CN1986042B - Improved tubular reactor - Google Patents
Improved tubular reactor Download PDFInfo
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- CN1986042B CN1986042B CN200510134766XA CN200510134766A CN1986042B CN 1986042 B CN1986042 B CN 1986042B CN 200510134766X A CN200510134766X A CN 200510134766XA CN 200510134766 A CN200510134766 A CN 200510134766A CN 1986042 B CN1986042 B CN 1986042B
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Abstract
The improved tubular reactor includes one reactant mixing section, one reactant reacting section and one reaction product outputting nozzle. It features the reactant mixing section with one spiral jetting mixer and the reactant reacting section with one spiral mixer. The material contact order and the spiral jetting mixer in the reactant mixing section are regulated properly to control the mixing degree, contact area and reaction speed to ensure homogeneous mixing of the materials and moderate reaction speed. The spiral mixer in the reactant reacting section mix the gas phase, the liquid phase and the solid phase gradually for homogeneous, smooth, mild and full reaction to form high quality well atomized slurry.
Description
Technical field:
The invention belongs to the key equipment in the chemical fertilizer production technology, the solution-air phase in specifically a kind of chemical synthesis compound fertilizer production technology or the tubular reactor of liquid-liquid phase reaction, the tubular reactor that particularly has gas ammonia or liquefied ammonia and acid or mixed acid to react.
Background technology:
In compound fertilizer production technology, what product quality was the highest is chemical synthesis technology, and the main chemical reaction in the production is ammonia and acid or nitration mixture, as the reaction of phosphoric acid, sulfuric acid, nitric acid, the existing ammoniation reactor that uses has two kinds of normal pressure and pressurization ammoniation reactors.
The normal pressure ammoniation reactor uses tank diameter mostly, in be provided with paddle, fluid flows and to be mixed flow, can fully mix between the reactant, but reaction pressure is low, back-mixing is serious, reaction speed is slow, and equipment is huge, and degree of neutralization is lower, the ammonia loss is big, reaction heat is difficult to make full use of, and the slip water content is big, and returning charge is more higher than high, dry power consumption in the follow-up drum granulating process.
The pressurized reactor capital equipment is a tubular reactor, utilize the mixing that atomizes fully of the heat that produces in the aminating reaction process and steam, owing to improved reaction pressure and mixed effect, the reactivity height of ammonia, loss are little, and make full use of reacting heat evaporation moisture, and the slip water content of generation is low, granulating rate height in granulation process, returning charge is than low, and energy consumption for drying is low, and the equipment operating cost is low.Owing to used the higher slip crystallization granulation of temperature, the intensity of product is higher, and outward appearance is better, and nutrient is regulated fast.Do not need preneutralization groove, agitator, shurry pump, pipeline etc., flow process is simple, and equipment investment is saved, and it is simple to operation.So tubular reactor is the key equipment in the chemical synthesis production technology.But the material in reactor must fully mix, otherwise occur easily scabbing, overheated, phenomenons such as the burn into reactivity is low, asthma, vibration, be difficult to steadily operate normally.
Key reaction in tubular reactor is:
H
3PO
4+NH
3＝NH
4H
2PO
4
NH
4H
2PO
4+NH
3＝(NH
4)
2HPO
4
2NH
3+H
2SO
4＝(NH
4)
2SO
4
NH
3+HNO
3＝NH
4NO
3
The reaction that ammonia and phosphoric acid generate MAP is irreversible exothermic reaction fast, MAP and ammonia continue reaction speed that reaction generates Diammonium phosphate (DAP) then slowly many, sulfuric acid is quick irreversible exothermic reaction with the reaction that ammonia generates ammonium sulfate, nitric acid and ammonia generation ammonium nitrate.
In entering the various materials of tubular reactor, the concentration of washings acid is minimum, moisture content is the highest, and at washing system process part neutralization, it mainly is in MAP and the ammonia and the reaction of generation Diammonium phosphate (DAP), so the reacting dose minimum, main effect is to regulate slurry temperature, viscosity, liquid phase total amount; The phosphoric acid moisture content is higher, and phosphoric acid and ammonia react are produced MAP and Diammonium phosphate (DAP) is the main reaction of tubular reactor, and main effect provides reaction heat, forms the suitable phosphor ammonium slurry of degree of neutralization; The amount of sulfuric acid, nitric acid is less, but reaction speed is fast, exothermic heat of reaction is big, and main effect provides N/P, assurance pulp quality, the adjustment nutrients ratio of reaction heat, control slip.
The reaction of topmost phosphoric acid and ammonia in tubular reactor belongs to the mass transfer limited quick gas liquid reaction of air film, and overall reaction rate is directly proportional with the phase boundary mass transfer area, reduces with the rising of reaction temperature, increases with the enhancing of gas-liquid phase mixing velocity.Allly can increase gas-liquid mixed and contact area, the measure that suitably reduce reaction temperature, improves reaction pressure all can be strengthened course of reaction, improves equipment capacity, reduces overflowing of ammonia.Adopting and to spray ammonia at a high speed, strengthen gas-liquid and mix, make the reactor inner fluid become the rill shape to flow, is the effective measures of strengthening this process.
Existing tubular reactor is generally established blender, discharge end by feed end and is established not constituting with the pipeline section of filler of shower nozzle, its internal diameter is between 10～300mm, length is between 1～10m, length/diameter is not less than 50 than generally, main effect is to make gas phase or liquid phase feed carry out abundant hybrid reaction, and the slip of Sheng Chenging is through shower nozzle atomizing ejection the most at last.
