CN115784164A - Method for preparing nano basic magnesium hypochlorite stable turbid liquid by using waste chlorine - Google Patents
Method for preparing nano basic magnesium hypochlorite stable turbid liquid by using waste chlorine Download PDFInfo
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- CN115784164A CN115784164A CN202211648976.0A CN202211648976A CN115784164A CN 115784164 A CN115784164 A CN 115784164A CN 202211648976 A CN202211648976 A CN 202211648976A CN 115784164 A CN115784164 A CN 115784164A
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- Prior art keywords
- hypochlorite
- solution
- chlorine
- basic magnesium
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- 239000000460 chlorine Substances 0.000 title claims abstract description 49
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 229910052801 chlorine Inorganic materials 0.000 title claims abstract description 48
- YZQBYALVHAANGI-UHFFFAOYSA-N magnesium;dihypochlorite Chemical compound [Mg+2].Cl[O-].Cl[O-] YZQBYALVHAANGI-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 40
- 239000002699 waste material Substances 0.000 title claims abstract description 21
- 239000007788 liquid Substances 0.000 title description 2
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims abstract description 56
- WQYVRQLZKVEZGA-UHFFFAOYSA-N hypochlorite Chemical compound Cl[O-] WQYVRQLZKVEZGA-UHFFFAOYSA-N 0.000 claims abstract description 42
- 238000006243 chemical reaction Methods 0.000 claims abstract description 32
- 239000000725 suspension Substances 0.000 claims abstract description 30
- 229910001629 magnesium chloride Inorganic materials 0.000 claims abstract description 28
- 239000003513 alkali Substances 0.000 claims abstract description 12
- 230000008569 process Effects 0.000 claims abstract description 12
- 238000005530 etching Methods 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 239000002253 acid Substances 0.000 claims abstract description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 3
- 239000000243 solution Substances 0.000 claims 9
- 239000012670 alkaline solution Substances 0.000 claims 2
- 239000005708 Sodium hypochlorite Substances 0.000 abstract description 13
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 abstract description 13
- 238000011084 recovery Methods 0.000 abstract description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 5
- 229910052802 copper Inorganic materials 0.000 abstract description 5
- 239000010949 copper Substances 0.000 abstract description 5
- 238000005868 electrolysis reaction Methods 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- 230000003647 oxidation Effects 0.000 abstract description 2
- 238000007254 oxidation reaction Methods 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 229960002337 magnesium chloride Drugs 0.000 description 22
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 8
- 239000011777 magnesium Substances 0.000 description 6
- SATVIFGJTRRDQU-UHFFFAOYSA-N potassium hypochlorite Chemical compound [K+].Cl[O-] SATVIFGJTRRDQU-UHFFFAOYSA-N 0.000 description 6
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 5
- 229910052749 magnesium Inorganic materials 0.000 description 5
- 229940091250 magnesium supplement Drugs 0.000 description 5
- 230000002378 acidificating effect Effects 0.000 description 4
- GRFBKUDKDYCTIW-UHFFFAOYSA-M disodium;hydroxide;hypochlorite Chemical compound [OH-].[Na+].[Na+].Cl[O-] GRFBKUDKDYCTIW-UHFFFAOYSA-M 0.000 description 3
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- ZKQDCIXGCQPQNV-UHFFFAOYSA-N Calcium hypochlorite Chemical compound [Ca+2].Cl[O-].Cl[O-] ZKQDCIXGCQPQNV-UHFFFAOYSA-N 0.000 description 1
- UZHXGDONXYJIJZ-UHFFFAOYSA-M [OH-].[K+].Cl[O-].[K+] Chemical compound [OH-].[K+].Cl[O-].[K+] UZHXGDONXYJIJZ-UHFFFAOYSA-M 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004061 bleaching Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000000249 desinfective effect Effects 0.000 description 1
- ZOSVFAIIFHTUEG-UHFFFAOYSA-L dipotassium;dihydroxide Chemical compound [OH-].[OH-].[K+].[K+] ZOSVFAIIFHTUEG-UHFFFAOYSA-L 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 229940050906 magnesium chloride hexahydrate Drugs 0.000 description 1
- DHRRIBDTHFBPNG-UHFFFAOYSA-L magnesium dichloride hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[Cl-].[Cl-] DHRRIBDTHFBPNG-UHFFFAOYSA-L 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 1
