CN107161967A - It is a kind of to add the method and device that raffinate clear liquid produces high-class product diammonium phosphate product - Google Patents
It is a kind of to add the method and device that raffinate clear liquid produces high-class product diammonium phosphate product Download PDFInfo
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- CN107161967A CN107161967A CN201710516420.9A CN201710516420A CN107161967A CN 107161967 A CN107161967 A CN 107161967A CN 201710516420 A CN201710516420 A CN 201710516420A CN 107161967 A CN107161967 A CN 107161967A
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- raffinate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/28—Ammonium phosphates
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Abstract
The invention discloses a kind of method and device for the high-class product diammonium phosphate product for adding raffinate clear liquid production high-quality, raffinate stoste is specifically obtained into raffinate clear liquid after Filter Press；Process water is transported into washer again to mix in proportion with concentrated phosphoric acid, a nitration mixture washing lotion is configured, the waste gas from diammonium phosphate device main line dust-laden, ammonia is absorbed；Then nitration mixture washing lotion of raffinate clear liquid and washer is transported to tubular reactor storage tank mixing complex acid and reaches that proportion and degree of neutralization required for the reaction of Diammonium phosphate (DAP) tubular reactor obtain secondary nitration mixture；Granulation machine tool layer granulation is sprayed into rapidly with liquefied ammonia reaction generation slurry through the suitable secondary nitration mixture feeding tubular reactor of proportioning.The present invention counts addition raffinate clear liquid mass ratio 20%, is compared relative to the low ammonium of nutrient one is produced with raffinate, improves added value and guards based on 300 yuan/ton, yuan/year of annual increase income about 28,800,000.
Description
Technical field
The present invention relates to reclamation of phosphorus resource utilization, particularly as being by by the raffinate of wet phosphoric acid refining byproduct in process
Clear liquid is proportionally produced added to the anti-groove acid preparing system of diammonium phosphate device pipe as obtained by carrying out after separation of solid and liquid filter press
High-quality high-class product diammonium phosphate product.
Background technology
In wet phosphoric acid refining production process, a large amount of raffinates can be produced, raffinate solid content is high, sesquichloride
Height, general processing method is to be used to the by-product raffinate produce low side general calcium product or low nutrient specification monoammonium phosphate product,
And system jams can be caused, production run efficiency is had a strong impact on, the effective value of phosphor resource also fails to obtain high added value income,
Add production run cost.
In addition, when producing low side general calcium product or low nutrient specification monoammonium phosphate product using raffinate production, raffinate
It is sour dense too high, the dense rear progress subsequent production of acid need to be reduced, and if just may be used such as by the part raffinate for producing two ammonium products
Concentrated phosphoric acid consumption is saved on year-on-year basis, and the steam that a large amount of Phosphoric Acid Concentrations need can be saved every year, the purpose of energy-saving and emission-reduction is played.
Features of DAP production device routine complex acid technique is all that phosphoric acid is fed directly into washing system to complete complex acid, if will
Raffinate is directly added complex acid according to conventional production process, is influenceed by sesquichloride in raffinate, particularly MgO,
Al2O3Content height easily causes washing system and feed-line fouling, causes production system can not continuous and steady operation, the present invention
Raffinate clear liquid is directly added into inlet pipe anti-groove in proportion, without by raffinate added to washing acid preparing system, it is to avoid raffinate
Acid adds washing system and causes to be forced cleaned system after fouling, it is only necessary to which periodic cyclic cleaning pipe regurgitates slurry feed-line.
Sesquichloride content is one times of raffinate clear liquid in raffinate solid content, is directly used in production Diammonium phosphate (DAP) production
Product, if raffinate solid content is not filtered out, not only cause difficulty of transportation, and can not meet quality index requirement, it is impossible to produce
The high-class product Diammonium phosphate (DAP) of the specification high-quality of total nutrient >=64.0%.
The present invention had proportionally been added to the anti-groove complex acid of diammonium phosphate device pipe both using gained raffinate clear liquid after press filtration
The problem of conventional complex acid technique washing system fouling is avoided, high-quality high-class product diammonium phosphate product can be efficiently produced again,
Concentrated phosphoric acid consumption is reduced, reduced vapor is saved, while realizing that the high added value of phosphor resource is recycled.
