CN111138490A - Method for preparing n-butyl thiophosphoric triamide and integrated device thereof - Google Patents
Method for preparing n-butyl thiophosphoric triamide and integrated device thereof Download PDFInfo
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- CN111138490A CN111138490A CN202010155485.7A CN202010155485A CN111138490A CN 111138490 A CN111138490 A CN 111138490A CN 202010155485 A CN202010155485 A CN 202010155485A CN 111138490 A CN111138490 A CN 111138490A
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- butylamine
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- HEPPIYNOUFWEPP-UHFFFAOYSA-N n-diaminophosphinothioylbutan-1-amine Chemical compound CCCCNP(N)(N)=S HEPPIYNOUFWEPP-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 30
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 217
- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 claims abstract description 117
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 73
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims abstract description 63
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 189
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 78
- FNGLQNMQHOAIJQ-UHFFFAOYSA-N Cl[S](Cl)Cl Chemical compound Cl[S](Cl)Cl FNGLQNMQHOAIJQ-UHFFFAOYSA-N 0.000 claims description 43
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 42
- 229910052757 nitrogen Inorganic materials 0.000 claims description 39
- 238000003756 stirring Methods 0.000 claims description 30
- 238000002156 mixing Methods 0.000 claims description 26
- 238000012546 transfer Methods 0.000 claims description 24
- 239000000463 material Substances 0.000 claims description 21
- BMDVPRGEZHHGLJ-UHFFFAOYSA-N [S](Cl)(Cl)Cl.[P] Chemical compound [S](Cl)(Cl)Cl.[P] BMDVPRGEZHHGLJ-UHFFFAOYSA-N 0.000 claims description 15
- 230000000007 visual effect Effects 0.000 claims description 8
- 238000002360 preparation method Methods 0.000 claims description 5
- 239000012267 brine Substances 0.000 claims description 4
- 230000001276 controlling effect Effects 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 230000001105 regulatory effect Effects 0.000 claims description 4
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims description 4
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 3
- 239000012295 chemical reaction liquid Substances 0.000 claims description 2
- 239000000243 solution Substances 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 239000011148 porous material Substances 0.000 claims 3
- 239000000543 intermediate Substances 0.000 abstract description 33
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 239000003337 fertilizer Substances 0.000 abstract description 2
- 239000004973 liquid crystal related substance Substances 0.000 abstract description 2
- 239000012450 pharmaceutical intermediate Substances 0.000 abstract description 2
- 150000003839 salts Chemical class 0.000 description 8
- 238000007599 discharging Methods 0.000 description 3
- 238000009434 installation Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- FAIAAWCVCHQXDN-UHFFFAOYSA-N phosphorus trichloride Chemical compound ClP(Cl)Cl FAIAAWCVCHQXDN-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/06—Phosphorus compounds without P—C bonds
- C07F9/22—Amides of acids of phosphorus
- C07F9/224—Phosphorus triamides
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for preparing N-butyl thiophosphoryl triamide and an integrated device thereof, belonging to the technical field of producing high-efficiency green slow-release fertilizer synergists, liquid crystal intermediates and pharmaceutical intermediates, and mainly comprising the steps of generating N-N-butyl dichlorophos through the reaction of trichlorothion and N-butyl amine, and generating a target product N-butyl thiophosphoryl triamide through the reaction of the N-N-butyl dichlorophos and liquid ammonia, and particularly relating to a method for preparing the trichlorothion and a device thereof, wherein the core content and the technical scheme are that a novel ammoniation method production process technical flow is adopted on the basis of the existing method for preparing the N-butyl thiophosphoryl triamide, a liquid ammonia feeding and limiting orifice plate is added, the flow of ammonia fed into an ammonia feeding kettle is effectively controlled, a liquid ammonia metering tank is added, the quality of the ammonia fed into the ammonia feeding kettle is effectively controlled, a batching kettle, effectively controlling the reaction temperature in the n-butyl kettle, and achieving the purposes of complete process reaction, good product stability and low unit cost.
Description
Technical Field
The invention belongs to the technical field of production of efficient green slow-release fertilizer synergists, liquid crystal intermediates and pharmaceutical intermediates, and particularly relates to a method for preparing n-butyl thiophosphoryl triamide and an integrated device thereof.
Background
At present, the preparation of n-butyl thiophosphoric triamide (NBPT) at home and abroad has the defects of incomplete process reaction, poor production stability and continuity, high unit cost, manual operation and poor safety performance.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: aiming at the problems in the background technology, a novel ammoniation method production process technical flow is adopted on the basis of the existing preparation method of the n-butyl thiophosphoric triamide, liquid ammonia is added to be introduced into a flow limiting orifice plate, the flow of ammonia introduced into an ammonia introduction kettle is effectively controlled, a liquid ammonia metering tank is added, the quality of the ammonia introduced into the ammonia introduction kettle is effectively controlled, a batching kettle is added, materials in the batching kettle are precooled, the reaction temperature in the n-butyl kettle is effectively controlled, and the purposes of complete process reaction, good product stability and low unit cost are achieved.
