CN104892061A - Preparation method for sulfur-containing phosphate fertilizer - Google Patents
Preparation method for sulfur-containing phosphate fertilizer Download PDFInfo
- Publication number
- CN104892061A CN104892061A CN201510249522.XA CN201510249522A CN104892061A CN 104892061 A CN104892061 A CN 104892061A CN 201510249522 A CN201510249522 A CN 201510249522A CN 104892061 A CN104892061 A CN 104892061A
- Authority
- CN
- China
- Prior art keywords
- sulfur
- phosphate fertilizer
- bearing
- phosphoric acid
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Abstract
The invention discloses a preparation method for a sulfur-containing phosphate fertilizer. The method includes: firstly adding additives into an absorption liquid of sulfuric acid tail gas, endowing the absorption liquid with dispersibility to sulfur granules, performing mixing, then adding the mixture into phosphoric acid, using an existing phosphate fertilizer production device, and carrying out reaction, granulation and drying, thus obtaining the product. The method provided by uses sulfuric acid plant tail gas absorption liquid cyclically, utilizes existing ammonium phosphate, triple superphosphate plant and other traditional phosphate fertilizer devices to prepare the fertilizer containing over two nutrient elements of nitrogen, phosphorus, potassium and sulfur, and provides a low cost product upgrading method for traditional device.
Description
Technical field
The invention belongs to production of phosphate fertilizer technical field, specifically relate to a kind of preparation method of sulfur-bearing phosphate fertilizer.
Background technology
Sulfur fertilizer refers to the fertilizer containing element sulphur.Traditional produces sulfur fertilizer with phosphate fertilizer device, is generally take the material after ammonification to spray liquid-state sulfur or the mode at product external parcel one deck liquid-state sulfur.It is uneven all to there is mixing in these modes, even forms the phenomenon of block after sulphur cooling, causes quality product to occur fluctuation.
Find through retrieval, describe " sulfur-containing fertilizer and preparation method thereof " in Chinese patent 96193527.8, solidifying again by thawing sulphur being passed in reactor with after the mixing of phosphate fertilizer slip, being granulated.Describing in 201080005679.3 " sulfur-containing fertilizer and preparation method thereof ", introducing molten sulfur again, then granulation by being mixed into tensio-active agent in the slurries mainly containing phosphate base fertilizer mass.200380103202.9 " production methods of sulfur-bearing ammophos ", which depict by containing elementary sulfur liquid phase in the reactor and containing ammonia, phosphoric acid, water liquid-phase mixing or introduce in granulator device.Describe in 99120285.6 " compound sulfur-containing fertilizer and manufacture method thereof " and various fertilizer is mixed in proportion.200610172825.7 and 01801260.4 " sulfur-containing fertilizer composition and preparation method thereof " describes the surface of slurries spraying containing the fertilizer such as phosphoric acid salt or nitrate with sulfur-bearing.200910102988.1 " adding the method that SULPHUR POWDER produces sulfur fertilizer with di(2-ethylhexyl)phosphate sulphur device ", described and are mixed in sulfuric acid by SULPHUR POWDER, and reactor and diammonium phosphate slurry mixing are introduced in ammonification after melting.
Although these patent documentations above-mentioned disclose a lot of improvement, but also have problems, such as: mix uneven in the reactor, need the qualification rate being controlled the finished product by returning charge, cause containing elemental sulfur phosphoric acid salt in the fabrication process, elemental sulfur dust explosion hazardness is larger.And how to solve in prior art and there is not yet way well.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, a kind of preparation method of sulfur-bearing phosphate fertilizer is provided, after Homogeneous phase mixing simple substance sulphur particle in phosphoric acid, significantly reduce returning charge frequency, reduce the possibility of dust explosion.
Object of the present invention is achieved by the following technical programs.
Except as otherwise noted, percentage ratio of the present invention is mass percent.
A preparation method for sulfur-bearing phosphate fertilizer, comprises the following steps:
(1) calcium sulfate, phosphoric acid are added in sulfuric acid tail gas absorption liquid, after mixing, obtain solution A, control sulfate radical content 0.5 ~ 1.5% in solution A, calcium ion mass concentration 0.1 ~ 0.3%, Vanadium Pentoxide in FLAKES mass concentration 8.0 ~ 12.0%;
(2) in solution A, add the sulfur granule of 10 ~ 50%, grain diameter≤180 micron, stir and make sulfur granule in the solution dispersed, obtain the mixing solutions B of sulfur-bearing;
(3) mixing solutions B is evenly mixed in phosphoric acid, the consumption of mixing solutions B is 10% ~ 20% of phosphoric acid quality, the sulfur-bearing phosphoric acid obtained reacts by traditional production of phosphate fertilizer technique and ammonia or ground phosphate rock again, namely obtains required sulfur-bearing phosphate fertilizer after granulation, drying.