The content of the invention
The present invention is intended to provide a kind of add the method that raffinate produces diammonium phosphate product, to realize the recovery of raffinate
Recycle, on the premise of ensuring that production normal table is continuously run, produce high-quality high-class product diammonium phosphate product, improve
The added value that raffinate is recycled.
The present invention is mainly by nitration mixture washing lotion after two ammonium device dust-ladens, the waste gas washing absorption of ammonia and the raffinate after press filtration
Clear liquid proportioning reaches the proportion and degree of neutralization required for the anti-technique granulation of Diammonium phosphate (DAP) pipe, is re-fed into tubular reactor anti-with liquefied ammonia
Rapid spray into reaction slurry after slurry should be generated and granulate machine tool layer granulation.
Comprise steps that：
1st, raffinate stoste is obtained into raffinate clear liquid after Filter Press；2nd, process water is transported to washer and dense phosphorus
Acid configures a nitration mixture washing lotion after mixing in proportion, absorb the waste gas from diammonium phosphate device main line dust-laden, ammonia；3rd, will extraction
Nitration mixture washing lotion of spent acid clear liquid and washer is transported to tubular reactor storage tank mixing complex acid and reaches Diammonium phosphate (DAP) pipe reaction
Proportion and degree of neutralization required for device reaction obtain secondary nitration mixture；4th, tubular reactor will be sent into through the suitable secondary nitration mixture of proportioning
Granulation machine tool layer granulation is sprayed into rapidly with liquefied ammonia reaction generation slurry.
In the step of the above method the 1st, the nitration mixture washing lotion 1.20-1.40g/ml, degree of neutralization≤0.4mol/mol.
In the step of the above method the 1st, the raffinate clear liquid P2O5Mass percent is 44--48%, and proportion is 1.58-
1.67g/ml, solid content is≤0.5%, and MgO mass percents are 3.0--4.5%, Al in sesquichloride2O3Mass percent
For 3.0--4.5%.
In the step of the above method the 2nd, the concentrated phosphoric acid P2O5Mass percent is 46--49%, and proportion is 1.6-1.65g/ml,
Solid content is≤0.8%, and MgO mass percents are 1.3--1.8%, Al in sesquichloride2O3Mass percent is 1.4--
2.0%。
In the step of the above method the 2nd, described process water feed flow is joined with concentrated phosphoric acid flow using flowmeter with regulating valve
Lock control.
In the step of the above method the 3rd, nitration mixture proportion is 1.5-1.6g/ml, degree of neutralization≤0.7mol/mol in the anti-groove of pipe.
In the step of the above method the 3rd, the raffinate clear liquid and secondary nitration mixture washing lotion proportioning all use flowmeter and regulating valve
Interlocked control.
In the step of the above method the 4th, nitration mixture feeding tubular reactor and liquefied ammonia reaction generation slurry using flowmeter with
Regulating valve and the anti-pump frequency interlocked control of pipe.
The above method, required phosphoric acid P2O5Raffinate clear liquid adds accounting≤35% in mass percent, for process units
Quality and production capacity optimal balance point, preferred scheme complex acid process P2O5Raffinate clear liquid addition accounting is 15- in mass percent
25%。
In the procedure of above-mentioned production Diammonium phosphate (DAP), it is excellent that the present invention provides a kind of addition raffinate clear liquid production
Deng the device of product diammonium phosphate product, raffinate stock solution pipe connects with raffinate clear liquid storage tank again after being connected with filter press
Connect；Raffinate clear liquid storage tank is connected through pipeline with managing anti-groove；
Pipeline from process water is connected with washing tank, and concentrated sulfuric acid pipeline is connected with scrubber column,
Scrubber column bottom is connected with washing tank；
The washing scrubbed device circulating pump of tank is connected with managing anti-groove；
Anti- groove is managed to be connected with tubular reactor through the anti-pump of pipe；
Tubular reactor is connected with comminutor.
The washing scrubbed device circulating pump of tank is connected with Venturi scrubber, and Venturi scrubber bottom is directly with washing
Wash the connection of device tower.
Tubular reactor is connected with managing anti-groove；Sulfuric acid is connected through pipeline with managing anti-groove.
Washing tank, raffinate clear liquid storage tank, manage in anti-groove and be provided with agitator.