U.S. TVA begins to develop T type tubular reactor at middle nineteen sixties, and ammonia adds from the side from unclassified stores such as central tube importing, phosphoric acid; Developed the cross tubular reactor afterwards again, (Pipe crossReactor is called for short PCR), ammonia adds from central tube, and phosphoric acid adds in the side, adds phosphoric acid,diluted that is imported by washing tail gas and the sulfuric acid of adding from the opposite side over against the phosphoric acid inlet.Mix owing to only depend on material to flow naturally, the undercompounding of material, reaction is incomplete, and local reaction is violent, and burn into scabs and stops up easily.At the shortcoming of tubular reactor, a lot of researchers have carried out a large amount of improvement to tubular reactor, have formed a lot of patented technologies.
United States Patent (USP) 3954942,3310371, French Patent (FRP) 217172826,2199478 has all been done adjustment to the feeding manner and the structure of tubular reactor, but still the phenomenon that has corrosion easily and occur blocking.United States Patent (USP) 3419378 has used the structure of phosphoric acid spiral rotation, and mixed effect is better, but phosphoric acid to spiral nozzle wash away and corrode very serious, the mixing of the front obstruction easily that closes up also.
The structure of 87107537 pairs of mixing arrangements of Chinese patent is comparatively successful: main reactant phosphoric acid and sulfuric acid are mixed enters the mixed zone through the sleeve pipe feeder, at first contact and carry out partial reaction with the ammonia atomizing, mix with the washings that central tube enters then, the conversion zone that enters tubular reactor at last fully reacts.Adopt such sleeve pipe jet mixing device, make the mixing of various materials more even, but still the problem of Cun Zaiing is: phosphoric acid mixes earlier with sulfuric acid, because temperature rising, corrosivity increase behind the Dilution of sulphuric acid, so mixed nitration mixture is still serious to the corrosion of the sleeve pipe of T type mixing tube and logical ammonia; Contact at first with ammonia with the fastest sulfuric acid of reaction speed owing to main reactant phosphoric acid in the mixed zone, too early reacts, make ammonia and water vaporize in a large number, cause local slip overheated, violent turbulence appears in the mixed zone, cause and scab, pant and vibrate, and cause material corrosion, aging.
At the conversion zone of tubular reactor, along with the reacting dose increase of phosphoric acid and ammonia, in the reactor second half section, especially the slip before the outlet shower nozzle begins to occur the state that gas, liquid, solid separate, and makes reaction incomplete, and reactivity is low.Therefore, United States Patent (USP) 4861352,4931225,4867918,5061406,5211916,5302325, used venturi (convergent-divergent joint) or can be coalescent, deflection cone carries out secondary to slip and mixes, and guarantees that mixing of materials is even.
Chinese patent 87107538 adopts identical principle the conversion zone of tubular reactor to be done the improvement of structure: the conversion zone import at tubular reactor is provided with venturi, in pipe, venturi is set or assembles joint with outlet, slip is repeatedly mixed, guarantee to mix fully, react evenly.But, higher in the section import department concentration of reactants of tubular reactor, because the mixability of venturi is higher, cause reaction aggravation suddenly, hot-spot appears easily, cause the aging and thermal deformation of burn into of material; The resistance of venturi or convergence joint is bigger, in the second half section of the conversion zone of tubular reactor, especially before advancing shower nozzle, solid content that carries out slip and viscosity increasing along with reaction, clogging appears in closing in place at venturi or convergence joint easily, cause and scab and pressure oscillation that when impurity content was high in the low or phosphoric acid in N/P ratio height, the water content of reactant batching, this phenomenon was more serious.
Though done above-mentioned improvement, still there is following problem in existing tubular reactor:
Sulfuric acid dilutes earlier, because acidity strengthens behind the Dilution of sulphuric acid, corrosivity strengthens, temperature raises, thereby the corrosivity of nitration mixture strengthens greatly;
Acid or nitration mixture earlier with the ammonia haptoreaction because reaction speed is fast, reaction is violent, be easy to generate localized hyperthermia and violent turbulence;
What have in the mixed zone is not provided with mixing arrangement, the employing that has the sleeve pipe jet mixing device, the effect of mixing is undesirable, causes that local reaction is too violent, slip is overheated, causes and scabs, pants and vibrate.
Mixed material is when entering main reaction region, and what have does not have a mixing arrangement, reacts inhomogeneous, scabs easily and stops up, and reacts also insufficient, reactivity is low; The venturi of the employing change actual internal area that has or polycondensation joint, deflection cone mix, because concentration of reactants is big, mixing is too abundant, reaction is too violent, local temperature is too high, occurs easily scabbing and the vibration of reactor, and the reactor operation is not steady;
What have in conversion zone does not establish mixing arrangement, and the state that gas, liquid, solid separate appears in slip, makes reaction not exclusively, and reactivity is low, scab easily; The employing that has change the venturi of actual internal area or assemble joint, deflection cone mixes, resistance greatly, easily scab, easily scab, be not suitable for the phosphor ammonium slurry of thickness.