The calcium sulfate added in solution A described in step (1), its grain diameter≤150 micron, controlling calcium ion mass concentration in solution A is 0.2%.
It is 10.0% that step (1) controls Vanadium Pentoxide in FLAKES mass concentration in solution A.
In mixing solutions B described in step (2), the additional proportion of sulfur granule is preferably 50%.
Drying described in step (3), hot blast temperature≤250 DEG C, outlet material moisture≤2.0%;
Relative to prior art, the present invention has the following advantages:
1, instant invention overcomes the shortcoming that traditional sulfur fertilizer is produced, utilize existing phosphate fertilizer device (comprising the devices such as phosphorus ammonium, coarse whiting) to add sulfur granule and produce sulfur fertilizer, there is the wider scope of application.The quality index finally obtaining sulfur fertilizer product can reach: effectively P
2o
5>=40%; Total nitrogen>=6%; Moisture≤2.0%; Screening after product granularity 2-4mm>=90%; Sulphur content>=10%.
2, recycle of the present invention sulfuric acid tail gas absorption liquid, this absorption liquid contains ammonium sulfate and ammonium sulphite, is sulfuric acid tail gas to be absorbed logical ammonia to obtain, and in actual production, this absorption liquid recycle economic benefit is not high.Contriver is on experiment basis many times, the mixed solution formed after finding to add a small amount of phosphoric acid, calcium sulfate in sulfuric acid tail gas absorption liquid, can dispersed simple substance sulphur particle, and the liquid of this dispersed sulfur granule is mixed in phosphoric acid again, can still keeps good dispersion effect.
3, the simple substance sulphur particle that the present invention is used is not high to Particle size requirements, can adopt water mill or dry grinding, makes its fineness reach more than 80 orders.
Accompanying drawing explanation
Fig. 1 produces by the inventive method the process flow diagram adding sulphur ammonium hydrogen phosphate.
Fig. 2 produces by the inventive method the process flow diagram adding sulphur coarse whiting.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in further detail, but drawings and Examples are not limited to the technical solution.
Embodiment 1
Production adds sulphur monoammonium phosphate, as shown in Figure 1:
The first step: first get sulfuric acid tail gas absorption liquid, adds phosphoric acid, the calcium sulfate of 150 microns, makes sulfate radical content 0.5%, calcium contents 0.1%, Vanadium Pentoxide in FLAKES 8%.Sulphur is finely ground to the SULPHUR POWDER that fineness is 180 microns, according to the demand (the ratio demand of elemental sulfur or sulfate radical) of sulfur-bearing in product, by SULPHUR POWDER in 50% ratio be mixed into the sulfuric acid tail gas absorption liquid mixing and stirring of auxiliary agent, then press in 15% introducing phosphoric acid of phosphoric acid quality.
Second step: produce and add sulphur monoammonium phosphate particle.The reactor applied is tubular reactor.Above-mentioned phosphoric acid is introduced tubular reactor; and pass into ammonia; mixture reacts at 120 DEG C; monoammonium phosphate (also diammonium phosphate can be obtained) is obtained by controlling degree of neutralization; slurryspraying granulation in tablets press is squeezed into finally by spray pump; obtain after crushing and screening and add ammonium phosphate sulfate, analytical results sees the following form 1.
Table 1, sulfur-bearing phosphate fertilizer analytical results
| Index name | Total N/ (%) | Effective P 2O 5/(％) | Total S/ (%) | H 2O/(％) | Ultimate compression strength/(N/ grain) |
| Analytical results | 10.9 | 41.3 | 12.5 | 1.4 | 47.2 |
Embodiment 2
Production adds sulphur monoammonium phosphate, as shown in Figure 1:
The first step: first get sulfuric acid tail gas absorption liquid, adds phosphoric acid, the calcium sulfate of 150 microns, makes sulfate radical content 1.0%, calcium contents 0.2%, Vanadium Pentoxide in FLAKES 10%.Sulphur is finely ground to the SULPHUR POWDER that fineness is 180 microns, according to the demand (the ratio demand of elemental sulfur or sulfate radical) of sulfur-bearing in product, by SULPHUR POWDER in 30% ratio be mixed into the sulfuric acid tail gas absorption liquid mixing and stirring of auxiliary agent, then press in 10% introducing phosphoric acid of phosphoric acid quality.
