AU2020101431A4 - Method for co-producing monoammonium phosphate and diammonium phosphate by phosphoric acid and associated system - Google Patents
Method for co-producing monoammonium phosphate and diammonium phosphate by phosphoric acid and associated system Download PDFInfo
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- mother liquor
- neutralization
- phosphoric acid
- phosphate
- diammonium phosphate
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- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 title claims abstract description 158
- 239000005696 Diammonium phosphate Substances 0.000 title claims abstract description 95
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 title claims abstract description 95
- 229910000388 diammonium phosphate Inorganic materials 0.000 title claims abstract description 95
- 235000019838 diammonium phosphate Nutrition 0.000 title claims abstract description 95
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 title claims abstract description 93
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 title claims abstract description 93
- 235000019837 monoammonium phosphate Nutrition 0.000 title claims abstract description 93
- 239000006012 monoammonium phosphate Substances 0.000 title claims abstract description 93
- 229910000147 aluminium phosphate Inorganic materials 0.000 title claims abstract description 79
- 238000000034 method Methods 0.000 title claims abstract description 13
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 150
- 239000012452 mother liquor Substances 0.000 claims abstract description 136
- 239000007788 liquid Substances 0.000 claims abstract description 50
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 46
- 238000004519 manufacturing process Methods 0.000 claims abstract description 37
- 239000012047 saturated solution Substances 0.000 claims abstract description 24
- 238000002156 mixing Methods 0.000 claims abstract description 16
- 238000005406 washing Methods 0.000 claims description 21
- 238000003860 storage Methods 0.000 claims description 18
- 238000000926 separation method Methods 0.000 claims description 17
- 238000006243 chemical reaction Methods 0.000 claims description 16
- 239000002002 slurry Substances 0.000 claims description 8
- 229910000402 monopotassium phosphate Inorganic materials 0.000 claims description 3
- 235000019796 monopotassium phosphate Nutrition 0.000 claims description 3
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 claims description 3
- 239000007789 gas Substances 0.000 description 28
- 238000003756 stirring Methods 0.000 description 14
- 238000002425 crystallisation Methods 0.000 description 8
- 230000008025 crystallization Effects 0.000 description 8
- 239000002994 raw material Substances 0.000 description 6
- 239000000243 solution Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 description 4
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 230000008016 vaporization Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 238000003973 irrigation Methods 0.000 description 1
- 230000002262 irrigation Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/28—Ammonium phosphates
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Fertilizers (AREA)
- Treating Waste Gases (AREA)
- Paper (AREA)
- Gas Separation By Absorption (AREA)
Abstract
The present invention discloses a method for producing monoammonium phosphate and
diammonium phosphate by phosphoric acid, and the associated system. The method includes:
(1) mixing, reacting and solid-liquid separating monoammonium phosphate saturated solution,
liquid ammonia and phosphoric acid to obtain monoammonium phosphate product and
crystallized mother liquor I; mixing, reacting and solid-liquid separating diammonium
phosphate saturated solution, liquid ammonia and phosphoric acid to obtain diammonium
phosphate product and mother liquor II; (2) mixing, reacting and solid-liquid separating
mother liquor I, mother liquor II, liquid ammonia and phosphoric acid to obtain
monoammonium phosphate product and mother liquor I; mixing, reacting and solid-liquid
separating mother liquor II, liquid ammonia and phosphoric acid to obtain diammonium
phosphate product and mother liquor II; (3) repeating step (2) with the mother liquor I and the
mother liquor II obtained in step (2); wherein tail gas generated in the neutralization reaction
of diammonium phosphate in the steps (1) and (2) is washed and absorbed with phosphoric
acid. The method of the present invention achieves a balance in mother liquor and the
co-production of monoammonium phosphate and diammonium phosphate.
