CN101519189A - Method and device for preparing basic magnesium hypochlorite by using waste chlorine - Google Patents
Method and device for preparing basic magnesium hypochlorite by using waste chlorine Download PDFInfo
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- CN101519189A CN101519189A CN 200910021883 CN200910021883A CN101519189A CN 101519189 A CN101519189 A CN 101519189A CN 200910021883 CN200910021883 CN 200910021883 CN 200910021883 A CN200910021883 A CN 200910021883A CN 101519189 A CN101519189 A CN 101519189A
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- chlorine
- hypochlorite
- basic magnesium
- alkali lye
- absorption tower
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Abstract
The invention discloses a method for preparing basic magnesium hypochlorite by using waste chlorine. Firstly, chlorine is absorbed by a solution of sodium hydroxide to form a solution of sodium hypochlorite; and secondly, the solution of sodium hypochlorite is reacted with a solution of magnesium chloride to form solid basic magnesium hypochlorite. In the basic magnesium hypochlorite product prepared by the method, the effective chlorine content is 38 to 42 percent, the magnesium content is 28 to 32 percent and the effective chlorine yield is 85 to 95 percent. The method uses chlorine-containing gases produced in the production processes of electrolytic industry or other industries and makes full use of the cheap but high-quality bischofite resources in salt lake areas. The prepared basic magnesium hypochlorite is stable in property and mild in oxidation and can avoid the adverse impact of pinhole damages when used on textiles. The waste liquid produced in the preparation process mainly contains sodium chloride and magnesium chloride and can be directly discharged into salt lakes after simple treatment without adverse impact on the resource structure of the salt lakes.
Description
Technical field
The present invention relates to and belongs to chemical technology field, relates to a kind of method for preparing basic magnesium hypochlorite, and relating in particular to a kind of is the method for main material production basic magnesium hypochlorite with the chlorine that produces in electrolytic process or other process; The present invention also relates to a kind of device that utilizes waste chlorine to prepare basic magnesium hypochlorite simultaneously.
Background technology
Basic magnesium hypochlorite (basic magnesium hypochlorite is called for short BMH) is a kind of white powder, is insoluble in water, and solubleness is about 0.02% in water, and is non-hygroscopic, and quite stable in air is heated to more than 200 ℃ and could decomposes.BMH meets acid and decomposes the generation nascent oxygen:
Mg
2ClO(OH)
3H
2O+H
+＝MgCl
2+HClO+2H
2O
HClO=HCl+O (active oxygen)
Thereby BMH has good sterilization, sterilization and bleaching action, these action temperature and and lasting.BMH can be used as sterilant, mould inhibitor, sanitas, deodorizing composition, preservation agent etc., has been widely used at aspects such as industry, agricultural, daily lifes.
The preparation of basic magnesium hypochlorite generally adopt magnesium oxide chlorination process or sal epsom and Losantin double decomposition, but the yield of these two kinds of methods is lower, is no more than 50% at present.
In electrolytic industry and other industrial production, can by-product a large amount of chlorine or chloride tail gas, for the processing of these chlorine or chloride tail gas, different according to the quantity of the chlorine-containing gas that is produced and composition, the resource distribution and the industrial structure is different near the plant area, can adopt different treatment processs.These methods mainly comprise preparation liquid chlorine (if the amount of chlorine that is produced is big and purity is higher), absorb the preparation chlorine bleach liquor, absorb preparation Losantin solid, absorb (if the chlorine content that produces are little and purity is lower) such as preparation ferric chloride Solutions with solution of ferrous chloride with sodium hydroxide and aqua calcis with sodium hydroxide solution.
Summary of the invention
The purpose of this invention is to provide a kind of chlorine-containing gas that produces in electrolytic industry or other Industrial processes that utilizes and be main raw material, produce the method for basic magnesium hypochlorite.
Another object of the present invention provides and a kind ofly realizes utilizing waste chlorine to prepare the device of basic magnesium hypochlorite.
