CN109264687A - A kind of phosphoric acid microwave flash distillation prepares the method and apparatus of polyphosphoric acid - Google Patents
A kind of phosphoric acid microwave flash distillation prepares the method and apparatus of polyphosphoric acid Download PDFInfo
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- CN109264687A CN109264687A CN201811213932.9A CN201811213932A CN109264687A CN 109264687 A CN109264687 A CN 109264687A CN 201811213932 A CN201811213932 A CN 201811213932A CN 109264687 A CN109264687 A CN 109264687A
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- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 title claims abstract description 154
- 229910000147 aluminium phosphate Inorganic materials 0.000 title claims abstract description 76
- 229920000137 polyphosphoric acid Polymers 0.000 title claims abstract description 59
- 238000000034 method Methods 0.000 title claims abstract description 53
- 238000007701 flash-distillation Methods 0.000 title claims abstract description 36
- 239000007788 liquid Substances 0.000 claims abstract description 73
- 238000001704 evaporation Methods 0.000 claims abstract description 25
- 238000010438 heat treatment Methods 0.000 claims abstract description 25
- 230000008020 evaporation Effects 0.000 claims abstract description 24
- 239000012141 concentrate Substances 0.000 claims abstract description 17
- 238000011084 recovery Methods 0.000 claims abstract description 6
- 239000007789 gas Substances 0.000 claims description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- 239000000463 material Substances 0.000 claims description 24
- 239000000243 solution Substances 0.000 claims description 16
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 12
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 12
- 239000002250 absorbent Substances 0.000 claims description 10
- 230000002745 absorbent Effects 0.000 claims description 10
- 239000003517 fume Substances 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- -1 polytetrafluoroethylene Polymers 0.000 claims description 8
- 239000012670 alkaline solution Substances 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 7
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical compound FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims 1
- 238000006116 polymerization reaction Methods 0.000 abstract description 11
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 238000005265 energy consumption Methods 0.000 abstract description 6
- 238000002360 preparation method Methods 0.000 abstract description 3
- 238000012546 transfer Methods 0.000 abstract description 3
- 238000012545 processing Methods 0.000 abstract description 2
- 238000007796 conventional method Methods 0.000 abstract 1
- 235000011007 phosphoric acid Nutrition 0.000 description 63
- 239000000047 product Substances 0.000 description 20
- 239000002253 acid Substances 0.000 description 7
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 6
- 230000007797 corrosion Effects 0.000 description 6
- 238000005260 corrosion Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 238000000605 extraction Methods 0.000 description 6
- 229910052698 phosphorus Inorganic materials 0.000 description 6
- 239000011574 phosphorus Substances 0.000 description 6
- 238000001816 cooling Methods 0.000 description 5
- 238000007599 discharging Methods 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 102000004160 Phosphoric Monoester Hydrolases Human genes 0.000 description 3
- 108090000608 Phosphoric Monoester Hydrolases Proteins 0.000 description 3
- 238000004442 gravimetric analysis Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 230000035515 penetration Effects 0.000 description 2
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000012024 dehydrating agents Substances 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 239000003779 heat-resistant material Substances 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 238000012643 polycondensation polymerization Methods 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 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
- C01B25/24—Condensed phosphoric acids
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The present invention discloses the method and apparatus that a kind of phosphoric acid microwave flash distillation prepares polyphosphoric acid, under vacuum conditions, using microwave heating, polymerize phosphoric acid stoste progress flash concentration to obtain polyphosphoric acid, exhaust gas of flash evaporation condensing recovery；Its equipment includes microwave generator, microwave waveguide, pressure transmitter, head tank, liquid flowing valve, infrared temperature sensor, flash tank, reactor tank, liquid valve door, concentrate liquid collecting tank, valve, condensing tower, condensate liquid collecting tank, collects tank valve, vacuum pump, device for absorbing tail gas；Present device is simple, the thermal efficiency is high, low energy consumption, process flow is short, and processing speed is fast, polyphosphoric acid produced coloration, in terms of be superior to conventional method, serialization can be used, the semicontinuous or independent mode of interruption is produced, production method multiplicity, solve the problems such as heat-transfer surface and forced circulation pump in traditional evaporation process easily corrode, power consumption is high, product purity is low, it can be achieved that high polymerization degree polyphosphoric acid efficient preparation.