Summary of the invention:
The objective of the invention is to, a kind of improved tubular reactor is provided, mixing section,, guarantee both to have made mixing of materials even, do not make reaction too violent again by the control of spiral spray mixing arrangement mixability, contact area and reaction speed; In reaction section, by the spiral mixing arrangement gas, liquid, solid are progressively mixed fully mutually, realization response evenly, steadily, gentle, carry out fully, form high-quality atomizing slip in order.
The objective of the invention is to be achieved through the following technical solutions:
A kind of tubular reactor that is used for carrying out the prepared in reaction ammonium compounds with acid or mixed acid and ammonia, contain a reactant mixing section, a reactant reaction section and a product delivery nozzle, it is characterized in that: be provided with a spiral spray mixing arrangement at described reactant mixing section; Be provided with the spiral mixing arrangement at described reactant reaction section.
A kind of optimal technical scheme is characterized in that: described spiral mixing arrangement is positioned at described reactant reaction section near described reactant mixing section one end.
A kind of optimal technical scheme is characterized in that: described reactant reaction section also is provided with a spiral mixing arrangement near described product delivery nozzle one end.
A kind of optimal technical scheme, it is characterized in that: described reactant mixing section comprises outermost layer sleeve pipe, intermediate casing and central tube, described outermost layer sleeve pipe is the mixed zone near the space of reactant reaction section one end, and described intermediate casing is between described outermost layer sleeve pipe and central tube; Described outermost layer sleeve pipe both sides are provided with one or two charging aperture, are used for the adding of phosphoric acid and washings, enter the mixed zone through the circular passage of outermost layer sleeve pipe; Described intermediate casing one side is provided with a charging aperture, is used for the charging of ammonia; Described central tube one end is provided with charging aperture, is used for the charging of sulfuric acid.
A kind of optimal technical scheme is characterized in that: described spiral spray mixing arrangement is the spirality distributing fin that is installed in the central tube outside or intermediate casing inboard.
A kind of optimal technical scheme is characterized in that: the spirality distributing fin of described mixing section is 3～10.
A kind of optimal technical scheme is characterized in that: the height of the spirality distributing fin of described mixing section is 10～100% of intermediate casing and a central tube spacing.
A kind of optimal technical scheme is characterized in that: the anglec of rotation θ between the spirality distributing fin of described mixing section and central tube are axial is 5～45 °, preferably 30～45 °; And the angle of inclination Φ of central tube between radially is 0～45 °, preferably 25～45 °.
A kind of optimal technical scheme, it is characterized in that: the spirality distributing fin of described mixing section and central tube between axially anglec of rotation θ and and the angle of inclination Φ of central tube between radially be stepping, the direction of preferably pressing the fluid overall flow by little to big variation.
A kind of optimal technical scheme is characterized in that: described spiral mixing arrangement is the spirality distributing fin that is installed in the reaction section pipeline.
A kind of optimal technical scheme is characterized in that: the spirality distributing fin in the described reaction section is 3～6.
A kind of optimal technical scheme is characterized in that: the height of the spirality distributing fin in the described reaction section is 10～30% of a tubular reactor conversion zone internal diameter of the pipeline.
A kind of optimal technical scheme is characterized in that: spirality distributing fin and the anglec of rotation α between the reaction section pipeline axial in the described reaction section are 5～45 °, preferably 10～30 °; And the inclination angle beta of reaction section pipeline between radially is 0～30 °, preferably 0～15 °.
A kind of optimal technical scheme, it is characterized in that: spirality distributing fin in the described reaction section and the anglec of rotation α between the reaction section pipeline axial and and the inclination angle beta of reaction section pipeline between radially be stepping, the direction of preferably pressing the fluid overall flow by little to big variation.
A kind of optimal technical scheme is characterized in that: between the described spiral mixing arrangement and with the direction of rotation of spiral spray mixing arrangement in the same way or oppositely.
Again from the charging aperture adding of outermost layer sleeve pipe, perhaps phosphoric acid and washings add from the charging aperture of outermost layer sleeve pipe both sides respectively, enter the mixed zone through the circular passage of outermost layer sleeve pipe after T type pipe carries out mixed diluting for phosphoric acid and washings elder generation; Ammonia enters from the charging aperture of middle sleeve pipe, because described spiral spray mixing arrangement is divided into several spirality channels with the circular passage of intermediate casing, enter the ammonia rotation ejection of intermediate casing, enter the mixed zone, carrying out atomizing fully mixing with phosphoric acid and washings forms the gas-liquid mixed slip; Sulfuric acid enters the mixed zone from the central tube charging aperture, after described gas-liquid mixed slip rapid mixing, enters the reactant reaction section and fully reacts.
Beneficial effect
The advantage of improved tubular reactor of the present invention:
(1) raw material ammonia is in the centre of each inlet feed, and the stirring of ammonia helps reducing the resistance of air film control, makes gas ammonia be dissolved in the liquid phase quickly; The high velocity jet of ammonia can prevent that suck-back is gone into sulfuric acid in the ammonia pipeline, generates ammonium sulfate crystallization and causes that the ammonia pipeline blocks; The corrosivity of ammonia is less, and corrosion and wearing and tearing that its rotation produces are little, heavy corrosion and the wearing and tearing of having avoided other liquid phase rotations to produce.