The present invention also provides a kind of device for adding raffinate clear liquid production high-class product diammonium phosphate product, raffinate
Stock solution pipe is connected with raffinate clear liquid storage tank again after being connected with filter press；Raffinate clear liquid storage tank is through pipeline and washer
Tower is connected；
Pipeline and sulfuric acid pipeline from process water are connected with washing tank respectively, concentrated sulfuric acid pipeline and scrubber column
Connection, from main line dust-laden, the pipeline of ammonia waste gas with being connected at the top of scrubber column, scrubber column bottom connects with washing tank
Connect；
The washing scrubbed device circulating pump of tank is connected with managing anti-groove；
Anti- groove is managed to be connected with tubular reactor through the anti-pump of pipe；
Tubular reactor is connected with comminutor.
The washing scrubbed device circulating pump of tank is connected with Venturi scrubber top, and Venturi scrubber bottom is directly with washing
Wash the connection of device tower.
Tubular reactor is connected with managing anti-groove；Sulfuric acid is connected through pipeline with managing anti-groove, and liquefied ammonia pipeline connects with tubular reactor
Connect.
Washing tank, raffinate clear liquid storage tank, manage in anti-groove and be provided with agitator.
The beneficial effects of the invention are as follows：1st, by reclaiming the discarded raffinate produced in wet phosphoric acid refining device production process
Acid production diammonium phosphate product, improves the recovery utilization rate of phosphor resource, improves the added value of raffinate recycling, guard
Based on addition raffinate clear liquid ratio 20%, it is compared relative to the low ammonium of nutrient one is produced with raffinate, improves added value and guard
Based on 300 yuan/ton, yuan/year of annual increase income about 28,800,000；2nd, concentrated phosphoric acid consumption is reduced, steam needed for saving Phosphoric Acid Concentration reaches
The purpose of energy-saving and emission-reduction, is guarded based on addition raffinate clear liquid ratio 20%, year reduces 46560 tons of concentrated phosphoric acid consumption, steam saving
856.7 ten thousand yuan/year；3rd, the discarded raffinate for solving to produce in wet phosphoric acid refining production process reprocesses the problem of difficulty is big.
Brief description of the drawings
During Fig. 1 is the schematic flow sheet of the present invention of embodiment 1,3, figure, 1 filter press；2 raffinate clear liquid storage tanks；3 raffinates
Sour clear liquid storage tank stirring；4 raffinate clear liquid pumps；5 scrubber columns；6 Venturi scrubbers；7 washing tanks；8 washers are stirred；9
Washer circulating pump；The 10 anti-grooves of pipe；The anti-groove stirring of 11 pipes；The 12 anti-pumps of pipe；13 tubular reactors；14 comminutors；15 plug valves 1；
16 plug valves 2.
During Fig. 2 is the schematic flow sheet of the present invention of embodiment 2, figure, 1 filter press；2 raffinate clear liquid storage tanks；3 raffinates
Clear liquid storage tank is stirred；4 raffinate clear liquid pumps；5 scrubber columns；6 Venturi scrubbers；7 washing tanks；8 washers are stirred；9 wash
Wash device circulating pump；The 10 anti-grooves of pipe；The anti-groove stirring of 11 pipes；The 12 anti-pumps of pipe；13 tubular reactors；14 comminutors；15 plug valves 1；16
Plug valve 2.
Embodiment
Embodiment 1
As in Fig. 1, with reference to accompanying drawing, the present invention will be further described：
High-class product diammonium phosphate product is produced by adding raffinate clear liquid in proportion using the present invention, concrete scheme is as follows：
Comprise steps that：
By raffinate stoste, gained raffinate clear liquid is delivered to raffinate clear liquid groove 2 after filter press 1 is filtered.
Process water is delivered to washing tank 7, concentrated phosphoric acid is added to scrubbing tower 5 with process water interlocking, stirred in washer
Mix after concentrated phosphoric acid and process water progress mixing match under 8 effects, Venturi scrubber 6 be delivered to by washer circulating pump 9,
Absorb the waste gas from two ammonium device main line dust-ladens, ammonia and configure a nitration mixture washing lotion；
Nitration mixture washing lotion of washing tank 7 is delivered to the anti-groove 10 of pipe by washer circulating pump 9, from raffinate
The raffinate clear liquid of sour clear liquid groove 2 is conveyed by raffinate clear liquid pump 4, with a nitration mixture washing lotion from washing tank 7
Interlocking is added to anti-groove 10 is managed, and progress is sufficiently mixed proportioning and obtains secondary nitration mixture in the presence of the anti-groove stirring 11 of pipe；
The secondary nitration mixture matched in the anti-groove 10 of pipe is sent into tubular reactor 13 by the anti-pump 12 of pipe；By liquefied ammonia
Flow is interlocked with managing the anti-frequency of pump 12 and nitration mixture flow, and it is fast that liquefied ammonia is delivered into tubular reactor 13 according to required degree of neutralization
Speed sprays into the bed of comminutor 14 with nitration mixture reaction generation slurry and granulated.