Description
Technical field
The present invention relates to a kind of microwave reinforced evaporation process high viscosity, the new technology of low heat conductivity or strong corrosive solution,
The method and apparatus that polyphosphoric acid is prepared more particularly to a kind of phosphoric acid microwave flash distillation, belongs to chemical production technical field.
Background technique
Polyphosphoric acid is a kind of colorless and transparent thick liquid, easily deliquesces, does not crystallize, and has corrosivity, can hydrolyze, be dissolved in water
Become orthophosphoric acid.Fusing point under normal pressure be 48 ~ 50 DEG C, 856 DEG C of boiling point, density 2100kg/m3, relative molecular mass is
337.93.In the industry, generally by P2O5Phosphoric acid of the content higher than 68% is known as polyphosphoric acid.
Polyphosphoric acid is widely used in the industries such as pigment, fragrance, pharmacy, leather, fire retardant manufacture, in organic synthesis
It is used in journey as cyclizing agent, acidulant, dehydrating agent.The chemical industry intermediate products important as one, while being also one important
Chemical products, production method mainly has thermal method and two kinds of wet process, wherein wet process is that will be phosphoric acid by single-stage or multistage
The method of evaporation carries out heating concentration and removes moisture to obtain, low in cost, but the impurity content of product of the product of acquisition
Height is mainly used for agrochemical and prepares the phosphate of feed using being limited.The good product quality that thermal method obtains, impurity content
It is low, but it is expensive.The production technology of polyphosphoric acid mainly has high-temperature heating concentration method, electric energy method, absorption process, synthetic method, wet
Method phosphoric acid purification extraction etc..And these production methods need to expend huge heat, the extractant extraction of wet cleaning extraction process
Take process there is also process flows it is long, the problems such as being difficult to control.
Since phosphoric acid by wet process needs to be heated using high-temperature steam by evaporator, concentration increases after Phosphoric Acid Concentration,
Viscosity increases, and increases the workload of circulating pump, and in integrated artistic process, equipment energy consumption is big, and tube surface polyphosphoric acid
Assemble after generation, generates the diabatic process for affecting equipment while fouling, need periodically to clean equipment, to keep flowing
Dynamic fluency and the stability of equipment work.
When traditional evaporation process processing high viscosity, low heat conductivity or strong corrosive solution, there are equipment more, long flow path is accounted for
The problems such as ground is big, and energy consumption height, fouling, burn into product impurity content height, coal-fired steam heating cause environmental pollution.Traditional
In phosphoric acid by wet process thermal dehydration polymerization technique, generallys use shell and tube heating evaporation device and combined with forced circulation vacuum evaporator
Mode heating evaporation carried out to phosphoric acid, the traditional equipment of this type constructs complicated, and technique is tediously long, and heat resistant material is generally graphite
Or alloy, wherein Graphite thermal tube heat transfer is stablized, but is easy to produce surface scale, and graphite material is more crisp, uses one section
It cracks, is replaced after time.Compo pipe is during heating vulnerable to phosphoric acid corrosion, to generate damage.
Microwave heating is as a kind of efficient heating means, when microwave penetration substance, passes through the energy inside material and consumes
The features such as scattered realize heats the selectivity of material, has and is evenly heated, high thermal efficiency, short heating time.Microwave flash evaporation technology
Flash distillation chamber is optimized as microwave cavity, inhales microwave energy intracavitary by target solution by presenting mouth and entering to flash
It receives, realizes that solution temperature quick in situ is promoted, supply enough energy and make target solution constantly boiling, to reach enhanced water evaporation
The purpose of process, microwave single stage flash just can reach evaporation and require, it can be achieved that short route, high-efficiency evaporating.Microwave can penetrate high viscous
Degree, low heat conductivity, strong corrosive material carry out active isomer heating.
Summary of the invention
The present invention provides the method and apparatus that a kind of phosphoric acid microwave flash distillation prepares polyphosphoric acid, in order to reduce traditional handicraft phosphoric acid
The energy consumption of concentration realizes that phosphoric acid is dense present invention incorporates microwave heating technique, vacuum flashing technology, vapor-liquid separation technology
Condensation polymerization prepares the purpose of polyphosphoric acid, meanwhile, present device has simple and reliable for structure, energy conservation and environmental protection, stable, cost
The features such as low.