The present invention utilizes waste chlorine to prepare the method for basic magnesium hypochlorite, is that the chlorine that at first absorbs in the chlorine-containing gas with sodium hydroxide solution obtains the chlorine bleach liquor, makes the reaction of chlorine bleach liquor and magnesium chloride solution obtain the basic magnesium hypochlorite solid product then.Concrete preparation technology is as follows:
(1) sends in the alkali lye absorption tower after waste chlorine is cooled to 20～40 ℃, adopt the sodium hydroxide solution of mass concentration 15～30% to absorb chlorine, obtain containing the sodium hydroxide solution of clorox; Its reaction formula is as follows:
2NaOH+Cl
2＝NaClO+NaCl+H
2O
Because chlorination reaction is thermopositive reaction, when absorbing chlorine, adopt the lower alkali lye of temperature, cool off absorbing circulation fluid in case of necessity.By following reaction decomposes, the temperature of chlorination absorption reaction is controlled at below 35 ℃ for fear of hypochlorite:
3ClO
-＝ClO3
-+2Cl
-
2ClO
-＝2Cl
-+O
2
(2) available chlorine content reaches more than 10% in the alkali lye after absorbing chlorine, and when the mol ratio of sodium hydroxide and clorox is 2:1～4:1, the sodium hydroxide solution that will contain clorox is sent into reactor, with magnesium chloride solution reaction 3～6 hours, obtains the basic magnesium hypochlorite precipitation.
Described magnesium chloride solution adopts the salt lake to carry the old halogen (based on the saturated solution of magnesium chloride) of by-product behind the potassium or spontaneous evaporation and the bischofite of separating out from the old halogen in salt lake.The mass concentration of magnesium chloride solution is at 95～285g/L, and its add-on is 1～3 times of hypochlorite molar weight for its add-on.Its reaction equation is as follows:
2MgCl
2+3NaOH+NaClO+H
2O＝Mg
2ClO(OH)
3H
2O+4NaCl
(3) with after the sedimentary feed liquid centrifugation of basic magnesium hypochlorite, washing, oven dry promptly get the basic magnesium hypochlorite solid phase prod.
In the basic magnesium hypochlorite solid phase prod of the present invention's preparation, available chlorine content is 38～42%, and Mg content is 28～32%, available chlorine yield 85～95%.
The present invention utilizes waste chlorine to prepare the equipment of basic magnesium hypochlorite, comprises interchanger successively, watercooler, alkali lye absorption tower, reservoir, reactor and whizzer; Wherein interchanger is by the pipe connection watercooler, and watercooler connects the bottom on alkali lye absorption tower by pipeline, blower fan; Described reservoir is arranged on a side on alkali lye absorption tower, and reservoir is communicated with the top on alkali lye absorption tower by submerged pump and pipeline, and the bottom of reservoir is connected with reactor by liquid-feeding pump and pipeline; In the described reactor agitator is installed, the bottom of reactor is provided with valve, is provided with whizzer under the reactor.
Described alkali lye absorption tower can be provided with two or more according to the difference of the content of chlorine in the useless chlorine, to guarantee that cl content reaches emission standard from the tail gas that discharge at the top, absorption tower.
When adopting a plurality of alkali lye absorption tower, top, previous alkali lye absorption tower is connected by the bottom of pipeline with next alkali lye absorption tower.
Adopt this equipment to prepare the sedimentary process of basic magnesium hypochlorite to be: will make temperature reduce to 20～40 ℃ from the chlorine-containing gas of commercial runs such as fused salt electrolysis through after air heat exchanger and the watercooler.Cooled chlorine-containing gas is sent into the bottom on alkali lye absorption tower by blower fan, reacts with the sodium hydroxide lye counter current contact that is gone out by the absorption tower top spray, obtains containing the sodium hydroxide solution of clorox.The available chlorine content that absorbs clorox in the alkali lye when circulation reaches more than 10%, by liquid-feeding pump the chlorine bleach liquor is sent into reactor, with magnesium chloride solution that adds and sodium hydroxide solution reaction, obtains the basic magnesium hypochlorite precipitation.Open the valve of reactor bottom, the whizzer that will contain the sedimentary feed liquid injecting reactor of basic magnesium hypochlorite below separates, and obtains the basic magnesium hypochlorite solid product, and its washing, oven dry are promptly got the basic magnesium hypochlorite solid phase prod.The solution that produces after the centrifugation can be used as the additional liquid of circulating absorption solution, or is used to prepare the reaction soln of precipitin reaction, but also directly is discharged in the salt lake after the simple process.
The relative prior art of the present invention has following beneficial effect:
1, the present invention is a main raw material with the chlorine-containing gas that produces in electrolytic industry or other Industrial processes, and make full use of that salt lake area is cheap, fine bischofite resource, adopt simple equipment, prepare stable in properties, oxygenizement gentleness, persistent basic magnesium hypochlorite, when being applied to bleached woven fabric, in the time of can avoiding bleaching some fabric, on fabric, cause the negative impact of pin hole infringement with Losantin;
2, the waste liquid of preparation process generation mainly contains sodium-chlor and magnesium chloride, can directly be discharged in the salt lake after simple process, can not cause negative impact to the resource structures in salt lake.
