containing an oxidizing agent such as a sodium chlorite solution is known (for example, Patent Document 2). With this method, stainless steel with excellent corrosion resistance can be obtained, but when equipment made of this stainless steel is used to store hydrogen peroxide water used in the food hygiene field, it is difficult to stabilize the hydrogen peroxide water. There was a problem with the degree of deterioration.
以上の状況を踏まえ、本発明は、硝酸等の強酸を用いず、作業性が良好である、ステンレス鋼を表面処理する方法を提供することを目的とする。さらに、過酸化水素水に接液させた場合に、過酸化水素の安定度を低下させないステンレス鋼を提供することも本発明の目的である。 In view of the above circumstances, an object of the present invention is to provide a method for surface treating stainless steel that does not use strong acids such as nitric acid and has good workability. Furthermore, it is another object of the present invention to provide a stainless steel that does not reduce the stability of hydrogen peroxide when it comes into contact with a hydrogen peroxide solution.
そこで本発明者等は鋭意検討し、リン酸類又はその塩をステンレス鋼に接触させて付着させる工程、特定の温度にステンレス鋼を加熱する工程、並びにクエン酸アンモニウム類及びクエン酸トリアルキルを含む水溶液でステンレス鋼を洗浄する工程、を含むステンレス鋼の表面処理方法により上記課題を解決できることを見出し、本発明に至った。 Therefore, the inventors of the present invention conducted extensive research and developed a process for bringing phosphoric acids or their salts into contact with stainless steel and depositing them, a process for heating stainless steel to a specific temperature, and an aqueous solution containing ammonium citrates and trialkyl citrate. The inventors have discovered that the above-mentioned problems can be solved by a method for surface treatment of stainless steel, which includes a step of cleaning the stainless steel, and have arrived at the present invention.
即ち、本発明は、
（１）リン酸類又はその塩をステンレス鋼に接触させる工程、
（２）ステンレス鋼を１００℃～５００℃に加熱する工程、及び
（３）（Ａ）成分：クエン酸アンモニウム類から選択される少なくとも１種の化合物、（Ｂ）成分：クエン酸トリアルキルから選択される少なくとも１種の化合物及び（Ｃ）成分：水を含む溶液でステンレス鋼を洗浄する工程
を含む、ステンレス鋼の表面処理方法である。
That is, the present invention
(1) A step of bringing phosphoric acids or their salts into contact with stainless steel,
(2) heating stainless steel to 100°C to 500°C, and (3) component (A): at least one compound selected from ammonium citrates, component (B): selected from trialkyl citrate. This is a method for surface treatment of stainless steel, which includes a step of cleaning stainless steel with a solution containing at least one compound and component (C): water.
本発明のステンレスの表面処理方法により、強酸を使用せず、取り扱いが容易な化学物質のみを用いてステンレス鋼に不働態皮膜を形成することができる。そして、本発明の表面処理方法で得られたステンレス鋼は、過酸化水素水を接液させても、過酸化水素の安定度が低下しないことから、食品衛生分野で使用される過酸化水素水用の機材に適用することができる。 According to the stainless steel surface treatment method of the present invention, a passive film can be formed on stainless steel using only easy-to-handle chemical substances without using strong acids. The stainless steel obtained by the surface treatment method of the present invention does not reduce the stability of hydrogen peroxide even when it comes into contact with hydrogen peroxide solution, so it is used in hydrogen peroxide solution used in the food hygiene field. It can be applied to equipment for
本発明は、以下の（１）～（３）の工程を含むステンレス鋼の表面処理方法である。
（１）リン酸類又はその塩をステンレス鋼に接触させる工程：
（２）ステンレス鋼を１００℃～５００℃に加熱する工程：
（３）（Ａ）成分：クエン酸アンモニウム類から選択される少なくとも１種の化合物、（Ｂ）成分：クエン酸トリアルキルから選択される少なくとも１種の化合物及び（Ｃ）成分：水を含む溶液でステンレス鋼を洗浄する工程：
The present invention is a method for surface treatment of stainless steel, which includes the following steps (1) to (3).
(1) Step of bringing phosphoric acids or their salts into contact with stainless steel:
(2) Process of heating stainless steel to 100°C to 500°C:
(3) Component (A): at least one compound selected from ammonium citrates, component (B): at least one compound selected from trialkyl citrate, and component (C): a solution containing water. The process of cleaning stainless steel with:
本発明における（１）の工程で使用されるリン酸類とは、例えば、リン酸（オルトリン酸）、亜リン酸、次亜リン酸、ピロリン酸、及び三リン酸などのポリリン酸、並びにこれらのリン酸類の塩を挙げることができる。
上記リン酸類の塩としては、例えば、上記に例示されたリン酸類のリチウム塩、ナトリウム塩、カリウム塩、マグネシウム塩、カルシウム塩、アルミニウム塩などを挙げることができる。
上記に挙げたリン酸類、又はリン酸類の塩は１種を単独で使用してもよく、２種以上を併用してもよい。
The phosphoric acids used in step (1) of the present invention include, for example, phosphoric acid (orthophosphoric acid), phosphorous acid, hypophosphorous acid, pyrophosphoric acid, polyphosphoric acid such as triphosphoric acid, and these Examples include salts of phosphoric acids.
Examples of the salts of the phosphoric acids include the lithium salts, sodium salts, potassium salts, magnesium salts, calcium salts, and aluminum salts of the phosphoric acids listed above.
The above-mentioned phosphoric acids or salts of phosphoric acids may be used alone or in combination of two or more.
上記に挙げたリン酸類、又はリン酸類の塩の中では、ステンレス鋼表面の不動態化、及び過酸化水素の安定化の観点から、リン酸類の塩を使用することが好ましく、リン酸アルミニウムを使用することが特に好ましい。 Among the phosphoric acids and salts of phosphoric acids mentioned above, it is preferable to use salts of phosphoric acids from the viewpoint of passivating the stainless steel surface and stabilizing hydrogen peroxide. Particularly preferred is the use of
本発明における（１）の工程では、上記リン酸類又はその塩をステンレス鋼に接触させるが、その方法は特に限定されないが、例えば、以下の方法を用いることができる。
（１－１）リン酸類、若しくはリン酸類の塩を含む溶液、又はリン酸塩の分散液をステンレス鋼に塗布する方法。
（１－２）リン酸類、若しくはリン酸類の塩を含む溶液、又はリン酸塩の分散液にステンレス鋼を浸漬させる方法。
（１－３）固形のリン酸塩をステンレス鋼に付着させる方法。
本発明の（１）の工程はこれらの方法のうち少なくとも１つ用いることが好ましい。
In step (1) of the present invention, the phosphoric acid or its salt is brought into contact with stainless steel, and the method is not particularly limited, but for example, the following method can be used.
(1-1) A method of applying a solution containing phosphoric acids or salts of phosphoric acids, or a dispersion of phosphates to stainless steel.
(1-2) A method of immersing stainless steel in a solution containing phosphoric acids or salts of phosphoric acids, or a dispersion of phosphates.
(1-3) A method of attaching solid phosphate to stainless steel.
It is preferable to use at least one of these methods in step (1) of the present invention.