Microwave is introduced phosphoric acid by wet process and heats concentration process by the present invention, in conjunction with vacuum distillation and steam discharge technology, in vacuum item
Under part, gradually by the heating of microwave, temperature increases phosphoric acid, and the bubble point of liquid reduces under environment under low pressure, continuous heating so that
Phosphoric acid boils, and after the hydrone inside phosphoric acid is heated, is detached from phosphoric acid ontology in a low pressure environment, and vapor is achieved separation,
Phosphoric Acid Concentration simultaneously, volume reduce, and concentration increases, and viscosity increases, and obtain polyphosphoric acid product；Matched microwave flash distillation phosphoric acid generates
The equipment of polyphosphoric acid realizes the heating and polymerization to phosphoric acid by single stage operation.
The present invention provides a kind of method that the flash distillation of phosphoric acid microwave prepares polyphosphoric acid, under vacuum conditions, using microwave heating,
It polymerize phosphoric acid stoste progress flash concentration to obtain polyphosphoric acid, exhaust gas of flash evaporation condensing recovery.
The pressure of the vacuum condition is 100Pa-85KPa.
The flash temperature is 250 DEG C -350 DEG C.
The present invention also provides the equipment that the phosphoric acid by wet process microwave flash distillation prepares polyphosphoric acid, including microwave generator 2, microwave
Waveguide 3, pressure transmitter 4, head tank 5, liquid flowing valve 6, infrared temperature sensor 7, flash tank 8, reactor tank 9, liquid valve door
10, concentrate liquid collecting tank 11, discharge valve 12, steam (vapor) outlet 14, condensing tower 15, condensate liquid collecting tank 16, collect tank valve 17,
Vacuum pump 18, device for absorbing tail gas 19；
It is connected at the top of 5 bottom of head tank and flash tank 8, liquid flowing valve 6 is equipped between head tank 5 and flash tank 8, flash tank 8 pushes up
Portion is equipped with infrared temperature sensor 7 and steam (vapor) outlet 14, is equipped with pressure transmitter 4, reactor tank 9, infrared temperature inside flash tank 8
Inside 7 face reactor tank 9 of sensor, for measuring the temperature of 9 materials inside of reactor tank, pressure transmitter 4 is for measuring flash distillation
8 internal pressure of tank is equipped with microwave waveguide 3 outside flash tank 8, and microwave waveguide 3 is connect with microwave generator 2, and 9 bottom of reactor tank goes out
Mouthful be overlapped with 8 outlet at bottom of flash tank, 8 outlet at bottom of flash tank is connect with concentrate liquid collecting tank 11,8 outlet at bottom of flash tank and
Liquid valve door 10 is equipped between concentrate liquid collecting tank 11,11 bottom of concentrate liquid collecting tank is equipped with discharge valve 12；8 top of flash tank
Steam (vapor) outlet 14 and condensing tower 15 at the top of connect, 15 bottom of condensing tower connect condensate liquid collecting tank 16, condensate liquid collecting tank 16
Bottom, which is equipped with, collects tank valve 17, and 16 top of condensate liquid collecting tank is connect with vacuum pump 18, vacuum pump 18 and device for absorbing tail gas
19 connections.
Temperature transmitter 13 is additionally provided with inside the flash tank 8, temperature transmitter 13 is for measuring 8 inside temperature of flash tank
Degree.
The equipment further includes control system 1, microwave generator 2, pressure transmitter 4, infrared temperature sensor 7, vacuum
Pump 18 is connect with control system 1 respectively, and control system 1 includes PLC integrated manipulator, circuit, the model of PLC integrated manipulator
SIEMENS S7 Series Controller.
The device for absorbing tail gas 19 is the device equipped with fume absorbent material, and fume absorbent material is that water or alkalinity are molten
Liquid, alkaline solution are sodium hydroxide solution, sodium carbonate liquor etc..
The reactor tank 9 be polytetrafluoroethylene (PTFE) reactor tank, quartz glass reaction tank etc. not with the reactor tank of phosphatase reaction.
The flash tank 8 be 316L stainless steel flash tank or polytetrafluoroethylene (PTFE) flash tank etc. not with the flash distillation of phosphatase reaction
Tank.
