CN106115643B - A kind of technique using boiler slag purification of wet process phosphoric acid production feed-level calcium biphosphate - Google Patents
A kind of technique using boiler slag purification of wet process phosphoric acid production feed-level calcium biphosphate Download PDFInfo
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- CN106115643B CN106115643B CN201610481405.0A CN201610481405A CN106115643B CN 106115643 B CN106115643 B CN 106115643B CN 201610481405 A CN201610481405 A CN 201610481405A CN 106115643 B CN106115643 B CN 106115643B
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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
- C01B25/32—Phosphates of magnesium, calcium, strontium, or barium
Abstract
The invention discloses a kind of technique using boiler slag purification of wet process phosphoric acid production high-efficiency feed level calcium biphosphate, the present invention includes herein below：The waste residue that boiler desulfurization obtains, with the concentrated phosphoric acid hybrid reaction desulfurization obtained after wet-process phosphoric acid concentration after break process, phosphoric acid is handled again through defluorinate after reaction, and filtering phosphoric acid defluorination slurry obtains finished product phosphoric acid；After finished product phosphoric acid and calcium ore pulp hybrid reaction, spray-dried tower carries out granulating and drying, then is dried under reduced pressure to obtain product through revolution.The present invention realizes the recycling to boiler desulfurization waste residue, efficiently utilizes the active CaO and SiO in waste residue2, Solid state fermentation cost is reduced, reduces production defluorinate auxiliary agent consumption, while the feed-level calcium biphosphate product that appearance is mellow and full, particle internal moisture is low, product purity is high, prevented from caking is obtained, product competitiveness in the market is improved, cost efficiency is realized for enterprise.
Description
Technical field
The present invention relates to belong to technical field of phosphorous chemical industry, and in particular to a kind of to be produced using boiler slag purification of wet process phosphoric acid
The technique of feed-level calcium biphosphate.
Background technology
Phosphorus is important biological element, and phosphoric acid salt additive is widely used as food and feed additive.Due to hot method phosphorus
Sour cost is higher, and feed-grade calcium phosphate product salt is nearly all produced using phosphoric acid by wet process as raw material currently on the market, but due to
Wet Processes of Phosphoric Acid limits, and causes impurity in product more, influences product quality.
With the continuous progress of industry, raising the requirement index of calcium product will also be continuously improved, according to the feed of newest revision
Level calcium biphosphate national standard (GB 22548-2008) requirement, total phosphorus >=22%, water-soluble phosphorus >=20%, calcium content >=13%,
The product purity that it is converted, wherein containing substantial amounts of impurity, seriously affects the quality of product only proximate to 90%.According to overseas market
Demand, requirement index total phosphorus of the portions of client to feed-level calcium biphosphate need to reach more than 23.5%, and corresponding product purity reaches
To more than 95%, hence it is evident that higher than domestic index.Therefore, product purity and quality are improved, the higher product of production active ingredient will
It is the important directions of following enterprise development.
Simultaneously because the characteristic that feed-level calcium biphosphate product is hygroscopic, in production, packaging, storage and transportational process
Once ambient humidity is larger, product easily absorbs ambient moisture, and particle surface occurs secondary response recrystallization, causes product easily
Caking, great inconvenience is brought to the use of client；Meanwhile the uneven distribution of particle internal moisture and the office of dry technology
Sex-limited, recrystallization phenomenon occurs for interiors of products water translocation, and the problem of product is caused to lump, there is presently no related public technologies
It can solve.How production technology is optimized, control Product Activity, solving external environment and internal factor causes to produce
The problem of product lump avoids the product before client's use from the emphasis direction that caking is also business research occur.