The scheme of the invention for specifically solving the background technical problems is as follows: a method for preparing n-butyl thiophosphoric triamide and an integrated device thereof are characterized in that: the n-butyl thiophosphoryl triamide integrated device is composed of a first n-butylamine conveying pump, a first n-butylamine conveying pump outlet pipe, a first n-butylamine conveying pump outlet valve, an n-butylamine intermediate tank, a second n-butylamine conveying pump inlet valve, a burdening kettle ice salt water inlet pipe, a burdening kettle ice salt water inlet valve, an ammonia-introducing kettle nitrogen inlet pipe, a burdening kettle nitrogen inlet pipe, a nitrogen buffer tank, a nitrogen outlet three-way valve, a transfer pump outlet pipe, a burdening kettle jacket, a dichloromethane conveying pump outlet pipe, a burdening kettle stirring motor device, a burdening kettle visual cup, a burdening kettle connecting pipe, a burdening kettle connecting and adjusting valve, a burdening kettle inlet pipe, a burdening kettle inlet valve, an n-butylamine head tank outlet pipe, a dichloromethane metering tank, an n-butylamine head tank, a dichloromethane metering tank inlet valve, an n-butylamine head tank inlet valve, trichlorothion elevated tank inlet pipe, trichlorothion delivery pump, n-butylamine elevated tank outlet valve, trichlorothion elevated tank outlet pipe, trichlorothion elevated tank outlet valve, dichloromethane metering tank bottom left outlet pipe, batching kettle, dichloromethane metering tank bottom left outlet valve, n-butyl kettle jacket, n-butyl kettle viewing cup, n-butyl kettle stirring motor device, n-butyl kettle ice salt inlet pipe, n-butyl kettle outlet valve, n-butyl kettle outlet pipe, n-butyl kettle ice salt inlet valve, material transfer pump, ammonia kettle ice salt inlet pipe, ammonia kettle jacket, ammonia kettle ice salt inlet three-way valve, trichlorothion intermediate tank outlet valve, n-butyl thiophosphoryl triamide discharge pipe, ice salt water pump, trichlorothion-butyl thiophosphoryl triamide discharge valve, ammonia kettle stirring motor device, ammonia kettle liquid ammonia inlet pipe, flow limiting orifice plate, liquid ammonia outlet valve, ammonia liquid, The device comprises a liquid ammonia blowdown valve, a liquid ammonia intermediate tank, a liquid ammonia delivery pump outlet pipe, a liquid ammonia delivery pump outlet valve, a liquid ammonia delivery pump inlet pipe, a second n-butylamine delivery pump inlet pipe, a trichloro-sulfur intermediate tank outlet pipe and a trichloro-sulfur elevated tank.
The method for preparing n-butyl thiophosphoric triamide and the integrated device thereof comprise a core device, a dosing kettle, a n-butyl kettle and an ammonia introducing kettle, wherein a dosing kettle nitrogen inlet pipe, a dosing kettle feed pipe and an n-butylamine elevated tank outlet pipe are arranged at the top end of a dosing kettle of the core device, the dosing kettle nitrogen inlet pipe at the top end of the dosing kettle is communicated with a nitrogen buffer tank through a nitrogen outlet three-way valve, the dosing kettle feed pipe at the top end of the dosing kettle is communicated with a dichloromethane metering tank through a dosing kettle feed valve, the dichloromethane metering tank inlet valve is arranged at the top end of the dichloromethane metering tank and is communicated with a dichloromethane delivery pump through a dichloromethane delivery pump outlet pipe, the n-butylamine elevated tank outlet pipe at the top end of the dosing kettle is communicated with the n-butylamine elevated tank through an n-butylamine elevated tank outlet valve, the n-butylamine elevated tank inlet pipe, a n-butylamine delivery pump inlet pipe, a, An inlet pipe of a second n-butylamine conveying pump, an inlet valve of a second n-butylamine conveying pump and an n-butylamine intermediate tank are communicated, the n-butylamine intermediate tank is communicated with a first n-butylamine conveying pump outlet pipe, a first n-butylamine conveying pump outlet valve and a first n-butylamine conveying pump, a blending kettle connecting pipe is installed on the left side surface of a blending kettle and is communicated with the n-butyl kettle through a blending kettle connecting adjusting valve, a blending kettle visual cup and a blending kettle icy salt inlet pipe are installed on the right side surface of the blending kettle, the blending kettle icy salt inlet pipe is communicated with an icy salt water pump through a blending kettle icy salt inlet valve, a blending kettle stirring motor device is installed in the middle of the bottom of the blending kettle, a trichlorothion head tank outlet valve and a dichloromethane metering tank bottom left side outlet valve are installed at the top end of the second n-butyl kettle of the core equipment, and the dichloromethane metering tank, an outlet valve of a trichlorothion elevated tank is communicated with the trichlorothion elevated tank through an outlet pipe of the trichlorothion elevated tank, the trichlorothion elevated tank is communicated with a trichlorothion intermediate tank through an inlet valve of the trichlorothion elevated tank, an inlet pipe of the trichlorothion elevated tank, a trichlorothion delivery pump, an outlet pipe of the trichlorothion intermediate tank, an outlet valve of the trichlorothion intermediate tank and the trichlorothion intermediate tank, a matching kettle connecting pipe is arranged on the right side of a normal-butyl kettle and is communicated with a batching kettle through a matching kettle connecting regulating valve, the left side of the normal-butyl kettle is provided with a normal-butyl kettle visual cup, a normal-butyl kettle icy salt inlet pipe and a normal-butyl kettle outlet pipe, the normal-butyl kettle icy salt inlet pipe is communicated with an icy salt water pump through a normal-butyl kettle outlet valve, a material transfer pump is arranged in the middle of the bottom of the normal-butyl kettle and is communicated with the top of an ammonia-, the ammonia introducing kettle comprises an ammonia introducing kettle ice salt inlet pipe and an n-butyl thiophosphoric triamide discharging pipe, wherein the left side of the ammonia introducing kettle is provided with the ammonia introducing kettle ice salt inlet pipe and is communicated with an ice salt water pump through an ammonia introducing kettle ice salt water inlet three-way valve, the n-butyl thiophosphoric triamide discharging pipe enters the next process through an n-butyl thiophosphoric triamide discharging valve, the right side of the ammonia introducing kettle is provided with an ammonia introducing kettle nitrogen inlet pipe and is communicated with a nitrogen buffer tank through a nitrogen outlet three-way valve, the right middle of the bottom of the ammonia introducing kettle is provided with an ammonia introducing kettle stirring motor device, the right side of the bottom of the ammonia introducing kettle is provided with an ammonia introducing kettle liquid ammonia inlet pipe and is communicated with a liquid ammonia intermediate tank through a flow limiting orifice plate, a liquid ammonia outlet pipe valve is communicated with a liquid ammonia intermediate tank, the left lower.