8ea~o~eie 62 ReaodeviceA
442 41
Figure1I
Description
8ea~o~eie 62 ReaodeviceA
442 41
Figure1I
[0001] The present application claims priority to Chinese Patent Application No. 201911294763.0, titled "METHOD FOR PRODUCING INDUSTRIAL-GRADE MONOAMMONIUM PHOSPHATE AND INDUSTRIAL-GRADE DIAMMONIUM PHOSPHATE BY WET-PROCESS PHOSPHORIC ACID AND ASSOCIATED SYSTEM", filed on December 16, 2019 with the State Intellectual Property Office of People's Republic of China, which is incorporated herein by reference in its entirety.
[0002] The present invention relates to the technical field of chemical industry, and specifically to a method for co-producing monoammonium phosphate and diammonium phosphate by phosphoric acid, and the associated system.
[0003] monoammonium phosphate and diammonium phosphate are widely used in various aspects of fire protection, drip irrigation fertilizer, medicine and food or the like. At present, a process by thermal phosphoric acid or purified phosphoric acid is generally employed in the production of monoammonium phosphate and diammonium phosphate, which has disadvantages of high production cost, complicated process, high energy consumption and large pollution. However, the existing production device and production process using a production process by phosphoric acid are relatively single, most of which can only produce monoammonium phosphate or diammonium phosphate, making it difficult to achieve the co-production of monoammonium phosphate and diammonium phosphate.
[0004] In view of this, the present application provides a method for co-producing monoammonium phosphate and diammonium phosphate by phosphoric acid, which achieves a balance in mother liquor and the co-production of monoammonium phosphate and diammonium phosphate, and the associated system.
[0005] In order to solve the above technical problems, the technical solution provided by the present application is a method for co-producing monoammonium phosphate and diammonium phosphate by phosphoric acid including:
[0006] (1)
[0007] mixing monoammonium phosphate saturated solution, liquid ammonia and phosphoric acid in a neutralization device A for the neutralization reaction of monoammonium phosphate, and solid-liquid separating to obtain monoammonium phosphate product and mother liquor I;
[0008] mixing diammonium phosphate saturated solution, liquid ammonia and phosphoric acid in a neutralization device B for the neutralization reaction of diammonium phosphate, and solid-liquid separating to obtain diammonium phosphate product and mother liquor II;
[0009] (2)
[0010] mixing mother liquor I, mother liquor II, liquid ammonia and phosphoric acid in the neutralization device A for the neutralization reaction of monoammonium phosphate, and solid-liquid separating to obtain monoammonium phosphate product and mother liquor I';
[0011] mixing mother liquor II, liquid ammonia and phosphoric acid in the neutralization device B for the neutralization reaction of diammonium phosphate, and solid-liquid separating to obtain diammonium phosphate product and mother liquor II';
[0012] (3) repeating step (2) with the mother liquor I' and the mother liquor II' obtained in step (2);
[0013] wherein,
[0014] tail gas generated in the neutralization reaction of diammonium phosphate in the steps (1) and (2) is washed and absorbed with phosphoric acid, and the absorbed slurry is sent to the neutralization device B.
[0015] Preferably, the remaining gas of the tail gas generated in the neutralization reaction of diammonium phosphate in the steps (1) and (2) after being washed and absorbed with phosphoric acid is discharged into a chimney.
[0016] Preferably, the tail gas generated in the neutralization reaction of monoammonium phosphate in the steps (1) and (2) is discharged into a chimney.
[0017] Preferably, in the steps (1) and (2), during the neutralization reaction of monoammonium phosphate, the liquid ammonia is added in a flow rate of 1300 KG/h to 1500 KG/h, and the phosphoric acid is added in an amount such that the pH value of the reaction process is controlled to be 3.5 to 4.0; and during the neutralization reaction of diammonium phosphate, the liquid ammonia is added in a flow rate of 800 KG/h to 900 KG/h, and the phosphoric acid is added in an amount such that the pH value of the reaction process is controlled to be 6.5 to 8.0.
[0018] Preferably, in the steps (1) and (2), the reaction temperature of the neutralization reaction is 108°C to 113°C for monoammonium phosphate, and 90°C to 95°C for diammoniumphosphate.
[0019] Preferably, in the step (1), the addition amount is 10 m3 to 11 m 3 for the monoammonium phosphate saturated solution, and 10 m 3 to 11 m 3 for the diammonium phosphate saturated solution.