In wet method phosphoric acid manufacture process, most enterprises be using Production By Sulfuric Acid Process technique, in production process in order to
The coarse crystal of calcium sulfate convenient for filtering is obtained, SO in diluted acid need to be controlled3Content is 2% or so, if not taking appropriate technique
It is removed, part SO3Product quality will be influenced as phosphoric acid is together into product.According to domestic main feed grade phosphorus
The product analysis of acid dihydride calcium (MCP) manufacturing enterprise shows SO in wherein product3Content all control substantially 2.0~4.0% it
Between, it corresponds to calcium sulphate content in product and reaches 3.4~6.8%, seriously affect the utilization ratio of calcium in product quality and product.
Therefore, SO3The regulation and control of content improve active ingredient proportion, have product to improving product competitiveness to improving product quality
The meaning of pole.
The technique of phosphoric acid by wet process desulfurization is mainly removed using the compound containing calcium, reaction production calcium sulfate precipitation
After separated, realize the purification to sulfur trioxide in phosphoric acid.Number of patent application is public in 201410370866.1 Chinese patents
A kind of technique of phosphoric acid by wet process desulfurization is opened, primarily directed to the work of two sections of neutralisation production calcium hydrophosphate fodder products
Skill proposes that the mother liquor after neutralizing is neutralized again using milk of lime, and will precipitate back in phosphoric acid by wet process slurry.Although the technique energy
The phosphor resource lost in enough effectively recycling precipitations, but it is only raised calcium technique with two sections of neutralisation productions and can combine closely, and should
Technique productions cost is higher, and phosphor resource utilization rate is low, is gradually eliminated by industry.
Number of patent application is to disclose a kind of technique of phosphoric acid by wet process desulfurization in 201410818845.1 Chinese patents, is led
If for the sulfur trioxide in phosphoric acid by wet process to the quality of the downstream product such as production monoammonium phosphate, Diammonium phosphate (DAP), purifying phosphoric acid
It influences, proposes to use and contain 31~35%Ca, 20~25%P2O5, 19~26%F fluorine-containing waste residue handled, although to containing
Phosphorus and fluorine in fluorine waste residue are recycled, but for feeding calcium product tighter to fluorine content index request in product, it is fluorine-containing
It can increase fluorine content ratio in phosphoric acid after waste residue recycling, more strict requirements are proposed to the defluorinate of system, be not suitable for promoting and answer
With.
The problem of easily luming for product, also undisclosed related effective patented technology, uses for reference the anti-of relevant industries at present
Agglomeration techniques are usually all to add a certain amount of property-modifying additive in the product, such as 200910307557.9 China of Application No.
Organic modifiers hydrocarbon compound, grease etc. disclosed in patent and powdery material such as calcium silicates, flyash etc., but these are undoubtedly
The content of impurity in product will be increased, negative impact or even the toxic feed that cannot be present in will be caused to add to product quality
Add in agent.
Therefore, the difference of product index is required in order to meet different clients, the feed-level calcium biphosphate production produced
Product have the characteristics that efficiently easily to absorb, while can solve the technical barrier that feed-level calcium biphosphate product easily lumps again and become
The problem of industry focuses more on.
The content of the invention
In view of the above problems, it is an object of the invention to provide a kind of raising product purity and quality to meet more
The demand of more clients, while the technique for solving the production feed-level calcium biphosphate of product caking problem easy to moisture absorption.
A kind of technique using boiler slag purification of wet process phosphoric acid production feed-level calcium biphosphate, key are：Pot
The waste residue that stove desulfurization obtains, after break process with the concentrated phosphoric acid hybrid reaction desulfurization obtained after wet-process phosphoric acid concentration, after reaction
Phosphoric acid is handled again through defluorinate, and filtering phosphoric acid defluorination slurry obtains finished product phosphoric acid；After finished product phosphoric acid and calcium ore pulp hybrid reaction, through spray
Mist drying tower carries out granulating and drying, then is dried under reduced pressure to obtain product through revolution.
Above-mentioned boiler desulfurization waste residue is to remove SO in steam boiler using calcium carbonate2、SO3The solid slag obtained afterwards, master
Ingredient is wanted as CaO content 45~70%, wherein may participate in the active CaO content 35~60% of reaction, SiO2Content 5~20%,
SO3Content 2~5%, other metal oxides 5~10%, particle size range is great for the mass ratio of 100~300 mesh after crushing
In 80%.
