CN208454495U - A kind of device producing chlorine dioxide with high purity gas - Google Patents
A kind of device producing chlorine dioxide with high purity gas Download PDFInfo
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- CN208454495U CN208454495U CN201820747282.5U CN201820747282U CN208454495U CN 208454495 U CN208454495 U CN 208454495U CN 201820747282 U CN201820747282 U CN 201820747282U CN 208454495 U CN208454495 U CN 208454495U
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- mother liquor
- chlorine dioxide
- pipe
- generator
- crystallizing evaporator
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Abstract
The utility model discloses a kind of device for producing chlorine dioxide with high purity gas, the generator of the device connects with sulfuric acid pipe, dioxygen water pipe and sodium chlorate pipe, and generator connects mother liquor letdown tank;Circulation loop is formed between crystallizing evaporator and heater, which communicates with mother liquor letdown tank, and circulation pipe connect and is formed into a loop with filter device under mother liquor, filter device outlet connection drier;Crystallizing evaporator connects with generator inlet, is equipped with mother liquor tank on the pipeline.Utility model device is using hydrogen peroxide as reducing agent, when producing chlorine dioxide using generator, aeration stirring is carried out to reaction solution using air, and the chlorine dioxide produced is diluted, continuously produces the few chlorine dioxide of purity is high, moisture content;Crystallization, filtering, drying are evaporated to the byproduct saltcake of generation using crystallizing evaporator, drier simultaneously, anhydrous sodium sulphate is made.Utility model device is used, so that entire production process is generated without solid waste and waste liquid.
Description
Technical field
The utility model belongs to chlorine dioxide Preparation equipment technical field, specifically a kind of production chlorine dioxide with high purity gas
The device of body.
Background technique
Chlorine dioxide (ClO2) it is at normal temperatures and pressures orange-yellow gas, there is the stimulation similar to chlorine and ozone mixture
Property pungent, boiling point be 11 DEG C, freezing point be -59 DEG C, at 11 DEG C gaseous density be 3.09g/m3.Gaseous state ClO2It is unstable, high concentration
Shi Guangzhao or decomposition the production oxygen, chlorine of setting off an explosion that is in contact with organic matter.Under normal circumstances, it is prepared in situ, scene makes
With.It is relatively stable when being diluted to 12% volume content or less with air, vapor under room temperature or be low-temperature aqueous solution state.
ClO2With very Strong oxdiative ability, it can be used as bleaching agent, water treatment agent, novel air the purification freshener of paper pulp and textile etc.
With the disinfection, sterilization, deodorant for diet, epidemic prevention, health etc..
Currently, the method for industrial production chlorine dioxide mainly has methanol method, synthesis, wherein methanol method with methanol, sulfuric acid,
Sodium chlorate is raw material, prepares chlorine dioxide using vertical generator, the chlorine dioxide moisture content of generation is big, up to 80% (w/
W) more than, and chlorine containing small part;Synthesis, both can be with vertical generator or with horizontal hair using hydrochloric acid, sodium chlorate as raw material
Raw device, but the chlorine dioxide generated is big containing amount of chlorine, and the molar ratio of chlorine dioxide and chlorine is 2:1.For purity requirement
It is higher to use field (such as sodium chlorite preparation, food, medicine industry), the chlorine dioxide of both the above preparation method production
Purity is unable to reach requirement.
And the Chlorine dioxide production of traditional commercial silica chlorine preparation facilities preparation is with low temperature aqueous solution of chlorine dioxide
Form be pumped into point of use use, also reported at present there is not yet sending outside in gaseous form as product to the related of point of use
It leads.
Utility model content
The technical problem to be solved by the utility model is to provide a kind of devices for producing chlorine dioxide with high purity gas, should
Device can produce the low chlorine dioxide product and anhydrous sodium sulphate byproduct of purity is high, moisture content, and in production process
Without solid waste and waste liquid outlet.