上記リン酸類、又はリン酸類の塩を用いる場合は、水などの溶媒に溶解させた溶液、又は分散させた分散液を使用する場合、作業性が良好であるという点で好ましい。この時、溶液又は分散液中のリン酸類、又はリン酸類の塩の濃度としては、０．１～９０質量％が好ましく、１０～８５質量％であることがより好ましい。 When using the above-mentioned phosphoric acids or salts of phosphoric acids, it is preferable to use a solution dissolved in a solvent such as water or a dispersion liquid, since the workability is good. At this time, the concentration of phosphoric acids or salts of phosphoric acids in the solution or dispersion is preferably 0.1 to 90% by mass, more preferably 10 to 85% by mass.
上記（１－１）の、リン酸類、若しくはその塩を含む溶液、又はリン酸塩の分散液をステンレス鋼に塗布する方法としては、特に制限されず、公知の方法から適宜選択することが可能である。例えば、ロールコート法や、カーテンフロー法、スピンコート法、エアースプレー法、エアーレススプレー法などが挙げられる。 The method of applying the solution containing phosphoric acids or their salts or the dispersion of phosphates to stainless steel in (1-1) above is not particularly limited, and can be appropriately selected from known methods. It is. Examples include a roll coating method, a curtain flow method, a spin coating method, an air spray method, and an airless spray method.
上記（１－２）として、予めリン酸類、若しくはその塩を含む溶液、又はリン酸塩の分散液が入っている容器に、ステンレス鋼を、例えば１分～２時間浸漬させる、浸漬引き上げ法により、ステンレス鋼に溶液、又は分散液を付着させてもよい。
さらに、上記（１－３）として、上記リン酸塩を使用する場合は、ステンレス鋼の表面における不動態膜形成を効率よく行えるという観点から、固形のリン酸塩を直接ステンレス鋼の表面に付着させてもよい。
As for (1-2) above, stainless steel is immersed for 1 minute to 2 hours in a container containing a solution containing phosphoric acids or its salts, or a dispersion of phosphates, for example, by the immersion pulling method. , a solution or a dispersion may be applied to stainless steel.
Furthermore, as for (1-3) above, when using the above phosphate, solid phosphate is directly attached to the surface of stainless steel from the viewpoint of efficiently forming a passive film on the surface of stainless steel. You may let them.
本発明における（２）の工程は、ステンレス鋼を１００～５００℃に加熱する工程である。この工程では、（１）の工程でステンレス鋼の表面に付着した溶液、又は分散液に含まれるリン酸類、又はその塩により、ステンレス鋼の表面に鉄、クロム、又はニッケルの酸化物が形成する他、リン酸類が縮合したもの、又はその塩が生成する。また、リン酸類の塩を用いた場合は、リン酸類の塩の粒子同士が加熱により凝集し、粒子同士の隙間がなくなり、一つの層となることもある。これらの複合物が不動態被膜として機能する。加熱する温度としては、不働態被膜の生成効率の点から、１５０～４５０℃が好ましく、２００～４００℃がより好ましい。 Step (2) in the present invention is a step of heating stainless steel to 100 to 500°C. In this step, oxides of iron, chromium, or nickel are formed on the surface of stainless steel due to phosphoric acids or their salts contained in the solution or dispersion that adhered to the surface of stainless steel in step (1). In addition, condensed products of phosphoric acids or salts thereof are produced. In addition, when a salt of phosphoric acids is used, the particles of the salt of phosphoric acids may coagulate with each other due to heating, and the gaps between the particles may disappear, forming a single layer. These composites function as passive films. The heating temperature is preferably 150 to 450°C, more preferably 200 to 400°C, from the viewpoint of passive film production efficiency.
本発明における（３）の工程で使用される（Ａ）成分であるクエン酸アンモニウム類は、クエン酸モノアンモニウム、クエン酸ジアンモニウム、クエン酸トリアンモニウムを挙げることができる。この中でも、ステンレス鋼を過酸化水素水の保管、使用のための機材に用いた場合に、過酸化水素の安定度が高まるという観点から、クエン酸トリアンモニウムが好ましい。クエン酸トリアンモニウムは、クエン酸とアンモニア水を中和させて得ることができ、クエン酸モノアンモニウムまたはクエン酸ジアンモニウムとアンモニア水を中和させて得ることもできる。また、関東化学（株）や富士フィルム和光純薬（株）などで販売されている市販品を使用してもいい。 Examples of ammonium citrates which are component (A) used in step (3) of the present invention include monoammonium citrate, diammonium citrate, and triammonium citrate. Among these, triammonium citrate is preferred from the viewpoint of increasing the stability of hydrogen peroxide when stainless steel is used as equipment for storing and using hydrogen peroxide. Triammonium citrate can be obtained by neutralizing citric acid and aqueous ammonia, and can also be obtained by neutralizing monoammonium citrate or diammonium citrate and aqueous ammonia. Alternatively, commercial products sold by Kanto Kagaku Co., Ltd., Fuji Film Wako Pure Chemical Industries, Ltd., etc. may be used.
クエン酸アンモニウム類の使用量としては、（３）の工程で使用される溶液中にクエン酸アンモニウム類が０．１質量％～６０質量％の濃度で使用され、他の成分との相溶性の観点から０．１質量％～２５質量％の濃度で使用されることが好ましく、溶解速度の観点から、５質量％～１２．５質量％の濃度で使用されることがより好ましい。 The amount of ammonium citrate used is that ammonium citrate is used at a concentration of 0.1% by mass to 60% by mass in the solution used in step (3), and the amount of ammonium citrate used is 0.1% by mass to 60% by mass, depending on the compatibility with other components. From the viewpoint of the dissolution rate, it is preferably used at a concentration of 0.1% to 25% by mass, and from the viewpoint of dissolution rate, it is more preferably used at a concentration of 5% to 12.5% by mass.
本発明における（３）工程で使用される（Ｂ）成分であるクエン酸トリアルキルは、クエン酸に含まれる３つのカルボン酸が全てエステル化された化合物であり、ステンレス鋼の表面に付着した鉄を含む成分の除去に寄与するものである。クエン酸トリアルキル中のエステル化された部分のアルキル基としては、例えば、メチル基、エチル基、プロピル基、イソプロピル基、ブチル基、第２ブチル基、第３ブチル基、イソブチル基、ペンチル基、イソペンチル基、第２ペンチル基、第３ペンチル基、ヘキシル基などの炭素原子数が１～６のアルキル基が挙げられる。これらの中でも、ステンレス鋼を過酸化水素水の保管、使用のための機材に用いた場合に、過酸化水素の安定度が高まるという観点から、炭素原子数１～４のアルキル基が好ましく、メチル基、エチル基、プロピル基、イソプロピル基がより好ましく、食品添加物として使用できるという安全性の観点からエチル基が特に好ましい。 Trialkyl citrate, which is the component (B) used in step (3) in the present invention, is a compound in which all three carboxylic acids contained in citric acid are esterified, and it is a compound in which all three carboxylic acids contained in citric acid are esterified. This contributes to the removal of components including. Examples of the alkyl group in the esterified portion of trialkyl citrate include methyl group, ethyl group, propyl group, isopropyl group, butyl group, sec-butyl group, tertiary-butyl group, isobutyl group, pentyl group, Examples include alkyl groups having 1 to 6 carbon atoms such as an isopentyl group, a secondary pentyl group, a tertiary pentyl group, and a hexyl group. Among these, alkyl groups having 1 to 4 carbon atoms are preferred, and methyl , ethyl group, propyl group, and isopropyl group are more preferable, and ethyl group is particularly preferable from the viewpoint of safety so that it can be used as a food additive.