- 235000019341 magnesium sulphate Nutrition 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
Landscapes
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
Abstract
The invention discloses a method for preparing a stable suspension of nano basic magnesium hypochlorite by using waste chlorine, which belongs to the technical field of chemical industry and comprises the steps of introducing chlorine generated in an electrolytic acid etching solution process into a reaction tank containing alkali liquor to prepare hypochlorite solution; adding magnesium chloride into the reaction kettle, adding water, stirring and dissolving to prepare a magnesium chloride solution; when the available chlorine content of the hypochlorite solution in the first step reaches 9-12%, the mole ratio of the effective components of the alkali liquor to the hypochlorous acid is (2-4): 1, placing the hypochlorite solution in the reaction kettle in the second step for reacting for 1-2 hours to prepare the basic magnesium hypochlorite suspension. The basic magnesium hypochlorite with stable property and mild oxidation effect is prepared by using chlorine-containing gas generated in the copper electrolysis recovery process as a main raw material. Solves the technical pain point that the sodium hypochlorite prepared in the prior art has poor stability and low price for sale.
Description
Technical Field
The invention relates to the technical field of chemical industry, in particular to a method for preparing a stable suspension of nanometer basic magnesium hypochlorite by using waste chlorine.
Background
The basic magnesium hypochlorite is white powder, is difficult to dissolve in water, does not absorb moisture, can be stably stored in the air, and can be decomposed only by heating to more than 200 ℃. It has good disinfecting, sterilizing and bleaching functions, and has mild and lasting effect, and wide application in industry, daily life and other aspects.
At present, the basic magnesium hypochlorite is prepared by a magnesium oxide chlorination method or a magnesium sulfate and calcium hypochlorite double decomposition method generally, but the effective chlorine recovery rate of the two methods is lower and is generally lower than 50%.
In the PCB industry, a large amount of chlorine gas is produced as a byproduct in the process of recovering copper by electrolysis, and the chlorine gas treatment is generally prepared into a sodium hypochlorite solution for sale. But the sodium hypochlorite has poor stability, low selling price and no economic benefit.
Disclosure of Invention
The embodiment of the invention provides a method for preparing a stable suspension of nano basic magnesium hypochlorite by using waste chlorine, the method uses chlorine generated in the process of recovering copper by electrolysis as a main raw material to produce the basic magnesium hypochlorite suspension, and the contents of the invention are as follows:
the method for preparing the stable suspension of the nanometer basic magnesium hypochlorite by using the waste chlorine gas has the technical points that the method comprises the following steps:
step one, chlorine generated in the process of electrolyzing the acid etching solution is introduced into a reaction tank containing alkali liquor to prepare hypochlorite solution; the reaction formula is as follows:
2AOH+Cl 2 ＝AClO+ACl+H 2 O。
adding magnesium chloride into the reaction kettle, adding water, stirring and dissolving to prepare a magnesium chloride solution;
step three, when the effective chlorine content of the hypochlorite solution in the step one reaches 9-12%, the molar ratio of the effective components of the alkali liquor to the hypochlorous acid is (2-4): 1, placing the hypochlorite solution in the reaction kettle in the second step to react for 1-2h to prepare basic magnesium hypochlorite suspension, wherein the reaction equation is as follows:
2MgCl 2 +3AOH+AClO＝Mg 2 ClO(OH)+2H 2 O+4ACl。
in order to better realize the technical scheme, in the first step of the method for preparing the stable suspension of the nano basic magnesium hypochlorite by using the waste chlorine, the alkali liquor is sodium hydroxide solution or potassium hydroxide solution.