The utility model solves above-mentioned technical problem with following technical solution:
The device of the utility model production chlorine dioxide with high purity gas comprising generator, crystallizing evaporator, heating
The entrance of device, the generator connects with sulfuric acid pipe, dioxygen water pipe and sodium chlorate pipe, the reaction solution outlet connection mother liquor of generator
Letdown tank;It connects by circulation pipe under mother liquor upper circular tube and mother liquor between the crystallizing evaporator and heater and forms evaporation
Crystallisation cycle circuit, the circulation loop are connected with mother liquor letdown tank, reaction mother liquor are supplied by mother liquor letdown tank, under the mother liquor
Circulation pipe connect with filter device by the road and is formed filtrate cycle circuit, by filter device by crystallizing evaporator lower part and mother
The saltcake that circulation pipe generates under liquid is filtered, and the sludge outlet of filter device connects drier;The crystallizing evaporator it is upper
Portion connects with the entrance of generator by the road, is equipped with mother liquor tank on the pipeline.
The dioxygen water pipe and sodium chlorate manifold access generator after closing.
The generator connection heat source tube, air compressor machine, air blower and air-introduced machine.
On the connecting line of the crystallizing evaporator and generator, filter device charging pump turnover pipeline, evaporative crystallization follow
In the loop back path and outlet of mother liquor letdown tank is mounted on pump.
The reactor is horizontal reactor.
The utility model produces the device of chlorine dioxide with high purity gas, has the advantages that
1, utility model device between horizontal generator and crystallizing evaporator by configuring mother liquor letdown tank and mother liquor
Tank, makes chlorine dioxide reaction device and evaporated crystallization device relative separation, independence, at the same mother liquor letdown tank and mother liquor tank play it is slow
The effect of depositing enables chlorine dioxide preparation system continuous and stable to run;
2, the chlorine dioxide purity is high that utility model device uses hydrogen peroxide, sulfuric acid, sodium chlorate to produce for raw material;
Using horizontal generator, by 25 DEG C to 85 DEG C stepped heating reaction solutions under the conditions of tiny structure, reaction solution moisture can effectively avoid
Excessive evaporation, and saltcake is caused to crystallize in generator, generator is blocked, while can avoid reaction and acutely causing chlorine dioxide point
The chlorine dioxide moisture content of solution, preparation is lower than 8% (w/w), is substantially free of chlorine;It is sleeping that Dilution air is blasted by air blower
Chlorine dioxide in formula generator is not easily decomposed chlorine dioxide stabilization to 4~9% (V/V);By controlling evaporative crystallization
At 70~73 DEG C, the byproduct saltcake of generation can be carried out concentration knot in -79~-81KPa by vacuum degree control for temperature control in device
The anhydrous sodium sulphate that can be sold outside is made in crystalline substance after filtration drying;Filtered filtrate recycle, no solid waste outlet.
Detailed description of the invention
Fig. 1 is the overall structure figure of the device of the utility model production chlorine dioxide with high purity gas.
In figure: 1, sulfuric acid pipe;2, dioxygen water pipe;3, sodium chlorate pipe;4, horizontal generator;5, heat source tube;6, compressed air
Pipe;7, air blower;8, air-introduced machine;9, mother liquor letdown tank;10, crystallizer feeding pump;11, circulating pump;12, heater;13, it evaporates
Crystallizer;14, filter device charging pump;15, filter device;16, drier;17, mother liquor extracts pump;18, mother liquor tank;19, female
Liquid reflux pump;20, mother liquor reflux pipe;21, heat source tube;22, filtrate pipe;23, circulation pipe under mother liquor;24, mother liquor upper circular tube;
25, reaction solution delivery pipe;26, crystallizer feeding pump passes in and out liquid pipe;27, mother liquor extracts pump disengaging liquid pipe;28, filter device is fed
Pump inlet/outlet pipe;29, saltcake discharge nozzle;30, air compressor machine.
Specific embodiment
The utility model is described in detail with reference to the accompanying drawings and examples, described embodiment is only this
Utility model a part of the embodiment, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this field
Art personnel every other embodiment obtained without making creative work belongs to the utility model protection
Range.