[0020] Preferably, in the step (2), during the neutralization reaction of monoammonium phosphate, the addition amount is 30 m3/h for the mother liquor I, and 30 m 3/h for the mother liquor II; and during the neutralization reaction of diammonium phosphate, the addition amount of the mother liquor II is 30 m 3/h.
[0021] Preferably, in the steps (1) and (2), during the neutralization reaction of monoammonium phosphate, stirring is carried out at a stirring speed of 32 r/min; and during the neutralization reaction of diammonium phosphate, stirring is carried out at a stirring speed of 32 r/min.
[0022] The present invention further provides a system for co-producing monoammonium phosphate and diammonium phosphate by phosphoric acid including: a liquid ammonia delivery pipe, a phosphoric acid storage tank, a monoammonium phosphate production section, a potassium dihydrogen phosphate production section and a tail gas washing device;
[0023] wherein the monoammonium phosphate production section includes a neutralization device A, a solid-liquid separation device A and a mother liquor collection device A connected in sequence; the diammonium phosphate production section includes a neutralization device B, a solid-liquid separation device B and a mother liquor collection device B connected in sequence; the mother liquor collection device A is connected to the neutralization device A via a mother liquor I delivery pipe, and the mother liquor collection device B is connected to the neutralization device B and the mother liquor collection device A via a mother liquor II delivery pipe;
[0024] the liquid ammonia delivery pipe is connected to the neutralization device A and the neutralization device B, respectively; and the phosphoric acid storage tank is connected to the neutralization device A and the neutralization device B, respectively;
[0025] the tail gas washing device is connected to the neutralization device B, and the tail gas washing device is connected to the phosphoric acid storage tank through a circulation line.
[0026] Preferably, the neutralization device A and the tail gas washing device are connected to a chimney.
[0027] Preferably, a tail gas fan is provided between the neutralization device A and the chimney, and between the neutralization device B and the tail gas washing device.
[0028] Preferably, the neutralization device A and the neutralization device B are reaction kettles.
[0029] Preferably, the liquid inlet and the liquid outlet of the tail gas washing device are connected to the phosphoric acid storage tank.
[0030] The detailed description of the present application compared with the prior art is as follows.
[0031] In the system for producing monoammonium phosphate and diammonium phosphate by phosphoric acid of the present invention, the mother liquor collection device A is connected to the neutralization device A via the mother liquor I delivery pipe, and the mother liquor collection device B is connected to the neutralization device B and the mother liquor collection device A via the mother liquor II delivery pipe; the liquid ammonia delivery pipe is connected to the neutralization device A and the neutralization device B, respectively; and the phosphoric acid storage tank is connected to the neutralization device A and the neutralization device B, respectively. In the production method, monoammonium phosphate product and mother liquor I' are obtained after the neutralization reaction of monoammonium phosphate and solid-liquid separation, and the mother liquor I' is recycled as the raw material of the neutralization reaction of monoammonium phosphate. In the present invention, diammonium phosphate product and mother liquor II' are obtained after the neutralization reaction of diammonium phosphate and solid-liquid separation, and the mother liquor II' is recycled as the raw material for the neutralization reaction of diammonium phosphate and the neutralization reaction of monoammonium phosphate, achieving the recycle of the mother liquor and the recovery of the mother liquor. At the same time, due to the presence of ammonia gas overflowing from the tail gas generated in the neutralization reaction of diammonium phosphate, phosphoric acid is used to wash and absorb it, and the absorbed slurry is sent to the neutralization device B, so that the amount of liquid entering the diammonium phosphate production section is increased and the liquid is positively balanced. The neutralization reactions of monoammonium phosphate and diammonium phosphate in the present invention are exothermic reactions, and the evaporation of water vapor is large, and therefore the amount of liquid entering the monoammonium phosphate production section is low and the liquid is positively balanced. In the present invention, the mother liquor I' obtained after the neutralization reaction of diammonium phosphate and solid-liquid separation is recycled as the raw material for the neutralization reaction of diammonium phosphate and the neutralization reaction of monoammonium phosphate, increasing the inflow of the monoammonium phosphate production section and the outflow of the diammonium phosphate production section, and achieving a balance in mother liquor and the co-production of monoammonium phosphate and diammonium phosphate.
