CN109877097A - The cleaning method of wet phosphoric acid purifying technique concentration systems - Google Patents
The cleaning method of wet phosphoric acid purifying technique concentration systems Download PDFInfo
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- CN109877097A CN109877097A CN201910248731.0A CN201910248731A CN109877097A CN 109877097 A CN109877097 A CN 109877097A CN 201910248731 A CN201910248731 A CN 201910248731A CN 109877097 A CN109877097 A CN 109877097A
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Abstract
The invention discloses a kind of cleaning methods of wet phosphoric acid purifying technique concentration systems, it is the connection cleaning liquid pipe on the circulation pipe of pump inlet, it cleans and cleaning solution delivery pump and valve is set in liquid pipe, it prepares in cleaning solution access cleaning liquid pipe, opening valve starting cleaning solution delivery pump makes cleaning solution enter vaporization chamber, when vaporization chamber cleaning liquid inside reaches default liquid level, close the valve in cleaning liquid pipe, start circulating pump, make cleaning solution after concentration systems internal circulation flow 10-15min, open vent valves, starting emptying pump, which falls cleaning fluid discharge, to be completed to clean；The cleaning solution be containing sulfuric acid, fluosilicic acid, restrainer, sodium molybdate, bleeding agent, sulfamic acid mixed solution.The method of the present invention is simple to operate, saves labour, realizes concentration systems and effectively cleans, has both saved scavenging period, in turn avoids hitting damage of the dirty block to fall off to concentrator in conventional method, has ensured the operation ratio of equipment.
Description
Technical field
The present invention relates to the cleaning methods of wet phosphoric acid purifying technique concentration systems, belong to technical field of fine.
Background technique
Phosphoric acid is the core of phosphorous chemical industry ranks.In China, obtains yellow phosphorus and produce thermal phosphoric acid to be electrolysed phosphorus ore and form phosphorus
Hydrochlorate industry produces phosphoric acid by wet process with sulfuric acid decomposition phosphorus ore and then forms phosphate fertilizer industry.Low energy consumption compared with thermal phosphoric acid for phosphoric acid by wet process,
Pollute it is small, have the significant energy, environment and cost advantage.But phosphoric acid by wet process is impure more, purification techniques is more demanding,
Therefore domestic phosphoric acid by wet process is mainly also served only for the lower phosphatic compound fertilizer of added value at present.In recent years, due to the energy and electric power
In short supply, environmental requirement improves, and production and the development of electrothermal way phosphoric acid are severely limited.Purification of wet process phosphoric acid replaces thermal method
The superiority of phosphoric acid is increasingly significant, and technological development is studied to obtain most attention.Purification of wet process phosphoric acid replaces thermal phosphoric acid to be modern
The developing direction of phosphorous chemical industry.
In large-scale phosphoric acid by wet process and phosphatic compound fertilizer enterprise, industrial for purification of raw materials purification production using phosphoric acid by wet process,
Food grade phosphoric acid and its phosphate rationally classified utilization phosphoric acid by wet process, raising added value of product can replace thermal phosphoric acid, keep away
Exempt from energy waste and reduce environmental pollution, increases Business Economic Benefit.Raffinate after wet phosphoric acid refining can also be used to produce
Chemical fertilizer, phosphor resource are not lost, and do not reduce its fertile value.Fertile salt is implemented in combination with the best comprehensive utilization of resource, meets
Circular economy and Scientific Outlook on Development requirement.
Satisfactory phosphorus concentrate is reacted in reactive tank with sulfuric acid, obtains wet process using being filtered, washed, being concentrated
Raw phosphoric acid, in the preparation process of wet process raw phosphoric acid, most calcium, fluorine foreign ion are arranged by filtering or for its absorption
It removes, but also contains a small amount of sulphur, iron, arsenic impurities in acid, in order to guarantee that product quality is up to state standards requirements, also need further
Phosphoric acid by wet process is produced by purification process.Existing common wet phosphoric acid purifying method, predominantly solvent extraction, it be by
Wet process raw phosphoric acid passes sequentially through pretreatment process, extraction process, postprocessing working procedures and carries out three-level purification process.In postprocessing working procedures
In need to use concentration systems to phosphoric acid,diluted carry out concentrate processing, working principle is as shown in Figure 1, work of the phosphoric acid,diluted through thin acid pump
It is delivered in the vaporization chamber 1 of concentration systems with by acid inlet tube 5, when phosphoric acid,diluted, which is supplemented to, evaporates indoor default liquid level, is opened
Dynamic circulating pump 3, vacuumizes phosphoric acid,diluted, in recurrent state, then to vaporization chamber 1 again in whole system, will be in vaporization chamber 1
Pressure is evacuated to 10-12KPa, and phosphoric acid,diluted is after tubular heat exchanger 2 and high-temperature steam carry out heat conversion, and temperature increases, moisture steams
Hair, to achieve the purpose that promote concentration.Due to containing the media such as calcium, magnesium, sylvite in the phosphoric acid,diluted of concentration systems processing, with
The extension of circulation time, system is interior can reduce heat exchange efficiency after fouling, especially heat exchanger tube encrustation, influence system
Load, it is therefore desirable to dirty removing processing periodically be carried out to it.Existing descaling method is physics cleaning, is exactly made using giant
Water forms jet stream state to hit dirty block, and dirty block is made to fall off from tubulation inner wall, the method security risk is big, at high cost, time-consuming,
It is complicated for operation.