Circulating condensing water is equipped with outside the condensing tower 15, condensed water inside condensing tower 15 to cooling down.
Polytetrafluoroethylene (PTFE) etc. can be used as inner lining material solve the etching problem of pipeline in the connecting pipe.
The present invention can get it is following the utility model has the advantages that
(1) low energy consumption.Microwave energy directly acts on material itself, and energy consumption is lower；Material does not need to recycle at high temperature, avoids
The thermal loss of material transportation process.
(2) process is short.The polymerization reaction that phosphoric acid can be carried out using the material of non-defluorinate, by defluorinate with polymerize two mistakes
Journey shortens to during one；And multistage evaporation is become into single-stage evaporation.
(3) easy to operate.Only need the once-through operation in microwave cavity, so that it may obtain high-concentration polyphosphoric acid product, be not required to
It repeatedly to recycle, eliminate expensive forced circulation pump, find out a set of operating procedure at present.
(4) heat transfer efficiency is high.Energy is passed to phosphoric acid by microwave penetration container table wall in situ, i.e., thoroughly avoids fouling shadow
The problems such as the problem of ringing the thermal efficiency, in turn avoids the corrosion of material, the damage of equipment.
(5) product quality is high.Material corrosion is avoided, the purity of product, available colorless and transparent phosphoric acid are improved
Product can carry out the preparation of electron level and food grade phosphoric acid product in the future.
(6) will flash distillation cavity according to microwave heating Theoretical Design be multimode cavity, using not with the material of phosphatase reaction
As main material, the etching problem of evaporation process is avoided；The concentrate of high-purity is once obtained using microwave single stage flash,
Highly energy-consumings, perishable component, the microwave flash process such as expensive forced circulation pump can be cancelled to be expected to be applied to wastewater treatment, poly- phosphorus
The fields such as sour preparation, chemical industry solutions condensing crystallizing, sterilization, solution oil removing, organic mixed solution rectifying separation and organic matter removing.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of 1 device of the embodiment of the present invention；
1- control system in figure, 2- microwave generator, 3- microwave waveguide, 4- pressure transmitter, 5- head tank, 6- liquid flowing valve,
7- infrared temperature sensor, 8- flash tank, 9- reactor tank, 10- liquid valve door, 11- concentrate liquid collecting tank, 12- discharge valve,
13- temperature transmitter, 14- steam (vapor) outlet, 15- condensing tower, 16- condensate liquid collecting tank, 17- collection tank valve, 18- vacuum pump,
19- device for absorbing tail gas.
Specific embodiment
With reference to the accompanying drawing and specific embodiment, invention is further explained.
Embodiment 1
A kind of method that the flash distillation of phosphoric acid microwave prepares polyphosphoric acid, in the case where pressure is the vacuum condition of 100Pa, using microwave heating,
Phosphoric acid stoste is flashed, flash temperature is 280 DEG C, and concentration polymerization obtains polyphosphoric acid, exhaust gas of flash evaporation condensing recovery.