3, preparation technology is simple, and is easy to operate, and cost is low, is easy to suitability for industrialized production.
Description of drawings
Fig. 1 is process flow sheet and the equipment drawing for preparing basic magnesium hypochlorite for the present invention
1---air heat exchanger 2---watercooler 3---blower fan 4---alkali lye absorption tower
5---reservoir 6---submerged pump 7---liquid-feeding pump 8---reactors
9---agitator 10---whizzer
Embodiment
Embodiment 1: utilizing the chloride system fused salt electrolysis to prepare the chlorine-containing gas that produces in the rare earth metal process, to prepare the equipment and the technology of basic magnesium hypochlorite as follows:
(1) equipment
The present invention prepares the equipment of basic magnesium hypochlorite, comprise air heat exchanger 1, watercooler 2, absorption tower 4, reservoir 5 successively, reactor 8 and whizzer 10, wherein interchanger 1 is by pipe connection watercooler 2, and watercooler 2 connects the bottom on absorption tower 4 by pipeline, blower fan 3; Reservoir 5 is arranged on a side on absorption tower 4, and reservoir 5 tops are communicated with the top on liquid absorption tower 4 by submerged pump 6 and pipeline, and the bottom of reservoir 5 is connected with reactor 8 by liquid-feeding pump 7 and pipeline; In the reactor 8 agitator is installed, the bottom of reactor 8 is provided with valve, and the bottom of reactor 8 is provided with whizzer 10 (with reference to Fig. 1).
All with the metal titanium preparation, absorption tower, reservoir, 1 reactor, agitator, pipeline etc. can adopt PVC or glass reinforced plastic material for air heat exchanger and watercooler.
(2) technology
Utilize the chloride system fused salt electrolysis to prepare the Faradaic current 1000～2000A of rare earth metal, 800～900 ℃ of electrolysis temperatures per hour produce chlorine 2～4kg.
After the chlorine process air heat exchanger 1 and watercooler 2 with the electrolysis generation, make temperature reduce to 20～40 ℃.Cooled chlorine-containing gas is sent into the bottom of chlorine gas absorption tower 4 by blower fan 3, (can earlier the sodium hydroxide solution that is mixed with mass concentration 15～30% be stored in the reservoir 5 with the sodium hydroxide solution that goes out by absorption tower 4 top sprays, absorbing operation the time sends into 4 tops, absorption tower by submerged pump 6 and sprays) counter current contact carries out absorption reaction, obtains containing the sodium hydroxide solution of clorox.The temperature of chlorination absorption reaction is controlled at below 35 ℃.
Available chlorine content reaches more than 10% in the alkali lye after absorbing chlorine, and when the mol ratio of sodium hydroxide and clorox is 2:1～4:1, the absorption chlorine solution that will be contained clorox by liquid-feeding pump 7 is sent into reactor 8, the solution of the bischofite that in reactor, adds spontaneous evaporation from the old halogen in salt lake simultaneously and separate out, strength of solution is 160g/L, its add-on is that the mol ratio of magnesium chloride and hypochlorite is 1:1, under agitation reacts 4 hours, obtains the basic magnesium hypochlorite precipitation.
After will containing 10 separation of the sedimentary feed liquid usefulness of basic magnesium hypochlorite whizzer, washing, oven dry promptly get the basic magnesium hypochlorite solid phase prod.
Available chlorine content 39.5% in this product, Mg content 29.2%, available chlorine yield 85.2%.
The solution that produces after the centrifugation can be used as the additional liquid of circulating absorption solution, or is used to prepare the reaction soln of precipitin reaction, but also directly is discharged in the salt lake after the simple process.
Embodiment 2: utilize Magnesium Chloride Anhydrous and rare earth chloride to prepare basic magnesium hypochlorite for the chlorine-containing gas that produces in the main raw material electrolytic preparation rare-earth magnesium intermediate alloy process
(1) equipment
Substantially the same manner as Example 1, difference is that alkali lye absorption tower 4 need be provided with two, to guarantee that cl content reaches emission standard from the tail gas that discharge at the top, absorption tower.When adopting two a plurality of alkali lye absorption towers, top, previous alkali lye absorption tower is connected by the bottom of pipeline with next alkali lye absorption tower.
(2) technology
Utilize Magnesium Chloride Anhydrous and rare earth chloride in the main raw material electrolytic preparation rare-earth magnesium intermediate alloy process, Faradaic current 2000～4000A, 800～900 ℃ of electrolysis temperatures per hour produce chlorine 3～6kg.