[0032] Further, firstly, the addition amounts of monoammonium phosphate saturated solution, diammonium phosphate saturated solution, liquid ammonia, phosphoric acid, mother liquor I' and mother liquor II' are controlled so as to prevent a large amount of liquid ammonia from vaporizing, avoid blockage of the pipeline due to excessive crystallization, improve the continuity of neutralization, achieve continuous crystallization, and improve production efficiency and safety. Secondly, the addition of mother liquor I' and mother liquor II' avoids the excessively high concentration of neutralization liquor which is unfavorable for stirring and the accuracy of pH value control, and avoids the excessively violent reaction between liquid ammonia and phosphoric acid which affects crystallization. Thirdly, the addition amounts of monoammonium phosphate saturated solution, diammonium phosphate saturated solution, liquid ammonia, phosphoric acid, mother liquor I' and mother liquor II' are controlled so as to ensure a balance in mother liquor and the co-prodution of monoammonium phosphate and diammonium phosphate.
[0033] Further, the stirring speed and temperature conditions are defined so as to ensure the crystallization of monoammonium phosphate and diammonium phosphate under an appropriate stirring speed and temperature conditions.
[0034] In order to explain the examples of the present invention or the technical solutions in the prior art more clearly, the drawings required in the description of examples or the prior art will be briefly introduced below. Obviously, the drawings described below are only some examples of the present invention. Those of ordinary skill in the art can obtain other drawings based on these drawings without paying any creative work.
[0035] Figure 1 is a schematic diagram of a system for producing monoammonium phosphate and diammonium phosphate by phosphoric acid of the present invention.
[0036] For a better understand of the technical solutions of the present invention by those skilled in the art, the present invention will be further described in detail below in combination with specific examples.
[0037] In the present invention, "mother liquor I" and "mother liquor I"', and "mother liquor I" and "mother liquorII"' respectively represent monoammonium phosphate solutions and diammonium phosphate solutions obtained in different steps, and they are given different names just for clarity.
[0038] Example 1
[0039] A method for producing monoammonium phosphate and diammonium phosphate by phosphoric acid includs:
[0040] (1)
[0041] mixing monoammonium phosphate saturated solution, liquid ammonia and phosphoric acid in a neutralization device A31 for the neutralization reaction of monoammonium phosphate, and solid-liquid separating to obtain monoammonium phosphate product and mother liquor I;
[0042] mixing diammonium phosphate saturated solution, liquid ammonia and phosphoric acid in a neutralization device B32 for the neutralization reaction of diammonium phosphate, and solid-liquid separating to obtain diammonium phosphate product and mother liquor II;
[00431 (2)
[0044] mixing mother liquor I, mother liquor II, liquid ammonia and phosphoric acid in the neutralization device A31 for the neutralization reaction of monoammonium phosphate, and solid-liquid separating to obtain monoammonium phosphate product and mother liquor I';
[0045] mixing mother liquor II, liquid ammonia and phosphoric acid in the neutralization device B32 for the neutralization reaction of diammonium phosphate, and solid-liquid separating to obtain diammonium phosphate product and mother liquor II';
[0046] (3) repeating step (2) by recycling the mother liquor I' and the mother liquor II 'obtained in step (2);
[0047] wherein,
[0048] tail gas generated in the neutralization reaction of diammonium phosphate in the steps (1) and (2) is washed and absorbed with phosphoric acid, and the absorbed slurry is sent to the neutralization device B32;
[0049] the remaining gas of the tail gas generated in the neutralization reaction of diammonium phosphate in the steps (1) and (2) after being washed and absorbed with phosphoric acid is discharged into a chimney 8;
[0050] the tail gas generated in the neutralization reaction of monoammonium phosphate in the steps (1) and (2) is discharged into the chimney 8;
[0051] in the steps (1) and (2), during the neutralization reaction of monoammonium phosphate, the liquid ammonia is added in a flow rate of 1300 KG/h to 1500 KG/h, and the phosphoric acid is added in an amount such that the pH value of the reaction process is controlled to be 3.5 to 4.0; and during the neutralization reaction of diammonium phosphate, the liquid ammonia is added in a flow rate of 800 KG/h to 900 KG/h, and the phosphoric acid is added in an amount such that the pH value of the reaction process is controlled to be 6.5 to 8.0;
[0052] in the steps (1) and (2), the reaction temperature of the neutralization reaction is 108°C to 113°C for monoammonium phosphate, and 90°C to 95°C for diammonium phosphate..
