CN104891442A - Method for preparing high-purity chlorine dioxide - Google Patents
Method for preparing high-purity chlorine dioxide Download PDFInfo
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- CN104891442A CN104891442A CN201510224770.9A CN201510224770A CN104891442A CN 104891442 A CN104891442 A CN 104891442A CN 201510224770 A CN201510224770 A CN 201510224770A CN 104891442 A CN104891442 A CN 104891442A
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Abstract
The invention discloses a method for preparing high-purity chlorine dioxide. The method comprises mixing sodium chlorite and a mixing agent so that sodium chlorite is coated with the mixing agent to form raw material particles, coating the raw material particles with molecular filter membranes to obtain a coated material A for next use, mixing citric acid and a mixing agent, coating the mixture with molecular filter membranes to obtain a coated material B for next use, sealing the coated material A and the coated material B in a raw material bag, and putting the raw material bag into water so that the high-purity chlorine dioxide is obtained. The produced chlorine dioxide solution has purity of 99.99%, eliminates adverse effects caused by chlorine dioxide solution residual substances in the disinfection liquid use, is safe and reliable, realizes chlorine dioxide gas storage and transport, realizes on-site preparation, has good on-site usage effects and fills a gap in the field of direct disinfection of air in a space.
Description
Technical field
The present invention relates to the preparing technical field of dioxide peroxide, specifically refer to a kind of method preparing chlorine dioxide with high purity.
Background technology
Dioxide peroxide (ClO
2) be a kind of yellow-green colour to orange-yellow gas, be known as safety, nontoxic green disinfectant in the world.Dioxide peroxide has broad spectrum, efficiently can kill the thalline of virus, bacterium, protobiont, algae, fungi and various spore and sporulation, consumption is few, can kill all bacterial propagules and many pathogenic bacterium under 0.1ppm, 50ppm can kill vegetative forms of bacteria, hepatitis virus, phage and bacterial spore completely.
There is many-sided defect in the chlorine dioxide generation of prior art:
1, the hazardous substance such as raw material is sulfuric acid, hydrochloric acid, chlorine are used;
2, the chlorine dioxide purity produced is inadequate, generally about 85%; What produce contains hypochlorite, chlorine and clorox containing in the liquid of dioxide peroxide;
3, dioxide peroxide generation device structure is complicated, volume large and produce a large amount of reluctant waste water and residual contamination while generation;
4, existing installation can not solve dioxide peroxide storage and a transport difficult problem, gives when using dioxide peroxide and brings inconvenience; The not high meeting of chlorine dioxide liquid purity simultaneously owing to producing brings many negative residues at use dioxide peroxide;
These factors above-mentioned limit Chlorine dioxide production and use in a lot of field, bring obstruction to the popularization of this environment-protecting clean sterilizing agent of dioxide peroxide.
Summary of the invention
The product purity that the object of the invention is to overcome the existence of prior art chlorine dioxide generation is not high, trade effluent is difficult, production unit volume is large, and the defect of accumulating difficulty, provides a kind of method can preparing chlorine dioxide with high purity without the need to main equipment convenient, fast, efficiently.
For achieving the above object, the method preparing chlorine dioxide with high purity designed by the present invention, comprises the following steps:
1) mixed with mixture by Textone, both weight ratios are 1:1 ~ 6, make mixture wrap up Textone and obtain feed particulate material, then utilize molecule filter membrane enwrapped granule shape raw material, obtain A parcel for subsequent use;
2) by citric acid and catalyst mix, both weight ratios are 1:0.05 ~ 1, utilize step 1) described in molecule filter membrane parcel, obtain B parcel for subsequent use;
3) A environmental sealing is inserted in B parcel, then seals B parcel,
Or B environmental sealing is inserted in A parcel, then seal A parcel,
Or insert in another molecule filter membrane after A parcel and B parcel are sealed respectively, after sealing, obtain the raw material packet comprising A parcel and B parcel;
4) by step 3) raw material packet that obtains inserts in water, and can high-purity dioxide peroxide;
Wherein, described molecule filter membrane for having water permeability, the molecule filter membrane of aperture≤0.1 μm.
