CN105692559A - Preparation method of chlorine dioxide - Google Patents
Preparation method of chlorine dioxide Download PDFInfo
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- CN105692559A CN105692559A CN201610051491.1A CN201610051491A CN105692559A CN 105692559 A CN105692559 A CN 105692559A CN 201610051491 A CN201610051491 A CN 201610051491A CN 105692559 A CN105692559 A CN 105692559A
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- Prior art keywords
- chlorine dioxide
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- OSVXSBDYLRYLIG-UHFFFAOYSA-N dioxidochlorine(.) Chemical compound O=Cl=O OSVXSBDYLRYLIG-UHFFFAOYSA-N 0.000 title claims abstract description 162
- 239000004155 Chlorine dioxide Substances 0.000 title claims abstract description 81
- 235000019398 chlorine dioxide Nutrition 0.000 title claims abstract description 81
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 60
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 30
- XTEGARKTQYYJKE-UHFFFAOYSA-M Chlorate Chemical compound [O-]Cl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-M 0.000 claims abstract description 26
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 12
- 230000002378 acidificating effect Effects 0.000 claims abstract description 11
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 11
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims abstract description 10
- 235000006408 oxalic acid Nutrition 0.000 claims abstract description 10
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical group [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 8
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 7
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L magnesium chloride Substances [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims abstract description 5
- 235000010265 sodium sulphite Nutrition 0.000 claims abstract description 5
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims abstract description 4
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims abstract description 4
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000002253 acid Substances 0.000 claims abstract description 4
- JXRVKYBCWUJJBP-UHFFFAOYSA-L calcium;hydrogen sulfate Chemical compound [Ca+2].OS([O-])(=O)=O.OS([O-])(=O)=O JXRVKYBCWUJJBP-UHFFFAOYSA-L 0.000 claims abstract description 4
- 239000004202 carbamide Substances 0.000 claims abstract description 4
- 235000015165 citric acid Nutrition 0.000 claims abstract description 4
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 4
- KAQHZJVQFBJKCK-UHFFFAOYSA-L potassium pyrosulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OS([O-])(=O)=O KAQHZJVQFBJKCK-UHFFFAOYSA-L 0.000 claims abstract description 4
- BHZRJJOHZFYXTO-UHFFFAOYSA-L potassium sulfite Chemical compound [K+].[K+].[O-]S([O-])=O BHZRJJOHZFYXTO-UHFFFAOYSA-L 0.000 claims abstract description 4
- 235000019252 potassium sulphite Nutrition 0.000 claims abstract description 4
- WBHQBSYUUJJSRZ-UHFFFAOYSA-M sodium bisulfate Chemical group [Na+].OS([O-])(=O)=O WBHQBSYUUJJSRZ-UHFFFAOYSA-M 0.000 claims abstract description 4
- ZNCPFRVNHGOPAG-UHFFFAOYSA-L sodium oxalate Chemical compound [Na+].[Na+].[O-]C(=O)C([O-])=O ZNCPFRVNHGOPAG-UHFFFAOYSA-L 0.000 claims abstract description 4
- JXAZAUKOWVKTLO-UHFFFAOYSA-L sodium pyrosulfate Chemical compound [Na+].[Na+].[O-]S(=O)(=O)OS([O-])(=O)=O JXAZAUKOWVKTLO-UHFFFAOYSA-L 0.000 claims abstract description 4
- 239000011975 tartaric acid Substances 0.000 claims abstract description 4
- 235000002906 tartaric acid Nutrition 0.000 claims abstract description 4
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims abstract description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims abstract description 3
- IRXRGVFLQOSHOH-UHFFFAOYSA-L dipotassium;oxalate Chemical compound [K+].[K+].[O-]C(=O)C([O-])=O IRXRGVFLQOSHOH-UHFFFAOYSA-L 0.000 claims abstract description 3
- 229910001629 magnesium chloride Inorganic materials 0.000 claims abstract description 3
- CHKVPAROMQMJNQ-UHFFFAOYSA-M potassium bisulfate Chemical compound [K+].OS([O-])(=O)=O CHKVPAROMQMJNQ-UHFFFAOYSA-M 0.000 claims abstract description 3