In the step of the above method the 1st, the raffinate clear liquid P2O5Mass percent is 46%, and proportion is 1.62g/ml, containing solid
Measure as 0.2%, MgO mass percents are 3.8%, Al in sesquichloride2O3Mass percent is 3.3% content.
In the step of the above method the 2nd, the concentrated phosphoric acid P2O5Mass percent is 48%, and proportion is 1.63g/ml, and solid content is
0.4%, MgO mass percents are 1.5%, Al in sesquichloride2O3Mass percent is 1.6%.
In the step of the above method the 2nd, a nitration mixture washing lotion 1.30g/ml, degree of neutralization 0.32mol/mol.
In the above method the 3rd, 4 steps, secondary nitration mixture proportion is 1.52g/ml, degree of neutralization 0.33mol/ in the anti-groove of pipe
mol。
The above method, for process units quality and production capacity optimal balance point, preferred scheme complex acid process P2O5Quality percentage
Raffinate clear liquid addition accounting is 18% in number.
The above method, preferred scheme need to be opened in or so 25 working days of plant running periodically parking, cut-out tap valve 15
Plug valve 16, configuration dilution heat of sulfuric acid is conveyed by the anti-anti- groove of wash cycles pipe of pump 12 of pipe to tubular reactor in the anti-groove 10 of pipe
Pipeline, the dilution heat of sulfuric acid content is 3.8%, and the wash cycles time is 1--2 hours.
For above-mentioned technique, the present invention also provides the device that addition raffinate clear liquid produces high-class product diammonium phosphate product,
Raffinate stock solution pipe is connected with raffinate clear liquid storage tank 2 again after being connected with filter press 1；Raffinate clear liquid storage tank 2 through pipeline with
Anti- groove 10 is managed to connect；
Pipeline from process water is connected with washing tank 7, and concentrated sulfuric acid pipeline is connected with scrubber column 5, the bottom of scrubber column 5 and
Washing tank 7 is connected；
The washing scrubbed device circulating pump 9 of tank 7 is connected with managing anti-groove 10；
Anti- groove 10 is managed to be connected with tubular reactor 13 through the anti-pump 12 of pipe；
Tubular reactor 13 is connected with comminutor 14.
The scrubbed device circulating pump 9 of described washing tank 7 is connected with Venturi scrubber 6, and the bottom of Venturi scrubber 6 is straight
Connect and be connected with scrubber column 5.
Described tubular reactor 13 is connected with managing anti-groove 10；Sulfuric acid is connected through pipeline with managing anti-groove 10.Described washing
Tank 7, raffinate clear liquid storage tank 2, manage in anti-groove 10 and be provided with agitator.
Embodiment 2
As in Fig. 2, with reference to accompanying drawing 2, the present invention will be further described：
High-class product diammonium phosphate product is produced by adding raffinate clear liquid in proportion using the present invention, concrete scheme is as follows：
Comprise steps that：
By raffinate stoste, gained raffinate clear liquid is delivered to raffinate clear liquid groove 2 after filter press 1 is filtered.
Raffinate clear liquid from raffinate clear liquid groove 2 is added to scrubbing tower 5 by the way that raffinate clear liquid pump 4 is defeated.By technique
Water is delivered to washing tank 7, and raffinate clear liquid, concentrated phosphoric acid and process water interlocking are added to scrubbing tower 5,8 stirred in washer
Concentrated phosphoric acid, raffinate clear liquid and process water are carried out after mixing match under effect, venturi is delivered to by washer circulating pump 9
Washer 6, absorbs the waste gas from two ammonium device main line dust-ladens, ammonia and configures a nitration mixture washing lotion；
Nitration mixture washing lotion of washing tank 7 is delivered to the anti-groove 10 of pipe by washer circulating pump 9, by sulfuric acid with coming from washer
The nitration mixture washing lotion interlocking of groove 7 be sufficiently mixed matching added to anti-groove 10 is managed in the presence of the anti-groove stirring 11 of pipe
To secondary nitration mixture；
The secondary nitration mixture matched in the anti-groove 10 of pipe is sent into tubular reactor 13 by the anti-pump 12 of pipe；By liquefied ammonia
Flow is interlocked with managing the anti-frequency of pump 12 and nitration mixture flow, and it is fast that liquefied ammonia is delivered into tubular reactor 13 according to required degree of neutralization
Speed sprays into the bed of comminutor 14 with nitration mixture reaction generation slurry and granulated.