Alternatively, described mixture is vitriol, carbonate or oxymuriate.In theory, above-mentioned salt can as mixture, but variant in effect.
Preferably, described mixture is sodium sulfate or sodium chlorate.By sodium salt as mixture, do not increase other ions.
Preferably, described catalyzer is one or more mixture in aluminum chloride, magnesium sulfate, boric acid, potassium primary phosphate, oxalic acid.
The principle of the invention:
The present invention is by being rolled in molecule filter membrane by raw material packet, make to only have the dioxide peroxide of generation to evaporate in air by molecule filter membrane or to be dissolved in water, other by products are all stored in molecule filter membrane and can not reveal, ensure that while generating highly purified dioxide peroxide, do not produce unnecessary waste water, reduce environmental pollution.
In dioxide peroxide generating process, by V-shape mixing equipment, Textone crystal is implemented evenly parcel with mixture; The ratio of Textone and mixture is 1:1 ~ 6; 20 minutes unit time of mixing.The present invention gets rid of traditional use strong acid to obtain dioxide peroxide, by using the mixed catalyst containing oxymuriate to improve the ratio that commensurability's raw material obtains dioxide peroxide, rises to 80% by original 40%; Like this while reaching safety in production, also achieve the benefit not using strong acid to obtain dioxide peroxide.
Beneficial effect of the present invention:
1, the difficult problem that chlorine dioxide stores and transports is solved; Reach in situ preparation, the object of onsite application.
2, production purity 99.99% ClO 2 solution; To eliminate in ClO 2 solution in the past residuals to using the untoward reaction caused during this sterilizing-and-disinfecting liquid.
3, be directly used in space air sterilization, the method is in use safe and reliable; Fill up the blank at present to the direct sterilization of space air.
4, optimization production link, reduce production cost, improve quality product, expand product use range, reach production security and zero blowdown requirement.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail, and following examples are explanation of the invention and the present invention is not limited to following examples.
Embodiment 1
Prepare the method for chlorine dioxide with high purity, comprise the following steps:
1) prepare Textone and sodium sulfate, both weight ratios are 1:4, then utilize mixing machine to make sodium sulfate wrap up Textone and obtain feed particulate material, and the molecule filter membrane sealed envelope feed particulate material of recycling aperture≤0.1 μm, obtains A parcel for subsequent use; The molecule filter membrane in this aperture has water permeability, can stop again by product beyond dioxide peroxide and raw material through.
In the present embodiment, the ZK-V type mixing machine that commercially available Shanghai Qiao Feng mixing machine instrument factory is produced selected by mixing machine.
2) mixed with the part by weight of catalyzer according to 1:0.1 by citric acid, described catalyzer is the mixture of 1:0.2 of aluminum chloride, oxalic acid, then with the molecule filter membrane parcel of aperture≤0.1 μm, obtains B parcel for subsequent use;
3) A parcel is inserted in B parcel, then seals B parcel, obtains the raw material packet of the sealing comprising A parcel and B parcel;
4) by step 3) raw material packet that obtains inserts in water, and within 5 minutes, can see that the color of water starts to occur yellow-green colour, the appearance of this color is high-purity dioxide peroxide.
Chlorine dioxide high purity 99.99% prepared by the present invention, the mass ratio of raw material and dioxide peroxide is 5:4.
Embodiment 2
Prepare the method for chlorine dioxide with high purity, comprise the following steps:
1) prepare Textone and sodium chlorate, both weight ratios are 1:4, then utilize mixing machine to make sodium chlorate wrap up Textone and obtain feed particulate material, and the molecule filter membrane enwrapped granule shape raw material of recycling aperture≤0.1 μm, obtains A parcel for subsequent use; The molecule filter membrane in this aperture has water permeability, can stop again by product beyond dioxide peroxide and raw material through.