[0053] Preferably, in the step (1), the addition amount is 10 m3 to 11 m 3 for the monoammonium phosphate saturated solution, and 10 m 3 to 11 m 3 for the diammonium phosphate saturated solution;
[0054] in the step (2), during the neutralization reaction of monoammonium phosphate, the addition amount is 30 m3/h for the mother liquor I, and 30 m 3/h for the mother liquor II; and during the neutralization reaction of diammonium phosphate, the addition amount of the mother liquor II is 30 m3/h;
[0055] in the steps (1) and (2), during the neutralization reaction of monoammonium phosphate, stirring is carried out at a stirring speed of 32 r/min; and during the neutralization reaction of diammonium phosphate, stirring is carried out at a stirring speed of 32 r/min;
[0056] As shown in Figure 1, the present invention further provides the above-mentioned system for producing monoammonium phosphate and diammonium phosphate by phosphoric acid including: a liquid ammonia delivery pipe 1, a phosphoric acid storage tank 2, a monoammonium phosphate production section, a potassium dihydrogen phosphate production section and a tail gas washing device 7;
[0057] wherein the monoammonium phosphate production section includes a neutralization device A31, a solid-liquid separation device A41 and a mother liquor collection device A51 connected in sequence; the diammonium phosphate production section includes a neutralization device B32, a solid-liquid separation device B42 and a mother liquor collection device B52 connected in sequence; the mother liquor collection device A51 is connected to the neutralization device A31 via a mother liquor I delivery pipe 61, and the mother liquor -0 collection device B52 is connected to the neutralization device B32 and the mother liquor collection device A51 via a mother liquor II delivery pipe 62;
[0058] the liquid ammonia delivery pipe 1 is connected to the neutralization device A31 and the neutralization device B32, respectively; and the phosphoric acid storage tank 2 is connected to the neutralization device A31 and the neutralization device B32, respectively;
[0059] the tail gas washing device 7 is connected to the neutralization device B32, and the tail gas washing device 7 is connected to the phosphoric acid storage tank 2 through a circulation line 10;
[0060] the neutralization device A31 and the tail gas washing device 7 are connected to a chimney 8;
[0061] a tail gas fan 9 is provided between the neutralization device A31 and the chimney 8, and between the neutralization device B32 and the tail gas washing device 7.
[0062] The neutralization device A31 is a reaction kettle A, the neutralization device B32 is a reaction kettle B, the tail gas washing device 7 is a absorption tower; the solid-liquid separation device A41 and the solid-liquid separation device B42 are centrifugation separation device; and the mother liquor collection device A51 and the mother liquor collection device B52 are mother liquor collection tank.
[0063] The liquid inlet and the liquid outlet of the tail gas washing device 7 are connected to the phosphoric acid storage tank 2.
[0064] The obtained mother liquor I and mother liquor II are examined, and the results are as follows.
[0065] The mother liquor I' obtained in step (2) has a specific weight of 1.4 to 1.42, a phosphorus pentoxide content of 31 to 32 wt%, and a total nitrogen (calculated as N) content of 6 to 7 wt%, and the liquid volume of the mother liquor I' produced in step (2) is 8 to 9 m3 /h; the mother liquor II' obtained in step (2) has a specific weight of 1.35 to 1.38, a phosphorus pentoxide content of 31 to 32 wt%, and a total nitrogen (calculated as N) content of 11 to 12.5 wt%, and the liquid volume of the mother liquor II' produced in step (2) is 9 to 10 m3 /h.