本発明の（Ｂ）成分であるクエン酸トリアルキルは、市販品を使用することもでき、例えば、クエン酸トリメチル、クエン酸トリエチルなどは関東化学（株）や富士フィルム和光純薬（株）などで販売されている。
本発明の（Ｂ）成分であるクエン酸トリアルキルの使用量としては、（３）の工程で使用される溶液中にクエン酸トリアルキルが０．２５質量％～１０質量％の濃度で使用され、界面活性の観点から、０．５質量％～１０質量％の濃度で使用されることが好ましく、他成分との相溶性の観点から１質量％～２．５質量％の濃度で使用されることがより好ましい。
Trialkyl citrate, component (B) of the present invention, can be commercially available. For example, trimethyl citrate, triethyl citrate, etc. are available from Kanto Kagaku Co., Ltd., Fuji Film Wako Pure Chemical Industries, Ltd. It is sold at.
The amount of trialkyl citrate used as component (B) of the present invention is such that trialkyl citrate is used at a concentration of 0.25% by mass to 10% by mass in the solution used in step (3). From the viewpoint of surface activity, it is preferably used at a concentration of 0.5% by mass to 10% by mass, and from the viewpoint of compatibility with other components, it is used at a concentration of 1% by mass to 2.5% by mass. It is more preferable.
本発明の（３）の工程で使用される溶液中の、（Ａ）成分と（Ｂ）成分の配合比は、それぞれの成分が上記濃度範囲内であれば特に限定されないが、通常、（Ａ）成分１００質量部に対して、（Ｂ）成分が５質量部～５０質量部、好ましくは１０質量部～４０質量部、より好ましくは１０質量部～２５質量部で使用される。 The blending ratio of component (A) and component (B) in the solution used in step (3) of the present invention is not particularly limited as long as each component is within the above concentration range, but usually (A Component (B) is used in an amount of 5 to 50 parts by weight, preferably 10 to 40 parts by weight, and more preferably 10 to 25 parts by weight, relative to 100 parts by weight of component (B).
本発明における（３）の工程で使用する溶液でステンレス鋼を洗浄する方法は、特に制限されず、例えば、（Ａ）、（Ｂ）、（Ｃ）成分を含む溶液が入っている容器に、ステンレス鋼を、例えば１０分～５時間浸漬させる方法が挙げられる。 The method for cleaning stainless steel with the solution used in step (3) of the present invention is not particularly limited, and for example, a container containing a solution containing components (A), (B), and (C) is placed in a container. A method of immersing stainless steel, for example, for 10 minutes to 5 hours is exemplified.
上記浸漬させる方法による洗浄においては、ステンレス鋼を過酸化水素水の保管、使用のための機材に用いた場合に、過酸化水素の安定度が高まるという観点から、（Ａ）、（Ｂ）、（Ｃ）成分を含む溶液の温度が２５～９０℃であることが好ましく、４０～９０℃であることがより好ましい。 In cleaning by the above-mentioned immersion method, from the viewpoint of increasing the stability of hydrogen peroxide when stainless steel is used as equipment for storing and using hydrogen peroxide, (A), (B), The temperature of the solution containing component (C) is preferably 25 to 90°C, more preferably 40 to 90°C.
本発明の（３）工程で使用される溶液においては、さらに（Ｄ）成分としてｐＨ調整剤を使用してもよい。（Ｄ）ｐＨ調整剤を使用することにより、ステンレス鋼の表面に付着した鉄を含む成分の洗浄力を向上させることができる。（Ｄ）ｐＨ調整剤としては、無機酸類、有機酸類、塩基類を挙げることができる。
上記無機酸類としては、例えば、硫酸、硝酸、ホウ酸、炭酸、次亜リン酸、亜リン酸、リン酸等が挙げられる。
In the solution used in step (3) of the present invention, a pH adjuster may further be used as component (D). (D) By using a pH adjuster, the ability to clean iron-containing components adhering to the surface of stainless steel can be improved. (D) Examples of the pH adjuster include inorganic acids, organic acids, and bases.
Examples of the inorganic acids include sulfuric acid, nitric acid, boric acid, carbonic acid, hypophosphorous acid, phosphorous acid, and phosphoric acid.
上記有機酸類としては、例えば、ギ酸、酢酸、プロピオン酸、酪酸、吉草酸、２－メチル酪酸、ｎ－ヘキサン酸、３，３－ジメチル酪酸、２－エチル酪酸、４－メチルペンタン酸、ｎ－ヘプタン酸、２－メチルヘキサン酸、ｎ－オクタン酸、２－エチルヘキサン酸、安息香酸、グリコール酸、サリチル酸、グリセリン酸、シュウ酸、マロン酸、コハク酸、グルタル酸、アジピン酸、ピメリン酸、マレイン酸、フタル酸、リンゴ酸、酒石酸、クエン酸、乳酸、ジグリコール酸、２－フランカルボン酸、２，５－フランジカルボン酸、３－フランカルボン酸、２－テトラヒドロフランカルボン酸、メトキシ酢酸、メトキシフェニル酢酸、フェノキシ酢酸、ヒドロキシエチリデンジホスホン酸、ニトリロトリス（メチレンホスホン酸）、ホスホノブタントリカルボン酸、エチレンジアミンテトラ（メチレンホスホン酸）等が挙げられる。 Examples of the above organic acids include formic acid, acetic acid, propionic acid, butyric acid, valeric acid, 2-methylbutyric acid, n-hexanoic acid, 3,3-dimethylbutyric acid, 2-ethylbutyric acid, 4-methylpentanoic acid, n- Heptanoic acid, 2-methylhexanoic acid, n-octanoic acid, 2-ethylhexanoic acid, benzoic acid, glycolic acid, salicylic acid, glyceric acid, oxalic acid, malonic acid, succinic acid, glutaric acid, adipic acid, pimelic acid, maleic acid Acid, phthalic acid, malic acid, tartaric acid, citric acid, lactic acid, diglycolic acid, 2-furancarboxylic acid, 2,5-furandicarboxylic acid, 3-furancarboxylic acid, 2-tetrahydrofurancarboxylic acid, methoxyacetic acid, methoxyphenyl Examples include acetic acid, phenoxyacetic acid, hydroxyethylidene diphosphonic acid, nitrilotris (methylenephosphonic acid), phosphonobutanetricarboxylic acid, ethylenediaminetetra (methylenephosphonic acid), and the like.
上記塩基類としては、例えば、アミンや水酸化第四級アンモニウム等の有機塩基、ナトリウム、カリウムなどのアルカリ金属の水酸化物、マグネシウムやカルシウムなどのアルカリ土類金属の水酸化物、アンモニア等が挙げられる。 Examples of the bases include organic bases such as amines and quaternary ammonium hydroxide, hydroxides of alkali metals such as sodium and potassium, hydroxides of alkaline earth metals such as magnesium and calcium, and ammonia. Can be mentioned.
