CS204318B1 - Process for restricting formation of the siliceous muds in the solution of hydrochloric acid at pickling silicon steels and device for making this process - Google Patents
Process for restricting formation of the siliceous muds in the solution of hydrochloric acid at pickling silicon steels and device for making this process Download PDFInfo
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- CS204318B1 CS204318B1 CS583678A CS583678A CS204318B1 CS 204318 B1 CS204318 B1 CS 204318B1 CS 583678 A CS583678 A CS 583678A CS 583678 A CS583678 A CS 583678A CS 204318 B1 CS204318 B1 CS 204318B1
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- Prior art keywords
- pickling
- hydrochloric acid
- valve
- solution
- siliceous
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- 238000005554 pickling Methods 0.000 title claims description 17
- 238000000034 method Methods 0.000 title claims description 12
- 229910000831 Steel Inorganic materials 0.000 title claims description 11
- 239000010959 steel Substances 0.000 title claims description 11
- 239000010703 silicon Substances 0.000 title claims description 10
- 229910052710 silicon Inorganic materials 0.000 title claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 title claims description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims description 8
- 230000015572 biosynthetic process Effects 0.000 title claims description 7
- 239000004094 surface-active agent Substances 0.000 claims description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 11
- 229910052751 metal Inorganic materials 0.000 claims description 7
- 239000002184 metal Substances 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 6
- 239000000377 silicon dioxide Substances 0.000 claims description 5
- 238000003860 storage Methods 0.000 claims description 5
- -1 alkylbenzene sulphate salt Chemical class 0.000 claims description 3
- 239000010695 polyglycol Substances 0.000 claims description 3
- 229920000151 polyglycol Polymers 0.000 claims description 3
- 125000002877 alkyl aryl group Chemical group 0.000 claims description 2
- 239000003945 anionic surfactant Substances 0.000 claims description 2
- 150000002170 ethers Chemical class 0.000 claims description 2
- 239000002736 nonionic surfactant Substances 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 239000000243 solution Substances 0.000 description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- 239000000499 gel Substances 0.000 description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- 239000011780 sodium chloride Substances 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 230000002401 inhibitory effect Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- XMIJDTGORVPYLW-UHFFFAOYSA-N [SiH2] Chemical compound [SiH2] XMIJDTGORVPYLW-UHFFFAOYSA-N 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 150000008055 alkyl aryl sulfonates Chemical class 0.000 description 1
- 150000004996 alkyl benzenes Chemical class 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 1
- 230000029142 excretion Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 125000005624 silicic acid group Chemical class 0.000 description 1
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
- 239000000080 wetting agent Substances 0.000 description 1
Landscapes
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
Description
Vynález sa týká sposobu obmedzovania tvorby křemičitých usadenín v roztoku kyseliny chlorovodíkovej pri moření křemíkových ocelí, najma dynamo a trafo plechov a zariadenia pre uskutočnenie tohto spósobu.BACKGROUND OF THE INVENTION The present invention relates to a method for limiting the formation of siliceous deposits in a hydrochloric acid solution in the pickling of silicon steels, in particular to dynamo and transformer sheets, and to apparatus for carrying out this method.
Vývoj morenia ocelí před ich dalším povrchovým spracovaním smeruje k vylučovaniu morenia v roztoku kyseliny sírovej a jeho nahradeniu roztokom kyseliny soinej. Toto však nie je možné pri oceliach s vyšším obsahom kremíka, najmá určených pre elektrotechnický priemysel, pretože dochádza k tvorbě křemičitých gélov a ich usadzovaniu v technologických rozvodoch a iných zariadeniach línky. Nie je vyriešená technológia obmedzovania ich tvorby pri moření, ani ich odstránenía z rozvodov. Neobstáli ani pokusy s ich odstraněním za pomoci horúcich' alkalických roztokov. Z toho dovodu je nutné tieto ocele nadalej aoriťlen v roztoku kyseliny sírovej, hoci sú známe nevýhody tejto technologie, ako sú vyššie straty kovu, vyšsia spotřeba moridla v dósledku neúplnej regenerácie a tým aj vyšší výskyt odpadných splodín. Pri moření v l^SO^ sa nutné používá inhibitor, napr. Ryphalgan A,pre zníženie úČinkov kyseliny sírovej na