CN111004153A - Method for producing urea phosphate by using wet-process phosphoric acid as raw material - Google Patents
Method for producing urea phosphate by using wet-process phosphoric acid as raw material Download PDFInfo
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- CN111004153A CN111004153A CN201911250227.0A CN201911250227A CN111004153A CN 111004153 A CN111004153 A CN 111004153A CN 201911250227 A CN201911250227 A CN 201911250227A CN 111004153 A CN111004153 A CN 111004153A
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- phosphoric acid
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- process phosphoric
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- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 title claims abstract description 90
- 238000000034 method Methods 0.000 title claims abstract description 51
- 229910000147 aluminium phosphate Inorganic materials 0.000 title claims abstract description 44
- DZHMRSPXDUUJER-UHFFFAOYSA-N [amino(hydroxy)methylidene]azanium;dihydrogen phosphate Chemical compound NC(N)=O.OP(O)(O)=O DZHMRSPXDUUJER-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 21
- 239000002994 raw material Substances 0.000 title claims abstract description 20
- 238000002425 crystallisation Methods 0.000 claims abstract description 67
- 230000008025 crystallization Effects 0.000 claims abstract description 65
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 19
- 238000010992 reflux Methods 0.000 claims abstract description 15
- 239000013078 crystal Substances 0.000 claims abstract description 10
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000004202 carbamide Substances 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 4
- 239000012065 filter cake Substances 0.000 claims abstract description 4
- 238000000926 separation method Methods 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 9
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 9
- SCYULBFZEHDVBN-UHFFFAOYSA-N 1,1-Dichloroethane Chemical compound CC(Cl)Cl SCYULBFZEHDVBN-UHFFFAOYSA-N 0.000 claims description 4
- 229910019142 PO4 Inorganic materials 0.000 claims description 4
- 238000000605 extraction Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 3
- 239000010452 phosphate Substances 0.000 claims description 3
- 239000002002 slurry Substances 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 3
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 2
- 239000008096 xylene Substances 0.000 claims description 2
- 238000001704 evaporation Methods 0.000 abstract description 13
- 230000008020 evaporation Effects 0.000 abstract description 13
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 5
- 238000009835 boiling Methods 0.000 abstract 1
- 230000000694 effects Effects 0.000 abstract 1
- 238000004064 recycling Methods 0.000 abstract 1
- 238000004904 shortening Methods 0.000 abstract 1
- 239000012071 phase Substances 0.000 description 20
- 230000008569 process Effects 0.000 description 9
- 238000001816 cooling Methods 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 239000007791 liquid phase Substances 0.000 description 3
- 239000012452 mother liquor Substances 0.000 description 3
- 229910052698 phosphorus Inorganic materials 0.000 description 3
- 241001465754 Metazoa Species 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 241000219000 Populus Species 0.000 description 1
- 241000282849 Ruminantia Species 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 239000012736 aqueous medium Substances 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C273/00—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups
- C07C273/02—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups of urea, its salts, complexes or addition compounds
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C273/00—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups
- C07C273/02—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups of urea, its salts, complexes or addition compounds
- C07C273/14—Separation; Purification; Stabilisation; Use of additives
- C07C273/16—Separation; Purification
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
Abstract
The invention relates to a method for producing urea phosphate by using wet-process phosphoric acid as a raw material. The technical scheme is as follows: adding wet-process phosphoric acid, urea and a water-carrying agent into a crystallization kettle, carrying out constant-temperature total reflux reaction, and then carrying out constant-temperature partial reflux crystallization; and after the crystallization is finished, carrying out solid-liquid separation, washing and drying a filter cake to obtain the urea phosphate crystal. The invention adopts the azeotropic effect of the water-carrying agent to reduce the boiling point temperature of the urea phosphate normal-pressure evaporation crystallization operation, realizes the recycling of the water-carrying agent, can regulate and control the discharge speed of water according to the demand of the evaporation crystallization rate, ensures that the urea phosphate evaporation crystallization operation is smoothly carried out by refluxing all redundant water to the crystallization kettle, improves the evaporation crystallization efficiency, and has the advantages of obviously reducing the energy consumption of the urea phosphate crystallization operation by taking wet phosphoric acid as a raw material, shortening the production period and improving the crystallization yield.
Description
Technical Field
The invention belongs to the technical field of deep processing in phosphorus chemical industry, and particularly relates to a method for producing urea phosphate by using wet-process phosphoric acid as a raw material.
