CN110015638A - A kind of equipment and its production method based on chloric acid and Hydrogen Peroxide Production sodium chlorite - Google Patents
A kind of equipment and its production method based on chloric acid and Hydrogen Peroxide Production sodium chlorite Download PDFInfo
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- CN110015638A CN110015638A CN201910341113.0A CN201910341113A CN110015638A CN 110015638 A CN110015638 A CN 110015638A CN 201910341113 A CN201910341113 A CN 201910341113A CN 110015638 A CN110015638 A CN 110015638A
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- pipe
- sodium chlorite
- sodium
- generator
- absorption tower
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- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 title claims abstract description 67
- UKLNMMHNWFDKNT-UHFFFAOYSA-M sodium chlorite Chemical compound [Na+].[O-]Cl=O UKLNMMHNWFDKNT-UHFFFAOYSA-M 0.000 title claims abstract description 67
- 229960002218 sodium chlorite Drugs 0.000 title claims abstract description 67
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 37
- XTEGARKTQYYJKE-UHFFFAOYSA-N chloric acid Chemical compound OCl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 229940005991 chloric acid Drugs 0.000 title claims abstract description 17
- OSVXSBDYLRYLIG-UHFFFAOYSA-N dioxidochlorine(.) Chemical compound O=Cl=O OSVXSBDYLRYLIG-UHFFFAOYSA-N 0.000 claims abstract description 79
- 238000010521 absorption reaction Methods 0.000 claims abstract description 52
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 47
- 239000004155 Chlorine dioxide Substances 0.000 claims abstract description 39
- 235000019398 chlorine dioxide Nutrition 0.000 claims abstract description 39
- 239000007788 liquid Substances 0.000 claims abstract description 34
- BZSXEZOLBIJVQK-UHFFFAOYSA-N 2-methylsulfonylbenzoic acid Chemical compound CS(=O)(=O)C1=CC=CC=C1C(O)=O BZSXEZOLBIJVQK-UHFFFAOYSA-N 0.000 claims abstract description 31
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims abstract description 31
- 238000002360 preparation method Methods 0.000 claims abstract description 29
- 239000000463 material Substances 0.000 claims abstract description 26
- 238000001035 drying Methods 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000013078 crystal Substances 0.000 claims abstract description 17
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Substances [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 14
- 238000001914 filtration Methods 0.000 claims abstract description 11
- 229910052938 sodium sulfate Inorganic materials 0.000 claims abstract description 11
- 235000011152 sodium sulphate Nutrition 0.000 claims abstract description 10
- 239000011780 sodium chloride Substances 0.000 claims abstract description 8
- 238000000605 extraction Methods 0.000 claims abstract description 6
- 238000011017 operating method Methods 0.000 claims abstract 2
- 238000006243 chemical reaction Methods 0.000 claims description 35
- 238000003860 storage Methods 0.000 claims description 24
- 239000002994 raw material Substances 0.000 claims description 23
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 15
- 229910001882 dioxygen Inorganic materials 0.000 claims description 15
- 102000005393 Sodium-Potassium-Exchanging ATPase Human genes 0.000 claims description 12
- 108010006431 Sodium-Potassium-Exchanging ATPase Proteins 0.000 claims description 12
- 239000003513 alkali Substances 0.000 claims description 11
- 239000007789 gas Substances 0.000 claims description 10
- OEMUKJZHMHTYSL-UHFFFAOYSA-N [Na].OCl=O Chemical compound [Na].OCl=O OEMUKJZHMHTYSL-UHFFFAOYSA-N 0.000 claims description 9
- 238000009833 condensation Methods 0.000 claims description 9
- 230000005494 condensation Effects 0.000 claims description 9
- 238000005352 clarification Methods 0.000 claims description 8
- 239000000706 filtrate Substances 0.000 claims description 8
- 238000010992 reflux Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 6
- 238000001704 evaporation Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 239000001117 sulphuric acid Substances 0.000 claims description 6
- 235000011149 sulphuric acid Nutrition 0.000 claims description 6
- 238000005273 aeration Methods 0.000 claims description 5
- 230000006835 compression Effects 0.000 claims description 5
- 238000007906 compression Methods 0.000 claims description 5
- 238000002425 crystallisation Methods 0.000 claims description 5
- 230000008025 crystallization Effects 0.000 claims description 5
- 239000012065 filter cake Substances 0.000 claims description 5
- 238000005649 metathesis reaction Methods 0.000 claims description 5
- 230000008020 evaporation Effects 0.000 claims description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims 2
- RTACEFMOLQFJNG-UHFFFAOYSA-N [Cl].OO Chemical compound [Cl].OO RTACEFMOLQFJNG-UHFFFAOYSA-N 0.000 claims 1
- 239000004408 titanium dioxide Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 11
- 230000008569 process Effects 0.000 abstract description 6
- 239000002699 waste material Substances 0.000 abstract description 6
- 238000000926 separation method Methods 0.000 abstract description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 6