- 238000006243 chemical reaction Methods 0.000 claims description 36
- 239000006096 absorbing agent Substances 0.000 claims description 23
- 239000002585 base Substances 0.000 claims description 18
- 238000010521 absorption reaction Methods 0.000 claims description 16
- 239000012190 activator Substances 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 10
- 238000003825 pressing Methods 0.000 claims description 10
- VKJKEPKFPUWCAS-UHFFFAOYSA-M potassium chlorate Chemical compound [K+].[O-]Cl(=O)=O VKJKEPKFPUWCAS-UHFFFAOYSA-M 0.000 claims description 7
- BZSXEZOLBIJVQK-UHFFFAOYSA-N 2-methylsulfonylbenzoic acid Chemical group CS(=O)(=O)C1=CC=CC=C1C(O)=O BZSXEZOLBIJVQK-UHFFFAOYSA-N 0.000 claims description 5
- 230000000694 effects Effects 0.000 claims description 5
- 239000011505 plaster Substances 0.000 claims description 4
- 235000013877 carbamide Nutrition 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 229910000342 sodium bisulfate Inorganic materials 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- 229910000343 potassium bisulfate Inorganic materials 0.000 claims description 2
- 239000000126 substance Substances 0.000 abstract description 7
- 239000003795 chemical substances by application Substances 0.000 abstract description 5
- 230000003213 activating effect Effects 0.000 abstract 2
- 239000004285 Potassium sulphite Substances 0.000 abstract 1
- 239000001164 aluminium sulphate Substances 0.000 abstract 1
- 235000011128 aluminium sulphate Nutrition 0.000 abstract 1
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 abstract 1
- BUACSMWVFUNQET-UHFFFAOYSA-H dialuminum;trisulfate;hydrate Chemical compound O.[Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O BUACSMWVFUNQET-UHFFFAOYSA-H 0.000 abstract 1
- 229910052943 magnesium sulfate Inorganic materials 0.000 abstract 1
- 235000019341 magnesium sulphate Nutrition 0.000 abstract 1
- 239000001120 potassium sulphate Substances 0.000 abstract 1
- 229940039790 sodium oxalate Drugs 0.000 abstract 1
- PMZURENOXWZQFD-UHFFFAOYSA-L sodium sulphate Substances [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 abstract 1
- 229910021653 sulphate ion Inorganic materials 0.000 abstract 1
- 239000002994 raw material Substances 0.000 description 20
- 238000000034 method Methods 0.000 description 12
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- 239000002250 absorbent Substances 0.000 description 7
- 230000002745 absorbent Effects 0.000 description 7
- 238000004659 sterilization and disinfection Methods 0.000 description 7
- 239000003814 drug Substances 0.000 description 6
- 230000001954 sterilising effect Effects 0.000 description 5
- 239000008399 tap water Substances 0.000 description 5
- 235000020679 tap water Nutrition 0.000 description 5
- 229910001919 chlorite Inorganic materials 0.000 description 4
- 229910052619 chlorite group Inorganic materials 0.000 description 4
- QBWCMBCROVPCKQ-UHFFFAOYSA-N chlorous acid Chemical compound OCl=O QBWCMBCROVPCKQ-UHFFFAOYSA-N 0.000 description 4
- 235000013399 edible fruits Nutrition 0.000 description 4
- 235000013311 vegetables Nutrition 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 235000013305 food Nutrition 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 238000004332 deodorization Methods 0.000 description 2
- -1 deodorizer Substances 0.000 description 2
- 230000000249 desinfective effect Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 230000001473 noxious effect Effects 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 230000037452 priming Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- UKLNMMHNWFDKNT-UHFFFAOYSA-M sodium chlorite Chemical compound [Na+].[O-]Cl=O UKLNMMHNWFDKNT-UHFFFAOYSA-M 0.000 description 2
- 229960002218 sodium chlorite Drugs 0.000 description 2
- 230000009182 swimming Effects 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000002386 air freshener Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004061 bleaching Methods 0.000 description 1