The equipment that the present embodiment phosphoric acid by wet process microwave flash distillation prepares polyphosphoric acid, as shown in Figure 1, including control system 1, microwave
Generator 2, microwave waveguide 3, pressure transmitter 4, head tank 5, liquid flowing valve 6, infrared temperature sensor 7, flash tank 8, reaction
It is tank 9, liquid valve door 10, concentrate liquid collecting tank 11, discharge valve 12, temperature transmitter 13, steam (vapor) outlet 14, condensing tower 15, cold
Lime set collecting tank 16 collects tank valve 17, vacuum pump 18, device for absorbing tail gas 19；Connect at the top of 5 bottom of head tank and flash tank 8
It connects, flash tank 8 is 316L stainless steel flash tank, and liquid flowing valve 6 is equipped between head tank 5 and flash tank 8, is set at the top of flash tank 8
There are infrared temperature sensor 7 and steam (vapor) outlet 14, is equipped with pressure transmitter 4, reactor tank 9, temperature transmitter inside flash tank 8
13, reactor tank 9 is polytetrafluoroethylene (PTFE) reactor tank, and temperature transmitter 13 is for measuring 8 internal temperature of flash tank, infrared temperature sensing
Inside 7 face reactor tank 9 of device, for measuring the temperature of 9 materials inside of reactor tank, pressure transmitter 4 is for measuring in flash tank 8
Portion's pressure is equipped with microwave waveguide 3 outside flash tank 8, and microwave waveguide 3 is connect with microwave generator 2,9 outlet at bottom of reactor tank and
8 outlet at bottom of flash tank is overlapped, and 8 outlet at bottom of flash tank is connect with concentrate liquid collecting tank 11,8 outlet at bottom of flash tank and concentration
Liquid valve door 10 is equipped between liquid liquid collecting tank 11,11 bottom of concentrate liquid collecting tank is equipped with discharge valve 12；The steaming at 8 top of flash tank
Connected at the top of vapor outlet 14 and condensing tower 15, outside condensing tower 15 be equipped with circulating condensing water, condensed water to inside condensing tower 15 into
Row cooling, 15 bottom of condensing tower connect condensate liquid collecting tank 16, and 16 bottom of condensate liquid collecting tank, which is equipped with, collects tank valve 17, condensation
16 top of liquid collecting tank is connect with vacuum pump 18, and vacuum pump 18 is connect with device for absorbing tail gas 19, and device for absorbing tail gas 19 is dress
There is the device of fume absorbent material, fume absorbent material is water, microwave generator 2, pressure transmitter 4, infrared temperature sensor
7, vacuum pump 18 is connect with control system 1 respectively, and control system 1 includes PLC integrated manipulator, circuit, PLC integrated manipulator
Model SIEMENS S7 Series Controller, the letter that control system 1 receives pressure transmitter 4, infrared temperature sensor 7 is fed back
Number, the switch and watt level of microwave generator 2 are controlled, the switch of vacuum pump 18 is controlled.
The flash distillation of phosphoric acid microwave is carried out using the equipment continuous operation of the present embodiment and prepares polyphosphoric acid, the specific steps are as follows:
(1) liquid flowing valve 6 under head tank 5 is opened, P is made2O5The phosphoric acid by wet process stoste that content is 48% is flowed into flash tank 8
Reactor tank 9 in, control charging rate be 5L/min, liquid flowing valve 6 is in the open state at this time, liquid valve door 10, outlet valve
Door 12, collection tank valve 17 are in close state；
(2) control system 1 opens vacuum pump 18 to vacuumizing inside flash tank 8, and vacuum degree reaches pressure after setting value 100Pa
For transmitter 4 by pressure feedback to control system 1, control system 1 closes vacuum pump 18, opens microwave generator 2, control microwave is defeated
Entering power is 1000W, and microwave transparent flash tank 8 heats the phosphoric acid stoste inside reactor tank 9；
(3) after phosphoric acid stoste is heated, combination water and partially crystallizable water therein realize evaporation, the prompt flash distillation of pressure transmitter 4
Pressure in tank 8 changes, and after control system 1 receives signal, opens the vapor inside the extraction flash tank 8 of vacuum pump 18
And gas, with keep the environmental pressure in flash tank 8, vapor and gas from steam (vapor) outlet 14 release after enter condensing tower
15, condensed water is equipped with outside condensing tower 15, for condensed water to cooling down inside condensing tower 15, condensate liquid is collected into condensate liquid receipts
Collect in tank 16, the gas not being condensed is evacuated to device for absorbing tail gas 19 by vacuum pump 18 and is absorbed purification emptying；
(4) temperature of 7 real-time measurement phosphoric acid of infrared temperature sensor during heating when temperature is increased to 280 DEG C at that time, is adjusted
Whole microwave power is 500W, makes microwave constent temperature heated phosphoric stoste, the water evaporation contained in phosphoric acid and phosphoric acid polymerization is gathered simultaneously
Phosphoric acid opens the liquid valve door 10 of 8 bottom of flash tank, and control discharging speed is 3L/min, and adjusting liquid flowing valve 6 makes charging rate
For 3L/min, keep charging rate consistent with discharging speed, to realize that continuous operation carries out phosphoric acid by wet process microwave flash distillation system
For polyphosphoric acid, polyphosphoric acid product is obtained in the concentrate collecting tank 11 that polyphosphoric acid flows into below flash tank 8；
(5) after preparing, vacuum pump 18 is closed by control system 1, releases the vacuum of flash tank 8, opens discharge valve 12,
Polyphosphoric acid product is collected, opens and collects tank valve 17, collects the solution in condensate liquid collecting tank 16, after, using hot water pair
Each tank body is rinsed, and prevents acid solution and vapor from generating corrosion to tank body.