- 239000000460 chlorine Substances 0.000 description 6
- 229910052801 chlorine Inorganic materials 0.000 description 6
- 241000790917 Dioxys <bee> Species 0.000 description 5
- 230000008859 change Effects 0.000 description 5
- QBWCMBCROVPCKQ-UHFFFAOYSA-N chlorous acid Chemical compound OCl=O QBWCMBCROVPCKQ-UHFFFAOYSA-N 0.000 description 5
- 229940077239 chlorous acid Drugs 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- NHYCGSASNAIGLD-UHFFFAOYSA-N Chlorine monoxide Chemical compound Cl[O] NHYCGSASNAIGLD-UHFFFAOYSA-N 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- TVWHTOUAJSGEKT-UHFFFAOYSA-N chlorine trioxide Chemical compound [O]Cl(=O)=O TVWHTOUAJSGEKT-UHFFFAOYSA-N 0.000 description 2
- 239000012263 liquid product Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 241000251468 Actinopterygii Species 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 241000195493 Cryptophyta Species 0.000 description 1
- 241000208202 Linaceae Species 0.000 description 1
- 235000004431 Linum usitatissimum Nutrition 0.000 description 1
- 239000007832 Na2SO4 Substances 0.000 description 1
- 229920001131 Pulp (paper) Polymers 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000010808 liquid waste Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000004076 pulp bleaching Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection 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
- C01B11/08—Chlorous acid
- C01B11/10—Chlorites
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Treating Waste Gases (AREA)
Abstract
The invention discloses a kind of equipment and its production method based on chloric acid and Hydrogen Peroxide Production sodium chlorite, the equipment is made of material crystal processing system, chlorine dioxide preparation system and sodium chlorite preparation system, the operating procedure of production is: 1) sulfuric acid and sodium chlorate being sent in crystallizing evaporator and heated, sodium chloride crystal body is precipitated, anhydrous sodium sulphate is made through filter device filtering, drying;2) water vapour generated enters condensate draining after condenser condenses and stores;3) clarified solution of crystallizing evaporator send to generator and prepares chlorine dioxide, then chlorine dioxide is sent to absorption tower;4) sodium chlorite solution is made after absorbing in chlorine dioxide and hydrogen peroxide and lye.The saltcake that the present invention generates script in chlorine dioxide generator is generated in feedstock processing process in advance, and by becoming the anhydrous sodium sulphate that can be taken out after separation drying;Meanwhile Na+, SO42-, H+, ClO32- for reacting in extraction raffinate being enable to be recycled, the usage amount of sodium chlorate, sulfuric acid is not only reduced, but also without waste liquid outlet.
Description
Technical field
It is specifically a kind of to be based on chloric acid and Hydrogen Peroxide Production sodium chlorite the invention belongs to sodium chlorite preparation technical field
Equipment and its production method.
Background technique
Sodium chlorite is a kind of high-efficient oxidant, is had many uses general, is mainly used for that cotton spinning, flax, paper pulp bleaching, food disappears
Poison, water process, sterilization algae removal and fish medicine manufacture etc..Sodium chlorite product has solid and two kinds of liquid, but leads in many applications
Domain all uses liquid, and main cause is because solid product risk is big, and liquid product risk is small.Liquid product is used at present
Content is generally in 20~30% (w/w), and stable at normal temperature, the general shelf-life was up to 12 months or more.
Currently, the domestic industry production most common horizontal generator of sodium chlorite prepares chlorine dioxide production chlorous acid
The production method of sodium, there are the directly outer pollution discharging environment of acid waste liquid that chlorine dioxide preparation system generates, and the chlorine in spent acid
The problems such as sour sodium, sulfuric acid, byproduct saltcake can not efficiently use.
Therefore need to develop a kind of low and environmentally friendly sodium chlorite production method of consumption of raw materials and device.
Summary of the invention
Technical problem to be solved by the invention is to provide it is a kind of consume it is low and environmentally friendly based on chloric acid and Hydrogen Peroxide Production
The equipment and its production method of sodium chlorite, the equipment is in feedstock processing process configurations crystallizing evaporator, saltcake filtering and drying
Device, vapour condensation device generate the saltcake generated in chlorine dioxide generator originally in feedstock processing process in advance, and
By becoming the anhydrous sodium sulphate that can be taken out after separation drying;Meanwhile it sending the reaction solution after reaction back to crystallizing evaporator and being evaporated
Concentration, so that the Na in reaction extraction raffinate+、SO4 2-、H+、ClO3 2-It can be recycled, both reduce the usage amount of sodium chlorate, sulfuric acid,
Again without waste liquid outlet.