上記に挙げた（Ｄ）ｐＨ調整剤の中でも、安全性、コスト、洗浄性の観点から、アンモニア、クエン酸、乳酸を使用することが好ましく、アンモニア、クエン酸を使用することがより好ましい。また、上記に例示した（Ｄ）ｐＨ調整剤は、１種類を単独で用いてもよく、２種以上を併用してもよい。 Among the pH adjusters (D) listed above, it is preferable to use ammonia, citric acid, and lactic acid, and it is more preferable to use ammonia and citric acid, from the viewpoints of safety, cost, and cleanability. Furthermore, the pH adjusters (D) exemplified above may be used alone or in combination of two or more.
上記に挙げた（Ｄ）ｐＨ調整剤の使用量としては、洗浄力と洗浄液の粘性、コスト等のバランスの観点から、（３）の工程で使用される溶液中にｐＨ調整剤が０．０００１質量％～１５質量％の濃度で含まれることが好ましく、０．０５質量％～１０質量％の濃度で含まれることがより好ましく、０．０５質量％～５質量％の濃度で含まれることが更に好ましい。 The amount of the pH adjuster (D) mentioned above is determined to be 0.0001% in the solution used in step (3) from the viewpoint of balance between cleaning power, viscosity of the cleaning liquid, cost, etc. It is preferably contained in a concentration of 0.05% by mass to 10% by mass, more preferably contained in a concentration of 0.05% by mass to 5% by mass. More preferred.
本発明の（３）の工程で使用される溶液のｐＨは、特に制限されるものではないが、洗浄性の点から、４～１２が好ましく、取り扱いの安全性の観点から６～８がより好ましい。 The pH of the solution used in step (3) of the present invention is not particularly limited, but from the viewpoint of cleaning properties, it is preferably 4 to 12, and from the viewpoint of handling safety, 6 to 8 is more preferable. preferable.
本発明の（３）の工程で使用される溶液は、必要に応じて、増粘剤、界面活性剤、キレート剤を含んでもよい。
上記増粘剤としては、例えば、グアーガム、エチルセルロース、キサンタンガム、カルボマー、カラギーナン、キトサン、ヒドロキシエチルセルロース、微結晶性セルロース、高分子量の固体ポリエチレングリコール、アルギン酸、アルギン酸ナトリウム、カルボキシメチルセルロースカルシウム、ケイ酸アルミニウムマグネシウム、コロイド状二酸化ケイ素などを挙げることができる。
The solution used in step (3) of the present invention may contain a thickener, a surfactant, and a chelating agent, if necessary.
Examples of the thickener include guar gum, ethylcellulose, xanthan gum, carbomer, carrageenan, chitosan, hydroxyethylcellulose, microcrystalline cellulose, high molecular weight solid polyethylene glycol, alginic acid, sodium alginate, calcium carboxymethylcellulose, magnesium aluminum silicate, Examples include colloidal silicon dioxide.
上記界面活性剤としては、例えば、一般的なアニオン性界面活性剤及びノニオン性界面活性剤、第一級アミン塩、第二級アミン塩、第三級アミン塩、第四級アミン塩及びピリジニウム塩等のカチオン性界面活性剤、ベタイン型、硫酸エステル型及びスルホン酸型等の両性界面活性剤等を使用することができる。 Examples of the surfactant include general anionic surfactants and nonionic surfactants, primary amine salts, secondary amine salts, tertiary amine salts, quaternary amine salts, and pyridinium salts. Cationic surfactants such as, amphoteric surfactants such as betaine type, sulfuric acid ester type, and sulfonic acid type can be used.
上記アニオン性界面活性剤として、ナトリウムドデシルサルフェート、カリウムドデシルサルフェート、アンモニウムドデシルサルフェート等のアルキルサルフェート類、ナトリウムドデシルポリグリコールエーテルサルフェート及びアンモニウムポリオキシエチレンアルキルエーテルサルフェート等のポリオキシエチレンエーテルサルフェート類；ナトリウムスルホリシノレート、スルホン化パラフィンのアルカリ金属塩、スルホン化パラフィンのアンモニウム塩等のアルキルスルホン酸塩類；ナトリウムラウレート、トリエタノールアミンオレート、トリエタノールアミンアビエテート等の脂肪酸塩類；ナトリウムベンゼンスルホネート、アルカリフェノールヒドロキシエチレンのアルカリ金属サルフェート等のアルキルアリールスルホネート類を使用することができる。さらに、高アルキルナフタレンスルホン酸塩、ナフタレンスルホン酸ホルマリン縮合物、ジアルキルスルホコハク酸塩、ポリオキシエチレンアルキルサルフェート塩、ポリオキシエチレンアルキルアリールサルフェート塩、ポリオキシエチレンエーテルリン酸塩、ポリオキシエチレンアルキルエーテル酢酸塩、Ｎ－アシルアミノ酸塩、及びＮ－アシルメチルタウリン塩等も使用することができる。 Examples of the anionic surfactants include alkyl sulfates such as sodium dodecyl sulfate, potassium dodecyl sulfate, and ammonium dodecyl sulfate; polyoxyethylene ether sulfates such as sodium dodecyl polyglycol ether sulfate and ammonium polyoxyethylene alkyl ether sulfate; Alkyl sulfonates such as ricinoleate, alkali metal salts of sulfonated paraffins, ammonium salts of sulfonated paraffins; fatty acid salts such as sodium laurate, triethanolamine oleate, triethanolamine abietate; sodium benzenesulfonate, alkali phenol hydroxy Alkylaryl sulfonates such as alkali metal sulfates of ethylene can be used. Furthermore, high alkyl naphthalene sulfonate, naphthalene sulfonic acid formalin condensate, dialkyl sulfosuccinate, polyoxyethylene alkyl sulfate salt, polyoxyethylene alkylaryl sulfate salt, polyoxyethylene ether phosphate, polyoxyethylene alkyl ether acetic acid Salts, N-acyl amino acid salts, N-acylmethyl taurine salts, etc. can also be used.
上記ノニオン性界面活性剤として、ソルビタンモノラウレート、ソルビタンモノオレート等の多価アルコールの脂肪酸部分エステル類、ポリオキシエチレングリコール脂肪酸エステル類、ポリグリセリン脂肪酸エステル類を使用することができる。さらに炭素数１～１８のアルコールのエチレンオキサイド及び／又はプロピレンオキサイド付加物、アルキルフェノールのエチレンオキサイド及び／又はプロピレンオキサイド付加物、アルキレングリコール及び／又はアルキレンジアミンのエチレンオキサイド及び／又はプロピレンオキサイド付加物等も使用することができる。 As the nonionic surfactant, fatty acid partial esters of polyhydric alcohols such as sorbitan monolaurate and sorbitan monooleate, polyoxyethylene glycol fatty acid esters, and polyglycerin fatty acid esters can be used. Furthermore, ethylene oxide and/or propylene oxide adducts of alcohols having 1 to 18 carbon atoms, ethylene oxide and/or propylene oxide adducts of alkylphenols, ethylene oxide and/or propylene oxide adducts of alkylene glycols and/or alkylene diamines, etc. can be used.