(2) sulfuric acid adds by central tube, directly participate in reaction without dilution, make the corrosivity of sulfuric acid reduce greatly, reaction heat can be absorbed by slip very soon, be not easy to occur situation, utilize the fast reaction of sulfuric acid to absorb in time gas ammonia with phosphatase reaction, reduce sharply the vaporize Volume Changes of generation of liquefied ammonia and water because of localized hyperthermia, reacting balance, the scabbing of tubular reactor, pant, vibration, noise descend greatly.
(3) being uniformly dispersed of spiral spray mixing arrangement, but mixing intensity is less, drop is bigger, and main reactant phosphoric acid dilutes with washings earlier, has prevented that reaction speed is too fast, makes reaction temperature and steady.
(4) temperature was lower after phosphoric acid mixed with washings, had reduced the evaporating capacity of water, had reduced the resistance that gas ammonia spreads in solution, had increased solution and had absorbed the speed and the capacity of gas ammonia, thereby reduced the Volume Changes of total reactant.
(5) the spiral spray mixing arrangement does not need to change actual internal area basically, resistance than venturi is little, is not easy to scab, and also can be easy to be washed away totally by slip even have to scab on a small quantity, reduced scabbing, pant, vibrating of reactor, the stability of operation and security improve.
(6) slip in the reaction section produces centrifugal force, shearing force and rotation under the effect of the spirality distributing fin of spiral mixing arrangement, makes gas, liquid, solid mix mutually fully.
(7) the spiral mixing arrangement in the reaction section does not need to change actual internal area basically, and resistance is little;
(8) degree of the mixing of the spiral mixing arrangement in the reaction section is suitable, and reactor operates steadily.
(9) because reaction is even, the efficient of reactor improves, and the production capacity of tubular reactor improves.
(10) reactor has improved the adaptability to slip viscosity, the requirement of impurity content in raw material proportioning N/P ratio, water content and the phosphoric acid is relaxed, thereby improved tubular reactor to the adaptability of raw material and the elasticity of operation.
Sulfuric acid among the present invention can substitute with nitric acid, and use the advantage of nitric acid to be: aminating reaction heat is little than sulfuric acid ammonification reaction heat; Nitrogen content is than sulfuric acid content height, the easier adjusting of the prescription of production; Increased a kind of acid that reaction heat is provided, raw material be that adaptability increases; In product, increase nitrate nitrogen content, improved the adaptability of product.
The present invention will be further described below by the drawings and specific embodiments, but and do not mean that limiting the scope of the invention.
Description of drawings
Fig. 1 is the generalized section of tubular reactor of the present invention;
Fig. 2 is the generalized section of mixing section;
Fig. 3 mixes the interior A-A of section to schematic cross-section;
Fig. 4 is the generalized section of the spiral mixing arrangement in the reaction section;
Fig. 5 is that the B-B of the spiral mixing arrangement in the reaction section is to schematic cross-section.
The specific embodiment
Shown in Fig. 1-5, tubular reactor of the present invention comprises reactant mixing section 6, reactant reaction section 3, product delivery nozzle 1.At reactant mixing section 6, phosphoric acid and washings enter mixed zone 7 through T type pipe 11 from outermost layer sleeve pipe one side charging aperture; Ammonia enters circular passage in the intermediate casing by charging aperture 9, produces the rotation ejection through the guiding of spirality distributing fin 8, enters mixed zone 7; Sulfuric acid enters mixed zone 7 by central tube charging aperture 10, and all reactants mix in mixed zone 7, enters reactant reaction section 3 behind partial reaction.
Reactant reaction section 3 is made up of the pipeline of inside lining anti-corrosive material, is provided with a spiral mixing arrangement 4 in the reactant reaction section 3, and the spirality distributing fin 5 of slip on it produces rotation, and gas, liquid, solid progressively mix to make mutually and react completely; Reactant reaction section 3 is being provided with a spiral mixing arrangement 2 identical with spiral mixing arrangement 4 structures near product nozzle 1 one ends, make slip before entering product nozzle 1, spirality distributing fin 5 on it ' generation rotation, mix once more, guarantee that the slip of ejection fully atomizes.
Shown in Fig. 2,3, θ for the spirality distributing fin that mixes section with central tube the anglec of rotation between axial; Φ is the spirality distributing fin that mixes section and the central tube angle of inclination between radially.
Shown in Fig. 3,4, α is the spirality distributing fin and the anglec of rotation between the reaction section pipeline axial in the reaction section, and β is the interior spirality distributing fin of reaction section and the reaction section pipeline angle of inclination between radially.
The product delivery nozzle 1 of reactor can be the positive taper of symmetry, or asymmetric tilted conical, also can have 0～90 ° and curve, with the spray veer of guiding reactant.
Further specify below in conjunction with concrete operating position:
At internal diameter is 150mm, in the tubular reactor that length is 5.9 meters, adopts the reactor of original CN87107538 structure and the practical operation situation that adopts structure of the present invention to be compared as follows:
The comparative example 1
Use the maximum throwing amount of tubular reactor produced ability among the CN87107538 to be:
Ammonia 7.2t/h
98% sulfuric acid 16.6t/h
52% phosphatase 11 2.0t/h
The washings 17.0t/h of tail gas recycle
N/P 1.5
It is high to feed intake again, and then tubular reactor begins to occur scabbing, pant, vibrate, and the reactivity of ammonia descends, tubular reactor pressure 6～8kg/cm
2, 100 decibels of noises were using 10 days, the polytetrafluoroethylene (PTFE) seriously charing that enters first venturi of conversion zone, and color is pitch-black, a lot of crackles are arranged.The stainless steel T type pipe intermediate casing that feeds phosphoric acid, sulfuric acid uses after 6 months because erosion corrosion attenuation perforation, the central tube that enters washings has been shorter than logical ammonia sleeve pipe through corrosion, begin to occur the nitration mixture suck-back and go into the ammonia pipe, cause ammonium sulfate, ammonium phosphate crystallization to stop up, must be through purge vapor commonly used, it is undesired to operate, and can't keep in repair owing to remaining pipeline wall thickness is too thin, and T type pipe and central tube must all be changed again.