- 239000007844 bleaching agent Substances 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 239000000645 desinfectant Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000009920 food preservation Methods 0.000 description 1
- 235000012055 fruits and vegetables Nutrition 0.000 description 1
- 231100000734 genotoxic potential Toxicity 0.000 description 1
- ZDYUUBIMAGBMPY-UHFFFAOYSA-N oxalic acid;hydrate Chemical compound O.OC(=O)C(O)=O ZDYUUBIMAGBMPY-UHFFFAOYSA-N 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000004076 pulp bleaching Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B11/00—Oxides or oxyacids of halogens; Salts thereof
- C01B11/02—Oxides of chlorine
- C01B11/022—Chlorine dioxide (ClO2)
- C01B11/023—Preparation from chlorites or chlorates
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention discloses a preparation method of chlorine dioxide. The preparation method comprises the following steps of dropwise adding water in a mixture of chlorate, an acidic substance, an activating agent and a reducing agent, and reacting, thus obtaining the chlorine dioxide, wherein the reducing agent is sodium sulphite, potassium sulphite, oxalic acid, sodium oxalate, potassium oxalate or urea, the acidic substance for providing an acid environment is sodium hydrogen sulphate, potassium hydrogen sulphate, calcium hydrogen sulphate, sodium pyrosulphate, potassium pyrosulphate, the oxalic acid, citric acid or tartaric acid, and the activating agent is anhydrous calcium sulphate, anhydrous calcium chloride, anhydrous aluminium sulphate, anhydrous aluminium chloride, anhydrous ferric sulphate, anhydrous ferric chloride, anhydrous magnesium chloride or anhydrous magnesium sulphate. The preparation method of the chlorine dioxide, disclosed by the invention, is high is security, low in cost, less in loss of the chlorine dioxide and simple in operation.
Description
Technical field
The preparation method that the present invention relates to chlorine dioxide, is specifically related to a kind of chlorate, the method that chlorine dioxide prepared by reducing agent, acid, activator。
Background technology
Containing unpaired electron in chlorine dioxide, its chemical property is active, has sterilization, deodorization, bleaching, the function such as fresh-keeping。During as water treatment agent, it is possible to for tap water, swimming pool, hospital and chemical plant sewage disposal etc.；During as sterilizing preservative, food and drink, food fresh keeping, medical aid, cultivation field can be used for；As air freshener, then can be used for the deodorization such as indoor, freezer, refrigerator and improve air quality；Additionally, chlorine dioxide can be also used for association with pulp bleaching。
At present, the research and development of chlorine dioxide generating device and reagent combination also receive much concern, and conventional means can be divided into that use device context is relatively large to be produced and the priming reaction that added water by the medicament that formula is good produces two kinds。Use equipment is prepared relatively large chlorine dioxide and is namely mixed by a certain percentage with hydrochloric acid and sodium chlorite and namely produce gas；Reagent combination adds water to activate and namely mixes with chlorite and ackd salt, generates chlorine dioxide in aqueous, can use。The application of current above two method is relatively broad。The former is mainly used in the medium-and-large-sized enterprise such as waterworks, paper mill, and the latter is then used for cultivating sterilization, field of food preservation。But, due to both of which adopt chlorite as raw material, its price costly, and hydrochloric acid and sodium chlorite reaction product contain chlorine by-product, chloroform noxious substance can be produced, thus losing the superiority of chlorine dioxide treatment tap water processing tap water process。The activation and if reagent combination adds water, have chlorine dioxide and overflow diffusion in atmosphere, not only cause waste, and sharp aroma is difficult to stand, in gained ClO 2 solution product, also containing the noxious substances such as remaining chlorite, chlorite with ackd salt can react and cause medicament to lose efficacy in depositing simultaneously。