As shown in Figure 1, the device of the utility model production chlorine dioxide with high purity gas includes horizontal generator 4, air blast
Machine 7, air-introduced machine 8, mother liquor letdown tank 9, heater 12, crystallizing evaporator 13, filter device 15, drier 16, mother liquor tank 18, sky
Press 30, sulfuric acid pipe 1 connect with the feed(raw material)inlet of horizontal generator 4, and dioxygen water pipe 2 and sodium chlorate pipe 3 converge rear and horizontal hair
The feed(raw material)inlet of raw device 4 connects;Heat source tube 5 is connect with the entrance of horizontal generator 4;Air compressor machine 30 is through compressed air hose 6 and crouches
Formula generator 4 connects;Air blower 7 and air-introduced machine 8 are arranged in the two sides of horizontal generator 4 and connect with horizontal generator 4;It is sleeping
The outlet of formula generator 4 is connect by reaction solution delivery pipe 25 with mother liquor letdown tank 9;Between crystallizing evaporator 13 and heater 12
It is connected by circulation pipe 23 under mother liquor upper circular tube 24 and mother liquor and forms evaporative crystallization circulation loop, under mother liquor on circulation pipe 23
Circulating pump 11 is installed, heater 12 is connect with heat source tube 21, provides power supply heating by heat source tube 21;Mother liquor letdown tank 9 goes out
Mouth passes in and out liquid pipe 26 by crystallizer feeding pump and connect with circulation pipe 23 under mother liquor, installs in crystallizer feeding pump disengaging liquid pipe 26
There is crystallizer feeding pump 10, the reaction solution of mother liquor letdown tank 9 is sent by evaporative crystallization circulation loop by crystallizer feeding pump 10;
Circulation pipe 23 connects through filter device charging pump inlet/outlet pipe 28 with the entrance of filter device 15 under mother liquor, filter device charging pump into
Filter device charging pump 14 is installed, the filtrate (liquid of filter device 15 is through circulation pipe under filtrate pipe 22 and mother liquor in outlet pipe 28
23 connect, and make to form filtrate cycle circuit, the sludge outlet of filter device 15 under mother liquor between circulation pipe 23 and filter device 15
Connect through saltcake discharge nozzle 29 with drier 16, by filter device 15 by circulation pipe 23 under 13 lower part of crystallizing evaporator and mother liquor
The saltcake of generation is filtered;The top of crystallizing evaporator 13 extracts pump disengaging liquid pipe 27 through mother liquor and is connected with mother liquor tank 18,
Mother liquor, which extracts, is equipped with mother liquor extraction pump 17 in pump disengaging liquid pipe 27, the outlet of mother liquor tank 18 connects horizontal through mother liquor reflux pipe 20
The entrance of generator 4 is equipped with mother liquor reflux pump 19 on mother liquor reflux pipe 20.
Utility model device configures mother liquor letdown tank 9, mother liquor tank between horizontal generator 4 and crystallizing evaporator 13
18, make chlorine dioxide reaction device and evaporated crystallization device relative separation, independence, while mother liquor letdown tank 9, mother liquor tank 18 play
Caching effect, enables chlorine dioxide preparation system continuous and stable to run.
To make full use of saltcake and filtered filtrate, waste is not generated, filter device 15 is configured with filtrate pipe 22, awns
Nitre discharge nozzle 29 is connect with circulation pipe 23 under mother liquor and drier 16 respectively, forms filtrate return flow line and saltcake treatment channel.