In order to better realize the technical scheme, in the first step of the method for preparing the nano basic magnesium hypochlorite stable suspension by using the waste chlorine, the mass concentration of the alkali liquor is 15-20%.
In order to better realize the technical scheme, the mass concentration of the magnesium chloride solution in the second step of the method for preparing the stable suspension of the nano basic magnesium hypochlorite by using the waste chlorine is 115-200g/L.
In order to better realize the technical scheme, the dosage of the hypochlorite solution in the third step of the method for preparing the nano basic magnesium hypochlorite stable suspension by utilizing the waste chlorine gas is controlled according to the condition that the molar weight of hypochlorite is 30-45 percent of that of magnesium chloride.
Compared with the prior art, the method for preparing the stable suspension of the nanometer basic magnesium hypochlorite by using the waste chlorine gas has the following beneficial effects:
1. the method for preparing the stable suspension of the nano basic magnesium hypochlorite by utilizing the waste chlorine gas comprises the steps of introducing the chlorine gas generated in the process of electrolyzing the acid etching solution into a reaction tank containing alkali liquor to prepare hypochlorite solution; adding magnesium chloride into the reaction kettle, adding water, stirring and dissolving to prepare a magnesium chloride solution; when the available chlorine content of the hypochlorite solution in the first step reaches 9-12%, the mole ratio of the effective components of the alkali liquor to the hypochlorous acid is (2-4): and 1, placing the hypochlorite solution in the reaction kettle in the second step for reacting for 1-2 hours to prepare the basic magnesium hypochlorite suspension.
2. The basic magnesium hypochlorite with stable property and mild oxidation effect is prepared by using chlorine-containing gas generated in the copper electrolysis recovery process as a main raw material. Solves the technical pain point that the sodium hypochlorite prepared in the prior art has poor stability and low price for sale.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below with reference to specific embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the process of recovering copper by electrolyzing the acidic etching solution, 2-3kg of chlorine gas can be generated by each production line per hour, and the magnesium chloride adopted by the invention is commercially available magnesium chloride hexahydrate.
Example 1
The method for preparing the stable suspension of the nanometer basic magnesium hypochlorite by using the waste chlorine comprises the following steps:
step one, chlorine generated in the process of electrolyzing the acidic etching solution is introduced into a reaction tank containing a sodium hydroxide solution with the mass concentration of 15% to prepare a sodium hypochlorite-sodium hydroxide solution;
adding magnesium chloride into the reaction kettle, adding water, stirring and dissolving to prepare a magnesium chloride solution with the mass concentration of 115 g/L;
step three, when the effective chlorine content of the sodium hypochlorite solution in the step one reaches 9 percent, the molar ratio of the sodium hydroxide to the hypochlorous acid is 2: and 1, placing the sodium hypochlorite solution in the reaction kettle in the step two for reaction for 1 hour to prepare basic magnesium hypochlorite suspension. The amount of the sodium hypochlorite solution added was controlled so that the molar amount of hypochlorite was 37.5% of the molar amount of magnesium chloride.
The recovery rate of the effective chlorine of the basic magnesium hypochlorite prepared by the invention is 80%, the content of the effective chlorine is 5%, and the content of the magnesium is 10%.
Example 2
The method for preparing the stable suspension of the nanometer basic magnesium hypochlorite by using the waste chlorine comprises the following steps:
step one, chlorine generated in the process of electrolyzing the acidic etching solution is introduced into a reaction tank containing a sodium hydroxide solution with the mass concentration of 17.5% to prepare a sodium hypochlorite-sodium hydroxide solution;
adding magnesium chloride into the reaction kettle, adding water, stirring and dissolving to prepare a magnesium chloride solution with the mass concentration of 117.5 g/L;
step three, when the effective chlorine content of the sodium hypochlorite solution in the step one reaches 10.5 percent, the molar ratio of the sodium hydroxide to the hypochlorous acid is 3:1, placing the sodium hypochlorite solution in the reaction kettle in the second step for reacting for 1.5 hours to prepare basic magnesium hypochlorite suspension. The amount of the sodium hypochlorite solution added is controlled according to the mole amount of hypochlorite which is 30 percent of the mole amount of magnesium chloride.