Embodiment 1
Tubular reactor of the present invention is affixed 3 spirality distributing fins in the outside of central tube, direction of rotation is clockwise, anglec of rotation θ is 5 °, angle of inclination Φ is 0 °, conversion zone import at tubular reactor is provided with a spiral mixing arrangement 4, a spiral mixing arrangement 2 identical with spiral mixing arrangement 4 is installed before the reactant delivery nozzle, the spirality distributing fin is 3, direction of rotation is clockwise, anglec of rotation α is 5 °, and inclination angle beta is 0 °, under identical throwing amount, do not occur scabbing, asthma, vibration, tubular reactor pressure 3～5kg/cm
2, pressure is steady, and tubular reactor reaction and injection are normal, 50 decibels of noises, after using 30 days, the color jaundice only appears in the polytetrafluoroethylene (PTFE) that enters the ribbon mixer of conversion zone, does not have crackle.The stainless steel T type pipe that feeds phosphoric acid, washings uses not obviously corrosion in 1.0 years, reaches 2.5 years service life.The stainless steel central tube that feeds sulfuric acid uses 9 months post-etchings to shorten, can normally use but still be longer than logical ammonia sleeve pipe, the wall thickness of residue central tube does not have tangible attenuate, can continue to use behind the welding lengthening, and the central tube that feeds sulfuric acid can use 1.5 years repeatedly through maintenance.And under the situation that guarantees normal operation, production capacity can improve 25%, and largest production throwing amount reaches:
Ammonia 9.1t/h
98% sulfuric acid 20.7t/h
52% phosphatase 11 5.0t/h
The washings 19.0t/h of tail gas recycle
N/P 1.5
The comparative example 2
Inventory is with comparative example 1, and the problem of using the tubular reactor produced appearance among the CN87107538 is with comparative example 1.
Embodiment 2
Tubular reactor of the present invention is affixed 10 spirality distributing fins in the outside of central tube, direction of rotation is clockwise, anglec of rotation θ is 45 °, angle of inclination Φ is 45 °, conversion zone import at tubular reactor is provided with a spiral mixing arrangement 4, a spiral mixing arrangement 2 identical with spiral mixing arrangement 4 is installed before the reactant delivery nozzle, the spirality distributing fin is 6, direction of rotation is clockwise, anglec of rotation α is 45 °, and inclination angle beta is 30 °, under identical throwing amount, do not occur scabbing, asthma, vibration, tubular reactor pressure 3～5kg/cm
2, pressure is steady, and tubular reactor reaction and injection are normal, 55 decibels of noises, after using 30 days, the color jaundice only appears in the polytetrafluoroethylene (PTFE) that enters the ribbon mixer of conversion zone, does not have crackle.The stainless steel T type pipe that feeds phosphoric acid, washings uses not obviously corrosion in 1.0 years, reaches 2.5 years service life.The stainless steel central tube that feeds sulfuric acid uses 9 months post-etchings to shorten, can normally use but still be longer than logical ammonia sleeve pipe, the wall thickness of residue central tube does not have tangible attenuate, can continue to use behind the welding lengthening, and the central tube that feeds sulfuric acid can use 1.5 years repeatedly through maintenance.Identical with comparative example 1, under the situation that guarantees normal operation, production capacity can improve 25%.
The comparative example 3
Inventory is with comparative example 1, and the problem of using the tubular reactor produced appearance among the CN87107538 is with comparative example 1.
Embodiment 3
Tubular reactor of the present invention is affixed 5 spirality distributing fins in the outside of central tube, direction of rotation is clockwise, anglec of rotation θ is 30 °, angle of inclination Φ is 25 °, conversion zone import at tubular reactor is provided with a spiral mixing arrangement 4, a spiral mixing arrangement 2 identical with spiral mixing arrangement 4 is installed before the reactant delivery nozzle, the spirality distributing fin is 4, direction of rotation is clockwise, anglec of rotation α is 10 °, and inclination angle beta is 15 °, under identical throwing amount, do not occur scabbing, asthma, vibration, tubular reactor pressure 3～5kg/cm
2, pressure is steady, and tubular reactor reaction and injection are normal, 50 decibels of noises, after using 30 days, the color jaundice only appears in the polytetrafluoroethylene (PTFE) that enters the ribbon mixer of conversion zone, does not have crackle.The stainless steel T type pipe that feeds phosphoric acid, washings uses not obviously corrosion in 1.0 years, reaches 2.5 years service life.The stainless steel central tube that feeds sulfuric acid uses 9 months post-etchings to shorten, can normally use but still be longer than logical ammonia sleeve pipe, the wall thickness of residue central tube does not have tangible attenuate, can continue to use behind the welding lengthening, and the central tube that feeds sulfuric acid can use 1.5 years repeatedly through maintenance.Identical with comparative example 1, under the situation that guarantees normal operation, production capacity can improve 25%.