Utility model device is to use hydrogen peroxide, sulfuric acid, sodium chlorate to produce chlorine dioxide for raw material, while will dry awns
Nitrate is the specific application example that the chlorine dioxide of 3t/d is prepared using utility model device below at anhydrous sodium sulphate:
Embodiment 1, specific steps are as follows:
Step 1, by sulfuric acid by sulfuric acid pipe 1 enter horizontal generator 4, reducing agent-hydrogen peroxide by dioxygen water pipe 2 with
Enter horizontal generator 4 after sodium chlorate mixing in sodium chlorate pipe 3, generates chlorine dioxide after carrying out redox reaction;
Heat source makes reacting liquid temperature by 20 into horizontal 4 stepped heating reaction solution of generator by heat source tube 5 under micro-vacuum state
DEG C 80 DEG C are risen to step by step;Air enters horizontal generator 4 after the compression of air compressor machine 30, while agitation reaction solution makes to react uniform
Discharge simultaneously diluted chlorine dioxide gas;In addition, air is blasted horizontal generator 4, further diluted chlorine dioxide gas by air blower 7
Bulk concentration is to 4% (V/V);Chlorine dioxide after dilution, which is sent through the extraction of air-introduced machine 8 to point of use, to be used;Product contains through detection
Water rate is 7.8% (w/w), is substantially free of chlorine.
Step 2, while raw material enters horizontal generator 4 from one end, the reaction solution after reaction is expelled to mother from the other end
Liquid letdown tank 9 is stored, circulation pipe 23 under then crystallized device feeding pump 10 is sent to mother liquor, under the pump action of circulating pump 11,
It recycles, heat between crystallizing evaporator 13 and heater 12, evaporation, concentration;Temperature control is at 73 DEG C in crystallizing evaporator, very
Reciprocal of duty cycle is controlled in -79KPa.The concentrated rear crystallization of saltcake in mother liquor, and it is heavy in 13 bottom of crystallizing evaporator and lower circulation pipe 23
Product is sent to filter device 15 through filter device charging pump 14 and is filtered, washs, being concentrated.Solid saltcake after concentration enters dry
Dry device 16 forms the anhydrous sodium sulphate (can be used as product sale) that mass dryness fraction reaches 99.6% after drying;The filtrate filtered out is through filtering
Liquid pipe 22 returns to circulation pipe 23 under mother liquor and recycles.In entire production process, no solid waste and waste liquid outlet.
Step 3,13 top clarified mother liquor of crystallizing evaporator extracts pump 17 through mother liquor and send to the caching of mother liquor tank 18, then by
Mother liquor reflux pump 19 is sent to horizontal generator 4.
Embodiment 2, specific steps are as follows:
Step 1, sulfuric acid is entered into horizontal generator 4 by sulfuric acid pipe 1, reducing agent --- hydrogen peroxide passes through dioxygen water pipe 2
Enter horizontal generator 4 after mixing with the sodium chlorate in sodium chlorate pipe 3, generates chlorine dioxide after carrying out redox reaction
Body;Heat source by heat source tube 5 enter horizontal 4 stepped heating reaction solution of generator, under micro-vacuum state, make reacting liquid temperature by
25 DEG C rise to 83 DEG C step by step;Air enters horizontal generator 4 after the compression of air compressor machine 30, and agitation reaction solution keeps reaction uniform same
When release and diluted chlorine dioxide gas;In addition, air is blasted horizontal generator 4, further diluted chlorine dioxide by air blower 7
Gas concentration is to 6% (V/V);Chlorine dioxide after dilution, which is sent through the extraction of air-introduced machine 8 to point of use, to be used;Product is through detecting
Moisture content is 7.6% (w/w), is substantially free of chlorine.
Step 2, while raw material enters horizontal generator 4 from one end, the reaction solution after reaction is expelled to mother from the other end
Liquid letdown tank 9 is stored, circulation pipe 23 under then crystallized device feeding pump 10 is sent to mother liquor, under the pump action of circulating pump 11,
It recycles, heat between crystallizing evaporator 13 and heater 12, evaporation, concentration;Temperature control is at 72 DEG C in crystallizing evaporator, very
Reciprocal of duty cycle is controlled in -80KPa.The concentrated rear crystallization of saltcake in mother liquor, and it is heavy in 13 bottom of crystallizing evaporator and lower circulation pipe 23
Product is sent to filter device 15 through filter device charging pump 14 and is filtered, washs, being concentrated.Solid saltcake after concentration enters dry
Dry device 16 forms the anhydrous sodium sulphate (can be used as product sale) that mass dryness fraction reaches 99.65% after drying;The filtrate filtered out is through filtering
Liquid pipe 22 returns to circulation pipe 23 under mother liquor and recycles.In entire production process, no solid waste and waste liquid outlet.