Using the P in gravimetric analysis polyphosphoric acid product2O5Content obtains final P2O5Content is 72%, meets poly- phosphorus
The manufacturing technique requirent of acid.
Embodiment 2
A kind of method that the flash distillation of phosphoric acid microwave prepares polyphosphoric acid, in the case where pressure is the vacuum condition of 85KPa, using microwave heating,
Phosphoric acid stoste is flashed, flash temperature is 250 DEG C, and concentration polymerization obtains polyphosphoric acid, exhaust gas of flash evaporation condensing recovery.
The equipment that the present embodiment phosphoric acid microwave flash distillation prepares polyphosphoric acid, reactor tank 9 are quartz glass reaction tank, tail gas absorption
Device 19 is the device equipped with fume absorbent material, and fume absorbent material is alkaline solution, and alkaline solution is that concentration is 1mol/L
Sodium hydroxide solution, the connection relationship between other component and component is same as Example 1.
The flash distillation of phosphoric acid microwave is carried out using the equipment interruption independent mode of the present embodiment and prepares polyphosphoric acid, specific steps are such as
Under:
(1) liquid flowing valve 6 under head tank 5 is opened, P is made2O5The phosphoric acid by wet process stoste that content is 55% is flowed into flash tank 8
Reactor tank 9 in, control charging rate be 5L/min, charging after the completion of close liquid flowing valve 6, at this time liquid valve door 10, discharging
Valve 12, collection tank valve 17 are in close state；
(2) control system 1 opens vacuum pump 18 to vacuumizing inside flash tank 8, after vacuum degree reaches setting value 85KPa, presses
For power transmitter 4 by pressure feedback to control system 1, control system 1 closes vacuum pump 18, opens microwave generator 2, controls microwave
Input power is 1000W, and microwave transparent flash tank 8 heats the phosphoric acid stoste inside reactor tank 9；
(3) after phosphoric acid stoste is heated, combination water and partially crystallizable water therein realize evaporation, the prompt flash distillation of pressure transmitter 4
Pressure in tank 8 changes, and after control system 1 receives signal, opens the vapor inside the extraction flash tank 8 of vacuum pump 18
And gas, with keep the environmental pressure in flash tank, vapor and gas from steam (vapor) outlet 14 release after enter condensing tower 15,
Condensed water is equipped with outside condensing tower 15, for condensed water to cooling down inside condensing tower 15, condensate liquid is collected into condensate liquid collection
In tank 16, the gas not being condensed is evacuated to device for absorbing tail gas 19 by vacuum pump 18 and is absorbed purification emptying；
(4) temperature of 7 real-time measurement phosphoric acid of infrared temperature sensor during heating, when temperature is increased to 250 DEG C at that time, root
It is 500W according to adjustment microwave power, makes microwave constent temperature heated phosphoric stoste, the water evaporation contained in phosphoric acid and phosphoric acid polymerization obtains simultaneously
To polyphosphoric acid, the liquid valve door 10 of 8 bottom of flash tank is opened, polyphosphoric acid flows into the concentrate collecting tank 11 of 8 lower section of flash tank
Obtain polyphosphoric acid product；It is then shut off liquid valve door 10, liquid flowing valve 6 is opened and completes charging, starts to produce next time, thus real
Now interruption independent mode carries out the flash distillation of phosphoric acid by wet process microwave and prepares polyphosphoric acid；
(5) after preparing, vacuum pump 18 is closed by control system 1, releases the vacuum of flash tank 8, opens discharge valve 12,
Polyphosphoric acid product is collected, opens and collects tank valve 17, collects the solution in condensate liquid collecting tank 16, after, using hot water pair
Each tank body is rinsed, and prevents acid solution and vapor from generating corrosion to tank body.
Using the P in gravimetric analysis polyphosphoric acid product2O5Content obtains final P2O5Content is 75%, meets poly- phosphorus
The manufacturing technique requirent of acid.