kov, ktorý obsahuje 81 % chloridu sodného, 10 % inhibičnej zložky a 9 2 alkylarylsulf onátti ako zraáčadla a dispergátora. Vznik spomínaných gélov v kyselině soinej vyplývá zo skutoČností, že elementárny křemík obsiahnutý vo vrstvě okují a v kove sa rozpúšča v neoxidujúcich minerálnych kyselinách za vzniku plynného kreraíkovodíka SiH^, ktorý sa vo vodných roztokoch móže rozkládat podlá reakcie:The development of the pickling of steels prior to their further surface treatment tends to eliminate the pickling in the sulfuric acid solution and replace it with a saline acid solution. However, this is not possible with higher silicon steels, especially for the electrical industry, because siliceous gels are formed and deposited in process lines and other line equipment. There is no solved technology to reduce their formation by pickling or to remove them from distribution lines. Attempts have also been made to remove them with hot alkaline solutions. For this reason, these steels still need to be aoritlene in sulfuric acid solution, although the disadvantages of this technology, such as higher metal loss, higher consumption of mordant due to incomplete regeneration and hence higher incineration waste, are known. In pickling in 1 SO 2, an inhibitor such as Ryphalgan A is required to reduce the effects of sulfuric acid on the metal, which contains 81% sodium chloride, 10% inhibitory component and 92 alkylarylsulfonate as a wetting agent and dispersant. The formation of said gels in saline acid results from the fact that the elemental silicon contained in the layer is scaled and dissolved in non-oxidizing mineral acids to form gaseous hydrogen silicon SiH2, which can be decomposed in aqueous solutions according to the reaction:
SiH4 + 2Η2θ - + SiO2 za vzniku kysličníka křemičitého, alebo je tento přítomný vo vrstvě okují, kde vznikol v dósledku oxidačných pochodov pri tvárniacich teplotách ocele. Zo zákonitosti ich elektrónovej stavby vyplývá, že volné molekuly kysličníka alebo kyseliny kremičitej nemóžu samostatné exis204318 ' .SiH 4 + 2Η 2 θ - + SiO 2 to form silica, or it is present in the scale layer, where it was formed as a result of oxidation processes at the forming temperatures of the steel. It is inherent in their electron structure that free oxide or silicic acid molecules cannot separate exis204318 '.
tovač á majú tendenciu savzájomne spojovat! a polymerizovať, pričom kyselina křemičitá i vo vodnom roztoku stráca postupné “vodu a mění sa na vysokomolekulárne kyseliny křemičitá, ktoré svojím celkovým zložením stoja medzi Si/OH/^ a S1O2· Tento proces sá navonok prejavuje vylučováním obj etane j gélovej usadeniny a pri zahrievaní sa ešte urýchíuje.Tailors tend to connect to each other! and polymerize, whereby the silicic acid, even in aqueous solution, loses the gradual water and becomes high molecular weight silicic acids, whose total composition stands between Si / OH / ^ and S1O2. This process is manifested externally by excretion of the gel deposit and heating is even faster.
Úlohou vynálezu bolo vytvořit také podmienky alebo reakcie, ktoré obmedzia možnost spojovania a polymerizácie molekul kysličníka křemičitého rozkladom kremíkovodíka, zabránia usadzovaniu. kremič itých gélov v rozvodech vytvořením antistatických účinkov a ne.pdsobia negativné na proces morenia a pri regenerácii moriaceho roztoku.SUMMARY OF THE INVENTION It is an object of the present invention to provide conditions or reactions that limit the possibility of coupling and polymerization of silica molecules by decomposing silicon hydrogen, preventing deposition. Silica gels in the pipelines by creating antistatic effects and do not negatively affect the pickling process and the regeneration of the pickling solution.
Uvedené nedostatky odstraňuje, problém rieši a vytýčené úlohy splňuje spósob obmedzovania tvorby křemičitých usadenín pre uvedený účel podlá vynálezu, ktorého podstata spočívá v tom, že do přidávaného množstva roztoku kyseliny chlorovodíkovej sa v úseku výstupu mořeného kovu přidává anionaktívny tenzid na báze lineárnych alkylbenzensulfonátov, s výhodou sodné sol alkylbenzensulfonátu a/alebo neíónogénny tenzid na báze alkylarylpolyglykoléterov, a to v koncentrácii 0,01 až 0,2 7» hmotnostných voči přidávanému množstvu kyseliny.The problem is solved, the problem is solved and the object is achieved by the method of limiting the formation of siliceous deposits according to the invention, which comprises adding an anionic surfactant based on linear alkyl benzene sulphonates to the amount of hydrochloric acid solution to be added. an alkylbenzene sulfonate sodium salt and / or a nonionic surfactant based on alkylaryl polyglycol ethers, at a concentration of 0.01 to 0.2% by weight relative to the amount of acid added.