上記ノニオン性界面活性剤を構成する炭素数１～１８のアルコールは例えば、メタノール、エタノール、プロパノール、２－プロパノール、ブタノール、２－ブタノール、第３ブタノール、アミルアルコール、イソアミルアルコール、第３アミルアルコール、ヘキサノール、オクタノール、デカンアルコール、ラウリルアルコール、ミリスチルアルコール、パルミチルアルコール、及びステアリルアルコール等である。 Examples of alcohols having 1 to 18 carbon atoms constituting the nonionic surfactant include methanol, ethanol, propanol, 2-propanol, butanol, 2-butanol, tertiary butanol, amyl alcohol, isoamyl alcohol, tertiary amyl alcohol, These include hexanol, octanol, decane alcohol, lauryl alcohol, myristyl alcohol, palmityl alcohol, and stearyl alcohol.
上記アルキルフェノールは、例えば、フェノール、メチルフェノール、２，４－ジ第３ブチルフェノール、２，５－ジ第３ブチルフェノール、３，５－ジ第３ブチルフェノール、４－（１，３－テトラメチルブチル）フェノール、４－イソオクチルフェノール、４－ノニルフェノール、４－第３オクチルフェノール、４－ドデシルフェノール、２－（３，５－ジメチルヘプチル）フェノール、４－（３，５－ジメチルヘプチル）フェノール、ナフトール、ビスフェノールＡ、及びビスフェノールＦ等である。 Examples of the alkylphenol include phenol, methylphenol, 2,4-di-tert-butylphenol, 2,5-di-tert-butylphenol, 3,5-di-tert-butylphenol, and 4-(1,3-tetramethylbutyl)phenol. , 4-isooctylphenol, 4-nonylphenol, 4-tertiary octylphenol, 4-dodecylphenol, 2-(3,5-dimethylheptyl)phenol, 4-(3,5-dimethylheptyl)phenol, naphthol, bisphenol A, and bisphenol F, etc.
上記アルキレングリコールは、例えば、エチレングリコール、１，２－プロパンジオール、１，３－プロパンジオール、２－メチル－１，３－プロパンジオール、２－ブチル－２－エチル－１，３－プロパンジオール、１，４－ブタンジオール、ネオペンチルグリコール、１，５－ペンタンジオール、３－メチル－１，５－ペンタンジオール、２，４－ジエチル－１，５－ペンタンジオール、及び１，６－ヘキサンジオール等である。
上記アルキレンジアミンは、例えば先に説明したアルキレングリコールのアルコール性水酸基がアミノ基に置換された化合物である。上記エチレンオキサイド及びプロピレンオキサイド付加物としては、ランダム付加物とブロック付加物のいずれも使用することができる。
Examples of the alkylene glycol include ethylene glycol, 1,2-propanediol, 1,3-propanediol, 2-methyl-1,3-propanediol, 2-butyl-2-ethyl-1,3-propanediol, 1,4-butanediol, neopentyl glycol, 1,5-pentanediol, 3-methyl-1,5-pentanediol, 2,4-diethyl-1,5-pentanediol, and 1,6-hexanediol, etc. It is.
The alkylene diamine is, for example, a compound in which the alcoholic hydroxyl group of the alkylene glycol described above is substituted with an amino group. As the ethylene oxide and propylene oxide adducts, both random adducts and block adducts can be used.
上記カチオン性界面活性剤として例えば、ラウリルトリメチルアンモニウムクロライド、ステアリルトリメチルアンモニウムクロライド、ジステアリルジメチルアンモニウムクロライド、ジデシルジメチルアンモニウムクロライド、ラウリルベンジルジメチルアンモニウムクロライド、ジデシルジメチルアンモニウムクロライド、アルキルピリジニウムブロマイド及びイミダゾリニウムラウレート等を使用することができる。 Examples of the cationic surfactants include lauryltrimethylammonium chloride, stearyltrimethylammonium chloride, distearyldimethylammonium chloride, didecyldimethylammonium chloride, laurylbenzyldimethylammonium chloride, didecyldimethylammonium chloride, alkylpyridinium bromide, and imidazolinium. Laurate etc. can be used.
上記両性界面活性剤として例えば、ヤシ油脂肪酸アミドプロピルジメチル酢酸ベタイン、ラウリルジメチルアミノ酸ベタイン、２－アルキル－Ｎ－カルボキシメチル－Ｎ－ヒドロキシメチルイミダゾリニウムベタイン、ラウリルヒドロキシスルホベタイン、ラウロイルアミドエチルヒドロキシエチルカルボキシメチルベタイン、ヒドロキシプロピルリン酸の金属塩等のベタイン型両性界面活性剤、β－ラウリルアミノプロピオン酸の金属塩等のアミノ酸型両性界面活性剤、硫酸エステル型両性界面活性剤及びスルホン酸型両性界面活性剤を使用することができる。 Examples of the amphoteric surfactants include coconut oil fatty acid amidopropyl dimethyl acetate betaine, lauryl dimethyl amino acid betaine, 2-alkyl-N-carboxymethyl-N-hydroxymethylimidazolinium betaine, laurylhydroxysulfobetaine, lauroylamide ethyl hydroxyethyl Betaine type amphoteric surfactants such as carboxymethyl betaine and metal salts of hydroxypropyl phosphate, amino acid type amphoteric surfactants such as metal salts of β-lauryl aminopropionic acid, sulfate ester type amphoteric surfactants and sulfonic acid type amphoteric surfactants Surfactants can be used.
上記キレート剤としては、例えば、ニトリロ三酢酸、エチレンジアミン四酢酸、ジエチレントリアミン五酢酸、アスパラギン酸二酢酸、エチレンジアミンジコハク酸、若しくはこれらのアルカリ金属塩、又はアンモニウム塩などのアミノポリカルボン酸型キレート剤；カルボキシメチルオキシサクシネート、オキシジサクシネート、酒石酸モノサクシネート、酒石酸ジサクシネート、若しくはこれらのアルカリ金属塩、又はアンモニウム塩などのオキシカルボン酸型キレート剤、ニトリロトリメチレンホスホン酸、エチレンジアミンテトラメチレンホスホン酸、ヒドロキシエチリデンジホスホン酸、若しくはこれらのアルカリ金属塩、又はアンモニウム塩などのホスホン酸型キレート剤などが挙げられる。 Examples of the chelating agent include aminopolycarboxylic acid type chelating agents such as nitrilotriacetic acid, ethylenediaminetetraacetic acid, diethylenetriaminepentaacetic acid, aspartic acid diacetic acid, ethylenediamine disuccinic acid, or alkali metal salts or ammonium salts thereof; Oxycarboxylic acid type chelating agents such as carboxymethyl oxysuccinate, oxydisuccinate, tartrate monosuccinate, tartrate disuccinate, or alkali metal salts or ammonium salts thereof, nitrilotrimethylenephosphonic acid, ethylenediaminetetramethylenephosphonic acid, hydroxy Examples include phosphonic acid type chelating agents such as ethylidene diphosphonic acid, or alkali metal salts or ammonium salts thereof.