Step 3,13 top clarified mother liquor of crystallizing evaporator extracts pump 17 through mother liquor and send to the caching of mother liquor tank 18, then by
Mother liquor reflux pump 19 is sent to horizontal generator 4.
Embodiment 3, specific steps are as follows:
Step 1, sulfuric acid is entered into horizontal generator 4 by sulfuric acid pipe 1, reducing agent --- hydrogen peroxide passes through dioxygen water pipe 2
Enter horizontal generator 4 after mixing with the sodium chlorate in sodium chlorate pipe 3, generates chlorine dioxide after carrying out redox reaction
Body;Heat source makes reacting liquid temperature by 30 DEG C into horizontal 4 stepped heating reaction solution of generator by pipe 5 under micro-vacuum state
85 DEG C are risen to step by step;Air enters horizontal generator 4 after the compression of air compressor machine 3, and agitation reaction solution is released while making to react uniform
Put simultaneously diluted chlorine dioxide gas;In addition, air is blasted horizontal generator 4, further diluted chlorine dioxide gas by air blower 7
Concentration is to 9% (V/V);Chlorine dioxide after dilution, which is sent through the extraction of air-introduced machine 8 to point of use, to be used;Product is aqueous through detecting
Rate is 7.5% (w/w), is substantially free of chlorine.
Step 2, while raw material enters horizontal generator 4 from one end, the reaction solution after reaction is expelled to mother from the other end
Liquid letdown tank 9 is stored, circulation pipe 23 under then crystallized device feeding pump 10 is sent to mother liquor, under the pump action of circulating pump 11,
It recycles, heat between crystallizing evaporator 13 and heater 12, evaporation, concentration;Temperature control is at 70 DEG C in crystallizing evaporator, very
Reciprocal of duty cycle is controlled in -81KPa.The concentrated rear crystallization of saltcake in mother liquor, and it is heavy in 13 bottom of crystallizing evaporator and lower circulation pipe 23
Product is sent to filter device 15 through filter device charging pump 14 and is filtered, washs, being concentrated.Solid saltcake after concentration enters dry
Dry device 16 forms the anhydrous sodium sulphate (can be used as product sale) that mass dryness fraction reaches 99.6% after drying;The filtrate filtered out is through filtering
Liquid pipe 22 returns to circulation pipe 23 under mother liquor and recycles.In entire production process, no solid waste and waste liquid outlet.
Step 3,13 top clarified mother liquor of crystallizing evaporator extracts pump 17 through mother liquor and send to the caching of mother liquor tank 18, then by
Mother liquor reflux pump 19 is sent to horizontal generator 4.
The utility model uses hydrogen peroxide as reducing agent, when producing chlorine dioxide using generator, using air to anti-
It answers liquid to carry out aeration stirring, and the chlorine dioxide produced is diluted, it is few to continuously produce purity is high, moisture content
Chlorine dioxide;Crystallization, filtering, drying are evaporated to the byproduct saltcake of generation using crystallizing evaporator, drier, made
At anhydrous sodium sulphate.The entire production process of the utility model is generated without solid waste and waste liquid.
By utility model device, it is avoided that reaction is acutely in preparation process and chlorine dioxide concentration is excessively high, avoids
It decomposes;It is avoided that reaction temperature is excessively high simultaneously, transition evaporation water, saltcake crystallizes in horizontal generator 4, the titanium dioxide of preparation
Chlorine body moisture content is lower than 8% (w/w), and is substantially free of chlorine.
Detailed description is made to the utility model with specific embodiment above, although on the utility model basis
On, it needs, specific embodiment of the present utility model can be made some modifications or improvements, but to this field for engineering construction
It is obviously for technical staff, do not make the modification made under the premise of creative work, belongs to the utility model
The range of protection.