Zariadenie pre uskutočnenie sposobu podlá vynálezu pozostáva v podstatě zo zásobnej nádrže tenzidu s výtokovým potrubím zaústěným do výtlačného potrubia čerpadla přídavného regenerovaného moridla šikmo v smere výtoku a opatřeným elektrickým uzatváracím ventílom, ďalej z prívodného potrubia tlakového vzduchu s elektrickým uzatváracím ventílom, pričom oba elektrická úzatváracie ventily sú zapojené na pohon čerpadla přídavného regenerovaného moridla.The apparatus for carrying out the method of the invention consists essentially of a surfactant supply tank with an outlet conduit opening into the discharge conduit of an additional regenerated mordant pump at an angle in the outlet direction and provided with an electric shut-off valve, compressed air supply line with an electric shut-off valve are connected to drive an additional regenerated pickling pump.
Výhodou vynálezu je, Že využitím novozístených vlastností povrchovoaktívnych látok v kombinácií so sposobom, množstvom a miestom ich pridávanie sa dosahuje podstatné obmedzenie vzniku křemičitých gélov priamo pri procese morenia, ako aj obmedzenie ich usadzovania v okruhu zariadení moriárne. Tým sa umožní, rovnocenné s inými druhmi oceli, morenie aj křemíkových ocelí v roztokoch kyseliny. solnéj, modernizácia ujednotenie technologického zariadenia moriarní a podstatná úspora na investičných nákladoch, vČítane nákladov na inštaláciu zariadení pre odstraňovanie usadenín. Laboratorně aj prevádzkové skúšky potvrdili podstatné zníženie koncentrácie kremíka v moriacom roztoku a jeho obsahu v usadenine pri přidávaní tenzidov.už v koncentrácii blízkej 0,1 % hmotnostných.It is an advantage of the invention that by utilizing the newly discovered properties of the surfactants in combination with the manner, amount and place of their addition, a significant reduction in the formation of silica gels directly in the pickling process, as well as their deposition in the circuit of the marine plant, is achieved. This permits pickling of silicon steels in acid solutions, equivalent to other types of steel. salvage, modernization of the unification of technological equipment of mariners and substantial savings in investment costs, including installation costs for the removal of deposits. Both laboratory and field tests have shown a significant reduction in the concentration of silicon in the pickling solution and its content in the sediment when adding surfactants to a concentration close to 0.1% by weight.
Příklady uskutočnenia sposobu podlá vynálezu.DETAILED DESCRIPTION OF THE INVENTION.
Příklad 1Example 1
K regenerovanému moriacemu roztoku, obsahujúcemu 150 až 160 g/1 HC1, 30 až 40 g/1 Fe+^ resp. 1 * až 3 g/1 Pe+3, privádzanému zo zásobných nádrží do moriacej vane v poalednom stupni výstupu mořeného kovu sa přidává sodná sol dodecylbenzénsulfonátu 0^^25 SO^Na v takom množstve, aby koncentrácia v regenerovanom morxdle bola 0,1 7» .hmotnostných, t. j. 1 g tenzidu na 1 liter moridla, najvhodnéjŠie vždy pri doplňovaní, alebo obměně moridla.To the regenerated pickling solution containing 150-160 g / l HCl, 30-40 g / l Fe @ +, respectively. 1 * to 3 g / l Pe + 3, fed from the storage tanks to the pickling tank in the first stage of pickled metal output, is added sodium dodecylbenzene sulfonate 0 ^^ 25 SO ^ Na in such a quantity that the concentration in the regenerated morxdle is 0.1 7 The weight, i.e. 1 g of surfactant per liter of mordant, is always best when adding or changing the mordant.
Příklad rovnakom čase a rovnakým spósobora ako 9H19 /OCHgCHj/jOH v množstveExample at the same time and with the same factor as 9 H 19 / OCH 3 CH 3 / iOH in an amount
K regenerovanému moridlu řovnakého zloženia v v příklade 1 sa přidává alkylfenol-polyglykoléter C 0,5 g tenzidu na 1 liter moridla.To the regenerated mordant of the same composition in Example 1 is added an alkylphenol polyglycol ether C of 0.5 g surfactant per liter of mordant.
Přiklad uskutočnenia zariadenia podlá vynálezu je znázorněný na přiloženou výkrese v schématickou čiastočnom řeze.An exemplary embodiment of the device according to the invention is shown in the attached drawing in a schematic partial section.