Furthermore, the pipeline, the valve, the pump and the orifice plate are all known standard parts and common parts, the functions are also known, and the shape, the structure and the installation method are set by a user and do not belong to the protection scope of the patent.
Furthermore, the exterior of the batching kettle, the n-butyl kettle and the ammonia introducing kettle is cylindrical, the inner wall of the cylinder body is provided with a jacket and is also hollow cylindrical, the structure and the installation method of the device are set by a user, and the device does not belong to the protection scope of the patent.
Furthermore, the exterior of each intermediate tank, the dichloromethane metering tank, the nitrogen buffer tank and each head tank is in a cylinder shape, and is a known standard component, the function is also known, and the shape, the structure and the installation method are set by a user, so that the device does not belong to the protection scope of the patent.
The working principle of the invention is as follows:
the trichloro-sulfur phosphorus reacts with N-butylamine to generate N-N-butyl dichloro-sulfur phosphorus, the N-N-butyl dichloro-sulfur phosphorus reacts with liquid ammonia to generate a target product N-butyl thiophosphoryl triamide (NBPT), and the reaction equation is as follows:
the invention has the beneficial effects that: the process design is reasonable, the unit cost is saved, the production reaction is complete, the product stability and the production continuity are good, and the energy is saved and the environment is protected.
Drawings
The invention is further illustrated with reference to the figures and examples.
FIG. 1 is a process scheme flow chart of a method for preparing n-butyl thiophosphoric triamide and an integrated device thereof.
In fig. 1, the reference numerals mean: 1. a n-butylamine transport pump; 2. an outlet pipe of a first n-butylamine transfer pump; 3. an outlet valve of a first n-butylamine transfer pump; 4. a n-butylamine intermediate tank; 5. an inlet valve of a second n-butylamine conveying pump; 6. a water inlet pipe for ice salt in the batching kettle; 7. a water inlet valve for ice salt in the batching kettle; 8. introducing a nitrogen inlet pipe of an ammonia kettle; 9. a nitrogen inlet pipe of the batching kettle; 10. a nitrogen buffer tank; 11. a nitrogen outlet three-way valve; 12. an outlet pipe of the material transferring pump; 13. a material mixing kettle jacket; 14. a dichloromethane delivery pump; 15. a dichloromethane delivery pump outlet pipe; 16. a batching kettle stirring motor device; 17. a material mixing kettle visual cup; 18. a connecting pipe of the alignment kettle is arranged; 19. the positive preparation kettle is connected with the regulating valve; 20. a feeding pipe of the batching kettle; 21. a feed valve of the batching kettle; 22. an outlet pipe of the n-butylamine elevated tank; 23. a dichloromethane metering tank; 24. a n-butylamine head tank; 25. a dichloromethane metering tank inlet valve; 26. an inlet valve of the n-butylamine elevated tank; 27. an n-butylamine elevated tank inlet pipe; 28. an inlet valve of the trichloro sulfur phosphorus elevated tank; 29. an inlet pipe of a trichloro sulfur phosphorus elevated tank; 30. a phosphorus trichloride delivery pump; 31. an outlet valve of the n-butylamine head tank; 32. an outlet pipe of the trichloro sulfur phosphorus elevated tank; 33. an outlet valve of the trichlorothion head tank; 34. a left outlet pipe at the bottom of the dichloromethane metering tank; 35. a batching kettle; 36. a left outlet valve at the bottom of the dichloromethane metering tank; 37. n-butyl kettle; 38. a n-butyl kettle jacket; 39. a visual cup of the n-butyl kettle; 40. a stirring motor device of the n-butyl kettle; 41. a salt water inlet pipe is arranged in the n-butyl kettle; 42. an outlet valve of the n-butyl kettle; 43. an outlet pipe of the n-butyl kettle; 44. an ice salt water inlet valve of the n-butyl kettle; 45. a material transferring pump; 46. introducing ammonia into the kettle; 47. an ammonia kettle ice salt water inlet pipe is introduced; 48. introducing an ammonia kettle jacket; 49. an ammonia kettle ice salt water inlet three-way valve is introduced; 50. an outlet valve of the trichlorothion intermediate tank; 51. a discharge pipe of n-butyl thiophosphoric triamide; 52. an ice brine pump; 53. a trichloro sulfur phosphorus intermediate tank; 54. a discharge valve of n-butyl thiophosphoric triamide; 55. an ammonia kettle stirring motor device; 56. introducing ammonia kettle liquid ammonia into a pipe; 57. a restriction orifice plate; 58. a liquid ammonia outlet pipe valve; 59. a liquid ammonia blowdown valve; 60. a liquid ammonia intermediate tank; 61. an outlet pipe of the liquid ammonia delivery pump; 62. an outlet valve of the liquid ammonia delivery pump; 63. a liquid ammonia transfer pump; 64. an inlet pipe of a liquid ammonia delivery pump; 65. a second n-butylamine transfer pump; 66. an inlet pipe of a second n-butylamine conveying pump; 67. an outlet pipe of the trichloro sulfur phosphorus intermediate tank; 68. a trichloro sulfur phosphorus elevated tank.