Second step: undertaken operating to obtain product by embodiment 1 second step step, analytical results is shown in 2.
Table 2, sulfur-bearing phosphate fertilizer analytical results
| Index name | Total N/ (%) | Effective P 2O 5/(％) | Total S/ (%) | H 2O/(％) | Ultimate compression strength/(N/ grain) |
| Analytical results | 10.6 | 40.7 | 10.2 | 1.7 | 47.5 |
Embodiment 3
Production adds sulphur monoammonium phosphate, as shown in Figure 1:
The first step: first get sulfuric acid tail gas absorption liquid, adds phosphoric acid, the calcium sulfate of 150 microns, makes sulfate radical content 1.5%, calcium contents 0.3%, Vanadium Pentoxide in FLAKES 12%.Sulphur is finely ground to the SULPHUR POWDER that fineness is 180 microns, according to the demand (the ratio demand of elemental sulfur or sulfate radical) of sulfur-bearing in product, by SULPHUR POWDER by 10% be mixed into the sulfuric acid tail gas absorption liquid mixing and stirring of auxiliary agent, then press in 20% introducing phosphoric acid of phosphoric acid quality.
Second step: undertaken operating to obtain product by embodiment 1 second step step, analytical results is shown in 3.
Table 3, sulfur-bearing phosphate fertilizer analytical results
| Index name | Total N/ (%) | Effective P 2O 5/(％) | Total S/ (%) | H 2O/(％) | Ultimate compression strength/(N/ grain) |
| Analytical results | 7 | 40.1 | 10.2 | 1.5 | 46.4 |
Embodiment 4
Production adds sulphur coarse whiting, as shown in Figure 2:
The first step: by embodiment 1 the first step by simple substance sulphur Granular composite in phosphoric acid.
Second step: produce and add sulphur coarse whiting.Above-mentioned phosphoric acid is introduced mixing tank, adds breeze, granulation after slaking, obtain after crushing and screening adding sulphur coarse whiting
Table 4, sulfur-bearing phosphate fertilizer analytical results
| Index name | Effective P 2O 5/(％) | Total S/ (%) | H 2O/(％) | Ultimate compression strength/(N/ grain) |
| Analytical results | 40.1 | 12.4 | 3.5 | 7.1 |
Embodiment 5
Production adds sulphur coarse whiting, as shown in Figure 2:
The first step: by embodiment 2 the first step by simple substance sulphur Granular composite in phosphoric acid.
Second step: according to Fig. 2 technical process, produces and adds sulphur coarse whiting.Above-mentioned phosphoric acid is introduced mixing tank, adds breeze, granulation after slaking, obtain after crushing and screening adding sulphur coarse whiting
Table 5, sulfur-bearing phosphate fertilizer analytical results
| Index name | Effective P 2O 5/(％) | Total S/ (%) | H 2O/(％) | Ultimate compression strength/(N/ grain) |
| Analytical results | 40.1 | 11.2 | 3.8 | 8.4 |
Embodiment 6
Production adds sulphur coarse whiting, as shown in Figure 2:
The first step: by embodiment 3 the first step by simple substance sulphur Granular composite in phosphoric acid.
Second step: according to Fig. 2 technical process, produces and adds sulphur coarse whiting.Above-mentioned phosphoric acid is introduced mixing tank, adds breeze, granulation after slaking, obtain after crushing and screening adding sulphur coarse whiting
Table 6, sulfur-bearing phosphate fertilizer analytical results
| Index name | Effective P 2O 5/(％) | Total S/ (%) | H 2O/(％) | Ultimate compression strength/(N/ grain) |
| Analytical results | 40.1 | 7.8 | 2.5 | 7.8 |
Claims (5)
1. a preparation method for sulfur-bearing phosphate fertilizer, comprises the following steps:
(1) calcium sulfate, phosphoric acid are added in sulfuric acid tail gas absorption liquid, after mixing, obtain solution A, control sulfate radical content 0.5 ~ 1.5% in solution A, calcium ion mass concentration 0.1 ~ 0.3%, Vanadium Pentoxide in FLAKES mass concentration 8.0 ~ 12.0%;
(2) in solution A, add the sulfur granule of 10 ~ 50%, grain diameter≤180 micron, stir and make sulfur granule in the solution dispersed, obtain the mixing solutions B of sulfur-bearing;
(3) mixing solutions B is evenly mixed in phosphoric acid, the consumption of mixing solutions B is 10% ~ 20% of phosphoric acid quality, the sulfur-bearing phosphoric acid obtained reacts by traditional production of phosphate fertilizer technique and ammonia or ground phosphate rock again, namely obtains required sulfur-bearing phosphate fertilizer after granulation, drying.