The present invention solves above-mentioned technical problem with following technical solution:
A kind of equipment based on chloric acid and Hydrogen Peroxide Production sodium chlorite of the present invention, by material crystal processing system, dioxy
Change chlorine preparation system and sodium chlorite preparation system composition, the material crystal processing system includes crystallizing evaporator 1, heater
2, filter device 5, drying device 6 are connected between crystallizing evaporator 1 and heater 2 by upper circular tube 19 and lower circulation pipe 21,
Arrival end of the bottom of crystallizing evaporator 1 through lower circulation pipe 21 connection heater 2, the outlet end of heater 2 is through upper circular tube 19
Crystallizing evaporator 1 is connected, upper circular tube 19 and lower circulation pipe 21 are respectively connected to sulfuric acid pipe 20 and sodium chlorate's pipe 22, and lower circulation pipe
Circulating pump 3 is installed, the arrival end of filter device 5 is connected through feeder sleeve 23 with lower circulation pipe 21, and the feeder sleeve 23 on 21
On filter device charging pump 4 is installed, the discharge port of filter device 5 connects drying device 6, and the liquid outlet of filter device 5 is through filtering
Liquid return pipe 32 is connected with lower circulation pipe 21, and the top exit of crystallizing evaporator 1 is sequentially connected condensation through steam exhaust pipe 31
Device 15, condensate draining 16 and vacuum pump 17;The chlorine dioxide preparation system includes generator 8, the feed(raw material)inlet end of generator 8
Connect dioxygen water pipe 25 and raw feed materials pipe 24, the clarification on other end connection 1 top of crystallizing evaporator of raw feed materials pipe 24
Liquid outlet, and the raw feed materials pipe 24 is equipped with clarification liquid pump 7, the bottom of generator 8 connects air compressor through air hose 27
9, the reacted liquid return pipe 28 of the liquid outlet of generator 8 connects the lower circulation pipe 21 of material crystal processing system, and reaction solution returns
Reaction solution reflux pump 10 is installed, the gas vent of generator 8 drains into sodium chlorite through chlorine dioxide exhaust pipe 26 in flow tube 28
Preparation system;The sodium chlorite preparation system includes absorption tower 11, cooler 12 and sodium chlorite storage tank 14, absorption tower 11
Bottom inlet connects chlorine dioxide exhaust pipe 26, and the top entry on absorption tower 11 connects absorption tower dioxygen water pipe 29, absorption tower 11
Centre entrance connect alkali liquor pipe 30, the outlet at bottom on absorption tower 11 connects chlorous acid sodium pump 13, the outlet point of chlorous acid sodium pump 13
Two-way connects sodium chlorite storage tank 14 all the way, and another way connects cooler 12, and the outlet of cooler 12 connects alkali liquor pipe 30, absorbs
The top exit of tower 11 connects exhaust fan 18.
The generator is horizontal generator.
The present invention is based on the production methods that the equipment of chloric acid and Hydrogen Peroxide Production sodium chlorite uses, including operate step as follows
It is rapid:
Step 1, raw material sulphuric acid and sodium chlorate are put into crystallizing evaporator through sulfuric acid pipe and sodium chlorate pipe respectively, then
It is heated by heater, two kinds of raw materials is made to carry out metathesis reaction in crystallizing evaporator, sodium chloride crystal body is precipitated, evaporates simultaneously
The extra moisture of raw material;Then the material solution with charging pump by crystallizing evaporator bottom containing crystalline solid is evacuated to filter device mistake
Filter, the filter cake filtered out enter drying device drying and anhydrous sodium sulphate are made, filtrate is returned to crystallizing evaporator and is recycled;
Step 2, the water vapour that crystallizing evaporator is evaporated is extracted out by vacuum pump, after condenser condenses, into condensation
Sink storage, for dissolving sodium chlorate;
Step 3, the clarified solution on crystallizing evaporator top is pumped to generator by clarified solution, reacts with hydrogen peroxide and prepares dioxy
Change chlorine, and by the way that in generator bottom compression contracting air aeration, chlorine dioxide abjection is sent to absorption tower;After generator reaction
The reacted liquid reflux pumped back crystallizing evaporator of reaction solution, concentration cycles use;
Step 4, for chlorine dioxide in absorption tower, it is molten that sodium chlorite is made after absorbing in the hydrogen peroxide and lye being added into
Liquid, sodium chlorite solution are pumped out by sodium chlorite pump liquid, a part of solution be recycled back to absorption tower mixed with hydrogen peroxide, lye it is laggard
One step absorbs chlorine dioxide, and a part is pumped to the storage of sodium chlorite storage tank;The tail gas that absorption tower generates after absorbing passes through tail gas
Blower extraction emptying.