Background
Urea phosphate (urea phosphate) is a fine chemical product widely applied to the fields of animal husbandry, industry, agriculture and the like, is not only a type I additive legally prescribed by the European Union feed industry, but also a special nutrient additive for ruminants and a phosphorus supplement recommended by the food and agricultural organization of the United nations in the animal husbandry, and has wide market prospect and great potential. The urea phosphate is a complex compound obtained by equivalent reaction of phosphoric acid and urea, and has a chemical formula of CO (NH)2)2–H3PO4At present, wet-process phosphoric acid is mostly used as a raw material to synthesize urea phosphate abroad, and the mainstream process comprises a two-stage method (a U.S. TVA method), a secondary crystallization method and a concentration crystallization method; most of the domestic uses hot phosphoric acid as raw material to synthesize urea phosphate. However, the thermal phosphoric acid process has high energy consumption, which causes the production cost to be overhigh, thereby limiting the market competitiveness of the urea phosphate in China. In recent years, with the improvement of purification and concentration technologies of wet-process phosphoric acid, many manufacturers gradually turn to the production of urea phosphate products by using wet-process phosphoric acid as a raw material, namely, the urea phosphate is prepared by pretreating the wet-process phosphoric acid through purification (solvent extraction or chemical precipitation), and then carrying out reaction and crystallization.
However, wet process phosphoric acid, although lower in cost, has P as compared to hot process phosphoric acid2O5The content is low, the impurity content is high, and the operations of purifying, removing impurities, concentrating and the like are often carried out before the urea phosphate is prepared, so that the production process is more complicated, and the energy consumption is high.
The existing urea phosphate crystallization process mainly comprises cooling crystallization and evaporative crystallization. The cooling crystallization process of urea phosphate mostly adopts intermittent operation, and the cooling crystallization process of urea phosphate taking wet-process phosphoric acid as a raw material mostly needs concentration operation; in actual production, the urea phosphate crystals scale on the wall of the heat exchanger seriously, so that the heat exchange efficiency is reduced, the production period is prolonged, the yield is reduced, and the cost is increased. Because the urea phosphate has higher solubility in the aqueous solution, the utilization rate of P, N in the raw material wet-process phosphoric acid and urea is lower. Because the specific heat and the evaporation latent heat of water are larger, and the solubility of the urea phosphate in the aqueous solution is larger, the viscosity and the concentration of the urea phosphate evaporation crystallization liquid are higher, so that the energy consumption of the urea phosphate evaporation crystallization operation is higher, and although the evaporation operation temperature can be properly reduced by adopting the pressure reduction operation, the comprehensive production cost is still higher.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and aims to provide a method for producing urea phosphate by using wet-process phosphoric acid as a raw material.
In order to achieve the purpose, the technical scheme adopted by the invention is specifically completed according to the following steps:
firstly, adding wet-process phosphoric acid, urea and a water-carrying agent S into a crystallization kettle under the conditions of normal pressure and a rotating speed of 50-200 r/min, wherein the water-carrying agent S is immiscible or partially miscible with water, and the mass of added urea is P contained in the wet-process phosphoric acid in the crystallization kettle2O50.85-0.9 times of the mass, and the adding volume of the water-carrying agent S is equal to the H contained in the wet-process phosphoric acid in the crystallization kettle21.0-5.0 times of the volume of O;
step two, under the conditions of normal pressure and the rotating speed of 50-200 r/min, heating the solution in the crystallization kettle to 70-90 ℃, carrying out constant-temperature total reflux for 0.5-1.5 h, and then carrying out constant-temperature partial reflux; the full reflux is that condensate generated after steam generated in the crystallization kettle is completely condensed is divided into an oil phase and a water phase through an oil-water separator, and then the oil phase and the water phase are totally refluxed into the crystallization kettle; the partial reflux is that condensate generated after steam generated in the crystallization kettle is completely condensed is divided into an oil phase and a water phase through an oil-water separator, the oil phase is totally refluxed into the crystallization kettle, the extraction rate of the water phase is controlled to be 1-10 mL/min, and the rest water phase is refluxed into the crystallization kettle again;
step three, when the total volume of the water phase extracted in the step two reaches the H contained in the wet-process phosphoric acid in the crystallization kettle in the step one2And when the volume of O is 70-90%, taking out crystal slurry in the crystallization kettle for solid-liquid separation, washing and drying a filter cake to obtain the urea phosphate crystal.
The crystallization kettle is a jacket stirring reaction kettle with controllable temperature.
The wet-process phosphoric acid is prepared by decomposing phosphate ore by adopting concentrated sulfuric acid, wherein P is2O5The content is 20 to 50 wt%.
The water-carrying agent S is at least one of dichloroethane, ethyl acetate, toluene, benzene and xylene.