Above-mentioned broken rear boiler desulfurization waste residue is controlled with concentrated acid phosphoric acid hybrid reaction condition is：Material proportion is pressed living in waste residue
Property calcium and phosphoric acid in SO3In molar ratio 1.0~2.0:1, phosphoric acid concentration 40~50%, SO3Content 2~6%, reaction temperature 60~
80 DEG C, 0.5~3.0h of reaction time, mixing speed be 3~8m/s.
By the fluorine content that dissociates in removing phosphoric acid, excessively 20% active silica and sodium carbonate carry out for above-mentioned defluorinate processing
Defluorinate is handled, 50~70 DEG C of reaction temperature, 1~3h of reaction time.
Above-mentioned phosphoric acid is ore pulp moisture 40~60% with the control of calcium ore pulp reaction condition, and reaction mass presses calcium/phosphorus mass ratio
For 0.55~0.65 mixing, 60~80 DEG C of reaction temperature, 1.5~3.0h of reaction time.
Above-mentioned spray drying tower operating procedure condition be 500~600 DEG C of high-temperature region temperature, middle warm area temperature 250~350
DEG C, 80~110 DEG C of low-temperature space temperature.
Above-mentioned revolution vacuum drying apparatus operation element condition be 100~300 DEG C of material inlet temperature, material outlet temperature 60
~90 DEG C, 1~2h of residence time of material, vacuum degree is 0.001~0.02MPa.
The present invention is using boiler desulfurization waste residue as SO in precipitate phosphoric acid3Precipitating reagent, it is mainly anti-using having in waste residue
The CaO of activity is answered, including calcium oxide, calcium carbonate etc., Ca is generated in reaction process2+And and SO4 2-It reacts, generates CaSO4It is heavy
Form sediment, realize the recycling of the calcium in waste residue being reaction, reduce the direct discharge capacity of waste residue, reduce enterprise's Solid state fermentation into
This.
Desuifurized particle size range is filtered after stringent control of the invention is broken, when the quality proportion of 100~300 mesh of waste residue
During more than 80%, the active CaO reaction conversion ratios in waste residue can reach more than 95%, while 60~80 DEG C of controlling reaction temperature,
0.5~3.0h of reaction time, mixing speed are 3~8m/s, and the crystal of calcium sulfate particle generated under the conditions of being somebody's turn to do is coarse, is conducive to
It is separated by filtration.
The present invention utilizes SiO entrained in residue2It reacts with the free fluorine in phosphoric acid, part SiO2Through high temperature
After processing there is higher reactivity, active diatom soil in part in defluorinate process can be replaced, reduce the consumption of activated silica diatomaceous earth
30~50%, hence it is evident that reduce production cost.
After defluorinate of the present invention after the washed recovery section phosphoric acid of press filtration filter cake, residual residue carries about 8~10% P2O5,
It can be added in fertilizer, need not only reprocess waste residue, moreover it is possible to bring certain benefit for enterprise.
For the present invention using spray drying tower as reaction slurry drying equipment, the material that nozzle is sprayed can fast eliminating trip
Form spherical particle from water, obtained product compares the obtained product roundness degree higher of other techniques, particle and particle it
Between contact area smaller, product bonding probability be substantially reduced.
The present invention is dried using vacuum drying apparatus, can slow evaporation particle be wrapped in internal free water, and pass through
Surface micropore is discharged, and forms the particle with hollow structure；Water content reaches balance inside and outside particle after drying, can avoid in life
It produces, particle inside free water moves to particle surface and causes to recrystallize formation bonding between particle in packaging, storage and transportational process
Caking.
The present invention is formed by improving particle appearance pattern and internal structure, one is reducing contact surface, it is several to reduce caking
Rate；The second is reducing free moisture inside particle, migration is avoided to crystallize.After the two organically combines, it can not additionally add modification and add
Add agent to improve particle from caking problem, utmostly reduce particle anti-caking block cost, and do not influence product quality.