In step 1, temperature control is at 65~68 DEG C in the crystallizing evaporator, and vacuum degree control is in -80~-82Kpa.
In step 2, condenser condensate temperature control after cooling is at 38 DEG C or less.
In step 3, generator is by adding automatic steam control reaction temperature to rise to 80~85 DEG C step by step by 40~50 DEG C.
In step 4, temperature control is at 35 DEG C hereinafter, the mass concentration of the sodium chlorite solution of preparation passes through tune in absorption tower
The lye being added and dioxygen water management are saved 20%~35%.
It is anti-that raw material of the invention carries out double decomposition before preparing chlorine dioxide into generator, first in crystallizing evaporator
It answers (see reaction equation 1), and utilizes the lower characteristic of saltcake solubility, sodium chloride crystal body is precipitated in heating concentration.After evaporative crystallization
Clarified solution, main component are chloric acid (containing a small amount of Na+、SO4 2-), chlorine dioxide is produced after reacting into generator with hydrogen peroxide
(see reaction equation 2).
(1)H2SO4+2NaClO3→Na2SO4+2HClO3
(2)2HClO3+H2O2→ClO2+2H2O+O2
Reaction solution after reaction is mainly water, a small amount of Na+、SO4 2-And unreacted HClO3, by pumped back evaporative crystallization
Device carries out concentration cycles use.System is generated without waste liquid and solid waste.
The invention has the following advantages:
1, in feedstock processing process configurations crystallizing evaporator, saltcake filtering and drying device, vapour condensation device, make originally
The saltcake generated in chlorine dioxide generator is generated in feedstock processing process in advance, and by becoming to take out after separation drying
Anhydrous sodium sulphate.
2, it sends the reaction solution after reaction back to crystallizing evaporator and is evaporated concentration, so that the Na in reaction extraction raffinate+、
SO4 2-、H+、ClO3 2-It can be recycled, not only reduce the usage amount of sodium chlorate, sulfuric acid, but also without waste liquid outlet.
Detailed description of the invention
Fig. 1 is a kind of overall structure figure of the equipment based on chloric acid and Hydrogen Peroxide Production sodium chlorite of the present invention.
In Fig. 1: 1, crystallizing evaporator;2, heater;3, circulating pump;4, filter device charging pump;5, filter device;6, it does
Dry device;7, liquid pump is clarified;8, generator;9, air compressor;10, reaction solution reflux pump;11, absorption tower;12, cooler;
13, chlorous acid sodium pump;14, sodium chlorite storage tank;15, condenser;16, condensate draining;17, vacuum pump;18, exhaust fan;19,
Upper circular tube;20, sulfuric acid pipe;21, lower circulation pipe;22, sodium chlorate pipe;23, saltcake feeder sleeve;24, raw feed materials pipe;25, it sends out
Raw device dioxygen water pipe;26, chlorine dioxide exhaust pipe;27, air hose;28, reaction solution return pipe;29, absorption tower dioxygen water pipe;
30, absorption tower alkali liquor pipe;31, steam exhaust pipe;32, filtrate return pipe.
Specific embodiment
The present invention is described in detail below with reference to the accompanying drawings and embodiments, and described embodiment is only the present invention
A part of the embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not having
Every other embodiment obtained under the premise of creative work is made, shall fall within the protection scope of the present invention.
As shown in Figure 1, a kind of equipment based on chloric acid and Hydrogen Peroxide Production sodium chlorite of the present invention includes including evaporation knot
Brilliant device 1, heater 2, circulating pump 3, filter device charging pump 4, filter device 5, drying device 6, clarification liquid pump 7, generator 8,
Air compressor 9, reaction solution reflux pump 10, absorption tower 11, cooler 12, chlorous acid sodium pump 13, sodium chlorite storage tank 14, condensation
Device 15, condensate draining 16, vacuum pump 17, exhaust fan 18;Crystallizing evaporator 1, heater 2, circulating pump 3 in device, on follow
Endless tube 19, lower circulation pipe 21, sulfuric acid pipe 20, sodium chlorate pipe 22 connect and compose raw material evaporative crystallization circulation loop, with filter device
Charging pump 4, filter device 5, drying device 6, feeder sleeve 23, condenser 15, condensate draining 16, vacuum pump 17, steam exhaust pipe
31 constitutive material crystallization treatment systems together;Generator 8, air compressor 9, reaction solution reflux pump 10 and raw feed materials pipe 24,
Dioxygen water pipe 25, reaction solution return pipe 28 constitute chlorine dioxide preparation system together;Absorption tower 11, chlorous acid sodium pump 13, cooling
Device 12, sodium chlorite storage tank 14, exhaust fan 18, dioxygen water pipe 29, alkali liquor pipe 30 etc. form sodium chlorite preparation system.