Summary of the invention
In view of this, in view of the deficiencies of the prior art, the present invention provides a kind of wet phosphoric acid purifying technique concentration systems
The cleaning method of system, it is simple to operate, labour is saved, concentration systems is realized and effectively cleans, has both saved cleaning
Time in turn avoids hitting damage of the dirty block to fall off to concentrator in conventional method, has ensured the operation ratio of equipment.
In order to solve the above technical problems, the technical scheme is that a kind of wet phosphoric acid purifying technique concentration systems
Cleaning method, it be on the circulation pipe of pump inlet connection cleaning liquid pipe, clean liquid pipe on setting cleaning solution delivery pump and
Valve is prepared in cleaning solution access cleaning liquid pipe, and opening valve starting cleaning solution delivery pump makes cleaning solution enter vaporization chamber, works as steaming
When the indoor cleaning solution arrival vaporization chamber cleaning solution of hair presets liquid level, the valve cleaned in liquid pipe is closed, starts circulating pump, makes to clean
Liquid opens vent valves after concentration systems internal circulation flow 10-15min, and starting emptying pump, which falls cleaning fluid discharge, to be completed
Cleaning；Above-mentioned cleaning solution be containing sulfuric acid, fluosilicic acid, restrainer, sodium molybdate, bleeding agent, sulfamic acid mixed solution.
Further, the mass fraction of sulfuric acid is 2~4% in the mixed solution, the mass fraction of fluosilicic acid is 6~
8%, the mass fraction of restrainer is 0.1~0.3%, the mass fraction of sodium molybdate is 0.1~0.3%, the matter of bleeding agent
Amount score is 0.1~0.3%, the mass fraction of sulfamic acid is 0.1~0.3%.
More optimizedly, the mass fraction of sulfuric acid is 3% in the mixed solution, and the mass fraction of fluosilicic acid is 7%, pickling
The mass fraction of corrosion inhibiter is 0.1%, the mass fraction of sodium molybdate is 0.1%, the mass fraction of bleeding agent is 0.1%, amino
The mass fraction of sulfonic acid is 0.1%.
Further, bleeding agent preferred anionic type bleeding agent used in above-mentioned cleaning solution.
More preferably technical solution is that, when vaporization chamber cleaning liquid inside, which reaches vaporization chamber, presets liquid level, tubular heat exchanger is passed through
High-temperature steam, which is started to work, is heated to 80-85 DEG C for cleaning solution, can significantly improve cleaning effect.
Further, it is high to preset liquid level liquid level more default than the vaporization chamber that concentration of dilute phosphoric acid uses for the vaporization chamber cleaning solution
10-15cm guarantees the cleaning effect of cleaning solution.
Further, the gas pressure of the vaporization chamber is 70-80KPa.
Compared with prior art, the beneficial effects of the present invention are: being cleaned by adding cleaning solution to concentration systems, greatly
Labour is saved greatly, reduces production and operation cost, the labor intensity and security risk of operator is reduced, avoids simultaneously
Damage of the dirty block to fall off to concentrator is hit in conventional method；The cleaning solution of use forms, and raw material is easy to get, cleaning effect
Good, sodium molybdate and restrainer inhibit corrosion of metal, and sulfamic acid has the highly acid same with hydrochloric acid, sulfuric acid, right
Iron rust, the cleaning effect of scale are good, small to corrosion of metal, and the use of bleeding agent can reinforce the cleaning effect of sour agent, therefore
Cleaning solution of the present invention both ensure that both the molten of the dirty block on the dirty block that ensure that on concentrator, especially tubular heat exchanger inner wall
Solution is removed, and acid corrosion damage equipment is in turn avoided.And the method for the present invention takes full advantage of original device apparatus and process pipeline, only needs
Add cleaning solution associated conduit, simple process, low equipment investment.
To sum up, the method for the present invention uses cleaning solution wash cycles concentration systems, and scavenging period is greatly saved, reduces work
People's labor intensity improves cleaning and washes efficiency, realizes effective cleaning of concentration systems, and does not lose set in the process of cleaning
It is standby, ensure the operation ratio of equipment.
Detailed description of the invention
Fig. 1 is the flow diagram of wet phosphoric acid purifying technique concentration systems.