Summary of the invention
The preparation method that it is an object of the invention to provide the chlorine dioxide that a kind of safety is high, with low cost, chlorine dioxide loss is few, simple to operate。
Technical scheme is as follows: the preparation method of a kind of chlorine dioxide, in the mixture of chlorate, acidic materials, activator and reducing agent, drips water, is obtained by reacting；Described reducing agent is sodium sulfite, potassium sulfite, oxalic acid, Disodium oxalate., potassium oxalate or carbamide；The acidic materials providing sour environment are sodium bisulfate, potassium acid sulfate, calcium bisulfate, sodium pyrosulfate, potassium pyrosulfate, oxalic acid, citric acid or tartaric acid, and described activator is dead plaster, anhydrous calcium chloride, anhydrous slufuric acid aluminum, anhydrous Aluminum chloride, anhydrous ironic sulfate, anhydrous ferric chloride, anhydrous magnesium chloride or anhydrous magnesium sulfate。
As preferably, described chlorate is sodium chlorate or potassium chlorate。
As preferably, described chlorate, reducing agent, acidic materials, activator mol ratio be 1:0.45～1.2:0.4～1.6:0.4～2.0。
As preferably, the reaction unit adopted includes: include base, casing, elastic water pocket, kit and chlorine dioxide absorber bottle, described cabinet arrangement is directly over base, described elastic water pocket is positioned in casing, and the top of elastic water pocket is provided with hold-down devices, described kit is arranged between base and casing, and is provided with lifting apparatus between kit and base；It is connected to the first conduit in the bottom of elastic water pocket, described kit top is provided with diaphragm seal, the other end of the first conduit reaches directly over kit through casing, the second conduit and the 3rd conduit it is provided with in chlorine dioxide absorber bottle, one end of second conduit extends to outside chlorine dioxide absorber bottle and elastic water pocket connects, one end of 3rd conduit is upward through chlorine dioxide absorber bottle and extends to the surface of kit, when kit rises to intended height under the effect of lifting apparatus, first conduit and the 3rd conduit can puncture diaphragm seal and extend in kit, chlorine dioxide absorber bottle is additionally provided with depotition cock, and one end of depotition cock reaches in chlorine dioxide absorber bottle, it is used for deriving ClO 2 solution, first conduit and the second conduit are mounted on unidirectional stop valve；Described first conduit and the 3rd conduit are additionally provided with sealing-plug or sealing ring, the first conduit can be sealed with diaphragm seal junction with diaphragm seal junction, the 3rd conduit, it is prevented that gas leaks；
The absorption bottle of reaction unit adds water, kit loads the mixture of chlorate, reducing agent, acidic materials, activator, this kit is placed on reaction unit, water in the absorption bottle of reaction unit is entered by elastic water pocket and inspires reaction generation chlorine dioxide in kit, and chlorine dioxide enters in absorption bottle and obtains ClO 2 solution。
In technique scheme, in described elastic water pocket, the one-pass water yield is 0.2～3:1 with the mass ratio of the reacting material mixture in kit。
As preferably, the hold-down devices of described reaction unit includes water pocket button, spring and pressing plate, and pressing plate is arranged in elastic water pocket top, and is connected by described spring between pressing plate with box top, water pocket button is arranged at pressing plate top, and extends upward outside casing。
As preferably, the lifting apparatus of described reaction unit includes base plate and spring, and base plate is arranged at bottom kit, and is connected by described spring between base plate with base。