The material crystal processing system includes crystallizing evaporator 1, heater 2, filter device 5, drying device 6, evaporation
It is connected between crystallizer 1 and heater 2 by upper circular tube 19 and lower circulation pipe 21, the bottom of crystallizing evaporator 1 is through lower circulation
Pipe 21 connects the arrival end of heater 2, and the outlet end of heater 2 connects crystallizing evaporator 1, upper circular tube 19 through upper circular tube 19
It is respectively connected to sulfuric acid pipe 20 and sodium chlorate's pipe 22 with lower circulation pipe 21, and circulating pump 3, filter device are installed on lower circulation pipe 21
5 arrival end is connected through feeder sleeve 23 with lower circulation pipe 21, and is equipped with filter device charging pump 4, mistake on the feeder sleeve 23
The discharge port for filtering device 5 connects drying device 6, and the liquid outlet of filter device 5 is connected through filtrate return pipe 32 with lower circulation pipe 21
It connects, the top exit of crystallizing evaporator 1 is sequentially connected condenser 15, condensate draining 16 and vacuum pump 17 through steam exhaust pipe 31.
The chlorine dioxide preparation system includes generator 8, and the feed(raw material)inlet end of generator 8 connects generator dioxygen water pipe
25 and raw feed materials pipe 24, the clarified solution outlet on other end connection 1 top of crystallizing evaporator of raw feed materials pipe 24, and the original
Expect that feeder sleeve 24 is equipped with clarification liquid pump 7, the bottom of generator 8 connects air compressor 9, the liquid of generator 8 through air hose 27
Body exports the lower circulation pipe 21 that reacted liquid return pipe 28 connects material crystal processing system, installs on the reaction solution return pipe 28
There is reaction solution reflux pump 10, the gas vent of generator 8 drains into sodium chlorite preparation system through chlorine dioxide exhaust pipe 26.
The sodium chlorite preparation system includes absorption tower 11, cooler 12 and sodium chlorite storage tank 14, absorption tower 11
Bottom inlet connects chlorine dioxide exhaust pipe 26, and the top entry on absorption tower 11 connects absorption tower dioxygen water pipe 29, absorption tower 11
Centre entrance connect absorption tower alkali liquor pipe 30, the outlet at bottom on absorption tower 11 connects chlorous acid sodium pump 13, chlorous acid sodium pump 13
Outlet divides two-way, connects sodium chlorite storage tank 14 all the way, and another way connects cooler 12, and the outlet of cooler 12 connects alkali liquor pipe
30, the top exit on absorption tower 11 connects exhaust fan 18.
The generator 8 that the present invention uses is horizontal generator.
Production method of the invention produces sodium chlorite solution using hydrogen peroxide, sulfuric acid, sodium chlorate, lye as raw material, simultaneously
Anhydrous sodium sulphate is made in dry saltcake, is the specific application example that the sodium chlorite of 15t/d is prepared using above-mentioned apparatus below:
Embodiment 1, specific steps are as follows:
Step 1, raw material sulphuric acid, sodium chlorate are put into crystallizing evaporator through sulfuric acid pipe and sodium chlorate pipe respectively, is passed through
Heater heating, makes two kinds of raw materials carry out metathesis reaction in crystallizing evaporator, sodium chloride crystal body is precipitated, while evaporating raw material
Extra moisture;Then the material solution with charging pump by crystallizing evaporator bottom containing crystalline solid is evacuated to filter device filtering, mistake
The filter cake filtered out enters drying device drying and is made anhydrous sodium sulphate (can take out), and filtrate returns to crystallizing evaporator and is recycled, this
In step, the temperature in crystallizing evaporator is controlled at 65 DEG C, vacuum degree control is in -80Kpa;
Step 2, the water vapour that crystallizing evaporator is evaporated is extracted out by vacuum pump, after condenser condenses, into condensation
Sink storage, for dissolving sodium chlorate, wherein condenser condensate temperature control after cooling is at 37 DEG C;
Step 3, the clarified solution on crystallizing evaporator top is pumped by clarification liquid pump to generator, is reacted with hydrogen peroxide and is prepared dioxy
Change chlorine, and by the way that in generator bottom compression contracting air aeration, chlorine dioxide abjection is sent to absorption tower;In this step, it will send out
Raw device is by adding steam that reaction temperature is made to rise to 80 DEG C step by step by 40 DEG C;And the reaction solution after reacting generator is returned by reaction solution
Pumped back crystallizing evaporator is flowed, concentration cycles use is carried out;
Step 4, chlorine dioxide is in absorption tower, and the hydrogen peroxide that is added into, that sodium chlorite is made after absorbing in lye is molten
Liquid;Chlorous acid sodium pump pumps out solution, and a part of solution, which is recycled back to after absorption tower is mixed with hydrogen peroxide, lye, further absorbs two
Chlorine monoxid, a part are pumped to the storage of sodium chlorite storage tank;The tail gas generated after absorption is extracted out by exhaust fan and is emptied, this step
In rapid, by temperature control in absorption tower at 35 DEG C, sodium chlorite solution's concentration of preparation can be by adjusting the alkali being added, dioxygen
Water concentration is controlled in 30% (w/w).
