CN211078988U - Device for producing urea phosphate by taking wet-process phosphoric acid as raw material - Google Patents
Device for producing urea phosphate by taking wet-process phosphoric acid as raw material Download PDFInfo
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- CN211078988U CN211078988U CN201922183882.0U CN201922183882U CN211078988U CN 211078988 U CN211078988 U CN 211078988U CN 201922183882 U CN201922183882 U CN 201922183882U CN 211078988 U CN211078988 U CN 211078988U
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- storage tank
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- phosphoric acid
- process phosphoric
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Abstract
The utility model relates to an use wet process phosphoric acid as device of raw materials production urea phosphate, specifically including pressing from both sides cover reation kettle (1), wet process phosphoric acid storage tank (3), urea granule feed bin (4), water carrying agent storage tank (6), filter (7), condensation heat exchanger (8), profit phase splitter (9), first waste liquid storage tank (10), second waste liquid storage tank (11), back flow (12), I mass flow meter (13) and II mass flow meter (14) to and the pipe connection between the above-mentioned equipment. The utility model discloses the device adopts the azeotropic effect of water-carrying agent can effectively reduce urea phosphate ordinary pressure evaporation crystallization boiling point, has avoided pressing from both sides the pressure boost phenomenon that the cover reation kettle was interior not smooth arouses because of steam discharge, has realized the recycling of water-carrying agent, can be according to the discharge velocity of evaporation crystallization rate's demand regulation and control moisture, and unnecessary moisture also can flow back to pressing from both sides cover reation kettle (1), ensures that evaporation crystallization operation goes on smoothly, has improved evaporation crystallization efficiency.
Description
Technical Field
The invention belongs to the technical field of deep processing in phosphorus chemical industry, and particularly relates to a device 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 utility model aims to overcome the technical defects and provides a device for producing urea phosphate by using wet-process phosphoric acid as a raw material.
In order to achieve the purpose, the device for producing urea phosphate by using wet-process phosphoric acid as a raw material is characterized by specifically comprising a jacket reaction kettle (1), a wet-process phosphoric acid storage tank (3), a urea particle storage bin (4), a water carrying agent storage tank (6), a filter (7), a condensing heat exchanger (8), an oil-water phase separator (9), a first waste liquid storage tank (10), a second waste liquid storage tank (11), a return pipe (12), an I mass flowmeter (13) and an II mass flowmeter (14);
the top end of the jacket reaction kettle (1) is provided with 1 exhaust port guide pipe (101), the exhaust port guide pipe (101) is connected with a tube side steam inlet (801) of the vertically installed condensing heat exchanger (8) through a pipeline, and the top end of the oil-water phase separator (9) is connected with a shell side condensate outlet (803) of the vertically installed condensing heat exchanger (8) through a pipeline; the middle lower part of the oil-water phase separator (9) is connected with the jacket reaction kettle (1) through a pipeline provided with a return pipe (12); the return pipe (12) is a U-shaped or concave pipe, and the bottom of the return pipe (12) is connected with the first waste liquid storage tank (10) through a pipeline provided with an I-shaped mass flowmeter (13); the bottom end of the oil-water phase separator (9) is connected with a second waste liquid storage tank (11) through a pipeline provided with a second mass flowmeter (14); the bottom end of the second waste liquid storage tank (11) is connected with the jacket reaction kettle (1) through a pipeline provided with a third pump (203);
the wet-process phosphoric acid storage tank (3) is connected with the jacket reaction kettle (1) through a pipeline provided with an I pump (201); the water-carrying agent storage tank (6) is connected with the jacket reaction kettle (1) through a pipeline provided with a second pump (202); the urea particle bin (4) is connected with the jacket reaction kettle (1) through a pipeline provided with a spiral feeding pump (5); the bottom of the jacket reaction kettle (1) is connected with the filter (7) through a pipeline provided with a valve.
The jacket reaction kettle is a jacket stirring reaction kettle with controllable temperature.