2. the preparation method of sulfur-bearing phosphate fertilizer according to claim 1, is characterized in that: the calcium sulfate added in solution A described in step (1), its grain diameter≤150 micron, and controlling calcium ion mass concentration in solution A is 0.2%.
3. the preparation method of sulfur-bearing phosphate fertilizer according to claim 1, is characterized in that: it is 10.0% that step (1) controls Vanadium Pentoxide in FLAKES mass concentration in solution A.
4. the preparation method of sulfur-bearing phosphate fertilizer according to claim 1, is characterized in that: in the mixing solutions B described in step (2), the additional proportion of sulfur granule is preferably 50%.
5. the preparation method of sulfur-bearing phosphate fertilizer according to claim 1, is characterized in that: the drying described in step (3), hot blast temperature≤250 DEG C, outlet material moisture≤2.0%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510249522.XA CN104892061A (en) | 2015-05-15 | 2015-05-15 | Preparation method for sulfur-containing phosphate fertilizer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510249522.XA CN104892061A (en) | 2015-05-15 | 2015-05-15 | Preparation method for sulfur-containing phosphate fertilizer |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104892061A true CN104892061A (en) | 2015-09-09 |
Family
ID=54025092
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510249522.XA Pending CN104892061A (en) | 2015-05-15 | 2015-05-15 | Preparation method for sulfur-containing phosphate fertilizer |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104892061A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106430109A (en) * | 2016-08-31 | 2017-02-22 | 瓮福达州化工有限责任公司 | Sulfur shearing and dispersing technology |
| CN106810321A (en) * | 2017-01-21 | 2017-06-09 | 云南三环中化化肥有限公司 | A kind of molten sulfur is added to the device and method of production sulfur-bearing phosphate fertilizer in gas phase |
| CN111533614A (en) * | 2020-03-24 | 2020-08-14 | 贵州新东浩化工材料科技有限公司 | Preparation method for producing triple superphosphate containing elemental sulfur by using raffinate acid |
| CN111606739A (en) * | 2020-06-17 | 2020-09-01 | 云南磷化集团海口磷业有限公司 | Sulfur-containing enriched calcium superphosphate production device and preparation method |
| CN112457090A (en) * | 2020-11-06 | 2021-03-09 | 云南磷化集团海口磷业有限公司 | Contain sulphur phosphorus fertilizer apparatus for producing and contain sulphur ammonium phosphate apparatus for producing |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101723411A (en) * | 2009-12-18 | 2010-06-09 | 聊城鲁西化工第五化肥厂 | Process and equipment for producing potassium sulfate compound fertilizer by integrally utilizing tail gas generated in sulphuric acid production |
| CN101935254A (en) * | 2010-08-26 | 2011-01-05 | 宁夏鲁西化工化肥有限公司 | Multi-element compound diammonium phosphate and production method and system thereof |
| CN102395543A (en) * | 2009-04-16 | 2012-03-28 | 硫磺溶解股份有限公司 | Dispersible sulphur fertilizer pellets |
| CN103249696A (en) * | 2010-08-27 | 2013-08-14 | Ccr科技有限公司 | Method for producing fertilizers containing dispersed micronized sulphur |
| CN104583157A (en) * | 2012-07-09 | 2015-04-29 | 国际壳牌研究有限公司 | Process for preparing an emulsion of elemental sulphur particles |
-
2015
- 2015-05-15 CN CN201510249522.XA patent/CN104892061A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102395543A (en) * | 2009-04-16 | 2012-03-28 | 硫磺溶解股份有限公司 | Dispersible sulphur fertilizer pellets |
| CN101723411A (en) * | 2009-12-18 | 2010-06-09 | 聊城鲁西化工第五化肥厂 | Process and equipment for producing potassium sulfate compound fertilizer by integrally utilizing tail gas generated in sulphuric acid production |
| CN101935254A (en) * | 2010-08-26 | 2011-01-05 | 宁夏鲁西化工化肥有限公司 | Multi-element compound diammonium phosphate and production method and system thereof |