In the present embodiment, the ZK-V type mixing machine that commercially available Shanghai Qiao Feng mixing machine instrument factory is produced selected by mixing machine.
2) citric acid is mixed with the part by weight of aluminum chloride according to 1:0.05, then use the molecule filter membrane sealed envelope of aperture≤0.1 μm, obtain B parcel for subsequent use;
3) B parcel is inserted in A parcel, then seals A parcel, obtains the raw material packet of the sealing comprising A parcel and B parcel;
4) by step 3) raw material packet that obtains inserts in water, and within 6 minutes, can see that the color of water starts to occur yellow-green colour, the appearance of this color is high-purity dioxide peroxide.
Chlorine dioxide high purity 99.99% prepared by the present invention, the mass ratio of raw material and dioxide peroxide is 5:3.6.
Embodiment 3
Prepare the method for chlorine dioxide with high purity, comprise the following steps:
1) prepare Textone and sodium sulfate, both weight ratios are 1:5, then utilize mixing machine to make sodium sulfate wrap up Textone and obtain feed particulate material, and the molecule filter membrane sealed envelope feed particulate material of recycling aperture≤0.1 μm, obtains A parcel for subsequent use; The molecule filter membrane in this aperture has water permeability, can stop again by product beyond dioxide peroxide and raw material through.
In the present embodiment, the ZK-V type mixing machine that commercially available Shanghai Qiao Feng mixing machine instrument factory is produced selected by mixing machine.
2) mixed with the part by weight of catalyzer according to 1:0.08 by citric acid, described catalyzer is the mixture of the 1:1 of boric acid and oxalic acid, then with the molecule filter membrane parcel of aperture≤0.1 μm, obtains B parcel for subsequent use;
3) A parcel is inserted in B parcel, then seals B parcel, obtains the raw material packet of the sealing comprising A parcel and B parcel;
4) by step 3) raw material packet that obtains inserts in water, and within 10 minutes, can see that the color of water starts to occur yellow-green colour, the appearance of this color is high-purity dioxide peroxide.
Chlorine dioxide high purity 99.99% prepared by the present invention, the mass ratio of raw material and dioxide peroxide is 7:5.
Embodiment 4
Prepare the method for chlorine dioxide with high purity, comprise the following steps:
1) prepare Textone and sodium carbonate, both weight ratios are 1:6, then utilize mixing machine to make sodium carbonate wrap up Textone and obtain feed particulate material, and the molecule filter membrane enwrapped granule shape raw material of recycling aperture≤0.1 μm, obtains A parcel for subsequent use; The molecule filter membrane in this aperture has water permeability, can stop again by product beyond dioxide peroxide and raw material through.
In the present embodiment, the ZK-V type mixing machine that commercially available Shanghai Qiao Feng mixing machine instrument factory is produced selected by mixing machine.
2) citric acid is mixed with the part by weight of catalyzer oxalic acid according to 1:1, then use the molecule filter membrane sealed envelope of aperture≤0.1 μm, obtain B parcel for subsequent use;
3) B parcel is inserted in A parcel, then seals A parcel, obtains the raw material packet of the sealing comprising A parcel and B parcel;
4) by step 3) raw material packet that obtains inserts in water, and within 8 minutes, can see that the color of water starts to occur yellow-green colour, the appearance of this color is high-purity dioxide peroxide.
Chlorine dioxide high purity 99.99% prepared by the present invention, the mass ratio of raw material and dioxide peroxide is 7:4.