Owing to adopt above-mentioned technical scheme, compare prior art, the utility model discloses following positive effect has: the azeotropic effect of the water-carrying agent is adopted to reduce the boiling point of the urea phosphate normal-pressure operation, the steam generated in the jacket reaction kettle can well enter the condenser due to the introduction of the upper steam pipe, the pressurization phenomenon caused by unsmooth steam discharge in the jacket reaction kettle is avoided, the water-carrying agent is separated by the oil-water phase separator, the solvent in the liquid mixture (containing the water-carrying agent) flows back to the jacket reaction kettle, the water is discharged from the waste liquid tank according to the evaporation crystallization requirement, the redundant water can also flow back to the jacket reaction kettle, the smooth operation of the evaporation crystallization is ensured, and the evaporation crystallization efficiency is improved. And a large amount of separated waste water enters a waste liquid tank, can be properly treated subsequently, does not directly enter the environment, and avoids environmental pollution.
Drawings
Fig. 1 is a schematic view of the present invention.
Detailed Description
The invention will be further explained with reference to the drawings, without limiting its scope.
As shown in fig. 1, the device for producing urea phosphate by using wet-process phosphoric acid as a raw material according to the present invention specifically comprises a jacket reaction kettle (1), a wet-process phosphoric acid storage tank (3), a urea particle bin (4), a water carrying agent storage tank (6), a filter (7), a condensing heat exchanger (8), an oil-water phase separator (9), a first waste liquid storage tank (10), a second waste liquid storage tank (11), a return pipe (12), an I-th mass flowmeter (13), and an II-th mass flowmeter (14);
the top end of the jacket reaction kettle (1) is provided with 1 exhaust port guide pipe (101), the exhaust port guide pipe (101) is connected with a tube side steam inlet (801) of the vertically installed condensing heat exchanger (8) through a pipeline, and the top end of the oil-water phase separator (9) is connected with a shell side condensate outlet (803) of the vertically installed condensing heat exchanger (8) through a pipeline; the middle lower part of the oil-water phase separator (9) is connected with the jacket reaction kettle (1) through a pipeline provided with a return pipe (12); the return pipe (12) is a U-shaped or concave pipe, and the bottom of the return pipe (12) is connected with the first waste liquid storage tank (10) through a pipeline provided with an I-shaped mass flowmeter (13); the bottom end of the oil-water phase separator (9) is connected with a second waste liquid storage tank (11) through a pipeline provided with a second mass flowmeter (14); the bottom end of the second waste liquid storage tank (11) is connected with the jacket reaction kettle (1) through a pipeline provided with a third pump (203);
the wet-process phosphoric acid storage tank (3) is connected with the jacket reaction kettle (1) through a pipeline provided with an I pump (201); the water-carrying agent storage tank (6) is connected with the jacket reaction kettle (1) through a pipeline provided with a second pump (202); the urea particle bin (4) is connected with the jacket reaction kettle (1) through a pipeline provided with a spiral feeding pump (5); the bottom of the jacket reaction kettle (1) is connected with the filter (7) through a pipeline provided with a valve.
The jacket reaction kettle is a jacket stirring reaction kettle with controllable temperature.
The device for producing urea phosphate by using wet-process phosphoric acid as a raw material, which is related by the utility model, is described by combining specific process operation conditions, and the implementation process is as follows:
step one, setting the rotating speed of a jacket reaction kettle (1) to be 50 r/min under normal pressure, and adding wet-process phosphoric acid, dichloroethane and urea into the jacket reaction kettle (1) through an I pump (201), an II pump (202) and a spiral feed pump (5) respectively, wherein the adding quality of the urea is that P contained in the wet-process phosphoric acid in the jacket reaction kettle (1)2O50.9 times of the mass, the volume of the water-carrying agent S is equal to the H contained in the wet-process phosphoric acid in the jacket reaction kettle (1)21.0-5.0 times of the volume of O;
setting the temperature of the jacketed reaction kettle (1) to be 70-80 ℃, completely condensing steam generated in the jacketed reaction kettle (1) through a condensing heat exchanger (8), then entering an oil-water phase separator (9), separating the steam into an oil phase and a water phase, carrying out constant-temperature total reflux for 1 hour, and then carrying out constant-temperature partial reflux crystallization operation, wherein the total reflux refers to closing a mass flow meter I (13) and a mass flow meter II (14), and completely refluxing the oil phase and the water phase in the oil-water phase separator (9) into the jacketed reaction kettle (1), the partial reflux refers to completely refluxing the oil phase in the oil-water phase separator (9) into the jacketed reaction kettle (1) through the mass flow meter I (13), the mass flow meter II (14) and a pump III (203), controlling the extraction rate of the water phase in the oil-water phase separator (9) to be 1-10 m L/min, and refluxing the rest water phase into the jacketed reaction kettle (1);
step three, when the total volume of the water phase extracted from the oil-water phase separator (9) in the step two reaches the H contained in the wet-process phosphoric acid in the jacketed reaction kettle (1) in the step one2When the volume of O is 80%, the crystal slurry in the jacket reaction kettle (1) is led out to a filter (7) for solid-liquid separation, and filter cakes are washed and dried to obtain urea phosphate crystals.