Boiler desulfurization waste residue desulfurizing agent of the present invention is to the SO that dissociates in phosphoric acid3Removal efficiency can reach 80% with
On, the feed-level calcium biphosphate product SO of production3Content is less than 0.5%.
The present invention uses the feed-level calcium biphosphate product total phosphorus of technique productions to reach more than 23.5%, higher than country
Standard 22.0%, water-soluble phosphorus reach more than 21.0%, and product purity reaches 95% by phosphorus conversion, other indexs reach national mark
Accurate (GB 22548-2008) requirement, and product caking rate is less than 5% after pressing 60 days, is fully able to meet domestic and international client's
Demand.
The special proposition of present invention applicant is a kind of to produce feed-level calcium biphosphate using boiler slag purification of wet process phosphoric acid
Process carries out purified treatment to phosphoric acid by using production solid waste, reduces SO3Impurity content, while be granulated using spray tower
Technology is dried under reduced pressure to realize to the control of particle appearance pattern and the homogenizing of internal moisture, finally obtain total phosphorus content >=
23.5%, water-soluble phosphorus >=21.0%, calcium >=13.0%, feed-level calcium biphosphate product of the caking rate less than 5%.
Advantageous effect：First, realizing the recycling to industrial residue, fixed-end forces cost is reduced；It is helped second is that reducing defluorinate
Agent consumes, and reduces production cost；Third, do not generate new waste residue, residue is obtained after defluorinate can be added in fertilizer to sell, increase
The performance of enterprises；Fourth, the obtained product structure of production is special, spherical particle is not easy to bonding caking, and internal moisture, which is overflowed, to be formed
Hollow structure effectively removes free moisture inside particle, not only avoids water translocation spilling that recrystallization is caused to cause caking, also avoids
Add influence of the property-modifying additive to production cost and product quality；It is significantly improved fifth, obtaining product quality, product purity carries
It is high by about 5%, can meet the needs of different clients simultaneously, improve market competitiveness of enterprises.
Description of the drawings
Fig. 1 is the micro-structure diagram of feed-level calcium biphosphate product produced by the present invention.
Specific embodiment
Below by specific embodiment, the invention will be further described.
Embodiment 1：
Boiler desulfurization slag index：
Phosphoric acid index：
The boiler desulfurization waste residue of These parameters is with concentrated acid phosphatase reaction by calcium activated in waste residue and SO in phosphoric acid3In molar ratio
1:1,60 DEG C of reaction temperature, reaction time 3.0h, mixing speed 8m/s.The active dioxy of excessive addition 20% after the completion of reaction
SiClx and sodium carbonate carry out defluorinate processing, and finished product phosphoric acid is obtained by filtration in 50 DEG C of reaction temperature, reaction time 1h.Finished product phosphoric acid with
The control of calcium ore pulp reaction condition is ore pulp moisture 40%, and reaction mass is mixed by calcium/phosphorus mass ratio for 0.55, reaction temperature 80
DEG C, reaction time 3.0h, obtain MCP slurries.Slurry uses spray drying tower granulating and drying, 600 DEG C of high-temperature region temperature, middle warm area
Slurry is dried in 350 DEG C of temperature, 110 DEG C of low-temperature space temperature, while coordinates and be dried under reduced pressure using revolution, material inlet temperature
300 DEG C, 90 DEG C, residence time of material 1h, vacuum degree 0.001MPa of material outlet temperature obtains MCP products, MCP products are most
Screening packaging eventually.As shown in Figure 1, it is the feed-level calcium biphosphate MCP product micro-structure diagrams that embodiment 1 obtains, in having
Hollow structure is not easy the MCP products being bonded.