本発明のステンレス鋼の表面処理方法は、上記に挙げた（１）～（３）工程を、（１）、（２）、（３）の順序で行うことが好ましい。（１）の工程では、ステンレス鋼の表面にリン酸類、又はその塩が付着し、（２）の工程では、鉄、クロム、ニッケルの酸化物、リン酸類又はその塩の縮合物、リン酸類の塩の粒子同士が凝集した層を含む、不動態被膜を形成する。（３）の工程では、（２）の工程で生成した不動態膜中の鉄を含む成分を効率的に除去し、最終的に鉄成分ができるだけ残らない不動態被膜を形成したステンレス鋼を得ることができる。鉄は過酸化水素の分解の触媒として機能するため、表面に鉄成分が残っていないステンレス鋼を用いた機材は、過酸化水素水を接液させても過酸化水素の分解による濃度低下を抑制することから、過酸化水素水を使用するための機材として有用である。 In the stainless steel surface treatment method of the present invention, the steps (1) to (3) listed above are preferably performed in the order of (1), (2), and (3). In the step (1), phosphoric acids or their salts adhere to the surface of the stainless steel, and in the step (2), oxides of iron, chromium, and nickel, condensates of phosphoric acids or their salts, and phosphoric acids are deposited on the surface of the stainless steel. Forms a passive film containing a layer of agglomerated salt particles. In the step (3), the iron-containing components in the passive film produced in the step (2) are efficiently removed to finally obtain stainless steel with a passive film in which as little iron as possible remains. be able to. Iron acts as a catalyst for the decomposition of hydrogen peroxide, so equipment made of stainless steel with no iron components remaining on the surface prevents the concentration from decreasing due to decomposition of hydrogen peroxide even when it comes in contact with hydrogen peroxide solution. Therefore, it is useful as equipment for using hydrogen peroxide.
本発明のステンレス鋼の表面処理方法は、（１）、（２）、（３）の順序で、２～５回繰り返して行うことが好ましい。２～５回繰り返すことにより、鉄成分が除かれた不動態被膜の層が厚くなり、ステンレス鋼を過酸化水素水の保管、使用のための機材に用いた場合に、過酸化水素の安定度がより高まる。 The stainless steel surface treatment method of the present invention is preferably carried out in the order of (1), (2), and (3), repeated 2 to 5 times. By repeating this process 2 to 5 times, the layer of passive film from which the iron component is removed becomes thicker, and the stability of hydrogen peroxide increases when stainless steel is used as equipment for storing and using hydrogen peroxide. becomes higher.
本発明のステンレス鋼の表面処理方法においては、（１）～（３）の工程を行う前に、ステンレス鋼の表面に付着している油成分等を除くために、脱脂工程を含んでもよい。脱脂をするために使用される溶媒としては、例えば、ペンタン、ヘキサン、シクロヘキサン、四塩化炭素、トルエン、べンゼン、クロロホルム、塩化メチレン、テトラヒドロフラン、アセトン、酢酸エチル、メタノール、エタノール、プロパノール、イソプロパノールなどを挙げることができる。これらの脱脂工程をすることにより、（１）の工程で使用されるリン酸類、又はその塩を効率的に付着させることができる。 The stainless steel surface treatment method of the present invention may include a degreasing step before performing steps (1) to (3) in order to remove oil components etc. adhering to the surface of the stainless steel. Examples of solvents used for degreasing include pentane, hexane, cyclohexane, carbon tetrachloride, toluene, benzene, chloroform, methylene chloride, tetrahydrofuran, acetone, ethyl acetate, methanol, ethanol, propanol, isopropanol, etc. can be mentioned. By performing these degreasing steps, the phosphoric acids or salts thereof used in step (1) can be efficiently attached.
本発明のステンレス鋼の表面処理方法においては、（１）の工程で使用された未反応のリン酸類、又はその塩の除去、その他余分な不純物を除去するために、ステンレス鋼を水により洗浄する工程を含んでもよい。この時、洗浄する方法としては特に制限されず、流水によりステンレス鋼表面を洗い流してもよいし、水浴にステンレス鋼を浸漬させてもよい。 In the stainless steel surface treatment method of the present invention, the stainless steel is washed with water in order to remove unreacted phosphoric acids or their salts used in step (1) and other excess impurities. It may also include steps. At this time, the cleaning method is not particularly limited, and the stainless steel surface may be washed away with running water, or the stainless steel may be immersed in a water bath.
本発明のステンレス鋼の表面処理方法においては、ステンレス鋼表面に付着した水分等の揮発分を除去するために、乾燥工程を含んでもよく、例えば、１０～２４時間、４０～２００℃にてステンレス鋼を乾燥させることにより、揮発分を除去することができる。
なお、上記水による洗浄及び乾燥工程は、（３）の工程の後に行うことが好ましい。
In the stainless steel surface treatment method of the present invention, a drying step may be included in order to remove volatile components such as moisture adhering to the stainless steel surface. By drying the steel, volatile components can be removed.
Note that the water washing and drying steps are preferably performed after the step (3).
本発明におけるステンレス鋼は、主成分を鉄とする、ニッケルやクロムを含む合金であり、そのようなステンレス鋼としては、例えば、ＳＵＳＸＭ７、ＳＵＳ３０３、ＳＵＳ３０４、ＳＵＳ３０４Ｊ３、ＳＵＳ３０４Ｎ１、ＳＵＳ３０５ＪＩ、ＳＵＳ３１０Ｓ、ＳＵＳ３１６Ｌ、ＳＵＳ３１６、ＳＵＳ４０３、ＳＵＳ４１０、ＳＵＳ４３０などを挙げることができる。 The stainless steel in the present invention is an alloy whose main component is iron and contains nickel and chromium. Examples of such stainless steel include SUSXM7, SUS303, SUS304, SUS304J3, SUS304N1, SUS305JI, SUS310S, SUS316L, and SUS316. , SUS403, SUS410, SUS430, etc.
以下本発明を実施例により、具体的に説明する。尚、以下の実施例等において％は特に記載が無い限り質量基準である。 The present invention will be specifically explained below using examples. In addition, in the following examples and the like, % is based on mass unless otherwise specified.
［製造例１］
５００ｍｌビーカーにクエン酸トリアンモニウム（富士フィルム和光純薬（株）製）を５ｇ、クエン酸トリエチルを１ｇ、イオン交換水を９４ｇ加え、２５℃にて５分間攪拌を行い溶解させ洗浄液Ｘ－１を得た。
［製造例２］
５００ｍｌビーカーにクエン酸トリアンモニウム（富士フィルム和光純薬（株）製）を７．５ｇ、クエン酸トリエチルを１．５ｇ、イオン交換水を９１ｇ加え、２５℃にて５分間攪拌を行い溶解させ洗浄液Ｘ－２を得た。
[Manufacture example 1]
Add 5 g of triammonium citrate (manufactured by Fuji Film Wako Pure Chemical Industries, Ltd.), 1 g of triethyl citrate, and 94 g of ion-exchanged water to a 500 ml beaker, and stir at 25°C for 5 minutes to dissolve and prepare cleaning liquid X-1. Obtained.