Detailed Description
The invention is further described with reference to the following figures and specific examples.
In the attached figure 1, a method for preparing n-butyl thiophosphoric triamide and an integrated device thereof comprise a core device, a dosing kettle 35, a n-butyl kettle 37 and an ammonia introducing kettle 46, wherein the exterior of one of the core devices, the dosing kettle 35, is in a cylinder shape, the inner wall of the cylinder is provided with a dosing kettle jacket 13 which is also in a hollow cylinder shape, the top end of the dosing kettle 35 is provided with a dosing kettle nitrogen inlet pipe 9, a dosing kettle feed pipe 20 and a n-butyl amine elevated tank outlet pipe 22, the dosing kettle nitrogen inlet pipe 9 at the top end of the dosing kettle 35 is communicated with a nitrogen buffer tank 10 through a nitrogen outlet three-way valve 11, the dosing kettle feed pipe 20 at the top end of the dosing kettle 35 is communicated with a dichloromethane metering tank 23 through a dosing kettle feed valve 21, the top end of the dichloromethane metering tank 23 is provided with a dichloromethane metering tank valve 25 and is communicated with a dichloromethane delivery pump outlet pipe 15 and a dichloromethane delivery pump 14 through a dichloromethane delivery pump, and the n-butyl amine elevated The tank 24 is communicated, the n-butylamine elevated tank 24 is communicated with the n-butylamine intermediate tank 4 through an n-butylamine elevated tank inlet valve 26, an n-butylamine elevated tank inlet pipe 27, a second n-butylamine conveying pump 65, a second n-butylamine conveying pump inlet pipe 66, a second n-butylamine conveying pump inlet valve 5, the n-butylamine intermediate tank 4 is communicated with the n-butylamine intermediate tank 4 through a first n-butylamine conveying pump outlet pipe 2, a first n-butylamine conveying pump outlet valve 3 and a first n-butylamine conveying pump 1, a burdening kettle connecting pipe 18 is installed on the left side surface of the burdening kettle 35 and is communicated with the n-butylamine kettle 37 through a burdening kettle connecting adjusting valve 19, a burdening kettle viewing cup 17 and a burdening kettle ice salt water inlet pipe 6 are installed on the right side surface of the burdening kettle 35, the burdening kettle ice salt water inlet pipe 6 is communicated with an ice salt water pump 52 through a burdening kettle ice salt water inlet; the outside of the two n-butyl kettles 37 of the core equipment is in a cylindrical shape, the inner wall of the cylinder body is provided with an n-butyl kettle jacket 38 and is also in a hollow cylindrical shape, the top end of the n-butyl kettle 37 is provided with a trichlorosulfur elevated tank outlet valve 33 and a dichloromethane metering tank bottom left outlet valve 36, the dichloromethane metering tank bottom left outlet valve 36 is communicated with a dichloromethane metering tank 23 through a dichloromethane metering tank bottom left outlet pipe 34, the trichlorosulfur elevated tank outlet valve 33 is communicated with a trichlorosulfur elevated tank 68 through a trichlorosulfur elevated tank outlet pipe 32, the trichlorosulfur elevated tank 68 is communicated with a trichlorosulfur elevated tank inlet valve 28, a trichlorosulfur elevated tank inlet pipe 29, a trichlorosulfur transfer pump 30, a trichlorosulfur intermediate tank outlet pipe 67, a trichlorosulfur intermediate tank outlet valve 50 and a trichlorosulfur intermediate tank 53, the right side of the n-butyl kettle 37 is provided with a correction kettle connecting pipe 18 and is communicated with a batching kettle, a n-butyl kettle visual cup 39, a n-butyl kettle ice salt water inlet pipe 41 and a n-butyl kettle outlet pipe 43 are arranged on the left side of the n-butyl kettle 37, the n-butyl kettle ice salt water inlet pipe 41 is communicated with an ice salt water pump 52 through a n-butyl kettle ice salt water inlet valve 44, the n-butyl kettle outlet pipe 43 is communicated with the top of an ammonia introducing kettle 46 through a n-butyl kettle outlet valve 42 and a material transferring pump 45 through a material transferring pump outlet pipe 12, and a n-butyl stirring motor device 40 is arranged in the middle of the bottom of the; the outside of a three-way ammonia kettle 46 device of a core device is in a cylinder shape, the inner wall of a cylinder body is provided with an ammonia kettle jacket 48 and is also in a hollow cylinder shape, the top of the ammonia kettle 46 is provided with a material transfer pump outlet