In the step of the above method the 1st, the raffinate clear liquid P2O5Mass percent is 46%, and proportion is 1.62g/ml, containing solid
Measure as 0.2%, MgO mass percents are 3.8%, Al in sesquichloride2O3Mass percent is 3.3% content.
In the step of the above method the 2nd, the concentrated phosphoric acid P2O5Mass percent is 48%, and proportion is 1.63g/ml, and solid content is
0.4%, MgO mass percents are 1.5%, Al in sesquichloride2O3Mass percent is 1.6%.
In the step of the above method the 2nd, a nitration mixture washing lotion proportion 1.50--1.53g/ml, degree of neutralization 0.4--0.6mol/
mol。
In the above method the 3rd, 4 steps, secondary nitration mixture proportion is 1.51--1.55g/ml, degree of neutralization in the anti-groove of pipe
0.4--0.6mol/mol。
The above method, for process units quality and production capacity and process units operational efficiency optimal balance point, preferred scheme
Complex acid process P2O5Raffinate clear liquid addition accounting is 10% in mass percent.
The above method, the concentrated sulfuric acid of the addition anti-groove 10 of inlet pipe is micro addition regulation product nutrient, the concentrated sulfuric acid addition
Measure as 0.3--1.2m3/h
The above method, preferred scheme need to be in or so 15 working days of plant running periodically parking, emptying washing tank 7, in washing
Tank configures dilution heat of sulfuric acid and passes through the wash cycles Venturi scrubber 6 of scrubber pump 9 and washing pipeline；The dilution heat of sulfuric acid
Content is 3.8%, and the wash cycles time is 1--2 hours.
The above method, preferred scheme need to be opened in or so 15 working days of plant running periodically parking, cut-out tap valve 15
Plug valve 16, configuration dilution heat of sulfuric acid is conveyed by the anti-anti- groove of wash cycles pipe of pump 12 of pipe to tubular reactor in the anti-groove 10 of pipe
Pipeline, the dilution heat of sulfuric acid content is 3.8%, and the wash cycles time is 1--2 hours.
For above-mentioned technique, the present invention provides a kind of raffinate clear liquid that adds and produces high-class product diammonium phosphate product
Device, raffinate stock solution pipe is connected with raffinate clear liquid storage tank again after being connected with filter press；Raffinate clear liquid storage tank is passed through
Pipeline is connected with scrubber column；
Pipeline and sulfuric acid pipeline from process water are connected with washing tank respectively, concentrated sulfuric acid pipeline and scrubber column
Connection, from main line dust-laden, the pipeline of ammonia waste gas with being connected at the top of scrubber column, scrubber column bottom connects with washing tank
Connect；
The washing scrubbed device circulating pump of tank is connected with managing anti-groove；
Anti- groove is managed to be connected with tubular reactor through the anti-pump of pipe；
Tubular reactor is connected with comminutor.
The washing scrubbed device circulating pump of tank is connected with Venturi scrubber top, and Venturi scrubber bottom is directly with washing
Wash the connection of device tower.
Tubular reactor is connected with managing anti-groove；Sulfuric acid is connected through pipeline with managing anti-groove, and liquefied ammonia pipeline connects with tubular reactor
Connect.
Washing tank, raffinate clear liquid storage tank, manage in anti-groove and be provided with agitator.
Above-mentioned process embodiment（One）With（Two）Comparison, in the case of same phosphoric acid quality index, embodiment
（Two）Raffinate clear liquid is added to washer 5, the dirt from main line is absorbed, wash cycle scaling can be caused after ammonia gas
Block, be balanced production operational efficiency and raffinate clear liquid usage amount, embodiment（Two）Preferred scheme complex acid process P2O5Quality
Raffinate clear liquid addition accounting is set to 10% in percentage, it can be ensured that device continuous and steady operation is on or so 15 working days, simultaneously
Product total nutrient meeting ＞ more than 64.5%, need to add Determination of Trace Sulfur when being produced according to above phosphoric acid quality and raffinate addition tissue
Acid reduction product nutrient is so as to prevent the higher cost of idleness increase producing cost of product nutrient.