[Manufacture example 2]
Add 7.5 g of triammonium citrate (manufactured by Fuji Film Wako Pure Chemical Industries, Ltd.), 1.5 g of triethyl citrate, and 91 g of ion-exchanged water to a 500 ml beaker, and stir at 25°C for 5 minutes to dissolve and prepare the cleaning solution. Obtained X-2.
［実施例１］
５０ｍｍ×５ｍｍ×１ｍｍのＳＵＳ３１６の試験片の表面をアセトンにて脱脂し試験片の質量を測定した、１０ｇの８５％リン酸水溶液と上記試験片を試験管に加え、１０分間静置させた後、ピンセットで試験片を取り、試験片の表面の液体を液切りし、試験片の質量を測定した結果、浸漬前の試験片より０．１ｇの質量増加が確認された。
次に、３００℃のマッフル炉の中に試験片を入れ、２時間静置した。その後、試験片を蒸留水で洗浄した後、８０℃の洗浄液Ｘ－１の中に試験片を２時間浸漬させた。
[Example 1]
The surface of a 50 mm x 5 mm x 1 mm SUS316 test piece was degreased with acetone and the mass of the test piece was measured. 10 g of 85% phosphoric acid aqueous solution and the above test piece were added to a test tube and left to stand for 10 minutes. A test piece was taken with tweezers, the liquid on the surface of the test piece was drained, and the mass of the test piece was measured. As a result, it was confirmed that the mass increased by 0.1 g compared to the test piece before immersion.
Next, the test piece was placed in a muffle furnace at 300°C and left to stand for 2 hours. Thereafter, the test piece was washed with distilled water, and then immersed in cleaning solution X-1 at 80°C for 2 hours.
その後、５０ｍＬのビーカーに５０ｍＬの３５％過酸化水素水をとり、該過酸化水素水に上記試験片を９８℃、５時間浸漬させた後、試験片を入れた５０ｍＬビーカー中の過酸化水素水の濃度を下記の過マンガン酸カリウム滴定により測定した。また、試験片を入れる前の過酸化水素水の濃度Ｃ０と比較して、上記試験片を入れた過酸化水素水の濃度Ｃの比（過酸化水素の安定度：（Ｃ／Ｃ０）×１００（％））が８５％以上のものを合格とした。結果を表１に示す。 Then, put 50 mL of 35% hydrogen peroxide in a 50 mL beaker, immerse the above test piece in the hydrogen peroxide at 98°C for 5 hours, and then place the test piece in the 50 mL beaker with hydrogen peroxide. The concentration of was measured by potassium permanganate titration as described below. In addition, the ratio of the concentration C of the hydrogen peroxide solution into which the test piece was added compared to the concentration C0 of the hydrogen peroxide solution before the test piece was added (stability of hydrogen peroxide: (C/C0) x 100 (%)) of 85% or more was considered to be a pass. The results are shown in Table 1.
［実施例２］
１０ｇの８５％リン酸水溶液の代わりに、１ｇのリン酸アルミニウム（純正化学（株）製）をアルミナ乳鉢で５分間粉砕させたものを９ｇの８５％リン酸水溶液に加え、５分間攪拌させた分散液に変更したこと以外は、実施例１と同様の操作を行い、過酸化水素の安定度を測定した。結果を表１に示す。
［実施例３］
洗浄液Ｘ－１を洗浄液Ｘ－２に変更したこと以外は、実施例１と同様の操作を行い、過酸化水素の安定度を測定した。結果を表１に示す。
[Example 2]
Instead of 10 g of 85% phosphoric acid aqueous solution, 1 g of aluminum phosphate (manufactured by Junsei Kagaku Co., Ltd.) was ground in an alumina mortar for 5 minutes, then added to 9 g of 85% phosphoric acid aqueous solution, and stirred for 5 minutes. The stability of hydrogen peroxide was measured by performing the same operation as in Example 1 except for changing to a dispersion liquid. The results are shown in Table 1.
[Example 3]
The stability of hydrogen peroxide was measured by carrying out the same operation as in Example 1, except that cleaning liquid X-1 was changed to cleaning liquid X-2. The results are shown in Table 1.
［実施例４］
５０ｍｍ×５ｍｍ×１ｍｍのＳＵＳ３１６の試験片の表面をアセトンにて脱脂した後、１ｇのリン酸アルミニウム（純正化学（株）製）をアルミナ乳鉢で５分間粉砕させたものを９ｇの８５％リン酸水溶液に加え、５分間攪拌させた分散液に、上記試験片を１０分間浸漬させた。その後、ピンセットで試験片を取り、試験片の表面の液体を液切りし、試験片の質量を測定した結果、浸漬前の試験片より０．１ｇの質量増加が確認された。この試験片の表面にリン酸アルミニウム（純正化学）の粉末を均一にまぶした後に試験片の重量を量ったところ、０．１１ｇの重量増加を確認した。
[Example 4]
After degreasing the surface of a 50 mm x 5 mm x 1 mm SUS316 test piece with acetone, 1 g of aluminum phosphate (manufactured by Junsei Kagaku Co., Ltd.) was ground in an alumina mortar for 5 minutes, and then 9 g of 85% phosphoric acid was ground. The test piece was immersed for 10 minutes in the dispersion that was added to the aqueous solution and stirred for 5 minutes. After that, the test piece was taken with tweezers, the liquid on the surface of the test piece was drained, and the mass of the test piece was measured. As a result, it was confirmed that the mass of the test piece was increased by 0.1 g compared to the test piece before immersion. When the surface of this test piece was uniformly sprinkled with powder of aluminum phosphate (Junsei Kagaku) and then weighed, it was confirmed that the weight increased by 0.11 g.
次に、３００℃のマッフル炉の中に試験片を入れ、２時間静置した。その後、試験片を蒸留水で洗浄した後、８０℃の洗浄液Ｘ－１の中に試験片を２時間浸漬させた。上記試験片を過酸化水素水に入れた後の、過酸化水素の安定度について、実施例１と同様に測定を行った。結果を表１に示す。 Next, the test piece was placed in a muffle furnace at 300°C and left to stand for 2 hours. Thereafter, the test piece was washed with distilled water, and then immersed in cleaning solution X-1 at 80°C for 2 hours. The stability of hydrogen peroxide after the test piece was placed in a hydrogen peroxide solution was measured in the same manner as in Example 1. The results are shown in Table 1.
［実施例５］
実施例４における、リン酸アルミニウム分散液に浸漬する工程、粉末のリン酸アルミニウムを付着させる工程、３００℃のマッフル炉の中で２時間静置する工程、蒸留水で洗浄する工程、及び８０℃の洗浄液Ｘ－１に浸漬する工程、を１サイクルとしたときに、同サイクルを２回繰り返した試験片の過酸化水素の安定度について、実施例１と同様に測定を行った。結果を表１に示す。
[Example 5]
In Example 4, the step of immersing in an aluminum phosphate dispersion, the step of attaching powdered aluminum phosphate, the step of standing still for 2 hours in a muffle furnace at 300 ° C., the step of washing with distilled water, and the step of 80 ° C. The stability of hydrogen peroxide of the test piece was measured in the same manner as in Example 1 after the same cycle was repeated twice, with the step of immersing it in cleaning solution X-1 as one cycle. The results are shown in Table 1.