After the chlorine process air heat exchanger 1 and watercooler 2 with the electrolysis generation, make temperature reduce to 20～40 ℃.Cooled chlorine-containing gas is sent into the bottom on first alkali lye absorption tower 4 by blower fan 3, (can earlier the sodium hydroxide solution that is mixed with mass concentration 15～30% be stored in the reservoir 5 with the sodium hydroxide solution that goes out by absorption tower 4 top sprays, absorbing operation the time sends into 4 tops, absorption tower by submerged pump 6 and sprays) counter current contact carries out absorption reaction, obtains containing the sodium hydroxide solution of clorox; The tail gas that discharge at first top, alkali lye absorption tower enters the bottom on second alkali lye absorption tower by pipeline, and the sodium hydroxide solution counter current contact that continues to go out with alkali lye absorption tower top spray is carried out absorption reaction, obtains containing the sodium hydroxide solution of clorox.The temperature of chlorination absorption reaction is controlled at below 35 ℃.
Available chlorine content reaches more than 10% in the alkali lye after absorbing chlorine, and when the mol ratio of sodium hydroxide and clorox is 2:1～4:1, the absorption chlorine solution that will be contained clorox by liquid-feeding pump 7 is sent into reactor 8, the solution of the bischofite that in reactor, adds spontaneous evaporation from the old halogen in salt lake simultaneously and separate out, strength of solution is 180g/L, its add-on is that the mol ratio of magnesium chloride and hypochlorite is 1:1, under agitation reacts 5 hours, obtains the basic magnesium hypochlorite precipitation.
After will containing 10 separation of the sedimentary feed liquid usefulness of basic magnesium hypochlorite whizzer, washing, oven dry promptly get the basic magnesium hypochlorite solid phase prod.
Available chlorine content 40.3% in this product, Mg content 28.9%, available chlorine yield 87.1%.
The solution that produces after the centrifugation can be used as the additional liquid of circulating absorption solution, or is used to prepare the reaction soln of precipitin reaction, but also directly is discharged in the salt lake after the simple process.
Embodiment 3: utilize partial dehydration magnesium chloride and partial dehydration rare earth chloride to prepare basic magnesium hypochlorite for the chlorine-containing gas that produces in the main raw material electrolytic preparation rare-earth magnesium intermediate alloy process
Faradaic current 2000～4000A, 800～900 ℃ of electrolysis temperatures per hour produce chlorine 3～6kg.
Preparation facilities is identical with embodiment 2 with preparation process.
Available chlorine content 38.3% in this product, Mg content 29.6%, available chlorine yield 86.2%.
Claims (6)
1, a kind of method of utilizing waste chlorine to prepare basic magnesium hypochlorite comprises following processing step:
(1) sends in the alkali lye absorption tower after waste chlorine is cooled to 20～40 ℃, adopt the sodium hydroxide solution of mass concentration 15～30% to absorb chlorine, obtain containing the sodium hydroxide solution of clorox.
(2) available chlorine content reaches more than 10% in the alkali lye after absorbing chlorine, and when the mol ratio of sodium hydroxide and clorox is 2:1～4:1, the sodium hydroxide solution that will contain clorox is sent into reactor, with magnesium chloride solution reaction 3～6 hours, obtains the basic magnesium hypochlorite precipitation; The mass concentration of described magnesium chloride solution is 95～285g/L, and its add-on is that the mol ratio of magnesium chloride and hypochlorite is 1:1～3:1, and the reaction times is 3～6 hours.
(3) with after the sedimentary feed liquid centrifugation of basic magnesium hypochlorite, washing, oven dry promptly get the basic magnesium hypochlorite solid phase prod.
2, utilize waste chlorine to prepare the method for basic magnesium hypochlorite according to claim 1, it is characterized in that: the temperature of reaction of described absorption chlorine is controlled at 20～40 ℃.
3, utilize waste chlorine to prepare the method for basic magnesium hypochlorite according to claim 1, it is characterized in that: described magnesium chloride solution adopts the salt lake to carry the old halogen of by-product behind the potassium or spontaneous evaporation and the bischofite of separating out from the old halogen in salt lake.
4, utilize waste chlorine to prepare the method for basic magnesium hypochlorite according to claim 1, it is characterized in that: the mass concentration of the described magnesium chloride solution of step (2) is 95～285g/L, and its add-on is 1～3 times of hypochlorite molar weight.