Embodiment 3
A kind of method that the flash distillation of phosphoric acid microwave prepares polyphosphoric acid, in the case where pressure is the vacuum condition of 25kpa, using microwave heating,
Phosphoric acid stoste is flashed, flash temperature is 350 DEG C, and concentration polymerization obtains polyphosphoric acid, exhaust gas of flash evaporation condensing recovery.
The equipment that the present embodiment phosphoric acid microwave flash distillation prepares polyphosphoric acid, flash tank 8 are polytetrafluoroethylene (PTFE) flash tank, and tail gas is inhaled
Receiving apparatus 19 is the device equipped with fume absorbent material, and fume absorbent material is alkaline solution, and alkaline solution is that concentration is 1mol/
The sodium carbonate liquor of L, the connection relationship between other component and component are same as Example 1.
Using the equipment of the present embodiment it is semicontinuous carry out operation the flash distillation of phosphoric acid microwave prepare polyphosphoric acid, specific steps are such as
Under:
(1) liquid flowing valve 6 under head tank 5 is opened, P is made2O5The phosphoric acid by wet process stoste that content is 24% is flowed into flash tank 8
Reactor tank 9 in, control charging rate be 4L/min, after charging liquid flowing valve 6 close, at this time liquid valve door 10, discharging
Valve 12, collection tank valve 17 are in close state；
(2) control system 1 opens vacuum pump 18 to vacuumizing inside flash tank 8, and vacuum degree reaches pressure after setting value 25kPa
For transmitter 4 by pressure feedback to control system 1, control system 1 closes vacuum pump 18, opens microwave generator 2, control microwave is defeated
Entering power is 1000W, and microwave transparent flash tank 8 heats the phosphoric acid stoste inside reactor tank 9, and infrared temperature sensor 7 shows phosphorus
After sour stoste temperature is increased to 225 DEG C, at this point, opening liquid flowing valve 6 and keeping feed rate is 2L/min；
(3) after phosphoric acid stoste is heated, combination water and partially crystallizable water therein realize evaporation, the prompt flash distillation of pressure transmitter 4
Pressure in tank 8 changes, and after control system 1 receives signal, opens the vapor inside the extraction flash tank 8 of vacuum pump 18
And gas, with keep the environmental pressure in flash tank 8, vapor and gas from steam (vapor) outlet 14 release after enter condensing tower
15, condensed water is equipped with outside condensing tower 15, for condensed water to cooling down inside condensing tower 15, condensate liquid is collected into condensate liquid receipts
Collect in tank 16, the gas not being condensed is evacuated to device for absorbing tail gas 19 by vacuum pump 18 and is absorbed purification emptying；
(4) temperature of 7 real-time measurement phosphoric acid of infrared temperature sensor is adjusted when temperature is increased to 350 DEG C during heating
Microwave power is 500W, makes microwave constent temperature heated phosphoric stoste, the water evaporation contained in phosphoric acid and phosphoric acid polymerization obtains poly- phosphorus simultaneously
Acid opens the liquid valve door 10 of 8 bottom of flash tank, and adjusting flow velocity is 2L/min, and the polyphosphoric acid of 9 lower part of reactor tank flows into flash tank
Polyphosphoric acid product is obtained in the concentrate collecting tank 11 of 8 lower sections；The phosphoric acid stoste that 9 top of reactor tank newly flows into is by microwave heating
Evaporative polymerization becomes polyphosphoric acid, to realize that semicontinuous operation phosphoric acid by wet process microwave flash distillation prepares polyphosphoric acid；
(5) after preparing, vacuum pump 18 is closed by control system 1, releases the vacuum of flash tank 8, opens discharge valve 12,
Polyphosphoric acid product is collected, opens and collects tank valve 17, collects the solution in condensate liquid collecting tank 16, after, using hot water pair
Each tank body is rinsed, and prevents acid solution and vapor from generating corrosion to tank body.
Using the P in gravimetric analysis polyphosphoric acid product2O5Content obtains final P2O5Content is 70%, meets poly- phosphorus
The manufacturing technique requirent of acid.
Claims (9)
1. a kind of method that the flash distillation of phosphoric acid microwave prepares polyphosphoric acid, which is characterized in that under vacuum conditions, using microwave heating,
It polymerize phosphoric acid stoste progress flash concentration to obtain polyphosphoric acid, exhaust gas of flash evaporation condensing recovery.