Due to the adoption of the technical scheme, compared with the prior art, the invention has the following positive effects:
(1) the traditional method for producing urea phosphate by using wet-process phosphoric acid as raw material mostly adopts evaporative crystallization or evaporative concentration and cooling crystallization, and the concentration (P) of the wet-process phosphoric acid is obtained when the wet-process phosphoric acid is sent into an evaporator after pretreatment2O5The content is about 20-50 wt%), the normal pressure evaporation concentration operation temperature is high (generally more than or equal to 100 ℃), the water content to be evaporated is large, the energy consumption is high, and the vacuum evaporation can properly reduce the operation temperature, but the vacuum pump and the accessory equipment thereof increase the equipment investment and the operation cost. In the method for producing urea phosphate by using wet-process phosphoric acid as a raw material, the water-carrying agent S and water are added to form an azeotropic system, so that the evaporation operation temperature is remarkably reduced, and for example, the azeotropic temperatures of water, dichloroethane, ethyl acetate, toluene and benzene are 72 ℃, 70.4 ℃, 84.1 ℃ and 69.3 ℃ respectively. The water-carrying agent S is immiscible or partially miscible with water, and can be recycled without complex operation after being condensed and layered.
(2) The method for producing urea phosphate by using wet-process phosphoric acid as a raw material avoids the defects that the liquid phase volume of the crystallization mother liquor is gradually reduced and the solid phase suspension density is continuously increased in the evaporation crystallization process, the liquid phase volume of the crystallization mother liquor is larger than that of evaporation crystallization or cooling crystallization due to the addition and backflow of the water-carrying agent S, the phenomena of crushing and aggregation of crystal products can be greatly reduced, and the concentration of the product particle size distribution is facilitated.
(3) Urea phosphate has a relatively high solubility in water (76.4 wt.% at 60 ℃ and 49.2 wt.% at 15 ℃) [ poplar sails, field-opening, liufei ] solubility in water as determined by the laser method [ J ]. inorganic salt industry, 2016,48(4):69-71 ], whereas it has a relatively low solubility in aqueous media. The traditional urea phosphate evaporation crystallization and cooling crystallization processes both adopt water as a solvent, and a large amount of urea phosphate crystals are not crystallized and separated out in mother liquor when the crystallization is finished, so that the product yield is low. The method for producing urea phosphate by using wet-process phosphoric acid as a raw material has the advantages that a liquid phase contains a large amount of water-carrying agent and a small amount of water when the crystallization operation is finished, and the product yield of urea phosphate can be obviously improved.
Drawings
FIG. 1 is a schematic flow chart of the present invention.
Detailed Description
The invention is further described with reference to specific embodiments, without limiting its scope.
Example 1
A method for producing urea phosphate by taking wet-process phosphoric acid as a raw material comprises the following steps:
firstly, adding wet-process phosphoric acid, urea and a water-carrying agent S into a crystallization kettle under the conditions of normal pressure and 100 r/min of rotating speed, wherein the water-carrying agent S is immiscible or partially miscible with water, and the adding quality of the urea is P contained in the wet-process phosphoric acid in the crystallization kettle2O50.9 times of the mass, and the adding volume of the water-carrying agent S is equal to the H contained in the wet-process phosphoric acid in the crystallization kettle23.0-4.0 times of the volume of O;
step two, under the conditions of normal pressure and the rotating speed of 100 r/min, heating the solution in the crystallization kettle to 70-80 ℃, carrying out constant-temperature total reflux for 1 h, and then carrying out constant-temperature partial reflux; the full reflux is that condensate generated after steam generated in the crystallization kettle is completely condensed is divided into an oil phase and a water phase through an oil-water separator, and then the oil phase and the water phase are totally refluxed into the crystallization kettle; the partial reflux is that condensate generated after steam generated in the crystallization kettle is completely condensed is divided into an oil phase and a water phase through an oil-water separator, the oil phase is totally refluxed into the crystallization kettle, the extraction rate of the water phase is controlled to be 1-5 mL/min, and the rest water phase is refluxed into the crystallization kettle again;
step three, when the total volume of the water phase extracted in the step two reaches the H contained in the wet-process phosphoric acid in the crystallization kettle in the step one2And when the volume of O is 70-90%, taking out crystal slurry in the crystallization kettle for solid-liquid separation, washing and drying a filter cake to obtain the urea phosphate crystal.
The crystallization kettle is a jacket stirring reaction kettle with controllable temperature.
The wet-process phosphoric acid adopts concentrated sulfuric acid to decompose phosphate oreThe phosphoric acid obtained, wherein P2O5The content is 30-32 wt%.
The water-carrying agent S is dichloroethane.