Embodiment 2：
Boiler desulfurization slag index：
Phosphoric acid index：
The boiler desulfurization waste residue of These parameters is with concentrated acid phosphatase reaction by calcium activated in waste residue and SO in phosphoric acid3In molar ratio
2:1,70 DEG C of reaction temperature, reaction time 2h, mixing speed 6m/s.The reactive silica of excessive addition 20% after the completion of reaction
Silicon and sodium carbonate carry out defluorinate processing, and finished product phosphoric acid is obtained by filtration in 60 DEG C of reaction temperature, reaction time 2h.Finished product phosphoric acid and calcium
The control of ore pulp reaction condition is ore pulp moisture 50%, and reaction mass is mixed by calcium/phosphorus mass ratio for 0.59,70 DEG C of reaction temperature,
Reaction time 2.0h obtains MCP slurries.Slurry uses spray drying tower granulating and drying, 500 DEG C of high-temperature region temperature, middle warm area temperature
300 DEG C of degree, slurry is dried in 100 DEG C of low-temperature space temperature, while coordinates and be dried under reduced pressure using revolution, material inlet temperature
200 DEG C, 80 DEG C, residence time of material 2h, vacuum degree 0.02MPa of material outlet temperature obtains MCP products, and MCP products are final
Screening packaging.As shown in Figure 1, being the feed-level calcium biphosphate MCP product micro-structure diagrams that embodiment 2 obtains, have hollow
Structure is not easy the MCP products being bonded.
Embodiment 3：
Boiler desulfurization slag index：
Phosphoric acid index：
The boiler desulfurization waste residue of These parameters is with concentrated acid phosphatase reaction by calcium activated in waste residue and SO in phosphoric acid3In molar ratio
1.5:1,80 DEG C of reaction temperature, reaction time 0.5h, mixing speed 3m/s.The activity two of excessive addition 20% after the completion of reaction
Silica and sodium carbonate carry out defluorinate processing, and finished product phosphoric acid is obtained by filtration in 70 DEG C of reaction temperature, reaction time 3h.Finished product phosphoric acid
It is ore pulp moisture 60% with the control of calcium ore pulp reaction condition, reaction mass is mixed by calcium/phosphorus mass ratio for 0.65, reaction temperature 60
DEG C, reaction time 1.5h, obtain MCP slurries.Slurry uses spray drying tower granulating and drying, 500 DEG C of high-temperature region temperature, middle warm area
Slurry is dried in 250 DEG C of temperature, 80 DEG C of low-temperature space temperature, while coordinates and be dried under reduced pressure using revolution, material inlet temperature
100 DEG C, material outlet temperature 60 C, residence time of material 2h, vacuum degree 0.02MPa obtain MCP products, and MCP products are final
Screening packaging.As shown in Figure 1, being the feed-level calcium biphosphate MCP product micro-structure diagrams that embodiment 1 obtains, have hollow
Structure is not easy the MCP products being bonded.
Embodiment 4：
Boiler desulfurization slag index：
Phosphoric acid index：
The boiler desulfurization waste residue of These parameters is with concentrated acid phosphatase reaction by calcium activated in waste residue and SO in phosphoric acid3In molar ratio
1.7:1,80 DEG C of reaction temperature, reaction time 0.5h, mixing speed 8m/s.The activity two of excessive addition 20% after the completion of reaction
Silica and sodium carbonate carry out defluorinate processing, and finished product phosphoric acid is obtained by filtration in 55 DEG C of reaction temperature, reaction time 1.5h.Finished product phosphorus
Acid is ore pulp moisture 45% with the control of calcium ore pulp reaction condition, and reaction mass presses calcium/phosphorus mass ratio as 0.62 mixing, reaction temperature
65 DEG C, reaction time 3.0h, obtain MCP slurries.Slurry uses spray drying tower granulating and drying, 580 DEG C of high-temperature region temperature, medium temperature
Slurry is dried in 330 DEG C of area's temperature, 100 DEG C of low-temperature space temperature, while coordinates and be dried under reduced pressure using revolution, material inlet temperature
250 DEG C of degree, 85 DEG C, residence time of material 1.5h, vacuum degree 0.01MPa of material outlet temperature obtains MCP products, MCP products
Final sizing is packed.As shown in Figure 1, for the feed-level calcium biphosphate MCP product micro-structure diagrams that embodiment 1 obtains, have
Hollow structure is not easy the MCP products being bonded.