Use the result of the method for the present invention: sodium chlorite (100%) consumption sodium chlorate per ton is 1.295t, consumption sulfuric acid
0.71t, than mode few 0.015t, 1.2t respectively of conventionally employed horizontal generator preparation chlorine dioxide production sodium chlorite.
Embodiment 2, specific steps are as follows:
Step 1, raw material sulphuric acid, sodium chlorate are put into crystallizing evaporator through sulfuric acid pipe and sodium chlorate pipe respectively, by adding
Hot device heating, makes two kinds of raw materials carry out metathesis reaction in crystallizing evaporator, sodium chloride crystal body is precipitated, while it is more to evaporate raw material
Remaining moisture;Then the material solution with charging pump by crystallizing evaporator bottom containing crystalline solid is evacuated to filter device filtering, filtering
Filter cake out enters drying device drying and is made anhydrous sodium sulphate (can take out), and filtrate returns to crystallizing evaporator and is recycled, this step
In rapid, the temperature in crystallizing evaporator is controlled at 67 DEG C, vacuum degree control is in -81Kpa;
Step 2, the water vapour that crystallizing evaporator is evaporated is extracted out by vacuum pump, after condenser condenses, into condensation
Sink storage, for dissolving sodium chlorate, wherein condenser condensate temperature control after cooling is at 36 DEG C;
Step 3, the clarified solution on crystallizing evaporator top is pumped by clarification liquid pump to generator, is reacted with hydrogen peroxide and is prepared dioxy
Change chlorine, and by chlorine dioxide abjection being sent to absorption tower, in this step, will be sent out in generator bottom compression contracting air aeration
Raw device is by adding steam that reaction temperature is made to rise to 83 DEG C step by step by 47.5 DEG C;And the reaction solution after reacting generator is by reaction solution
Flow back pumped back crystallizing evaporator, carries out concentration cycles use;
Step 4, chlorine dioxide is in absorption tower, and the hydrogen peroxide that is added into, that sodium chlorite is made after absorbing in lye is molten
Liquid;Chlorous acid sodium pump pumps out solution, and a part of solution, which is recycled back to after absorption tower is mixed with hydrogen peroxide, lye, further absorbs two
Chlorine monoxid, a part are pumped to the storage of sodium chlorite storage tank;The tail gas generated after absorption is extracted out by exhaust fan and is emptied, this step
In rapid, by temperature control in absorption tower at 34 DEG C, sodium chlorite solution's concentration of preparation can be by adjusting the alkali being added, dioxygen
Water concentration is controlled 30.2%.
Use the result of the method for the present invention: sodium chlorite (100%) consumption sodium chlorate per ton is 1.296t, consumption sulfuric acid
0.70t, than mode few 0.014t, 1.21t respectively of conventionally employed horizontal generator preparation chlorine dioxide production sodium chlorite.
Embodiment 3, specific steps are as follows:
Step 1, raw material sulphuric acid, sodium chlorate are put into crystallizing evaporator through sulfuric acid pipe and sodium chlorate pipe respectively, by adding
Hot device heating, makes two kinds of raw materials carry out metathesis reaction in crystallizing evaporator, sodium chloride crystal body is precipitated, while it is more to evaporate raw material
Remaining moisture;Then the material solution with charging pump by crystallizing evaporator bottom containing crystalline solid is evacuated to filter device filtering, filtering
Filter cake out enters drying device drying and is made anhydrous sodium sulphate (can take out), and filtrate returns to crystallizing evaporator and is recycled, this step
In rapid, temperature in crystallizing evaporator is controlled at 68 DEG C, vacuum degree control is in -82Kpa.