pipe 12 which is communicated with a normal butyl kettle 37 through a material transfer pump 45, the left side of the ammonia kettle 46 is provided with an ammonia kettle ice salt inlet pipe 47 and a normal butyl thiophosphoric triamide discharge pipe 51, the ammonia kettle ice salt inlet pipe 47 is communicated with an ice salt water pump 52 through an ammonia kettle ice salt water inlet three-way valve 49, the normal butyl thiophosphoric triamide discharge pipe 51 enters the next working procedure through a normal butyl thiophosphoric triamide discharge valve 54, the right side of the ammonia kettle 46 is provided with an ammonia kettle nitrogen inlet pipe 8 and is communicated with a nitrogen buffer tank 10 through a nitrogen outlet three-way valve 11, the right middle of the bottom of the ammonia kettle 46 is provided with an ammonia kettle stirring motor device 55, the right of the bottom is provided with an, and a liquid ammonia blow-down valve 59 is arranged on the left lower side of the liquid ammonia intermediate tank 60, and a liquid ammonia delivery pump outlet pipe 61 is arranged on the right lower side of the liquid ammonia intermediate tank 60 and is communicated with the liquid ammonia delivery pump outlet valve 62, the liquid ammonia delivery pump 63 and a liquid ammonia delivery pump inlet pipe 64 through the previous working procedures.
The specific implementation method of the invention comprises the following steps:
n-butylamine from an n-butylamine tank area is pumped into an n-butylamine intermediate tank 4 through a first n-butylamine conveying pump 1, a first n-butylamine conveying pump outlet pipe 2 and a first n-butylamine conveying pump outlet valve 3, n-butylamine in the n-butylamine intermediate tank 4 is pumped into an n-butylamine elevated tank 24 through an n-butylamine elevated tank inlet pipe 27 and an n-butylamine elevated tank inlet valve 26 through a second n-butylamine conveying pump 65 and a second n-butylamine conveying pump inlet pipe 66 and then 264kg of n-butylamine for standby.
Methylene dichloride (solvent) from the methylene dichloride tank field is pumped into a methylene dichloride metering tank 23 (about 2500L) by a methylene dichloride conveying pump 14 through a methylene dichloride conveying pump outlet pipe 15 and a methylene dichloride metering tank inlet valve 25 for standby. The trichloro-sulfur phosphorus from the preparation process of trichloro-sulfur phosphorus is delivered from a trichloro-sulfur intermediate tank 53 through a trichloro-sulfur transfer pump 30, through an inlet pipe 29 of a trichloro-sulfur elevated tank, through an inlet valve 28 of the trichloro-sulfur elevated tank, and then is pumped into a trichloro-sulfur elevated tank 68 (about 600kg) for standby.
Opening a 3000L stirring motor device 16 of the batching kettle and a fully-opened batching kettle ice salt water inlet valve 7, opening an outlet valve 31 of a n-butylamine elevated tank to enable 264kg of n-butylamine to automatically flow to the batching kettle 35 from the n-butylamine elevated tank 24, opening a batching kettle feed valve 21 to enable 2500L of dichloromethane to automatically flow to the batching kettle 35 from a dichloromethane metering tank 23, stirring and cooling to 0 ℃, closing the batching kettle stirring motor device 16, and standing for later use.
Opening 6300L n-butyl kettle stirring motor device 40, fully opening n-butyl kettle ice salt water inlet valve 44 on ice salt water pipeline of n-butyl kettle jacket 38, opening trichloro-sulfur high-level tank outlet valve 33 to enable 600kg of trichloro-sulfur to automatically flow from trichloro-sulfur high-level tank 68 to n-butyl kettle 37, opening left outlet valve 36 at bottom of dichloromethane metering tank to enable 2500L of dichloromethane to automatically flow from dichloromethane metering tank 23 to n-butyl kettle 37, stirring and cooling to 8 ℃. Opening a nitrogen outlet three-way valve 11 on a nitrogen pipeline of the batching kettle, adjusting a batching kettle connecting adjusting valve 19 on a collecting pipeline of the batching kettle 35, observing through a batching visual cup 17, dripping the n-butylamine solution prepared in the batching kettle 35 into the n-butyl kettle 37 through a batching kettle connecting pipe 18, controlling the temperature of the n-butyl kettle to be not higher than 12 ℃, continuing stirring for 10min after finishing dripping for about 2h, closing a n-butyl kettle stirring motor device 40 and a batching kettle ice salt water inlet valve 7, and preparing for material transferring.