Embodiments of the present invention（Two）Beneficial effect can reach embodiment（One）The 1/2 of income, is embodied in：1st, pass through
The discarded raffinate production diammonium phosphate product produced in wet phosphoric acid refining device production process is reclaimed, phosphor resource is improved
Recovery utilization rate, improves the added value of raffinate recycling, based on addition raffinate clear liquid ratio 10%, relative to extraction
Spent acid produces the low ammonium of nutrient one and is compared, and improves added value and guards based on 300 yuan/ton, yuan/year of annual increase income about 14,400,000；2、
Concentrated phosphoric acid consumption is reduced, steam needed for saving Phosphoric Acid Concentration has reached the purpose of energy-saving and emission-reduction, guarded by addition raffinate clear liquid
Ratio 10% is counted, and year reduces 23280 tons of concentrated phosphoric acid consumption, yuan/year of steam saving 428.4 ten thousand；3rd, wet phosphoric acid refining production is solved
During produce discarded raffinate reprocessing difficulty it is big the problem of.
Embodiment 3
The present invention will be further described by Fig. 1：
High-class product diammonium phosphate product is produced by adding raffinate clear liquid in proportion using the present invention, concrete scheme is as follows：
Comprise steps that：
By raffinate stoste, gained raffinate clear liquid is delivered to raffinate clear liquid groove 2 after filter press 1 is filtered.
Process water is delivered to washing tank 7, concentrated phosphoric acid is added to scrubbing tower 5 with process water interlocking, stirred in washer
Mix after concentrated phosphoric acid and process water progress mixing match under 8 effects, Venturi scrubber 6 be delivered to by washer circulating pump 9,
Absorb the waste gas from two ammonium device main line dust-ladens, ammonia and configure a nitration mixture washing lotion；
Nitration mixture washing lotion of washing tank 7 is delivered to the anti-groove 10 of pipe by washer circulating pump 9, from raffinate
The raffinate clear liquid of sour clear liquid groove 2 is conveyed by raffinate clear liquid pump 4, with a nitration mixture washing lotion from washing tank 7
Interlocking is added to anti-groove 10 is managed, and progress is sufficiently mixed proportioning and obtains secondary nitration mixture in the presence of the anti-groove stirring 11 of pipe；
The secondary nitration mixture matched in the anti-groove 10 of pipe is sent into tubular reactor 13 by the anti-pump 12 of pipe；By liquefied ammonia
Flow is interlocked with managing the anti-frequency of pump 12 and nitration mixture flow, and it is fast that liquefied ammonia is delivered into tubular reactor 13 according to required degree of neutralization
Speed sprays into the bed of comminutor 14 with nitration mixture reaction generation slurry and granulated.
In the step of the above method the 1st, the raffinate clear liquid P2O5Mass percent is 46%, and proportion is 1.62g/ml, containing solid
Measure as 0.2%, MgO mass percents are 3.8%, Al in sesquichloride2O3Mass percent is 3.3% content.
In the step of the above method the 2nd, the concentrated phosphoric acid P2O5Mass percent is 48%, and proportion is 1.63g/ml, and solid content is
0.4%, MgO mass percents are 1.5%, Al in sesquichloride2O3Mass percent is 1.6%.
In the step of the above method the 2nd, a nitration mixture washing lotion 1.30g/ml, degree of neutralization 0.32mol/mol.
In the above method the 3rd, 4 steps, secondary nitration mixture proportion is 1.54g/ml, degree of neutralization 0.5mol/ in the anti-groove of pipe
mol。
The above method, for process units quality and production capacity optimal balance point, ensures in product in nutritional quality preferentially
In the case of, do not consider that product appearance is felt thoroughly, complex acid process P2O5Raffinate clear liquid addition accounting is that can reach in mass percent
50%。
The above method, preferred scheme need to be opened in or so 20 working days of plant running periodically parking, cut-out tap valve 15
Plug valve 16, configuration dilution heat of sulfuric acid is conveyed by the anti-anti- groove of wash cycles pipe of pump 12 of pipe to tubular reactor in the anti-groove 10 of pipe
Pipeline, the dilution heat of sulfuric acid content is 3.8%, and the wash cycles time is 1--2 hours.