As preferably, the base of described reaction unit, casing, chlorine dioxide absorber bottle are wholely set, and also have bottleneck on chlorine dioxide absorber bottle, and described bottleneck provides solution to prepare use water as water inlet, and is provided with bottle cap on bottleneck。
The invention has the beneficial effects as follows: the reaction raw materials cost preparing chlorine dioxide in the present invention is low, replace the strongly corrosion liquids such as hydrochloric acid with solid material, and safety is high；Suitable material matching, can stably preserve, add water and get final product priming reaction, compares some raw materials at present and is divided into A, B agent more convenient for avoiding reactant contact metamorphism；Except conventional use of chlorate, reducing substances, acidic materials, also add activator, activator can provide the heat needed for reaction, promotes reaction, improve conversion ratio and efficiency, reaction raw materials is packaged in kit, medicament is conveniently preserved, powder performance is stable, ready access upon use, take a kit during every secondary use to be placed on reaction unit and prepare chlorine dioxide, be especially suitable for family, hospital disinfection etc. and use on a small scale。The kit being packaged with reaction raw materials in the present invention can also individually be made the antistaling agents such as vegetable and fruit and use, and takes apart and pack during use, is sealed with vegetable and fruit by packing box and preserves, can play preservation。
Chlorine dioxide reaction apparatus structure in the present invention is simple, safe to use; preparation process generates chlorine dioxide with this device; directly absorbed by water again and obtain ClO 2 solution; without poisonous or corrosive substances such as chlorate unreacted in reactant liquor in existing method, hydrochloric acid; chlorine dioxide is not diffuse in air; both utility waste had been reduced; can prevent from again distributing the chlorine dioxide that zest is strong; protection environment; use more safe and reliable, and chlorine dioxide loss is few, easy to operate in preparation process。
Accompanying drawing explanation
Fig. 1 is the chlorine dioxide reaction apparatus structure schematic diagram in the present invention。
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described, but not thereby limiting the invention。
Experimental technique in following embodiment, if no special instructions, is conventional method。
Embodiment 1 prepares ClO 2 solution
ClO 2 solution is prepared with the chlorine dioxide reaction device shown in Fig. 1。Raw material in kit 5 is powdery, contains: sodium chlorate 12.06g (0.11mol), two oxalic acid hydrate 4.41g (0.049mol), sodium bisulfate 5.28g (0.044mol), anhydrous calcium chloride 24.4g (0.22mol)。
Operation in accordance with the following steps:
Step one: unload the depotition cock 12 of chlorine dioxide absorber bottle 3 or open the bottle cap of chlorine dioxide absorber bottle 3, it is added thereto to the tap water of 1L, ensure the liquid level conduit mouth higher than the second conduit 10 in chlorine dioxide absorber bottle 3 and depotition cock 12, but lower than the conduit mouth of the 3rd conduit 11 above kit 5, it is prevented that aqueous reflux。Generally, in kit 5, chlorate is 10～15:1000 with the mass ratio of the water of addition in absorption bottle 3。After adding water, pressing the water pocket button 7 above elastic water pocket 4, elastic water pocket 4 compresses, and the water section in absorption bottle 3 enters in elastic water pocket 4, and in elastic water pocket 4, the one-pass water yield is 0.2～3:1 with the mass ratio of the reacting material mixture in kit 5。
Step 2: kit 5 diaphragm seal installing medicament is placed on pressing plate 8 upward and makes spring-compressed, when spring is upspring, diaphragm seal is punctured by the first conduit 9 and the 3rd conduit 11, effect due to the effect of spring and sealing-plug or sealing ring, first conduit 9 is tightly connected with diaphragm seal junction with diaphragm seal junction, the 3rd conduit (11), and gas will not be caused to leak。