Step 2, the water vapour that crystallizing evaporator is evaporated is extracted out by vacuum pump, after condenser condenses, into condensation
Sink storage, for dissolving sodium chlorate, wherein condenser condensate temperature control after cooling is at 35 DEG C;
Step 3, the clarified solution on crystallizing evaporator top is pumped by clarification liquid pump to generator, is reacted with hydrogen peroxide and is prepared dioxy
Change chlorine, and by chlorine dioxide abjection being sent to absorption tower, in this step, will be sent out in generator bottom compression contracting air aeration
Raw device is by adding steam that reaction temperature is made to rise to 85 DEG C step by step by 50 DEG C, and the reaction solution after generator is reacted is returned by reaction solution
Pumped back crystallizing evaporator is flowed, concentration cycles use is carried out;
Step 4, chlorine dioxide is in absorption tower, and the hydrogen peroxide that is added into, that sodium chlorite is made after absorbing in lye is molten
Liquid;Chlorous acid sodium pump pumps out solution, and a part of solution, which is recycled back to after absorption tower is mixed with hydrogen peroxide, lye, further absorbs two
Chlorine monoxid, a part are pumped to the storage of sodium chlorite storage tank;The tail gas generated after absorption is extracted out by exhaust fan and is emptied, this step
In rapid, by temperature control in absorption tower at 33 DEG C, sodium chlorite solution's concentration of preparation can be by adjusting the alkali being added, dioxygen
Water concentration is controlled 30.2%.
Use the result of the method for the present invention: sodium chlorite (100%) consumption sodium chlorate per ton is 1.294t, consumption sulfuric acid
0.705t, than mode few 0.016t, 1.205t respectively of conventionally employed horizontal generator preparation chlorine dioxide production sodium chlorite.
The method of the present invention chlorine dioxide preparation before, by crystallizing evaporator by the ion in raw material sulphuric acid, sodium chlorate into
Row exchanges, and the sodium chloride crystal in solution is precipitated heating evaporation, to achieve the purpose that in advance to separate saltcake dry;And lead to
The recycling of the extraction raffinate blowback crystallizing evaporator after reacting generator is crossed, achievees the purpose that reduce sodium chlorate and sulfuric acid consumption,
And without waste outlet.
Having used specific embodiment above, the present invention is described in detail, although on the basis of the present invention, for
Engineering construction need, a specific embodiment of the invention can be made some modifications or improvements, but to those skilled in the art and
Speech is obviously, does not make the modification made under the premise of creative work, be shall fall within the protection scope of the present invention.
Claims (7)
1. a kind of equipment based on chloric acid and Hydrogen Peroxide Production sodium chlorite, which is characterized in that the device is handled by material crystal
System, chlorine dioxide preparation system and sodium chlorite preparation system composition, the material crystal processing system includes evaporative crystallization
Device (1), heater (2), filter device (5), drying device (6), by upper circulation between crystallizing evaporator (1) and heater (2)
Pipe (19) is connected with lower circulation pipe (21), bottom the entering through lower circulation pipe (21) connection heater (2) of crystallizing evaporator (1)
The outlet end at mouth end, heater (2) connects crystallizing evaporator (1) through upper circular tube (19), upper circular tube (19) and lower circulation pipe
(21) it is respectively connected to sulfuric acid pipe (20) and sodium chlorate manages (22), and circulating pump (3), filter device are installed on lower circulation pipe (21)
(5) arrival end is connected through feeder sleeve (23) with lower circulation pipe (21), and filter device confession is equipped on the feeder sleeve (23)
The discharge port of material pump (4), filter device (5) connects drying device (6), and the liquid outlet of filter device (5) is through filtrate return pipe
(32) it is connected with lower circulation pipe (21), the top exit of crystallizing evaporator (1) is sequentially connected condensation through steam exhaust pipe (31)
Device (15), condensate draining (16) and vacuum pump (17);The chlorine dioxide preparation system includes generator (8), generator (8)
Feed(raw material)inlet end connects dioxygen water pipe (25) and raw feed materials pipe (24), the other end connection evaporation knot of raw feed materials pipe (24)
The clarified solution on brilliant device (1) top exports, and the raw feed materials pipe (24) is equipped with clarification liquid pump (7), the bottom warp of generator (8)
Air hose (27) connects air compressor (9), and the reacted liquid return pipe (28) of the liquid outlet of generator (8) connects material crystal
The lower circulation pipe (21) of processing system is equipped with reaction solution reflux pump (10) on reaction solution return pipe (28), the gas of generator (8)
Body outlet drains into sodium chlorite preparation system through chlorine dioxide exhaust pipe (26);The sodium chlorite preparation system includes absorption tower
(11), the bottom inlet of cooler (12) and sodium chlorite storage tank (14), absorption tower (11) connects chlorine dioxide exhaust pipe (26),
The top entry on absorption tower (11) connects absorption tower dioxygen water pipe (29), and the centre entrance of absorption tower (11) connects alkali liquor pipe (30),
The outlet at bottom on absorption tower (11) connects chlorous acid sodium pump (13), and the outlet of chlorous acid sodium pump (13) divides two-way, and connection is sub- all the way
Sodium chlorate storage tank (14), another way connect cooler (12), and the outlet of cooler (12) connects alkali liquor pipe (30), absorption tower (11)
Top exit connects exhaust fan (18).
2. the equipment based on chloric acid and Hydrogen Peroxide Production sodium chlorite according to claim 1, it is characterised in that: the generation
Device is horizontal generator.