| CN103249696A (en) * | 2010-08-27 | 2013-08-14 | Ccr科技有限公司 | Method for producing fertilizers containing dispersed micronized sulphur |
| CN104583157A (en) * | 2012-07-09 | 2015-04-29 | 国际壳牌研究有限公司 | Process for preparing an emulsion of elemental sulphur particles |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106430109A (en) * | 2016-08-31 | 2017-02-22 | 瓮福达州化工有限责任公司 | Sulfur shearing and dispersing technology |
| CN106810321A (en) * | 2017-01-21 | 2017-06-09 | 云南三环中化化肥有限公司 | A kind of molten sulfur is added to the device and method of production sulfur-bearing phosphate fertilizer in gas phase |
| CN111533614A (en) * | 2020-03-24 | 2020-08-14 | 贵州新东浩化工材料科技有限公司 | Preparation method for producing triple superphosphate containing elemental sulfur by using raffinate acid |
| CN111606739A (en) * | 2020-06-17 | 2020-09-01 | 云南磷化集团海口磷业有限公司 | Sulfur-containing enriched calcium superphosphate production device and preparation method |
| CN112457090A (en) * | 2020-11-06 | 2021-03-09 | 云南磷化集团海口磷业有限公司 | Contain sulphur phosphorus fertilizer apparatus for producing and contain sulphur ammonium phosphate apparatus for producing |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104892061A (en) | Preparation method for sulfur-containing phosphate fertilizer | |
| CN101891504B (en) | Method for producing granular monoammonium phosphate with raffinate | |
| CN103848670B (en) | A kind of with the technique of phosphorus ammonium thickened pulp One-step production high-concentration compound fertilizer | |
| CN103318863B (en) | A kind of slurry process mid low grade phosphate rock stone produces the joint acid novel process of phosphorus ammonium | |
| CN103113139B (en) | Method for producing multivariate nitro compound fertilizer from wet-process phosphoric acid purification sludge | |
| CA2809598C (en) | Method for producing fertilizers containing dispersed micronized sulphur | |
| CN105800574A (en) | Preparation method of sulfur-containing ammonium phosphate | |
| CN110590439A (en) | High-tower slow-release compound fertilizer and preparation method thereof | |
| CN100584805C (en) | Method for producing sulfur-magnesium fertilizer by high magnesium phosphorus tails | |
| CN101570455A (en) | Method for preparing particle ammonium sulfate product by organic-inorganic binder | |
| CN100354235C (en) | Spray pelleting process of compound fertilizer | |
| CA2985851A1 (en) | Fertilizer pellets formed by compression of micronized sulphur | |
| CN101575222A (en) | Method for producing ammonium sulphate grain products by using inorganic caking agent | |
| WO2021103942A1 (en) | Secondary and trace element mixture and application thereof | |
| CN109265249A (en) | Delay the method for molten fertilizer for delaying the activator of molten object and using activator preparation | |
| WO2012115496A1 (en) | Method for production of granular compound fertilizers | |
| CN105254341A (en) | Preparation method of sulfur-containing heavy calcium | |
| CN102557834A (en) | Method for producing composite fertilizer fillers by using phosphorite tailings | |
| CN103360145A (en) | Technology of producing ammonium sulfate phosphate product from tailing slag | |
| CN105431396A (en) | Method for producing granulated nitrogen-potash fertilizer | |
| CN106146109A (en) | A kind of spray pelleting process of compound fertilizer | |
| CN101337847B (en) | Method for preparing high-nitrogen sulfonyl azophoska compound fertilizer | |
| CN102001872B (en) | method for producing granular potash fertilizer and product thereof | |
| CN101768026B (en) | Method for producing sulfur fertilizer by using diammonium phosphate device to add sulfur powder | |
| CN106316510B (en) | Method for producing sulfur-containing ammonium phosphate by adopting industrial byproduct desulfurization paste |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20150909 |
|
| WD01 | Invention patent application deemed withdrawn after publication |