Embodiment 5
Prepare the method for chlorine dioxide with high purity, comprise the following steps:
1) prepare Textone and sodium sulfate, both weight ratios are 1:2, then utilize mixing machine to make sodium sulfate wrap up Textone and obtain feed particulate material, and the molecule filter membrane sealed envelope feed particulate material of recycling aperture≤0.1 μm, obtains A parcel for subsequent use; The molecule filter membrane in this aperture has water permeability, can stop again by product beyond dioxide peroxide and raw material through.
In the present embodiment, the ZK-V type mixing machine that commercially available Shanghai Qiao Feng mixing machine instrument factory is produced selected by mixing machine.
2) mixed with the part by weight of catalyzer according to 1:1 by citric acid, described catalyzer is the mixture of 1:1:1 of aluminum chloride, magnesium sulfate, boric acid, then uses the molecule filter membrane sealed envelope of aperture≤0.1 μm, obtains B parcel for subsequent use;
3) by A parcel and another molecule filter membrane sealed envelope of B parcel, the raw material packet of the sealing comprising A parcel and B parcel is obtained;
4) by step 3) raw material packet that obtains inserts in water, and within 7 minutes, can see that the color of water starts to occur yellow-green colour, the appearance of this color is high-purity dioxide peroxide.Chlorine dioxide high purity 99.99% prepared by the present invention, the mass ratio of raw material and dioxide peroxide is 7:5.
Embodiment 6
Prepare the method for chlorine dioxide with high purity, comprise the following steps:
1) prepare Textone and sodium sulfate, both weight ratios are 1:2, then utilize mixing machine to make sodium sulfate wrap up Textone and obtain feed particulate material, and the molecule filter membrane enwrapped granule shape raw material of recycling aperture≤0.1 μm, obtains A parcel for subsequent use; The molecule filter membrane in this aperture has water permeability, can stop again by product beyond dioxide peroxide and raw material through.
In the present embodiment, the ZK-V type mixing machine that commercially available Shanghai Qiao Feng mixing machine instrument factory is produced selected by mixing machine.
2) mixed with the part by weight of catalyzer according to 1:1 by citric acid, described catalyzer is the mixture of 0.5:1 of potassium primary phosphate, oxalic acid, then uses the molecule filter membrane sealed envelope of aperture≤0.1 μm, obtains B parcel for subsequent use;
3) B parcel is inserted in A parcel, then seals A parcel, obtains the raw material packet of the sealing comprising A parcel and B parcel;
4) by step 3) raw material packet that obtains inserts in water, and within 9 minutes, can see that the color of water starts to occur yellow-green colour, the appearance of this color is high-purity dioxide peroxide.
Chlorine dioxide high purity 99.99% prepared by the present invention, the mass ratio of raw material and dioxide peroxide is 5:3.
Embodiment 7
Prepare the method for chlorine dioxide with high purity, comprise the following steps:
1) prepare Textone and calcium chlorate, both weight ratios are 1:1, then utilize mixing machine to make calcium chlorate wrap up Textone and obtain feed particulate material, and the molecule filter membrane enwrapped granule shape raw material of recycling aperture≤0.1 μm, obtains A parcel for subsequent use; The molecule filter membrane in this aperture has water permeability, can stop again by product beyond dioxide peroxide and raw material through.
In the present embodiment, the ZK-V type mixing machine that commercially available Shanghai Qiao Feng mixing machine instrument factory is produced selected by mixing machine.
2) citric acid is mixed with the part by weight of catalyzer potassium primary phosphate according to 1:0.2, then use the molecule filter membrane sealed envelope of aperture≤0.1 μm, obtain B parcel for subsequent use;
3) B parcel is inserted in A parcel, then seals A parcel, obtains the raw material packet of the sealing comprising A parcel and B parcel;
4) by step 3) raw material packet that obtains inserts in water, and within 10 minutes, can see that the color of water starts to occur yellow-green colour, the appearance of this color is high-purity dioxide peroxide.
Chlorine dioxide high purity 99.99% prepared by the present invention, the mass ratio of raw material and dioxide peroxide is 5:3.