[0066] In the present invention, the liquid ammonia delivery pipe 1 delivers liquid ammonia to the neutralization device A31 and the neutralization device B32, respectively; and the phosphoric acid storage tank 2 delivers phosphoric acid to the neutralization device A31 and the neutralization device B32, respectively;
[0067] monoammonium phosphate saturated solution, liquid ammonia and phosphoric acid are mixed in the neutralization device A31 for the neutralization reaction of monoammonium phosphate, and solid-liquid separated by the solid-liquid separation device A41 to obtain monoammonium phosphate product and mother liquor I; and the mother liquor I enters the mother liquor collection device A51;
[0068] diammonium phosphate saturated solution, liquid ammonia and phosphoric acid are mixed in the neutralization device B32 for the neutralization reaction of diammonium phosphate, and solid-liquid separated by the solid-liquid separation device B42 to obtain diammonium phosphate product and mother liquor II; and the mother liquor II enters the mother liquor collection device B52;
[0069] mother liquor I, mother liquor II, liquid ammonia and phosphoric acid are mixed in the neutralization device A31 for the neutralization reaction of monoammonium phosphate, and solid-liquid separated to obtain monoammonium phosphate product and mother liquor I';
[0070] the mother liquor I in the mother liquor collection device A51 is delivered to the neutralization device A31 via the mother liquor I delivery pipe 61, and the mother liquor II in the mother liquor collection device B52 is delivered to the neutralization device B32 and the mother liquor collection device A51 via the mother liquor II delivery pipe 62;
[0071] the phosphoric acid storage tank 2 delivers phosphoric acid to the tail gas washing device 7 for washing via the circulation line 10, and the tail gas from the neutralization reaction of diammonium phosphate in the neutralization device B32 is delivered to the tail gas washing device 7 via the fan, and is washed and absorbed by phosphoric acid, and the absorbed slurry is returned to the phosphoric acid storage tank 2 via the circulation line 10.
[0072] The delivery of the absorbed slurry to the neutralization device B32 as described above is specifically that the absorbed slurry is sent to the phosphoric acid storage tank 2, and the phosphoric acid in the phosphoric acid storage tank 2 is delivered to the neutralization device B32.
[0073] In the system for producing monoammonium phosphate and diammonium phosphate by phosphoric acid of the present invention, the mother liquor collection device A51 is connected to the neutralization device A31 via the mother liquor I delivery pipe 61, and the mother liquor collection device B52 is connected to the neutralization device B32 and the mother liquor collection device A51 via the mother liquor II delivery pipe 62; the liquid -0 ammonia delivery pipe 1 is connected to the neutralization device A31 and the neutralization device B32, respectively; and the phosphoric acid storage tank 2 is connected to the neutralization device A31 and the neutralization device B32, respectively. In the production method, monoammonium phosphate product and mother liquor I' are obtained after the neutralization reaction of monoammonium phosphate and solid-liquid separation, and the mother liquor I' is recycled as the raw material of the neutralization reaction of monoammonium phosphate. In the present invention, diammonium phosphate product and mother liquor II' are obtained after the neutralization reaction of diammonium phosphate and solid-liquid separation, and the mother liquor II' is recycled as the raw material for the neutralization reaction of diammonium phosphate and the neutralization reaction of monoammonium phosphate, achieving the recycle of the mother liquor and the recovery of the mother liquor. At the same time, due to the presence of ammonia gas overflowing from the tail gas generated in the neutralization reaction of diammonium phosphate, phosphoric acid is used to wash and absorb it, and the absorbed slurry is sent to the neutralization device B32, so that the amount of liquid entering the diammonium phosphate production section is increased and the liquid is positively balanced. The neutralization reactions of monoammonium phosphate and diammonium phosphate in the present invention are exothermic reactions, and the evaporation of water vapor is large, and therefore the amount of liquid entering the monoammonium phosphate production section is low and the liquid is positively balanced. In the present invention, the mother liquor I' obtained after the neutralization reaction of diammonium phosphate and solid-liquid separation is recycled as the raw material for the neutralization reaction of diammonium phosphate and the neutralization reaction of monoammonium phosphate, increasing the inflow of the monoammonium phosphate production section and the outflow of the diammonium phosphate production section, and achieving a balance in mother liquor and the co-production of monoammonium phosphate and diammonium phosphate.