The comparative example 4
Inventory is with comparative example 1, and the problem of using the tubular reactor produced appearance among the CN87107538 is with comparative example 1.
Tubular reactor of the present invention is affixed 5 spirality distributing fins in the outside of central tube, direction of rotation is clockwise, anglec of rotation θ is 45 °, angle of inclination Φ is 45 °, conversion zone import and conversion zone 1/2 place at tubular reactor respectively are provided with a spiral mixing arrangement 4, a spiral mixing arrangement 2 is installed before the reactant delivery nozzle, the spirality distributing fin is 4, direction of rotation is clockwise, anglec of rotation α is 30 °, and inclination angle beta is 0 °, under identical throwing amount, tubular reactor pressure 3～5kg/cm does not appear scabbing, pant, vibrating
2, pressure is steady, and tubular reactor reaction and injection are normal, 50 decibels of noises, after using 30 days, the color jaundice only appears in the polytetrafluoroethylene (PTFE) that enters the ribbon mixer of conversion zone, does not have crackle.The stainless steel T type pipe that feeds phosphoric acid, washings uses not obviously corrosion in 1.0 years, reaches 2.5 years service life.The stainless steel central tube that feeds sulfuric acid uses 9 months post-etchings to shorten, can normally use but still be longer than logical ammonia sleeve pipe, the wall thickness of residue central tube does not have tangible attenuate, can continue to use behind the welding lengthening, and the central tube that feeds sulfuric acid can use 1.5 years repeatedly through maintenance.Identical with comparative example 1, under the situation that guarantees normal operation, production capacity can improve 25%.
The comparative example 5
Inventory is with comparative example 1, and the problem of using the tubular reactor produced appearance among the CN87107538 is with comparative example 1.
Tubular reactor of the present invention is affixed 5 spirality distributing fins in the outside of central tube, direction of rotation is clockwise, anglec of rotation θ carries out the transition to 45 ° gradually from 30 °, angle of inclination Φ carries out the transition to 45 ° gradually from 25 °, conversion zone import and conversion zone 1/2 place at tubular reactor respectively are provided with a spiral mixing arrangement 4, a spiral mixing arrangement 2 is installed before the reactant delivery nozzle, the spirality distributing fin is 4, direction of rotation is clockwise, anglec of rotation α carries out the transition to 30 ° gradually from 10 °, and inclination angle beta carries out the transition to 15 ° gradually from 0 °, under identical throwing amount, do not occur scabbing, asthma, vibration, tubular reactor pressure 3～5kg/cm
2, pressure is steady, and tubular reactor reaction and injection are normal, 40 decibels of noises, after using 30 days, the color jaundice only appears in the polytetrafluoroethylene (PTFE) that enters the ribbon mixer of conversion zone, does not have crackle.The stainless steel T type pipe that feeds phosphoric acid, washings uses not obviously corrosion in 1.0 years, reaches 2.5 years service life.The stainless steel central tube that feeds sulfuric acid uses 9 months post-etchings to shorten, can normally use but still be longer than logical ammonia sleeve pipe, the wall thickness of residue central tube does not have tangible attenuate, can continue to use behind the welding lengthening, and the central tube that feeds sulfuric acid can use 1.5 years repeatedly through maintenance.Identical with comparative example 1, under the situation that guarantees normal operation, production capacity can improve 25%.
The comparative example 6
Tubular reactor among the use CN87107538 is identical with the production throwing amount of tubular reactor of the present invention, is:
Ammonia 9.2t/h
93% sulfuric acid 17.7t/h
42% phosphatase 11 8.34t/h
The washings 18.0t/h of tail gas recycle
N/P 1.9
Use the N/P of the tubular reactor actual product among the CN87107538 to have only 1.0-1.5, and fluctuation range is big, the ammonia spill-out is big, washing tail gas water N/P has reached 1.8～1.9, PH reaches 6.5～7.5, washing system reclaims the ammonia difficulty, ammonia utilization rate 95%, and washings density reaches 1350～1450kg/m
3, viscosity height, mobile poor, difficulty of transportation need efflux washings and cause significant loss, and tubular reactor occurs scabbing, pants, vibrates, tubular reactor pressure 4～8kg/cm
2, and fluctuation is very big, and slip sprays discontinuous, and reactor can't normally move, needs steam blowing tubular reactor 1 time in per 1 hour, 150 decibels of reactor operation noises.Feed the stainless steel T type pipe of phosphoric acid, sulfuric acid and the central tube of feeding washings and use erosion corrosion attenuation after 8 months, central tube has been shorter than logical ammonia sleeve pipe very much, begin to occur the nitration mixture suck-back and go into the ammonia pipe, cause ammonium sulfate, ammonium phosphate crystallization to stop up, must be through purge vapor commonly used, it is undesired to operate, and can't keep in repair owing to remaining pipeline wall thickness is too thin, and T type pipe and central tube must all be changed again.