The recovery rate of the effective chlorine of the basic magnesium hypochlorite prepared by the invention is 87.1 percent, the effective chlorine content is 6.4 percent, and the magnesium content is 23.9 percent.
Example 3
The method for preparing the stable suspension of the nanometer basic magnesium hypochlorite by using the waste chlorine comprises the following steps:
step one, chlorine generated in the process of electrolyzing the acidic etching solution is introduced into a reaction tank containing a sodium hydroxide solution with the mass concentration of 16% to prepare a sodium hypochlorite-sodium hydroxide solution;
adding magnesium chloride into the reaction kettle, adding water, stirring and dissolving to prepare a magnesium chloride solution with the mass concentration of 118 g/L;
step three, when the effective chlorine content of the sodium hypochlorite solution in the step one reaches 10%, the molar ratio of the sodium hydroxide to the hypochlorous acid is 4: and 1, placing the sodium hypochlorite solution in the reaction kettle in the step two for reaction for 2 hours to prepare basic magnesium hypochlorite suspension. The amount of the sodium hypochlorite solution added is controlled according to the mole amount of hypochlorite which is 40 percent of that of magnesium chloride.
The recovery rate of the effective chlorine of the basic magnesium hypochlorite prepared by the method is 85%, the effective chlorine content is 6%, and the magnesium content is 20%.
Example 4
The method for preparing the stable suspension of the nanometer basic magnesium hypochlorite by using the waste chlorine comprises the following steps:
step one, chlorine generated in the process of electrolyzing the acid etching solution is introduced into a reaction tank containing a potassium hydroxide solution with the mass concentration of 17% to prepare a potassium-potassium hydroxide solution;
adding magnesium chloride into the reaction kettle, adding water, stirring and dissolving to prepare a magnesium chloride solution with the mass concentration of 117 g/L;
step three, when the effective chlorine content of the potassium hypochlorite solution in the step one reaches 11 percent, the molar ratio of the effective components of the alkali liquor to the hypochlorous acid is 2.5:1, placing the potassium hypochlorite solution in the reaction kettle in the second step to react for 2 hours to prepare basic magnesium hypochlorite suspension. The amount of potassium hypochlorite solution added was controlled so that the molar amount of hypochlorite was 40% of the molar amount of magnesium chloride.
The recovery rate of the effective chlorine of the basic magnesium hypochlorite prepared by the invention is 89.1%, the content of the effective chlorine is 5.5%, and the content of the magnesium is 15.6%.
Example 5
The method for preparing the stable suspension of the nanometer basic magnesium hypochlorite by using the waste chlorine comprises the following steps:
step one, chlorine generated in the process of electrolyzing the acid etching solution is introduced into a reaction tank containing a sodium hydroxide solution with the mass concentration of 15-20% to prepare a potassium hypochlorite-potassium hydroxide solution;
adding magnesium chloride into the reaction kettle, adding water, stirring and dissolving to prepare a magnesium chloride solution with the mass concentration of 200 g/L;
step three, when the effective chlorine content of the potassium hypochlorite solution in the step one reaches 12%, the molar ratio of the effective components of the alkali liquor to the hypochlorous acid is 4:1, placing the potassium hypochlorite solution in the reaction kettle in the second step to react for 2 hours to prepare basic magnesium hypochlorite suspension. The amount of potassium hypochlorite solution added was controlled based on the molar amount of hypochlorite to be 45% of the molar amount of magnesium chloride.
The recovery rate of the effective chlorine of the basic magnesium hypochlorite prepared by the invention is 87.5 percent, the effective chlorine content is 7 percent, and the magnesium content is 30 percent.