Liquid ammonia (318kg) from a liquid ammonia tank area is pumped into a liquid ammonia intermediate tank 60 through a liquid ammonia transfer pump 63, a liquid ammonia transfer pump outlet pipe 61 and a liquid ammonia transfer pump outlet valve 62, and the temperature and pressure ranges (0-30 ℃, 0.43-1.17 MPa) are controlled for standby.
The nitrogen replaces the ammonia introducing kettle 46, the reaction liquid in the n-butyl kettle 37 is transferred into the 6300L ammonia introducing kettle 46 through the material transferring pump 45 and the material transferring pump outlet pipe 12, the stirring motor device 55 of the ammonia introducing kettle is started, the three-way valve 49 of the ammonia introducing kettle ice salt water inlet on the jacket 48 of the ammonia introducing kettle is opened completely, the temperature is controlled to be 15-25 ℃, the pressure in the ammonia introducing kettle 46 is not higher than 0.1MPa, the liquid ammonia from the liquid ammonia intermediate tank 60 passes through the liquid ammonia outlet pipe valve 58 and the flow limiting orifice 57 and then enters the ammonia introducing kettle 46 from the bottom of the ammonia introducing kettle 46 through the liquid ammonia inlet pipe 56 at the speed of 60-100kg/h, and 318kg of liquid ammonia which is measured is introduced.
The above description is only exemplary of the invention and should not be taken as limiting the invention, as any modification, equivalent replacement or improvement made within the spirit and principle of the invention should be included in the protection scope of the invention.
Claims (3)
1. A method for preparing n-butyl thiophosphoric triamide and an integrated device thereof are characterized in that: the device is characterized by comprising a first n-butylamine conveying pump (1), a first n-butylamine conveying pump outlet pipe (2), a first n-butylamine conveying pump outlet valve (3), a n-butylamine intermediate tank (4), a second n-butylamine conveying pump inlet valve (5), a batching kettle ice salt inlet pipe (6), a batching kettle ice salt inlet valve (7), an ammonia-introducing kettle nitrogen inlet pipe (8), a batching kettle nitrogen inlet pipe (9), a nitrogen buffer tank (10), a nitrogen outlet three-way valve (11), a material transferring pump outlet pipe (12), a batching kettle jacket (13), a dichloromethane conveying pump (14), a dichloromethane conveying pump outlet pipe (15), a batching kettle stirring motor device (16), a batching kettle viewing cup (17), a batching kettle connecting pipe (18), a batching kettle connecting regulating valve (19), a batching kettle inlet pipe (21), a batching kettle inlet valve (21), a n-butylamine elevated tank outlet pipe (22), A dichloromethane metering tank (23), an n-butylamine elevated tank (24), a dichloromethane metering tank inlet valve (25), an n-butylamine elevated tank inlet valve (26), an n-butylamine elevated tank inlet pipe (27), a trichlorosulfur elevated tank inlet valve (28), a trichlorosulfur elevated tank inlet pipe (29), a trichlorosulfur transfer pump (30), an n-butylamine elevated tank outlet valve (31), a trichlorosulfur elevated tank outlet pipe (32), a trichlorosulfur elevated tank outlet valve (33), a dichloromethane metering tank bottom left outlet pipe (34), a batching kettle (35), a dichloromethane metering tank bottom left outlet valve (36), a n-butyl kettle (37), a n-butyl kettle jacket (38), a n-butyl kettle viewing cup (39), a n-butyl kettle stirring motor device (40), a n-butyl kettle ice salt inlet pipe (41), a n-butyl kettle outlet valve (42), a n-butyl kettle outlet pipe (43), a n-butyl kettle ice salt inlet valve (44), A material transfer pump (45), an ammonia kettle (46), an ammonia kettle brine ice inlet pipe (47), an ammonia kettle jacket (48), an ammonia kettle brine inlet three-way valve (49), a trichloro-thion intermediate tank outlet valve (50), a n-butyl thiophosphoric triamide discharge pipe (51), an brine ice pump (52), a trichloro-thion intermediate tank (53), a n-butyl thiophosphoric triamide discharge valve (54), an ammonia kettle stirring motor device (55), an ammonia kettle liquid ammonia inlet pipe (56), a flow limiting pore plate (57), a liquid ammonia outlet pipe valve (58), a blow-off valve (59), a liquid ammonia intermediate tank (60), a liquid ammonia delivery pump outlet pipe (61), a liquid ammonia delivery pump outlet valve (62), a liquid ammonia delivery pump (63), a liquid ammonia delivery pump inlet pipe (64), a No. two n-butylamine delivery pumps (65), a No. two n-butylamine delivery pump inlet pipes (66), a trichloro-thion intermediate tank outlet pipe, A trichloro sulfur phosphorus elevated tank (68).