Tubular reactor of the present invention has been installed 3 spirality distributing fins in the outside of central tube, direction of rotation is clockwise, anglec of rotation θ is 30 °, angle of inclination Φ is 25 °, conversion zone import and conversion zone 1/2 place at tubular reactor respectively are provided with a spiral mixing arrangement 4, a spiral mixing arrangement 2 is installed before the reactant delivery nozzle, the spirality distributing fin is 3, direction of rotation is clockwise, anglec of rotation α is 10 °, and inclination angle beta is 0 °, under identical throwing amount, tubular reactor pressure 3～5kg/cm does not appear scabbing, pant, vibrating
2, pressure is steady, and tubular reactor reaction and injection are normal, 60 decibels of noises.The N/P of reactor product reaches and has 1.5～1.7, and fluctuation range is little, and the ammonia spill-out is little, washing tail gas water N/P N/P1.2～1.55, PH6.0～6.7, density 1350～1450kg/m
3, ammonia utilization rate 98.5%, washings viscosity is suitable, good fluidity, conveying are normal, and washing system can reach balance, does not need to efflux washings.The stainless steel T type pipe that feeds phosphoric acid, washings uses not obviously corrosion in 1.0 years, reaches 2.5 years service life.The stainless steel central tube that feeds sulfuric acid uses 10 months post-etchings to shorten, can normally use but still be longer than logical ammonia sleeve pipe, the wall thickness of residue central tube does not have tangible attenuate, can continue to use behind the welding lengthening, and the central tube that feeds sulfuric acid can use 2 years repeatedly through maintenance.
The comparative example 7
The tubular reactor among the use CN87107538 and the production throwing amount of tubular reactor of the present invention are with comparative example 6, and the tubular reactor actual operating state among the use CN87107538 is with comparative example 6.
Embodiment 7
Tubular reactor of the present invention is affixed 10 spirality distributing fins in the outside of central tube, direction of rotation is clockwise, anglec of rotation θ is 45 °, angle of inclination Φ is 45 °, conversion zone import and conversion zone 1/2 place at tubular reactor respectively are provided with a spiral mixing arrangement 4, a spiral mixing arrangement 2 is installed before the reactant delivery nozzle, the spirality distributing fin is 6, direction of rotation is clockwise, anglec of rotation α is 30 °, and inclination angle beta is 15 °, under identical throwing amount, do not occur scabbing, asthma, vibration, tubular reactor pressure 3～5kg/cm
2, pressure is steady, and tubular reactor reaction and injection are normal, 65 decibels of noises.The N/P of reactor product reaches and has 1.55～1.7, and fluctuation range is little, and the ammonia spill-out is little, washing tail gas water N/P N/P1.2～1.55, PH6.0～6.8, density 1350～1450kg/m
3, ammonia utilization rate 98.0%, washings viscosity is suitable, good fluidity, conveying are normal, and washing system can reach balance, does not need to efflux washings.The stainless steel T type pipe that feeds phosphoric acid, washings uses not obviously corrosion in 1.0 years, reaches 2.5 years service life.The stainless steel central tube that feeds sulfuric acid uses 10 months post-etchings to shorten, can normally use but still be longer than logical ammonia sleeve pipe, the wall thickness of residue central tube does not have tangible attenuate, can continue to use behind the welding lengthening, and the central tube that feeds sulfuric acid can use 2 years repeatedly through maintenance.
The comparative example 8
The tubular reactor among the use CN87107538 and the production throwing amount of tubular reactor of the present invention are with comparative example 6, and the tubular reactor actual operating state among the use CN87107538 is with comparative example 6.
Tubular reactor of the present invention is at inboard affixed 7 spirality distributing fins of the intermediate casing of logical ammonia, direction of rotation is clockwise, anglec of rotation θ is 35 °, angle of inclination Φ is 25 °, conversion zone import and conversion zone 1/2 place at tubular reactor respectively are provided with a spiral mixing arrangement 4, a spiral mixing arrangement 2 is installed before the reactant delivery nozzle, the spirality distributing fin is 5, direction of rotation is clockwise, anglec of rotation α is 30 °, and inclination angle beta is 15 °, under identical throwing amount, do not occur scabbing, asthma, vibration, tubular reactor pressure 3～5kg/cm
2, pressure is steady, and tubular reactor reaction and injection are normal, 65 decibels of noises.The N/P of reactor product reaches and has 1.55～1.7, and fluctuation range is little, and the ammonia spill-out is little, washing tail gas water N/P N/P1.2～1.50, PH5.8～6.5, density 1350～1450kg/m
3, ammonia utilization rate 98.3%, washings viscosity is suitable, good fluidity, conveying are normal, and washing system can reach balance, does not need to efflux washings.The stainless steel T type pipe that feeds phosphoric acid, washings uses not obviously corrosion in 1.0 years, reaches 2.5 years service life.The stainless steel central tube that feeds sulfuric acid uses 10 months post-etchings to shorten, can normally use but still be longer than logical ammonia sleeve pipe, the wall thickness of residue central tube does not have tangible attenuate, can continue to use behind the welding lengthening, and the central tube that feeds sulfuric acid can use 2 years repeatedly through maintenance.
The comparative example 9
The tubular reactor among the use CN87107538 and the production throwing amount of tubular reactor of the present invention are with comparative example 6, and the tubular reactor actual operating state among the use CN87107538 is with comparative example 6.