Claims (4)
1. A method for producing urea phosphate by taking wet-process phosphoric acid as a raw material is characterized by comprising the following steps:
firstly, adding wet-process phosphoric acid, urea and a water-carrying agent S into a crystallization kettle under the conditions of normal pressure and a rotating speed of 50-200 r/min, wherein the water-carrying agent S is immiscible or partially miscible with water, and the mass of added urea is P contained in the wet-process phosphoric acid in the crystallization kettle2O50.85-0.9 times of the mass, and the adding volume of the water-carrying agent S is equal to the H contained in the wet-process phosphoric acid in the crystallization kettle21.0-5.0 times of the volume of O;
step two, under the conditions of normal pressure and the rotating speed of 50-200 r/min, heating the solution in the crystallization kettle to 70-90 ℃, carrying out constant-temperature total reflux for 0.5-1.5 h, and then carrying out constant-temperature partial reflux; the full reflux is that condensate generated after steam generated in the crystallization kettle is completely condensed is divided into an oil phase and a water phase through an oil-water separator, and then the oil phase and the water phase are totally refluxed into the crystallization kettle; the partial reflux is that condensate generated after steam generated in the crystallization kettle is completely condensed is divided into an oil phase and a water phase through an oil-water separator, the oil phase is totally refluxed into the crystallization kettle, the extraction rate of the water phase is controlled to be 1-10 mL/min, and the rest water phase is refluxed into the crystallization kettle again;
step three, when the total volume of the water phase extracted in the step two reaches the H contained in the wet-process phosphoric acid in the crystallization kettle in the step one2And when the volume of O is 70-90%, taking out crystal slurry in the crystallization kettle for solid-liquid separation, washing and drying a filter cake to obtain the urea phosphate crystal.
2. The method for producing urea phosphate by using wet-process phosphoric acid as a raw material according to claim 1, wherein the crystallization kettle is a temperature-controllable jacketed stirred tank reactor.
3. The method for producing urea phosphate by using wet-process phosphoric acid as raw material according to claim 1The method is characterized in that the wet-process phosphoric acid is prepared by decomposing phosphate ore by adopting concentrated sulfuric acid, wherein P is2O5The content is 20 to 50 wt%.
4. The method for producing urea phosphate by using wet-process phosphoric acid as a raw material according to claim 1, wherein the water-carrying agent S is at least one of dichloroethane, ethyl acetate, toluene, benzene, and xylene.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911250227.0A CN111004153A (en) | 2019-12-09 | 2019-12-09 | Method for producing urea phosphate by using wet-process phosphoric acid as raw material |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101318914A (en) * | 2008-07-23 | 2008-12-10 | 瓮福（集团）有限责任公司 | Method for preparing urea phosphoric acid with wet-process phosphoric acid |
| CN104151203A (en) * | 2014-07-17 | 2014-11-19 | 瓮福（集团）有限责任公司 | Method for continuously producing urea phosphate by vacuum evaporation crystallization |
| CN106349116A (en) * | 2016-08-25 | 2017-01-25 | 湖北三宁化工股份有限公司 | Method for continuously producing feed-grade urea phosphate from wet-method purified phosphoric acid strip liquor or washing residual liquid |
| CN107473990A (en) * | 2017-07-24 | 2017-12-15 | 湖北三宁化工股份有限公司 | A kind of urea phosphate mother liquor water soluble fertilizer and preparation method |
| CN108285427A (en) * | 2018-01-08 | 2018-07-17 | 湖北三宁化工股份有限公司 | A kind of method of phosphoric acid by wet process round-robin method continuous production big particle industrial grade urea phosphate |
-
2019
- 2019-12-09 CN CN201911250227.0A patent/CN111004153A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101318914A (en) * | 2008-07-23 | 2008-12-10 | 瓮福（集团）有限责任公司 | Method for preparing urea phosphoric acid with wet-process phosphoric acid |
| CN104151203A (en) * | 2014-07-17 | 2014-11-19 | 瓮福（集团）有限责任公司 | Method for continuously producing urea phosphate by vacuum evaporation crystallization |
| CN106349116A (en) * | 2016-08-25 | 2017-01-25 | 湖北三宁化工股份有限公司 | Method for continuously producing feed-grade urea phosphate from wet-method purified phosphoric acid strip liquor or washing residual liquid |
| CN107473990A (en) * | 2017-07-24 | 2017-12-15 | 湖北三宁化工股份有限公司 | A kind of urea phosphate mother liquor water soluble fertilizer and preparation method |
| CN108285427A (en) * | 2018-01-08 | 2018-07-17 | 湖北三宁化工股份有限公司 | A kind of method of phosphoric acid by wet process round-robin method continuous production big particle industrial grade urea phosphate |
Non-Patent Citations (1)
| Title |
|---|
| 李敬等: "湿法磷酸合成磷酸脲的工艺研究" * |
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Application publication date: 20200414 |