2. The method and the integrated device for preparing n-butyl thiophosphoric triamide according to claim 1 are characterized in that: comprises a core device, a batching kettle (35), a normal butyl kettle (37) and an ammonia introducing kettle (46), wherein the exterior of the batching kettle (35) of the core device is in a cylinder shape, a batching kettle jacket (13) is arranged on the inner wall of a cylinder body and is also in a hollow cylinder shape, a batching kettle nitrogen inlet pipe (9), a batching kettle feeding pipe (20) and an n-butylamine elevated tank outlet pipe (22) are arranged at the top end of the batching kettle (35), the batching kettle nitrogen inlet pipe (9) at the top end of the batching kettle (35) is communicated with a nitrogen buffer tank (10) through a nitrogen outlet three-way valve (11), the batching kettle feeding pipe (20) at the top end of the batching kettle (35) is communicated with a dichloromethane metering tank (23) through a batching kettle feeding valve (21), the dichloromethane metering tank inlet valve (25) is arranged at the top end of the dichloromethane metering tank (23) and is communicated with a dichloromethane delivery pump outlet pipe (15), an n-butylamine elevated tank outlet pipe (22) at the top end of a batching kettle (35) is communicated with an n-butylamine elevated tank (24) through an n-butylamine elevated tank outlet valve (31), the n-butylamine elevated tank (24) is communicated with an n-butylamine elevated tank inlet pipe (27), a second n-butylamine conveying pump (65), a second n-butylamine conveying pump inlet pipe (66), a second n-butylamine conveying pump inlet valve (5) and an n-butylamine intermediate tank (4), the n-butylamine intermediate tank (4) is communicated with a first n-butylamine conveying pump outlet pipe (2), a first n-butylamine conveying pump outlet valve (3) and a first n-butylamine conveying pump (1), a batching kettle connecting pipe (18) is arranged on the left side surface of the batching kettle (35) and communicated with a n-butylamine kettle (37) through a batching kettle connecting regulating valve (19), a batching kettle vision cup (17) and a batching ice salt water inlet pipe (6) are arranged on the right side surface of the batching kettle (35), the ice salt water inlet pipe (6) of the batching kettle is communicated with an ice salt water pump (52) through an ice salt water inlet valve (7) of the batching kettle, and a batching kettle stirring motor device (16) is arranged in the middle of the bottom of the batching kettle (35); the outside of the two n-butyl kettles (37) of the core equipment is in a cylindrical shape, the inner wall of a cylinder body is provided with an n-butyl kettle jacket (38) and is also in a hollow cylindrical shape, the top end of the n-butyl kettle (37) is provided with a trichlorosulfur elevated tank outlet valve (33) and a dichloromethane metering tank bottom left outlet valve (36), the dichloromethane metering tank bottom left outlet valve (36) is communicated with a dichloromethane metering tank (23) through a dichloromethane metering tank bottom left outlet pipe (34), the trichlorosulfur elevated tank outlet valve (33) is communicated with a trichlorosulfur elevated tank (68) through a trichlorosulfur elevated tank outlet pipe (32), the trichlorosulfur elevated tank (68) is communicated with a trichlorosulfur intermediate tank (53) through a trichlorosulfur elevated tank inlet valve (28), a trichlorosulfur elevated tank inlet pipe (29), a trichlorosulfur transfer pump (30), a trichlorosulfur intermediate tank outlet pipe (67), a trichlorosulfur intermediate tank outlet valve (50) and the trichlorosulfur, a positive mixing kettle connecting pipe (18) is arranged on the right side of the positive mixing kettle (37) and is communicated with the mixing kettle (35) through a positive mixing kettle connecting adjusting valve (19), a positive mixing kettle viewing cup (39), a positive mixing kettle ice salt water inlet pipe (41) and a positive mixing kettle outlet pipe (43) are arranged on the left side of the positive mixing kettle (37), the positive mixing kettle ice salt water inlet pipe (41) is communicated with an ice salt water pump (52) through a positive mixing kettle ice salt water inlet valve (44), the positive mixing kettle outlet pipe (43) is communicated with the top of the ammonia introducing kettle (46) through a positive mixing kettle outlet valve (42) and a transfer pump (45) through a transfer pump outlet pipe (12), and a positive mixing motor device (40) is arranged in the middle of the bottom of the positive mixing; the device outside of a triple-ammonia-introduction kettle (46) of core equipment is in a cylinder shape, an ammonia-introduction kettle jacket (48) is installed on the inner wall of a cylinder body, the triple-ammonia-introduction kettle is also in a hollow cylinder shape, a material transfer pump outlet pipe (12) is installed at the top of the ammonia-introduction kettle (46) and is communicated with a normal butyl kettle (37) through a material transfer pump (45), an ammonia-introduction kettle ice salt inlet pipe (47) and an n-butyl thiophosphoryl triamide discharge pipe (51) are installed on the left side of the ammonia-introduction kettle (46), the ammonia-introduction kettle ice salt inlet pipe (47) is communicated with an ice salt water pump (52) through an ammonia-introduction kettle ice salt three-way valve (490), the n-butyl thiophosphoryl triamide discharge pipe (51) enters the next working procedure through an n-butyl thiophosphoryl triamide discharge valve (54), an ammonia-introduction kettle nitrogen inlet pipe (8) is installed on the right side of the ammonia-introduction kettle (46) and is communicated with a nitrogen buffer, The right side of the bottom is provided with an ammonia inlet pipe (56) for introducing ammonia kettle liquid ammonia and communicated with a liquid ammonia middle tank (60) through a flow limiting pore plate (57), a liquid ammonia outlet pipe valve (58), a liquid ammonia blow-down valve (59) is arranged on the left lower side of the liquid ammonia middle tank (60), a liquid ammonia delivery pump outlet pipe (61) is arranged on the right lower side of the liquid ammonia middle tank (60), and the liquid ammonia delivery pump outlet pipe (62), the liquid ammonia delivery pump (63) and the liquid ammonia delivery pump inlet pipe (64) are communicated with each other in the last process.