The above description is only an example of the present invention, and is not intended to limit the present invention. Various modifications and alterations to this invention will become apparent to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the claims of the present invention.
Claims (5)
1. The method for preparing the stable suspension of the nanometer basic magnesium hypochlorite by using the waste chlorine is characterized by comprising the following steps of:
step one, chlorine generated in the process of electrolyzing the acid etching solution is introduced into a reaction tank containing alkali liquor to prepare hypochlorite solution;
adding magnesium chloride into the reaction kettle, adding water, stirring and dissolving to prepare a magnesium chloride solution;
step three, when the effective chlorine content of the hypochlorite solution in the step one reaches 9-12%, the molar ratio of the effective components of the alkali liquor to the hypochlorous acid is (2-4): and 1, placing the hypochlorite solution in the reaction kettle in the step two for reaction for 1-2 hours to prepare basic magnesium hypochlorite suspension.
2. The method for preparing stable suspension of nanometer basic magnesium hypochlorite according to claim 1, wherein the alkaline solution is sodium hydroxide solution or potassium hydroxide solution.
3. The method for preparing stable suspension of nanometer basic magnesium hypochlorite by using waste chlorine as claimed in claim 1, wherein the concentration of the alkaline solution in the first step is 15-20% by mass.
4. The method for preparing stable suspension of nanometer basic magnesium hypochlorite by using waste chlorine as claimed in claim 1, wherein the mass concentration of the magnesium chloride solution in the second step is 115-200g/L.
5. The method for preparing stable suspension of nano basic magnesium hypochlorite using waste chlorine as claimed in claim 1, wherein the amount of hypochlorite solution added in said step three is controlled based on the mole amount of hypochlorite solution is 30-45% of the mole amount of magnesium chloride.
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|---|---|---|---|
| CN202211648976.0A CN115784164A (en) | 2022-12-21 | 2022-12-21 | Method for preparing nano basic magnesium hypochlorite stable turbid liquid by using waste chlorine |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202211648976.0A CN115784164A (en) | 2022-12-21 | 2022-12-21 | Method for preparing nano basic magnesium hypochlorite stable turbid liquid by using waste chlorine |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09227104A (en) * | 1996-02-20 | 1997-09-02 | Kureha Chem Ind Co Ltd | Production of tribasic magnesium hypochlorite |
| CN101519189A (en) * | 2009-04-08 | 2009-09-02 | 中国科学院青海盐湖研究所 | Method and device for preparing basic magnesium hypochlorite by using waste chlorine |
| CN101683970A (en) * | 2008-09-26 | 2010-03-31 | 天津市黎虹化工有限公司 | Alkali liquid chlorination method for producing sodium hypochlorite solution with high concentration |
| CN108557768A (en) * | 2018-02-27 | 2018-09-21 | 广东先导稀材股份有限公司 | The preparation method of lithium hypochlorite |
-
2022
- 2022-12-21 CN CN202211648976.0A patent/CN115784164A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09227104A (en) * | 1996-02-20 | 1997-09-02 | Kureha Chem Ind Co Ltd | Production of tribasic magnesium hypochlorite |
| CN101683970A (en) * | 2008-09-26 | 2010-03-31 | 天津市黎虹化工有限公司 | Alkali liquid chlorination method for producing sodium hypochlorite solution with high concentration |
| CN101519189A (en) * | 2009-04-08 | 2009-09-02 | 中国科学院青海盐湖研究所 | Method and device for preparing basic magnesium hypochlorite by using waste chlorine |
| CN108557768A (en) * | 2018-02-27 | 2018-09-21 | 广东先导稀材股份有限公司 | The preparation method of lithium hypochlorite |
Non-Patent Citations (1)
| Title |
|---|
| 陈建文: "抗菌剂碱式次氯酸镁", 精细与专用化学品, no. 09 * |
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