[0074] Further, firstly, the addition amount of monoammonium phosphate saturated solution, diammonium phosphate saturated solution, liquid ammonia, phosphoric acid, mother liquor I and mother liquor II are controlled to prevent a large amount of liquid ammonia from vaporizing, avoid excessive crystallization result in blockage of the pipeline, improve the continuity of neutralization, achieve continuous crystallization, and improve production efficiency and safety. Secondly, the addition of mother liquor I and mother liquor II avoids the excessively high concentration of neutralization liquor, which is not conducive to stirring and the accuracy of pH value control, and avoids the excessively violent reaction between liquid ammonia and phosphoric acid, which affects crystallization. Thirdly, the addition amount of monoammonium phosphate saturated solution, diammonium phosphate saturated solution, liquid ammonia, phosphoric acid, mother liquor I and mother liquor II are controlled to ensure mother liquor balance.
[0075] Further, the stirring speed and temperature conditions are defined so as to ensure the crystallization of monoammonium phosphate and diammonium phosphate under an appropriate stirring speed and temperature conditions.
[0076] The above descriptions are only preferred embodiments of the present invention. It should be noted that the above preferred embodiments should not be regarded as limiting the present invention, and the protection scope of the present invention should be subject to the scope defined by the claims. A number of improvements and modifications can be made by those of ordinary skill in the art without departing from the spirit and scope of the present invention, which should also be regarded as the protection scope of the present invention.
Claims (4)
1. A method for co-producing monoammonium phosphate and diammonium phosphate, comprising:
(1)
mixing a monoammonium phosphate saturated solution, liquid ammonia and phosphoric acid in a neutralization device A for the neutralization reaction of monoammonium phosphate, and solid-liquid separating to obtain monoammonium phosphate product and mother liquor I;
mixing a diammonium phosphate saturated solution, liquid ammonia and phosphoric acid in a neutralization device B for the neutralization reaction of diammonium phosphate, and solid-liquid separating to obtain diammonium phosphate product and mother liquor II;
(2)
mixing the mother liquor I, the mother liquor II, liquid ammonia and phosphoric acid in the neutralization device A for the neutralization reaction of monoammonium phosphate, and solid-liquid separating to obtain the monoammonium phosphate product and a mother liquor I';
mixing the mother liquor II, liquid ammonia and phosphoric acid in the neutralization device B for the neutralization reaction of diammonium phosphate, and solid-liquid separating to obtain diammonium phosphate product and mother liquor II';
(3)
repeating step (2) with the mother liquor I' and the mother liquor II' obtained in step (2);
wherein,
tail gas generated in the neutralization reaction of diammonium phosphate in the steps (1) and (2) is washed and absorbed with phosphoric acid, and the absorbed slurry is sent to the neutralization device B
in the steps (1) and (2), during the neutralization reaction of monoammonium phosphate, the liquid ammonia is added in a flow rate of 1300 KG/h to 1500 KG/h, and the phosphoric acid is added in an amount such that the pH value of the reaction process is controlled to be 3.5 to 4.0; and during the neutralization reaction of diammonium phosphate, the liquid ammonia is added in a flow rate of 800 KG/h to 900 KG/h, and the phosphoric acid is added in an amount such that the pH value of the reaction process is controlled to be 6.5 to 8.0.
in the steps (1) and (2), the reaction temperature of the neutralization reaction is 108°C to 113°C for monoammonium phosphate, and 90°C to 95°C for diammonium phosphate.
wherein in the step (1), the addition amount is 10 m3 to 11 m 3 for the monoammonium phosphate saturated solution, and 10 m 3 to 11 m 3 for the diammonium phosphate saturated solution.
wherein in the step (2), during the neutralization reaction of monoammonium phosphate, the addition amount is 30 m3/h for the mother liquor I, and 30 m 3/h for the mother liquor II; and during the neutralization reaction of diammonium phosphate, the addition amount of the mother liquor II is 30 m3/h.