Step 3: press the water pocket button 7 above elastic water pocket 4, elastic water pocket 4 compresses, water therein is entered kit 5 by unidirectional cutoff valve action by the first conduit 9, react with kit 5 Chinese medicine, generation chlorine dioxide enters chlorine dioxide absorber bottle 3 by the 3rd conduit 11 and dissolves, and forms ClO 2 solution；While unclamping water pocket button 7, having negative pressure in elastic water pocket 4, the water in chlorine dioxide absorber bottle 3 stores along the second conduit and by the elastic water pocket 4 of unidirectional stop valve entrance, uses in order to next time；Because the first conduit 9 and the second conduit 10 are provided with unidirectional stop valve, so current can only flow into elastic water pocket 4 from chlorine dioxide absorber bottle 3, then are flowed in kit 5 by elastic water pocket 4, and can not flow backwards。
Step 4: after 10min, presses depotition cock 12, can release ClO 2 solution and use, and recording chlorine dioxide concentration in solution is 292ppm, and chlorine gas concentration is 15ppm。
By above step gained solution, can use as disinfectant, deodorizer, bleach, for Water Disinfections such as tap water, swimming pool, hospital sewages, can be also used for the disinfecting utensils such as tableware, medical apparatus and instruments, or the food sterilization such as water fruits and vegetables, aquatic products is fresh-keeping, cultivation, dentist's oral disinfecting etc.。
Further, it is also possible to disassembled from reaction unit by chlorine dioxide absorber bottle 3, absorption bottle 3 connects spray nozzle, indoor and public arena spraying can be carried out, air is carried out disinfection, improves environmental quality。
It addition, the kit 5 provided in the present embodiment, it is also possible to fresh-keeping for vegetable and fruit, the diaphragm seal tearing kit 5 off packs together with needing the vegetable and fruit of insurance, storing, the medicament in kit 5 generates chlorine dioxide etc. with steam effect lasts, can play sterilization, preservation。
Embodiment 2 prepares ClO 2 solution
Chlorine dioxide is prepared according to the identical method in embodiment 1, simply the raw material in kit 5 is different, and raw material contains: potassium chlorate 12.25g (0.1mol), oxalic acid 10.8g (0.12mol), potassium pyrosulfate 40.7g (0.16mol), anhydrous Aluminum chloride 5.33g (0.04mol)。
After reaction 12min, the absorbent solution taken in absorption bottle 3 is tested, and recording chlorine dioxide concentration is 438ppm, and chlorine gas concentration is 26ppm。
Embodiment 3 prepares ClO 2 solution
Chlorine dioxide is prepared according to the identical method in embodiment 1, simply the raw material in kit 5 is different, and raw material contains: sodium chlorate 10.64g (0.1mol), sodium sulfite 12.6g (0.1mol), oxalic acid 9.0g (0.1mol), anhydrous magnesium chloride 9.5g (0.1mol)。
After reaction 12min, the absorbent solution taken in absorption bottle 3 is tested, and recording chlorine dioxide concentration is 316ppm, and chlorine gas concentration is 32ppm。
Embodiment 4 prepares ClO 2 solution
Chlorine dioxide is prepared according to the identical method in embodiment 1, simply the raw material in kit 5 is different, and raw material contains: potassium chlorate 12.25g (0.1mol), Disodium oxalate. 9.38g (0.07mol), sodium pyrosulfate 13.3g (0.06mol), dead plaster 16.3g (0.12mol)。
After reaction 15min, the absorbent solution taken in absorption bottle 3 is tested, and recording chlorine dioxide concentration is 342ppm, and chlorine gas concentration is 16ppm。
Embodiment 5 prepares ClO 2 solution
Chlorine dioxide is prepared according to the identical method in embodiment 1, simply the raw material in kit 5 is different, and raw material contains: potassium chlorate 12.25g (0.1mol), potassium sulfite 12.67g (0.08mol), oxalic acid 9.0g (0.1mol), anhydrous ferric chloride 22.7g (0.14mol)。