Claims (10)
1. a kind of add the method that raffinate clear liquid produces high-class product diammonium phosphate product, it is characterised in that comprises the following steps：
（1）Raffinate stoste is obtained into raffinate clear liquid after Filter Press；
（2）Process water is transported into washer to mix in proportion with concentrated phosphoric acid, a nitration mixture washing lotion is configured, absorbs and comes from phosphoric acid
Two ammonium device main line dust-ladens, the waste gas of ammonia；
（3）Nitration mixture washing lotion of raffinate clear liquid and washer is transported to tubular reactor storage tank mixing complex acid and reaches di(2-ethylhexyl)phosphate
Proportion and degree of neutralization required for the reaction of ammonium tubular reactor obtain secondary nitration mixture；
（4）Tubular reactor will be sent into through the suitable secondary nitration mixture of proportioning and liquefied ammonia reaction generation slurry sprays into rapidly granulation lathe
Layer granulation.
2. the method that the addition raffinate clear liquid according to claim 1 produces high-class product diammonium phosphate product, its feature
It is, described step（1）In, raffinate clear liquid P2O5Mass percent is 44-48%, and proportion is 1.58-1.67g/ml, containing solid
Measure as≤0.5%, MgO mass percents are 3.0-4.5%, Al in sesquichloride2O3Mass percent is 3.0-4.5% contents.
3. the method that the addition raffinate clear liquid according to claim 1 produces high-class product diammonium phosphate product, its feature
It is, described step（2）In, the concentrated phosphoric acid P2O5Mass percent is 46-49%, and proportion is 1.6-1.65g/ml, containing solid
Measure as≤0.8%, MgO mass percents are 1.3-1.8%, Al in sesquichloride2O3Mass percent is 1.4-2.0% contents.
4. the method that the addition raffinate clear liquid according to claim 1 produces high-class product diammonium phosphate product, its feature
It is, the step（2）In, the mass concentration of a nitration mixture washing lotion is 1.20-1.40g/ml, degree of neutralization≤0.4mol/mol.
5. the method that addition raffinate clear liquid according to claim 1 produces high-class product diammonium phosphate product, its feature exists
In step（3）、（4）In, nitration mixture proportion is 1.5-1.6g/ml, degree of neutralization≤0.7mol/mol in the anti-groove of pipe.
6. the method that addition raffinate clear liquid according to claim 1 produces high-class product diammonium phosphate product, its feature exists
In required phosphoric acid P2O5Raffinate clear liquid adds accounting≤35%, preferred scheme complex acid process P in mass percent2O5Quality hundred
Raffinate clear liquid addition accounting is 15-25% in fraction.
7. a kind of add the device that raffinate clear liquid produces high-class product diammonium phosphate product, it is characterised in that
Raffinate stock solution pipe and filter press（1）After connection again with raffinate clear liquid storage tank（2）Connection；Raffinate clear liquid storage tank
（2）Through pipeline with managing anti-groove（10）Connection；
Pipeline and washing tank from process water（7）Connection, concentrated sulfuric acid pipeline and scrubber column（5）Connection, scrubber column（5）
Bottom and washing tank（7）Connection；
Wash tank（7）Scrubbed device circulating pump（9）With the anti-groove of pipe（10）Connection；
Manage anti-groove（10）Through the anti-pump of pipe（12）With tubular reactor（13）Connection；
Tubular reactor（13）With comminutor（14）Connection.
8. the addition raffinate clear liquid described in claim 7 produces the device of high-class product diammonium phosphate product, it is characterised in that wash
Wash tank（7）Scrubbed device circulating pump（9）With Venturi scrubber（6）Connection, Venturi scrubber（6）Bottom directly with washing
Device tower（5）Connection.
9. the addition raffinate clear liquid described in claim 7 produces the device of high-class product diammonium phosphate product, it is characterised in that pipe
Formula reactor（13）With the anti-groove of pipe（10）Connection；Sulfuric acid is through pipeline with managing anti-groove（10）Connection.
10. the addition raffinate clear liquid described in claim 7 produces the device of high-class product diammonium phosphate product, it is characterised in that
Wash tank（7）, raffinate clear liquid storage tank（2）, manage anti-groove（10）Inside it is provided with agitator.
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