2. The method according to claim 1, wherein the remaining gas of the tail gas generated in the neutralization reaction of diammonium phosphate in the steps (1) and (2) after being washed and absorbed with phosphoric acid is discharged into a chimney.
3. The method according to claim 1, wherein the tail gas generated in the neutralization reaction of monoammonium phosphate in the steps (1) and (2) is discharged into a chimney.
4. A system for co-producing monoammonium phosphate and diammonium phosphate by phosphoric acid, including: a liquid ammonia delivery pipe, a phosphoric acid storage tank, a monoammonium phosphate production section, a potassium dihydrogen phosphate production section and a tail gas washing device;
wherein the monoammonium phosphate production section includes a neutralization device A, a solid-liquid separation device A and a mother liquor collection device A connected in sequence; the diammonium phosphate production section includes a neutralization device B, a solid-liquid separation device B and a mother liquor collection device B connected in sequence; the mother liquor collection device A is connected to the neutralization device A via a mother liquor I delivery pipe, and the mother liquor collection device B is connected to the neutralization device B and the mother liquor collection device A via a mother liquor II delivery pipe;
the liquid ammonia delivery pipe is connected to the neutralization device A and the neutralization device B, respectively; and the phosphoric acid storage tank is connected to the neutralization device A and the neutralization device B, respectively; the tail gas washing device is connected to the neutralization device B, and the tail gas washing device is connected to the phosphoric acid storage tank through a circulation line; wherein the neutralization device A and the tail gas washing device are connected to a chimney; and a tail gas fan is provided between the neutralization device A and the chimney, and between the neutralization device B and the tail gas washing device.
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| CN201911294763.0 | 2019-12-16 | ||
| CN201911294763.0A CN110877901B (en) | 2019-12-16 | 2019-12-16 | Method and system for producing industrial-grade monoammonium phosphate and industrial-grade diammonium phosphate by wet-process phosphoric acid |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4239739A (en) * | 1979-11-06 | 1980-12-16 | Tennessee Valley Authority | Manufacture of purified diammonium phosphate |
| US4236911A (en) * | 1979-11-08 | 1980-12-02 | Tennessee Valley Authority | Purification and conversion of phosphoric acid to ammonium phosphates |
| JPS60204609A (en) * | 1984-03-28 | 1985-10-16 | Chisso Corp | Method for producing purified diammonium phosphate from wet-process phosphoric acid |
| US4610853A (en) * | 1985-03-08 | 1986-09-09 | Chisso Corporation | Process for producing purified monoammonium phosphate from wet process phosphoric acid |
| CN101337664A (en) * | 2008-08-11 | 2009-01-07 | 湖北祥云(集团)化工股份有限公司 | Process for co-producing diammonium phosphate and monoammonium phosphate by slurry concentration method |
| CN101857213B (en) * | 2010-06-04 | 2013-02-20 | 广西钦州桂金诺磷化工有限公司 | Method for preparing food-grade diammonium phosphate from wet-process phosphoric acid |
| CN101857210B (en) * | 2010-06-04 | 2012-02-15 | 广西钦州桂金诺磷化工有限公司 | Method for producing industrial grade diammonium phosphate from wet-process phosphoric acid |
| SE536607C2 (en) | 2012-06-21 | 2014-03-25 | Easymining Sweden Ab | Preparation of ammonium phosphates |
| CN103011113B (en) * | 2012-12-25 | 2015-05-20 | 贵州开磷（集团）有限责任公司 | Method for co-producing industrial grade diammonium phosphate during production of industrial grade monoammonium phosphate of phosphoric acid by wet process |
| CN103058157A (en) * | 2013-02-26 | 2013-04-24 | 贵州开磷（集团）有限责任公司 | Production method of industrial grade diammonium phosphate with wet-process phosphoric acid |
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| CN110877901B (en) | 2023-02-28 |
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