After reaction 15min, the absorbent solution taken in absorption bottle 3 is tested, and recording chlorine dioxide concentration is 323ppm, and chlorine gas concentration is 20ppm。
Embodiment 6 prepares ClO 2 solution
Chlorine dioxide is prepared according to the identical method in embodiment 1, simply the raw material in kit 5 is different, and raw material contains: potassium chlorate 12.25g (0.1mol), oxalic acid 10.8g (0.12mol), citric acid 14.7g (0.08), anhydrous Aluminum chloride 5.33g (0.04mol)。
After reaction 12min, the absorbent solution taken in absorption bottle 3 is tested, and recording chlorine dioxide concentration is 438ppm, and chlorine gas concentration is 26ppm。
Embodiment 7 prepares ClO 2 solution
Chlorine dioxide is prepared according to the identical method in embodiment 1, simply the raw material in kit 5 is different, raw material contains: sodium chlorate 10.64g (0.1mol), carbamide 3.02g (0.05mol), calcium bisulfate 12.06g (0.05mol), anhydrous magnesium chloride 10.42g (0.11mol)。
After reaction 12min, the absorbent solution taken in absorption bottle 3 is tested, and recording chlorine dioxide concentration is 286ppm, and chlorine gas concentration is 14ppm。
Embodiment 8 prepares ClO 2 solution
Chlorine dioxide is prepared according to the identical method in embodiment 1, simply the raw material in kit 5 is different, raw material contains: potassium chlorate 12.25g (0.1mol), sodium sulfite 11.5g (0.09mol), tartaric acid 14.0g (0.09mol), dead plaster 15.60g (0.11mol)。
After reaction 12min, the absorbent solution taken in absorption bottle 3 is tested, and it is 356ppm that side obtains chlorine dioxide concentration, and chlorine gas concentration is 16ppm。
Above example all can obtain concentration and reach high concentration of chlorine dioxide, and purity is high, and by-product chlorine is less。Owing to existing in absorbing liquid without other unreacted impurity in addition to chlorine dioxide, therefore eliminate the bad hidden danger that impurity genotoxic potential brings。
Claims (8)
1. the preparation method of a chlorine dioxide, it is characterised in that: in the mixture of chlorate, acidic materials, activator and reducing agent, drip water, be obtained by reacting；
Described reducing agent is sodium sulfite, potassium sulfite, oxalic acid, Disodium oxalate., potassium oxalate or carbamide；The acidic materials providing sour environment are sodium bisulfate, potassium acid sulfate, calcium bisulfate, sodium pyrosulfate, potassium pyrosulfate, oxalic acid, citric acid or tartaric acid, and described activator is dead plaster, anhydrous calcium chloride, anhydrous slufuric acid aluminum, anhydrous Aluminum chloride, anhydrous ironic sulfate, anhydrous ferric chloride, anhydrous magnesium chloride or anhydrous magnesium sulfate。
2. the preparation method of chlorine dioxide as claimed in claim 1, it is characterised in that: described chlorate is sodium chlorate or potassium chlorate。
3. the preparation method of chlorine dioxide as claimed in claim 1, it is characterised in that: described chlorate, reducing agent, acidic materials, activator mol ratio be 1:0.45～1.2:0.4～1.6:0.4～2.0。
4. the preparation method of chlorine dioxide as claimed any one in claims 1 to 3, it is characterized in that: the reaction unit of employing includes: include base (1), casing (2), elastic water pocket (4), kit (5) and chlorine dioxide absorber bottle (3), described casing (2) is arranged in directly over base (1), described elastic water pocket (4) is positioned in casing (2), and the top of elastic water pocket (4) is provided with hold-down devices, described kit (5) is arranged between base (1) and casing (2), and it is provided with lifting apparatus between kit (5) and base (1)；It is connected to the first conduit (9) in the bottom of elastic water pocket (4), described kit (5) top is provided with diaphragm seal, the other end of the first conduit (9) reaches directly over kit (5) through casing (2), the second conduit (10) and the 3rd conduit (11) it is provided with in