［実施例６］
上記サイクルを３回繰り返したこと以外は、実施例５と同様の操作を行い、過酸化水素の安定度を測定した。結果を表１に示す。
［実施例７］
実施例１における、８５％リン酸水溶液に浸漬する工程、３００℃のマッフル炉の中で２時間静置する工程、蒸留水で洗浄する工程、及び８０℃の洗浄液Ｘ－１に浸漬する工程、を１サイクルとしたときに、同サイクルを３回繰り返した試験片の過酸化水素の安定度について、実施例１と同様に測定を行った。結果を表１に示す。
[Example 6]
The same operation as in Example 5 was performed except that the above cycle was repeated three times, and the stability of hydrogen peroxide was measured. The results are shown in Table 1.
[Example 7]
In Example 1, the step of immersing in an 85% phosphoric acid aqueous solution, the step of leaving it standing in a muffle furnace at 300 ° C. for 2 hours, the step of washing with distilled water, and the step of immersing in 80 ° C. cleaning liquid X-1, The stability of hydrogen peroxide in a test piece obtained by repeating the same cycle three times was measured in the same manner as in Example 1. The results are shown in Table 1.
［比較例１］
無処理の５０ｍｍ×５ｍｍ×１ｍｍのＳＵＳ３１６の試験片の過酸化水素の安定度について、実施例１と同様に測定を行った。結果を表１に示す。
［比較例２］
８０℃の洗浄液Ｘ－１に浸漬する工程を行わなかったこと以外は、実施例１と同様の操作を行い、過酸化水素の安定度を測定した。結果を表１に示す。
［比較例３］
８０℃の洗浄液Ｘ－１に浸漬する工程を行わなかったこと以外は、実施例２と同様の操作を行い、過酸化水素の安定度を測定した。結果を表１に示す。
[Comparative example 1]
The stability of hydrogen peroxide in an untreated 50 mm x 5 mm x 1 mm SUS316 test piece was measured in the same manner as in Example 1. The results are shown in Table 1.
[Comparative example 2]
The stability of hydrogen peroxide was measured by carrying out the same operation as in Example 1, except that the step of immersing it in 80° C. cleaning solution X-1 was not performed. The results are shown in Table 1.
[Comparative example 3]
The stability of hydrogen peroxide was measured by carrying out the same operation as in Example 2, except that the step of immersing it in 80° C. cleaning solution X-1 was not performed. The results are shown in Table 1.
表１の通り、本発明の方法で表面処理されたＳＵＳ３１６は、過酸化水素の安定度が高く、食品衛生分野の殺菌等で使用される過酸化水素水の機材として有用であることがわかった。未処理のＳＵＳ３１６は、比較例１で示される通り、過酸化水素の安定度が満足するものではなく、（３）の工程を行わなかった比較例２、比較例３においては、比較例１よりもさらに過酸化水素の安定度が悪く、（１）の工程において、ＳＵＳ３１６の表面における鉄の濃度が高くなってしまったことが要因であると推定される。 As shown in Table 1, SUS316 surface-treated by the method of the present invention has high hydrogen peroxide stability, and was found to be useful as a hydrogen peroxide solution equipment used for sterilization in the food hygiene field. . As shown in Comparative Example 1, untreated SUS316 does not have satisfactory hydrogen peroxide stability, and in Comparative Examples 2 and 3, in which step (3) was not performed, Furthermore, the stability of hydrogen peroxide is poor, and it is presumed that this is due to the fact that the concentration of iron on the surface of SUS316 increased in the step (1).
Claims (8)
（２）ステンレス鋼を１００℃～５００℃に加熱する工程、及び
（３）（Ａ）成分：クエン酸アンモニウム類から選択される少なくとも１種の化合物、（Ｂ）成分：クエン酸トリアルキルから選択される少なくとも１種の化合物及び（Ｃ）成分：水を含む溶液でステンレス鋼を洗浄する工程
を含み、前記（１）～（３）の工程を、（１）、（２）、（３）の順序で行う、ステンレス鋼の表面処理方法。 (1) A step of bringing phosphoric acids or their salts into contact with stainless steel,
(2) heating stainless steel to 100°C to 500°C, and (3) component (A): at least one compound selected from ammonium citrates, component (B): selected from trialkyl citrate. At least one compound and (C) component: The step of cleaning stainless steel with a solution containing water , and the steps (1) to (3) described above are ) Surface treatment method for stainless steel.
（１－１）リン酸類、若しくはリン酸類の塩を含む溶液、又はリン酸塩の分散液をステンレス鋼に塗布する工程、
（１－２）リン酸類、若しくはリン酸類の塩を含む溶液、又はリン酸塩の分散液にステンレス鋼を浸漬させる工程、及び
（１－３）固形のリン酸塩をステンレス鋼に付着させる工程、
の中から選択される少なくとも１つの工程を含む、請求項１に記載のステンレス鋼の表面処理方法。 The step (1) above is
(1-1) A step of applying a solution containing phosphoric acids or salts of phosphoric acids, or a dispersion of phosphates to stainless steel,
(1-2) A step of immersing stainless steel in a solution containing phosphoric acids or salts of phosphoric acids, or a dispersion of phosphate; and (1-3) A step of adhering solid phosphate to stainless steel. ,
The method for surface treatment of stainless steel according to claim 1, comprising at least one step selected from the following.
（２）ステンレス鋼を１００℃～５００℃に加熱する工程、及び(2) heating stainless steel to 100°C to 500°C, and
（３）（Ａ）成分：クエン酸アンモニウム類から選択される少なくとも１種の化合物、（Ｂ）成分：クエン酸トリアルキルから選択される少なくとも１種の化合物及び（Ｃ）成分：水を含む溶液でステンレス鋼を洗浄する工程(3) Component (A): at least one compound selected from ammonium citrates, component (B): at least one compound selected from trialkyl citrate, and component (C): a solution containing water. The process of cleaning stainless steel with
を含み、前記（１）～（３）の工程を、（１）、（２）、（３）の順序で行う、表面処理されたステンレス鋼の製造方法。A method for producing surface-treated stainless steel, comprising performing the steps (1) to (3) in the order of (1), (2), and (3).
（１）リン酸類又はその塩をステンレス鋼に接触させる工程、(1) A step of bringing phosphoric acids or their salts into contact with stainless steel,
（２）ステンレス鋼を１００℃～５００℃に加熱する工程、及び(2) heating stainless steel to 100°C to 500°C, and
（３）ステンレス鋼を洗浄する工程を含み、前記（１）～（３）の工程を、（１）、（２）、（３）の順序で行う、ステンレス鋼の表面処理方法又は表面処理されたステンレス鋼の製造方法における（３）のステンレス鋼を洗浄する工程に用いるための溶液。(3) A method for surface treatment of stainless steel or a method for surface treatment of stainless steel, including the step of cleaning the stainless steel, and performing the steps (1) to (3) above in the order of (1), (2), and (3). A solution for use in the step (3) of cleaning stainless steel in the method for manufacturing stainless steel.
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