3. the production method according to claim 1 or claim 2 used based on the equipment of chloric acid and Hydrogen Peroxide Production sodium chlorite,
It is characterized in that, it includes following operating procedure:
Step 1, raw material sulphuric acid and sodium chlorate are put into crystallizing evaporator through sulfuric acid pipe and sodium chlorate pipe respectively, is then passed through
Heater heating, makes two kinds of raw materials carry out metathesis reaction in crystallizing evaporator, sodium chloride crystal body is precipitated, while evaporating raw material
Extra moisture;Then the material solution with charging pump by crystallizing evaporator bottom containing crystalline solid is evacuated to filter device filtering, mistake
The filter cake filtered out enters drying device drying and anhydrous sodium sulphate is made, and filtrate is returned to crystallizing evaporator and is recycled;
Step 2, the water vapour that crystallizing evaporator is evaporated is extracted out by vacuum pump, after condenser condenses, into condensate draining
Storage, for dissolving sodium chlorate;
Step 3, the clarified solution on crystallizing evaporator top is pumped to generator by clarified solution, and preparation titanium dioxide is reacted with hydrogen peroxide
Chlorine, and by the way that in generator bottom compression contracting air aeration, chlorine dioxide abjection is sent to absorption tower;It is anti-after generator reaction
The reacted liquid reflux pumped back crystallizing evaporator of liquid is answered, concentration cycles use;
Step 4, for chlorine dioxide in absorption tower, sodium chlorite solution is made after absorbing in the hydrogen peroxide and lye being added into,
Sodium chlorite solution is pumped out by sodium chlorite pump liquid, and a part of solution is recycled back to absorption tower and mixes laggard one with hydrogen peroxide, lye
Step absorbs chlorine dioxide, and a part is pumped to the storage of sodium chlorite storage tank;The tail gas that absorption tower generates after absorbing passes through tail gas wind
Machine extraction emptying.
4. the production method used according to claim 3 based on the equipment of chloric acid and Hydrogen Peroxide Production sodium chlorite, special
Sign is: in step 1, temperature control is at 65~68 DEG C in the crystallizing evaporator, and vacuum degree control is in -80~-82Kpa.
5. the production method used according to claim 3 based on the equipment of chloric acid and Hydrogen Peroxide Production sodium chlorite, special
Sign is: in step 2, condenser condensate temperature control after cooling is at 38 DEG C or less.
6. the production method used according to claim 3 based on the equipment of chloric acid and Hydrogen Peroxide Production sodium chlorite, special
Sign is: in step 3, generator is by adding automatic steam control reaction temperature to rise to 80~85 DEG C step by step by 40~50 DEG C.
7. the production method used according to claim 3 based on the equipment of chloric acid and Hydrogen Peroxide Production sodium chlorite, special
Sign is: in step 4, temperature control is at 35 DEG C hereinafter, the mass concentration of the sodium chlorite solution of preparation passes through tune in absorption tower
The lye being added and dioxygen water management are saved 20%~35%.
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US3563702A (en) * | 1968-03-05 | 1971-02-16 | Hooker Chemical Corp | Production of chlorine dioxide |
CN105439096A (en) * | 2015-12-02 | 2016-03-30 | 广西大学 | Environment-friendly sodium chlorite preparing method and device by means of hydrogen peroxide method chlorine dioxide technology |
CN108439341A (en) * | 2018-05-18 | 2018-08-24 | 广西大学 | A kind of method and device producing chlorine dioxide with high purity gas |
CN108529562A (en) * | 2018-05-14 | 2018-09-14 | 湖南恒光科技股份有限公司 | A kind of chloric acid mother liquid of sodium embrane method freezing denitrating technique |
CN208454495U (en) * | 2018-05-18 | 2019-02-01 | 广西大学 | A kind of device producing chlorine dioxide with high purity gas |
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- 2019-04-25 CN CN201910341113.0A patent/CN110015638A/en active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
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US3563702A (en) * | 1968-03-05 | 1971-02-16 | Hooker Chemical Corp | Production of chlorine dioxide |
CN105439096A (en) * | 2015-12-02 | 2016-03-30 | 广西大学 | Environment-friendly sodium chlorite preparing method and device by means of hydrogen peroxide method chlorine dioxide technology |
CN108529562A (en) * | 2018-05-14 | 2018-09-14 | 湖南恒光科技股份有限公司 | A kind of chloric acid mother liquid of sodium embrane method freezing denitrating technique |
CN108439341A (en) * | 2018-05-18 | 2018-08-24 | 广西大学 | A kind of method and device producing chlorine dioxide with high purity gas |
CN208454495U (en) * | 2018-05-18 | 2019-02-01 | 广西大学 | A kind of device producing chlorine dioxide with high purity gas |
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