chlorine dioxide absorber bottle (3), one end of second conduit (10) extends to chlorine dioxide absorber bottle (3) and connects with elastic water pocket (4) outward, one end of 3rd conduit (11) is upward through chlorine dioxide absorber bottle (3) and extends to the surface of kit (5), when kit (5) rises to intended height under the effect of lifting apparatus, first conduit (9) and the 3rd conduit (11) can puncture diaphragm seal and extend in kit (5), chlorine dioxide absorber bottle (3) is additionally provided with depotition cock (12), and one end of depotition cock (12) reaches in chlorine dioxide absorber bottle (3), it is used for deriving ClO 2 solution, first conduit (9) and the second conduit (10) are mounted on unidirectional stop valve；Described first conduit (9) and the 3rd conduit (11) are additionally provided with sealing-plug or sealing ring, first conduit (9) can be sealed with diaphragm seal junction with diaphragm seal junction, the 3rd conduit (11), it is prevented that gas leaks；
The absorption bottle (3) of reaction unit adds water, kit (5) loads the mixture of chlorate, reducing agent, acidic materials, activator, this kit (5) is placed on reaction unit, water in the absorption bottle (3) of reaction unit is entered by elastic water pocket (4) and inspires reaction generation chlorine dioxide in kit (5), and chlorine dioxide enters in absorption bottle (3) and obtains ClO 2 solution。
5. the preparation method of chlorine dioxide as claimed in claim 4, it is characterised in that: in described elastic water pocket (4), the one-pass water yield is 0.2～3:1 with the mass ratio of the reacting material mixture in kit (5)。
6. the preparation method of chlorine dioxide as claimed in claim 4, it is characterized in that: the hold-down devices of described reaction unit includes water pocket button (7), spring and pressing plate (6), pressing plate (6) is arranged in elastic water pocket (4) top, and be connected by described spring between pressing plate (6) with casing (2) end face, water pocket button (7) is arranged at pressing plate (6) top, and extends upward casing (2) outward。
7. the preparation method of chlorine dioxide as claimed in claim 4, it is characterized in that: the lifting apparatus of described reaction unit includes base plate (8) and spring, base plate (8) is arranged at kit (5) bottom, and is connected by described spring between base plate (8) with base (1)。
8. the preparation method of chlorine dioxide as claimed in claim 4, it is characterized in that: the base (1) of described reaction unit, casing (2), chlorine dioxide absorber bottle (3) are wholely set, and chlorine dioxide absorber bottle (3) also has bottleneck, described bottleneck provides solution to prepare use water as water inlet, and is provided with bottle cap on bottleneck。
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110558318A (en) * | 2019-09-19 | 2019-12-13 | 河南省化工研究所有限责任公司 | Stable chlorine dioxide effervescent agent and preparation method thereof |
| CN115072667A (en) * | 2022-06-14 | 2022-09-20 | 华南理工大学 | Preparation method of reactive chlorine dioxide solid preparation using sodium chlorate as raw material |
| CN115893321A (en) * | 2022-12-29 | 2023-04-04 | 深圳凯士洁生物技术有限公司 | Method for regulating stable release of chlorine dioxide |
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| WO2014064782A1 (en) * | 2012-10-24 | 2014-05-01 | 株式会社アマテラ | Chlorine dioxide gas generating agent pack, and manufacturing method and storage method thereof |
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| CN115072667A (en) * | 2022-06-14 | 2022-09-20 | 华南理工大学 | Preparation method of reactive chlorine dioxide solid preparation using sodium chlorate as raw material |
| CN115072667B (en) * | 2022-06-14 | 2024-01-16 | 华南理工大学 | Preparation method of reactive chlorine dioxide solid preparation using sodium chlorate as raw material |
| CN115893321A (en) * | 2022-12-29 | 2023-04-04 | 深圳凯士洁生物技术有限公司 | Method for regulating stable release of chlorine dioxide |
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