5, a kind of equipment that utilizes waste chlorine to prepare basic magnesium hypochlorite is characterized in that: comprise air heat exchanger (1), watercooler (2), alkali lye absorption tower (4), reservoir (5) successively, reactor (8) and whizzer (10); Wherein interchanger (1) is by pipe connection watercooler (2), and watercooler (2) connects the bottom on alkali lye absorption tower (4) by pipeline, blower fan (3); Described reservoir (5) is arranged on a side on alkali lye absorption tower (4), and reservoir (5) passes through submerged pump (6) and pipeline is communicated with the top of alkali lye absorption tower (4), and the bottom of reservoir (5) is connected with reactor (8) by liquid-feeding pump (7) and pipeline; Agitator (9) is installed in the described reactor (8), and the bottom of reactor is provided with valve, is provided with whizzer (10) under the reactor.
6, utilize waste chlorine to prepare the equipment of basic magnesium hypochlorite as described in claim 5, it is characterized in that: described alkali lye absorption tower (4) is provided with two or more.
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|---|---|---|---|
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102728195A (en) * | 2011-04-12 | 2012-10-17 | 陆宏卿 | Chlorine gas absorption device |
| CN103691284A (en) * | 2013-12-24 | 2014-04-02 | 滨州坤宝化工有限责任公司 | Method for producing sodium hypochlorite by using aluminum trichloride production waste gas |
| CN104338427A (en) * | 2013-08-09 | 2015-02-11 | 攀钢集团钛业有限责任公司 | Method for treating magnesium electrolysis chlorine-containing waste gas |
| CN104529376A (en) * | 2014-12-03 | 2015-04-22 | 中国科学院青海盐湖研究所 | Antifreezing magnesium oxychloride cement and preparation method and application thereof |
| CN105063622A (en) * | 2015-08-28 | 2015-11-18 | 上海八菱环保科技有限公司 | Chlorine treatment device in acid etching solution circulating reclaimed copper recovery system |
| CN109562935A (en) * | 2016-08-05 | 2019-04-02 | 陈朝光 | The system and method for sodium hypochlorite are recycled from chlorine exhaust gas |
| CN112174093A (en) * | 2020-09-30 | 2021-01-05 | 河南神马氯碱发展有限责任公司 | Method for producing bleaching powder by using carbide slag |
| CN112956488A (en) * | 2020-12-22 | 2021-06-15 | 天津海源汇科技有限公司 | Preparation method of sea salt disinfectant |
| CN115784164A (en) * | 2022-12-21 | 2023-03-14 | 广东臻鼎环境科技有限公司 | Method for preparing nano basic magnesium hypochlorite stable turbid liquid by using waste chlorine |
-
2009
- 2009-04-08 CN CN 200910021883 patent/CN101519189A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102728195A (en) * | 2011-04-12 | 2012-10-17 | 陆宏卿 | Chlorine gas absorption device |
| CN104338427A (en) * | 2013-08-09 | 2015-02-11 | 攀钢集团钛业有限责任公司 | Method for treating magnesium electrolysis chlorine-containing waste gas |
| CN103691284A (en) * | 2013-12-24 | 2014-04-02 | 滨州坤宝化工有限责任公司 | Method for producing sodium hypochlorite by using aluminum trichloride production waste gas |
| CN104529376A (en) * | 2014-12-03 | 2015-04-22 | 中国科学院青海盐湖研究所 | Antifreezing magnesium oxychloride cement and preparation method and application thereof |
| CN105063622A (en) * | 2015-08-28 | 2015-11-18 | 上海八菱环保科技有限公司 | Chlorine treatment device in acid etching solution circulating reclaimed copper recovery system |
| CN109562935A (en) * | 2016-08-05 | 2019-04-02 | 陈朝光 | The system and method for sodium hypochlorite are recycled from chlorine exhaust gas |
| CN112174093A (en) * | 2020-09-30 | 2021-01-05 | 河南神马氯碱发展有限责任公司 | Method for producing bleaching powder by using carbide slag |
| CN112174093B (en) * | 2020-09-30 | 2022-07-08 | 河南神马氯碱发展有限责任公司 | Method for producing bleaching powder by using carbide slag |
| CN112956488A (en) * | 2020-12-22 | 2021-06-15 | 天津海源汇科技有限公司 | Preparation method of sea salt disinfectant |
| CN115784164A (en) * | 2022-12-21 | 2023-03-14 | 广东臻鼎环境科技有限公司 | Method for preparing nano basic magnesium hypochlorite stable turbid liquid by using waste chlorine |
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Open date: 20090902 |