Embodiment 8
Prepare the method for chlorine dioxide with high purity, comprise the following steps:
1) prepare Textone and calcium chlorate, both weight ratios are 1:3, then utilize mixing machine to make calcium chlorate wrap up Textone and obtain feed particulate material, and the molecule filter membrane sealed envelope feed particulate material of recycling aperture≤0.1 μm, obtains A parcel for subsequent use; The molecule filter membrane in this aperture has water permeability, can stop again by product beyond dioxide peroxide and raw material through.
In the present embodiment, the ZK-V type mixing machine that commercially available Shanghai Qiao Feng mixing machine instrument factory is produced selected by mixing machine.
2) citric acid is mixed with the part by weight of catalyzer oxalic acid according to 1:0.5, then with the molecule filter membrane parcel of aperture≤0.1 μm, obtain B parcel for subsequent use;
3) A parcel is inserted in B parcel, then seals B parcel, obtains the raw material packet of the sealing comprising A parcel and B parcel;
4) by step 3) raw material packet that obtains inserts in water, and within 10 minutes, can see that the color of water starts to occur yellow-green colour, the appearance of this color is high-purity dioxide peroxide.
Chlorine dioxide high purity 99.99% prepared by the present invention, the mass ratio of raw material and dioxide peroxide is 4:3.
Claims (5)
1. prepare a method for chlorine dioxide with high purity, comprise the following steps:
1) mixed with mixture by Textone, both weight ratios are 1:1 ~ 6, make mixture wrap up Textone and obtain feed particulate material, then utilize molecule filter membrane enwrapped granule shape raw material, obtain A parcel for subsequent use;
2) by citric acid and catalyst mix, both weight ratios are 1:0.05 ~ 1, utilize molecule filter membrane to wrap up, and obtain B parcel for subsequent use;
3) A environmental sealing is inserted in B parcel, then seals B parcel,
Or B environmental sealing is inserted in A parcel, then seal A parcel,
Or insert in another molecule filter membrane after A parcel and B parcel are sealed respectively, after sealing, obtain the raw material packet comprising A parcel and B parcel;
4) by step 3) raw material packet that obtains inserts in water, and can high-purity dioxide peroxide;
Wherein, described molecule filter membrane for having water permeability, the molecule filter membrane of aperture≤0.1 μm.
2. prepare the method for chlorine dioxide with high purity according to claim 1, it is characterized in that: described mixture is vitriol, carbonate or oxymuriate.
3. prepare the method for chlorine dioxide with high purity according to claim 1, it is characterized in that: described mixture is sodium sulfate or sodium chlorate.
4. according to claim 1 or 2 or 3, prepare the method for chlorine dioxide with high purity, it is characterized in that: described catalyzer is one or more mixture in aluminum chloride, oxalic acid, sodium sulfate, S-WAT.
5. according to claim 1 or 2 or 3, prepare the method for chlorine dioxide with high purity, it is characterized in that: described citric acid and catalyst weight are than being 1:0.1, and described catalyzer is the mixture of 1:0.2 of aluminum chloride, oxalic acid.
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| CN201510224770.9A CN104891442A (en) | 2015-05-06 | 2015-05-06 | Method for preparing high-purity chlorine dioxide |
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| CN201510224770.9A CN104891442A (en) | 2015-05-06 | 2015-05-06 | Method for preparing high-purity chlorine dioxide |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105692559A (en) * | 2016-01-26 | 2016-06-22 | 张旭 | Preparation method of chlorine dioxide |
| CN106395749A (en) * | 2016-09-14 | 2017-02-15 | 华东师范大学 | Method for preparing high-purity chlorine dioxide through solid-state heterogeneous catalysis |
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| CN106395749A (en) * | 2016-09-14 | 2017-02-15 | 华东师范大学 | Method for preparing high-purity chlorine dioxide through solid-state heterogeneous catalysis |
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Application publication date: 20150909 |