Marginal data:
1, vaporization chamber；2, tubular heat exchanger；3, circulating pump；4, emptying pump；5, acid inlet tube；6, circulation pipe；7, delivery pipe；8,
Clean liquid pipe；71, vent valves；81, cleaning solution delivery pump；82, valve.
Specific embodiment
It is with reference to the accompanying drawing and specific real in order to make those skilled in the art more fully understand technical solution of the present invention
Applying mode, the present invention is described in further detail.
Embodiment 1:
A kind of cleaning method of wet phosphoric acid purifying technique concentration systems, comprising the following steps:
The connection cleaning liquid pipe 8 on the circulation pipe 6 of 3 import of circulating pump, cleans in liquid pipe 8 and is provided with cleaning solution delivery pump 81
With valve 82, prepare in cleaning solution access cleaning liquid pipe 8.
Above-mentioned cleaning solution is that the mixing containing sulfuric acid, fluosilicic acid, restrainer, sodium molybdate, bleeding agent, sulfamic acid is molten
Liquid.Wherein the mass fraction of sulfuric acid is 2% in mixed solution, and the mass fraction of fluosilicic acid is 6%, the quality point of restrainer
Number is 0.2%, the mass fraction of sodium molybdate is 0.2%, the mass fraction of bleeding agent is 0.2%, the mass fraction of sulfamic acid
It is 0.2%.
The detailed process of cleaning are as follows: referring to Fig. 1, open valve 82, cleaning solution is conveyed by starting cleaning solution delivery pump 81
In vaporization chamber 1, when 1 cleaning liquid inside of vaporization chamber, which reaches vaporization chamber cleaning solution, presets liquid level, the valve in cleaning liquid pipe 8 is closed
82, it is passed through high-temperature steam in tubular heat exchanger 2 starts to work cleaning solution is heated to 80-85 DEG C, pressure is evacuated in vaporization chamber 1
Power is 70-80KPa, starts circulating pump 3, makes cleaning solution after concentration systems internal circulation flow cleans 15min, opens vent valves
71, starting emptying pump 4, which falls cleaning fluid discharge, to be completed to clean；After cleaning, concentration systems restore initial load.
Embodiment 2:
A kind of cleaning method of wet phosphoric acid purifying technique concentration systems, comprising the following steps:
The connection cleaning liquid pipe 8 on the circulation pipe 6 of 3 import of circulating pump, cleans in liquid pipe 8 and is provided with cleaning solution delivery pump 81
With valve 82, prepare in cleaning solution access cleaning liquid pipe 8.
Above-mentioned cleaning solution is that the mixing containing sulfuric acid, fluosilicic acid, restrainer, sodium molybdate, bleeding agent, sulfamic acid is molten
Liquid.Wherein the mass fraction of sulfuric acid is 3% in mixed solution, and the mass fraction of fluosilicic acid is 7%, the quality point of restrainer
Number is 0.1%, the mass fraction of sodium molybdate is 0.1%, the mass fraction of bleeding agent is 0.1%, the mass fraction of sulfamic acid
It is 0.1%.
The detailed process of cleaning are as follows: referring to Fig. 1, open valve 82, cleaning solution is conveyed by starting cleaning solution delivery pump 81
In vaporization chamber 1, when 1 cleaning liquid inside of vaporization chamber, which reaches vaporization chamber cleaning solution, presets liquid level, the valve in cleaning liquid pipe 8 is closed
82, it is passed through high-temperature steam in tubular heat exchanger 2 starts to work cleaning solution is heated to 80-85 DEG C, pressure is evacuated in vaporization chamber 1
Power is 70-80KPa, starts circulating pump 3, makes cleaning solution after concentration systems internal circulation flow cleans 10min, opens vent valves
71, starting emptying pump 4, which falls cleaning fluid discharge, to be completed to clean；After cleaning, concentration systems restore initial load.
Embodiment 3:
A kind of cleaning method of wet phosphoric acid purifying technique concentration systems, comprising the following steps:
The connection cleaning liquid pipe 8 on the circulation pipe 6 of 3 import of circulating pump, cleans in liquid pipe 8 and is provided with cleaning solution delivery pump 81
With valve 82, prepare in cleaning solution access cleaning liquid pipe 8.
Above-mentioned cleaning solution is that the mixing containing sulfuric acid, fluosilicic acid, restrainer, sodium molybdate, bleeding agent, sulfamic acid is molten
Liquid.Wherein the mass fraction of sulfuric acid is 4% in mixed solution, and the mass fraction of fluosilicic acid is 8%, the quality point of restrainer
Number is 0.3%, the mass fraction of sodium molybdate is 0.3%, the mass fraction of bleeding agent is 0.3%, the mass fraction of sulfamic acid
It is 0.3%.