Claims (4)
1. a kind of device for producing chlorine dioxide with high purity gas comprising horizontal generator (4), adds crystallizing evaporator (13)
Hot device (12), it is characterised in that: entrance and sulfuric acid pipe (1), the dioxygen water pipe (2) and sodium chlorate pipe of the horizontal generator (4)
(3) connect, reaction solution outlet connection mother liquor letdown tank (9) of horizontal generator (4);The crystallizing evaporator (13) and heater
(12) it is connected between by circulation pipe (23) under mother liquor upper circular tube (24) and mother liquor and forms evaporative crystallization circulation loop, this is followed
Loop back path is connected with mother liquor letdown tank (9), supplies reaction mother liquor, circulation pipe (23) under the mother liquor by mother liquor letdown tank (9)
Filtrate cycle circuit is connect and formed with filter device (15) by the road, it will be under crystallizing evaporator (13) by filter device (15)
The saltcake that circulation pipe (23) generates under portion and mother liquor is filtered, and the sludge outlet of filter device (15) connects drier (16);
The top of the crystallizing evaporator (13) connects with the entrance of horizontal generator (4) by the road, is equipped with mother liquor tank on the pipeline
(18).
2. producing the device of chlorine dioxide with high purity gas according to claim 1, it is characterised in that: the dioxygen water pipe
(2) horizontal generator (4) are accessed after converging with sodium chlorate pipe (3).
3. producing the device of chlorine dioxide with high purity gas according to claim 1, it is characterised in that: the horizontal generator
(4) heat source tube (5), air compressor machine (30), air blower (7) and air-introduced machine (8) are connected.
4. producing the device of chlorine dioxide with high purity gas according to claim 1, it is characterised in that: the crystallizing evaporator
(13) with the connecting line of horizontal generator (4) on, in filter device charging pump turnover pipeline (28), evaporative crystallization circulation loop
Upper and mother liquor letdown tank (9) outlet is mounted on pump.
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CN201820747282.5U CN208454495U (en) | 2018-05-18 | 2018-05-18 | A kind of device producing chlorine dioxide with high purity gas |
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CN201820747282.5U CN208454495U (en) | 2018-05-18 | 2018-05-18 | A kind of device producing chlorine dioxide with high purity gas |
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CN201820747282.5U Expired - Fee Related CN208454495U (en) | 2018-05-18 | 2018-05-18 | A kind of device producing chlorine dioxide with high purity gas |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110015638A (en) * | 2019-04-25 | 2019-07-16 | 兰州泰邦化工科技有限公司 | A kind of equipment and its production method based on chloric acid and Hydrogen Peroxide Production sodium chlorite |
CN110040689A (en) * | 2019-04-25 | 2019-07-23 | 兰州泰邦化工科技有限公司 | A kind of big production capacity and sodium chlorite production equipment and its production method without spent acid discharge |
CN115385304A (en) * | 2022-04-12 | 2022-11-25 | 四川齐力绿源水处理科技有限公司 | Preparation method and preservation method of high-purity chlorine dioxide solution |
-
2018
- 2018-05-18 CN CN201820747282.5U patent/CN208454495U/en not_active Expired - Fee Related
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110015638A (en) * | 2019-04-25 | 2019-07-16 | 兰州泰邦化工科技有限公司 | A kind of equipment and its production method based on chloric acid and Hydrogen Peroxide Production sodium chlorite |
CN110040689A (en) * | 2019-04-25 | 2019-07-23 | 兰州泰邦化工科技有限公司 | A kind of big production capacity and sodium chlorite production equipment and its production method without spent acid discharge |
CN115385304A (en) * | 2022-04-12 | 2022-11-25 | 四川齐力绿源水处理科技有限公司 | Preparation method and preservation method of high-purity chlorine dioxide solution |
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Granted publication date: 20190201 Termination date: 20210518 |