3. The method and the integrated device for preparing n-butyl thiophosphoric triamide according to claim 1 and claim 2 are characterized in that: n-butylamine from an n-butylamine tank area is pumped into an n-butylamine intermediate tank (4) through a first n-butylamine conveying pump outlet pipe (2) and a first n-butylamine conveying pump outlet valve (3) by a first n-butylamine conveying pump (1), 264kg of n-butylamine is pumped into an n-butylamine elevated tank 24 by the n-butylamine in the n-butylamine intermediate tank (4) through an n-butylamine conveying pump inlet valve (5), a second n-butylamine conveying pump inlet pipe (66) and a second n-butylamine conveying pump (65) through an n-butylamine elevated tank inlet pipe (27) and an n-butylamine elevated tank inlet valve (26) for standby; dichloromethane (solvent) from a dichloromethane tank area is pumped into a dichloromethane metering tank (23) by a dichloromethane delivery pump (14) through a dichloromethane delivery pump outlet pipe (15) and a dichloromethane metering tank inlet valve (25) for about 2500L for standby; the trichloro-sulfur phosphorus from the preparation process of the trichloro-sulfur phosphorus is pumped into a trichloro-sulfur phosphorus elevated tank (68) for about 600kg from a trichloro-sulfur intermediate tank (53) through a trichloro-sulfur phosphorus delivery pump (30) through an inlet pipe (29) of the trichloro-sulfur phosphorus elevated tank through an inlet valve (28) of the trichloro-sulfur elevated tank for standby; opening a 3000L stirring motor device (16) of the batching kettle and a fully-opened batching kettle ice salt water inlet valve (7), opening an outlet valve (31) of a n-butylamine elevated tank to enable 264kg of n-butylamine to automatically flow to the batching kettle (35) from the n-butylamine elevated tank (24), opening a batching kettle feed valve (21) to enable 2500L of dichloromethane to automatically flow to the batching kettle (35) from a dichloromethane metering tank (23), stirring and cooling to 0 ℃, closing the batching kettle stirring motor device (16), and standing for later use; opening a 6300L n-butyl kettle stirring motor device (40), fully opening an n-butyl kettle ice salt water inlet valve (44) on an ice salt water pipeline of an n-butyl kettle jacket (38), opening an outlet valve (33) of a trichloro-sulfur high-level tank to enable 600kg of trichloro-sulfur to automatically flow from the trichloro-sulfur high-level tank (68) to the n-butyl kettle (37), opening an outlet valve (36) at the left side of the bottom of a dichloromethane metering tank to enable 2500L of dichloromethane to automatically flow from the dichloromethane metering tank (23) to the n-butyl kettle (37), and stirring and cooling to 8 ℃. Opening a nitrogen outlet three-way valve (11) on a nitrogen pipeline of the batching kettle, adjusting a batching kettle on a collecting pipeline of the batching kettle (35) to be connected with an adjusting valve (19), observing through a batching visual cup (17), dropping n-butylamine solution prepared in the batching kettle (35) into the n-butyl kettle (37) through a batching kettle connecting pipe (18), controlling the temperature of the n-butyl kettle to be not higher than 12 ℃, continuing stirring for 10min after finishing dropping for about 2h, closing a n-butyl kettle stirring motor device (40) and a batching kettle ice salt water inlet valve (7), and preparing for material transferring; liquid ammonia (318kg) from a liquid ammonia tank area is pumped into a liquid ammonia intermediate tank (60) through a liquid ammonia transfer pump (63) via an outlet pipe (61) of the liquid ammonia transfer pump and an outlet valve (62) of the liquid ammonia transfer pump, and the temperature and pressure ranges (0-30 ℃ and 0.43-1.17 MPa) are controlled for standby application; the method comprises the steps of replacing an ammonia introducing kettle (46) with nitrogen, transferring reaction liquid in a normal-butyl kettle (37) into a 6300L ammonia introducing kettle (46) through a material transferring pump (45) and a material transferring pump outlet pipe (12), starting an ammonia introducing kettle stirring motor device (55), introducing an ammonia kettle ice salt water inlet three-way valve (49) on a full-open ammonia introducing kettle jacket (48), controlling the temperature to be 15-25 ℃, controlling the pressure in the ammonia introducing kettle (46) to be not higher than 0.1MPa, introducing liquid ammonia from a liquid ammonia intermediate tank (60) into the ammonia introducing kettle (46) from the bottom of the ammonia introducing kettle (46) at the speed of 60-100kg/h through a liquid ammonia outlet pipe valve (58) and a flow limiting pore plate (57) and introducing measured 318kg of liquid ammonia.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111560036A (en) * | 2020-05-14 | 2020-08-21 | 浙江今晖新材料股份有限公司 | NBPT production facility |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111560036A (en) * | 2020-05-14 | 2020-08-21 | 浙江今晖新材料股份有限公司 | NBPT production facility |
| CN111560036B (en) * | 2020-05-14 | 2022-11-01 | 浙江今晖新材料股份有限公司 | NBPT production facility |
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Application publication date: 20200512 |