2. the method that the flash distillation of phosphoric acid microwave prepares polyphosphoric acid according to claim 1, which is characterized in that the vacuum condition
Pressure is 100Pa-85KPa.
3. the method that the flash distillation of phosphoric acid microwave prepares polyphosphoric acid according to claim 1, which is characterized in that the flash temperature is
250℃-350℃。
4. the equipment that the flash distillation of phosphoric acid microwave prepares polyphosphoric acid described in claim 1, which is characterized in that including microwave generator (2),
Microwave waveguide (3), pressure transmitter (4), head tank (5), liquid flowing valve (6), infrared temperature sensor (7), flash tank (8),
Reactor tank (9), liquid valve door (10), concentrate liquid collecting tank (11), discharge valve (12), steam (vapor) outlet (14), condensing tower (15),
Condensate liquid collecting tank (16) collects tank valve (17), vacuum pump (18), device for absorbing tail gas (19)；
It is connect at the top of head tank (5) bottom and flash tank (8), is equipped with liquid flowing valve (6) between head tank (5) and flash tank (8),
It is equipped with infrared temperature sensor (7) and steam (vapor) outlet (14) at the top of flash tank (8), is equipped with pressure transmitter inside flash tank (8)
(4), reactor tank (9), infrared temperature sensor (7) face reactor tank (9) is internal, and microwave waveguide is equipped with outside flash tank (8)
(3), microwave waveguide (3) is connect with microwave generator (2), and reactor tank (9) outlet at bottom is overlapped with flash tank (8) outlet at bottom,
Flash tank (8) outlet at bottom is connect with concentrate liquid collecting tank (11), flash tank (8) outlet at bottom and concentrate liquid collecting tank (11) it
Between be equipped with liquid valve door (10), concentrate liquid collecting tank (11) bottom be equipped with discharge valve (12)；Steam at the top of flash tank (8) goes out
It is connect at the top of mouth (14) and condensing tower (15), condensing tower (15) bottom connects condensate liquid collecting tank (16), condensate liquid collecting tank
(16) bottom, which is equipped with, collects tank valve (17), is connect at the top of condensate liquid collecting tank (16) with vacuum pump (18), vacuum pump (18) and
Device for absorbing tail gas (19) connection.
5. the equipment for preparing polyphosphoric acid according to claim 4 phosphoric acid microwave flash distillation, which is characterized in that the flash tank (8) is internal
It is additionally provided with temperature transmitter (13).
6. the equipment for preparing polyphosphoric acid according to claim 4 phosphoric acid microwave flash distillation, which is characterized in that it further include control system (1),
Microwave generator (2), pressure transmitter (4), infrared temperature sensor (7), vacuum pump (18) connect with control system (1) respectively
It connects.
7. the equipment for preparing polyphosphoric acid according to claim 4 phosphoric acid microwave flash distillation, which is characterized in that the device for absorbing tail gas
It (19) is the device equipped with fume absorbent material, fume absorbent material is water or alkaline solution, and alkaline solution is sodium hydroxide
Solution or sodium carbonate liquor.
8. the equipment for preparing polyphosphoric acid according to claim 4 phosphoric acid microwave flash distillation, which is characterized in that the reactor tank (9) is poly-
Tetrafluoroethene reactor tank or quartz glass reaction tank.
9. the equipment for preparing polyphosphoric acid according to claim 4 phosphoric acid microwave flash distillation, which is characterized in that described；The flash tank (8)
For 316L stainless steel flash tank or polytetrafluoroethylene (PTFE) flash tank.
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| CN112850810A (en) * | 2020-12-25 | 2021-05-28 | 中国原子能科学研究院 | Transformation system of technetium-containing product feed liquid |
| CN115531902A (en) * | 2022-10-26 | 2022-12-30 | 天津中医药大学 | Traditional chinese medicine single drop radiation heat transfer flash distillation equipment |
| CN116281905A (en) * | 2023-03-02 | 2023-06-23 | 昆明川金诺化工股份有限公司 | Device and method for producing polyphosphoric acid by using surplus washing acid |
| CN116440803A (en) * | 2023-06-16 | 2023-07-18 | 北京湃普莱恩尼龙新材料技术有限公司 | Preparation process and preparation device of polyamide |
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