The detailed process of cleaning are as follows: referring to Fig. 1, open valve 82, cleaning solution is conveyed by starting cleaning solution delivery pump 81
In vaporization chamber 1, when 1 cleaning liquid inside of vaporization chamber, which reaches vaporization chamber cleaning solution, presets liquid level, the valve in cleaning liquid pipe 8 is closed
82, it is passed through high-temperature steam in tubular heat exchanger 2 starts to work cleaning solution is heated to 80-85 DEG C, pressure is evacuated in vaporization chamber 1
Power is 70-80KPa, starts circulating pump 3, makes cleaning solution after concentration systems internal circulation flow cleans 15min, opens vent valves
71, starting emptying pump 4, which falls cleaning fluid discharge, to be completed to clean；After cleaning, concentration systems restore initial load.
It should be pointed out that above embodiment is not construed as limitation of the present invention, protection scope of the present invention should
It is defined by the scope defined by the claims..For those skilled in the art, do not depart from it is of the invention
In spirit and scope, several improvements and modifications can also be made, these modifications and embellishments should also be considered as the scope of protection of the present invention.
Claims (7)
1. the cleaning method of wet phosphoric acid purifying technique concentration systems, it is characterised in that: on the circulation pipe of pump inlet
Connection cleaning liquid pipe, cleans and cleaning solution delivery pump and valve is arranged in liquid pipe, prepares in cleaning solution access cleaning liquid pipe, opens valve
Door starting cleaning solution delivery pump makes cleaning solution enter vaporization chamber, presets liquid level when vaporization chamber cleaning liquid inside reaches vaporization chamber cleaning solution
When, the valve in cleaning liquid pipe is closed, starts circulating pump, makes cleaning solution after concentration systems internal circulation flow 10-15min, beat
Vent valves are opened, starting emptying pump, which falls cleaning fluid discharge, to be completed to clean；
The cleaning solution be containing sulfuric acid, fluosilicic acid, restrainer, sodium molybdate, bleeding agent, sulfamic acid mixed solution.
2. the cleaning method of wet phosphoric acid purifying technique concentration systems according to claim 1, it is characterised in that: work as steaming
When the indoor cleaning solution arrival vaporization chamber of hair presets liquid level, tubular heat exchanger is passed through high-temperature steam start-up operation and is heated to cleaning solution
80-85℃。
3. the cleaning method of wet phosphoric acid purifying technique concentration systems according to claim 1, it is characterised in that: described
It is 10-15cm high that vaporization chamber cleaning solution presets liquid level liquid level more default than the vaporization chamber that concentration of dilute phosphoric acid uses.
4. the cleaning method of wet phosphoric acid purifying technique concentration systems according to claim 1, it is characterised in that: described
The gas pressure of vaporization chamber is 70-80KPa.
5. the cleaning method of wet phosphoric acid purifying technique concentration systems according to claim 1, it is characterised in that: described
The mass fraction of sulfuric acid is 2~4% in mixed solution, and the mass fraction of fluosilicic acid is 6~8%, the quality point of restrainer
Number is 0.1~0.3%, the mass fraction of sodium molybdate is 0.1~0.3%, the mass fraction of bleeding agent is 0.1~0.3%, amino
The mass fraction of sulfonic acid is 0.1~0.3%.
6. the cleaning method of wet phosphoric acid purifying technique concentration systems according to claim 5, it is characterised in that: described
The mass fraction of sulfuric acid is 3% in mixed solution, and the mass fraction of fluosilicic acid is 7%, and the mass fraction of restrainer is
0.1%, the mass fraction of sodium molybdate is 0.1%, the mass fraction of bleeding agent is 0.1%, the mass fraction of sulfamic acid is
0.1%.
7. according to claim 1, wet phosphoric acid purifying technique described in any one of claim 5 or claim 6 is concentrated
The cleaning method of system, it is characterised in that: the bleeding agent is anionic bleeding agent.
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| CN201910248731.0A CN109877097A (en) | 2019-03-29 | 2019-03-29 | The cleaning method of wet phosphoric acid purifying technique concentration systems |
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| CN201910248731.0A CN109877097A (en) | 2019-03-29 | 2019-03-29 | The cleaning method of wet phosphoric acid purifying technique concentration systems |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021168536A1 (en) * | 2020-02-28 | 2021-09-02 | Sixring Inc. | Sulfuric acid composition and uses thereof |
| CN113458064A (en) * | 2021-07-20 | 2021-10-01 | 内蒙古大地云天化工有限公司 | Cleaning method for concentration system of phosphorus chemical production device |
| US11760720B2 (en) | 2020-02-28 | 2023-09-19 | Sixring Inc. | Modified sulfuric acid and uses thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN113458064A (en) * | 2021-07-20 | 2021-10-01 | 内蒙古大地云天化工有限公司 | Cleaning method for concentration system of phosphorus chemical production device |
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