Product index detects：
The product leading indicator comparison that the different embodiments of subordinate list 1 produce
Claims (6)
1. a kind of technique using boiler slag purification of wet process phosphoric acid production feed-level calcium biphosphate, it is characterised in that：Boiler
The waste residue that desulfurization obtains, with the concentrated phosphoric acid hybrid reaction desulfurization obtained after wet-process phosphoric acid concentration after break process, phosphorus after reaction
Acid is handled again through defluorinate, and filtering phosphoric acid defluorination slurry obtains finished product phosphoric acid；After finished product phosphoric acid and calcium ore pulp hybrid reaction, through spraying
Drying tower carries out granulating and drying, then is dried under reduced pressure to obtain product through revolution；Above-mentioned boiler desulfurization waste residue is to be removed using calcium carbonate
SO in steam boiler2、SO3The solid slag obtained afterwards, main component is CaO content 45 ~ 70%, wherein may participate in the work of reaction
Property CaO content 35 ~ 60%, SiO2Content 5 ~ 20%, SO3Content 2 ~ 5%, other metal oxides 5 ~ 10%, after crushing particle size range
It is great in 80% for the mass ratio of 100 ~ 300 mesh.
2. a kind of work using boiler slag purification of wet process phosphoric acid production feed-level calcium biphosphate according to claim 1
Skill, it is characterised in that：The broken rear boiler desulfurization waste residue is controlled with concentrated acid phosphoric acid hybrid reaction condition is：Material proportion is by useless
Calcium activated and SO in phosphoric acid in slag3In molar ratio 1.0 ~ 2.0:1, phosphoric acid concentration 40 ~ 50%, SO3Content 2 ~ 6%, reaction temperature 60 ~
80 DEG C, 0.5 ~ 3.0h of reaction time, mixing speed be 3 ~ 8m/s.
3. a kind of work using boiler slag purification of wet process phosphoric acid production feed-level calcium biphosphate according to claim 1
Skill, it is characterised in that：The defluorinate processing is by the active silica and sodium carbonate for removing the fluorine content excessive 20% that dissociates in phosphoric acid
Carry out defluorinate processing, 50 ~ 70 DEG C of reaction temperature, 1 ~ 3h of reaction time.
4. a kind of work using boiler slag purification of wet process phosphoric acid production feed-level calcium biphosphate according to claim 1
Skill, it is characterised in that：The phosphoric acid is ore pulp moisture 40 ~ 60% with the control of calcium ore pulp reaction condition, and reaction mass presses calcium/phosphorus matter
Amount for 0.55 ~ 0.65 than mixing, 60 ~ 80 DEG C of reaction temperature, 1.5 ~ 3.0h of reaction time.
5. a kind of work using boiler slag purification of wet process phosphoric acid production feed-level calcium biphosphate according to claim 1
Skill, it is characterised in that：The spray drying tower operating procedure condition be 500 ~ 600 DEG C of high-temperature region temperature, middle warm area temperature 250 ~
350 DEG C, 80 ~ 110 DEG C of low-temperature space temperature.
6. a kind of work using boiler slag purification of wet process phosphoric acid production feed-level calcium biphosphate according to claim 1
Skill, it is characterised in that：The vacuum drying apparatus operation element condition of turning round is 100 ~ 300 DEG C of material inlet temperature, material outlet
60 ~ 90 DEG C, 1 ~ 2h of residence time of material of temperature, vacuum degree are 0.001 ~ 0.02MPa.
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| CN108910853B (en) * | 2018-09-11 | 2020-07-31 | 云南磷化集团有限公司 | Method for producing granular calcium dihydrogen phosphate by one-step granulation of concentrated phosphoric acid |
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