The jacket reaction kettle (1) 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 30-32 wt%.
Claims (2)
1. A device for producing urea phosphate by taking wet-process phosphoric acid as a raw material is characterized by specifically comprising a jacket reaction kettle (1), a wet-process phosphoric acid storage tank (3), a urea particle storage bin (4), a water carrying agent storage tank (6), a filter (7), a condensing heat exchanger (8), an oil-water phase separator (9), a first waste liquid storage tank (10), a second waste liquid storage tank (11), a return pipe (12), an I mass flowmeter (13) and an II mass flowmeter (14);
the top end of the jacket reaction kettle (1) is provided with 1 exhaust port guide pipe (101), the exhaust port guide pipe (101) is connected with a tube side steam inlet (801) of the vertically installed condensing heat exchanger (8) through a pipeline, and the top end of the oil-water phase separator (9) is connected with a shell side condensate outlet (803) of the vertically installed condensing heat exchanger (8) through a pipeline; the middle lower part of the oil-water phase separator (9) is connected with the jacket reaction kettle (1) through a pipeline provided with a return pipe (12); the return pipe (12) is a U-shaped or concave pipe, and the bottom of the return pipe (12) is connected with the first waste liquid storage tank (10) through a pipeline provided with an I-shaped mass flowmeter (13); the bottom end of the oil-water phase separator (9) is connected with a second waste liquid storage tank (11) through a pipeline provided with a second mass flowmeter (14); the bottom end of the second waste liquid storage tank (11) is connected with the jacket reaction kettle (1) through a pipeline provided with a third pump (203);
the wet-process phosphoric acid storage tank (3) is connected with the jacket reaction kettle (1) through a pipeline provided with an I pump (201); the water-carrying agent storage tank (6) is connected with the jacket reaction kettle (1) through a pipeline provided with a second pump (202); the urea particle bin (4) is connected with the jacket reaction kettle (1) through a pipeline provided with a spiral feeding pump (5); the bottom of the jacket reaction kettle (1) is connected with the filter (7) through a pipeline provided with a valve.
2. The apparatus for producing urea phosphate by using wet-process phosphoric acid as raw material according to claim 1, wherein the jacketed reaction kettle is a temperature-controllable jacketed stirred reaction kettle.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201922183882.0U CN211078988U (en) | 2019-12-09 | 2019-12-09 | Device for producing urea phosphate by taking wet-process phosphoric acid as raw material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201922183882.0U CN211078988U (en) | 2019-12-09 | 2019-12-09 | Device for producing urea phosphate by taking wet-process phosphoric acid as raw material |
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| Publication Number | Publication Date |
|---|---|
| CN211078988U true CN211078988U (en) | 2020-07-24 |
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|---|---|---|---|
| CN201922183882.0U Expired - Fee Related CN211078988U (en) | 2019-12-09 | 2019-12-09 | Device for producing urea phosphate by taking wet-process phosphoric acid as raw material |
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|---|---|
| CN (1) | CN211078988U (en) |
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2019
- 2019-12-09 CN CN201922183882.0U patent/CN211078988U/en not_active Expired - Fee Related
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| Date | Code | Title | Description |
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| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| EE01 | Entry into force of recordation of patent licensing contract | ||
| EE01 | Entry into force of recordation of patent licensing contract |
Assignee: Wuhan University of science and Technology Business Incubator Co., Ltd Assignor: WUHAN University OF SCIENCE AND TECHNOLOGY Contract record no.: X2020420000008 Denomination of utility model: A device for producing urea phosphate from wet process phosphoric acid Granted publication date: 20200724 License type: Common License Record date: 20201022 |
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| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20200724 Termination date: 20201209 |