Zásobná nádrž 10 tenzidu je umiestnená zvislo a je opatřená prívodným potrubím 11 s ventilom, prívodným potrubím 12 tlakového vzduchu s regulačným ventílom 13 a elektrickým uzatvácim ventílom > 4, ako aj elektrickým uzatváracím ventílom 15 tenzidu so spátným ventílom 16 vo výtokovom potrubí 20. Výtokové potrubie 20 je zaústěné otvorom 22 v zošikmenotn ohybe 2J^ \The surfactant storage tank 10 is located vertically and is provided with a valve inlet pipe 11, a compressed air inlet pipe 12 with a control valve 13 and an electric shut-off valve> 4, as well as an electric shut-off valve 15 of the surfactant with a return valve 16 in the outlet pipe 20. 20 is connected to the opening 22 in the bevel 20 '
do výtlačného potrubia 31 čerpadla 30 přídavného regenerovaného morídla. Od pohonu 41 je zapojená ovládacia svorka 42 elektrického uzatváracieho ventilu 14 vzduchu a súčasne je zapojená ovládacia svorka 43 elektrického uzatváracieho ventilu 15 výtoku tenzidů.into the discharge line 31 of the additional regenerated mordant pump 30. From the actuator 41, the control terminal 42 of the electric air shut-off valve 14 is connected and at the same time the control terminal 43 of the electric shut-off valve 15 of the surfactant outlet is connected.
Po naplnění zásobnej nádrže 10 tenzidom,resp. jeho pravidelnom doplnění sa v případe spustenia pohonu 41 čerpadla 30,t. j. pri přidávaní regěnerovaného moridla do moriacej vane, za pomoci signálu v rozvodoch 40 zapojenia cez svorky 42 a 43 otvárajú elektrické uzatváracie ventily 14 a 15 pre spustenie tlakového vzduchu do hornej časti zásobnej nádrže 10 a pre výtok roztoku tenzidů do výtokového potrubia 20. Množstvo přidávaného tenzidů je regulované v závislosti na množstve přidávaného regenerovaného moridla bud automaticky, alebo ručně vždy v závislosti na prietoku moridla vstupujuceho do posledného stupňa výstupu mořeného kovu.After filling the storage tank 10 with a surfactant, respectively. its regular replenishment in the case of starting the drive 41 of the pump 30, i. j. when adding the regenerated mordant to the pickling bath, by means of a signal in the wiring 40 through the terminals 42 and 43, they open the electric shut-off valves 14 and 15 to trigger pressurized air to the top of the storage tank 10 and The added surfactants are regulated depending on the amount of regenerated mordant to be added, either automatically or manually, depending on the flow rate of the mordant entering the last stage of the pickled metal output.
Vynález možno využit u spracovatelov kovov»a to pri výrobnom spracovaní válcováním v kontinuálnych, ale aj diskontinuálnych linkách, resp. zariadenie aj u výrobcov týchto liniek.The invention can be used in metal processors in the production process by rolling in continuous as well as discontinuous lines, respectively. equipment at the manufacturers of these lines.
Okrem používania vysokokremíkových ocelí, je možné využitie aj pri iných běžných druhoch ocelí a výrobkov z ních| najmá vzhladom na čiastočný inhibičný účinok tenzidov voči množstvu rozpustného kovu a zmáčací účinok pre vyššiu rychlost morenia.In addition to the use of high-silicon steels, it is also possible to use other common types of steels and their products | in particular due to the partial inhibitory effect of surfactants against the amount of soluble metal and the wetting effect for a higher pickling rate.
Claims (2)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS583678A CS204318B1 (en) | 1978-09-11 | 1978-09-11 | Process for restricting formation of the siliceous muds in the solution of hydrochloric acid at pickling silicon steels and device for making this process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS583678A CS204318B1 (en) | 1978-09-11 | 1978-09-11 | Process for restricting formation of the siliceous muds in the solution of hydrochloric acid at pickling silicon steels and device for making this process |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CS204318B1 true CS204318B1 (en) | 1981-04-30 |
Family
ID=5404014
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CS583678A CS204318B1 (en) | 1978-09-11 | 1978-09-11 | Process for restricting formation of the siliceous muds in the solution of hydrochloric acid at pickling silicon steels and device for making this process |
Country Status (1)
| Country | Link |
|---|---|
| CS (1) | CS204318B1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8128754B2 (en) | 2008-11-14 | 2012-03-06 | Ak Steel Properties, Inc. | Ferric pickling of silicon steel |
-
1978
- 1978-09-11 CS CS583678A patent/CS204318B1/en unknown
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8128754B2 (en) | 2008-11-14 | 2012-03-06 | Ak Steel Properties, Inc. | Ferric pickling of silicon steel |
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