Tubular reactor of the present invention is affixed 6 spirality distributing fins in the outside of central tube, direction of rotation is clockwise, anglec of rotation θ carries out the transition to 45 ° gradually from 30 °, angle of inclination Φ carries out the transition to 45 ° gradually from 25, in the conversion zone import of tubular reactor with at conversion zone 1/3, / 2/3 place respectively is provided with a spiral mixing arrangement 4, a spiral mixing arrangement 2 is installed before the reactant delivery nozzle, direction of rotation is counterclockwise, the spirality distributing fin is 4, anglec of rotation α carries out the transition to 30 ° gradually from 10 °, inclination angle beta carries out the transition to 15 ° gradually from 0 °, under identical throwing amount, do not occur scabbing, asthma, vibration, tubular reactor pressure 3～5kg/cm
2, pressure is steady, and tubular reactor reaction and injection are normal, 50 decibels of noises.The N/P of reactor product reaches and has 1.6～1.75, and fluctuation range is little, and the ammonia spill-out is little, washing tail gas water N/P1.1～1.50, PH5.5～6.5, density 1300～1450kg/m
3, ammonia utilization rate 99.0%, washings viscosity is suitable, good fluidity, conveying are normal, and washing system can reach balance, does not need to efflux washings.The stainless steel T type pipe that feeds phosphoric acid, washings uses not obviously corrosion in 1.0 years, reaches 2.5 years service life.The stainless steel central tube that feeds sulfuric acid uses 10 months post-etchings to shorten, can normally use but still be longer than logical ammonia sleeve pipe, the wall thickness of residue central tube does not have tangible attenuate, can continue to use behind the welding lengthening, and the central tube that feeds sulfuric acid can use 2 years repeatedly through maintenance.
The comparative example 10
The tubular reactor among the use CN87107538 and the production throwing amount of tubular reactor of the present invention are with comparative example 6, and the tubular reactor actual operating state among the use CN87107538 is with comparative example 6.
Tubular reactor of the present invention is affixed 8 spirality distributing fins in the outside of central tube, direction of rotation is clockwise, anglec of rotation θ carries out the transition to 45 ° gradually from 30 °, angle of inclination Φ carries out the transition to 45 ° gradually from 25, in the conversion zone import of tubular reactor a direction of rotation being set is clockwise spiral mixing arrangement, it is counterclockwise spiral mixing arrangement 4 that a direction of rotation is set at conversion zone 1/2 place, before the reactant delivery nozzle direction of rotation being installed is clockwise spiral mixing arrangement 2, the spirality distributing fin is 3, anglec of rotation α carries out the transition to 30 ° gradually from 10 °, inclination angle beta carries out the transition to 15 ° gradually from 0 °, under identical throwing amount, do not occur scabbing, asthma, vibration, tubular reactor pressure 3～5kg/cm
2, pressure is steady, and tubular reactor reaction and injection are normal, 50 decibels of noises.The N/P of reactor product reaches and has 1.6～1.8, and fluctuation range is little, and the ammonia spill-out is little, washing tail gas water N/P 1.1～1.5, PH5.5～6.5, density 1300～1450kg/m
3, ammonia utilization rate 99.0%, washings viscosity is suitable, good fluidity, conveying are normal, and washing system can reach balance, does not need to efflux washings.The stainless steel T type pipe that feeds phosphoric acid, washings uses not obviously corrosion in 1.0 years, reaches 2.5 years service life.The stainless steel central tube that feeds sulfuric acid uses 10 months post-etchings to shorten, can normally use but still be longer than logical ammonia sleeve pipe, the wall thickness of residue central tube does not have tangible attenuate, can continue to use behind the welding lengthening, and the central tube that feeds sulfuric acid can use 2 years repeatedly through maintenance.
In a word, aspects such as the production capacity of reactor of the present invention, reaction efficiency, operation conditions, operating flexibility, noise pollution, service life, tail gas recycle all are significantly improved.
Claims (7)
1. tubular reactor that is used for carrying out the prepared in reaction ammonium compounds with acid or mixed acid and ammonia, contain a reactant mixing section, a reactant reaction section and a product delivery nozzle, be provided with a spiral spray mixing arrangement at described reactant mixing section; Be provided with the spiral mixing arrangement at described reactant reaction section near described reactant mixing section one end, also be provided with a spiral mixing arrangement near described product delivery nozzle one end at described reactant reaction section; It is characterized in that: described reactant mixing section comprises outermost layer sleeve pipe, intermediate casing and central tube, and described outermost layer sleeve pipe is the mixed zone near the space of reactant reaction section one end, and described intermediate casing is between described outermost layer sleeve pipe and central tube; Described outermost layer sleeve pipe both sides are provided with one or two charging aperture, are used for the adding of phosphoric acid and washings, enter the mixed zone through the circular passage of outermost layer sleeve pipe; Described intermediate casing one side is provided with a charging aperture, is used for the charging of ammonia; Described central tube one end is provided with charging aperture, is used for the charging of sulfuric acid.
2. tubular reactor according to claim 1 is characterized in that: described spiral spray mixing arrangement is the spirality distributing fin that is installed in the central tube outside or intermediate casing inboard.
3. tubular reactor according to claim 2 is characterized in that: the anglec of rotation θ between the spirality distributing fin of described mixing section and central tube are axial is 5～45 °; And the angle of inclination Ф of central tube between radially is 0～45 °.
4. according to claim 2 or 3 described tubular reactors, it is characterized in that: the spirality distributing fin of described mixing section and central tube between axially anglec of rotation θ and and the angle of inclination Ф of central tube between radially press the fluid overall flow direction by little to big variation.
5. tubular reactor according to claim 1 is characterized in that: described spiral mixing arrangement is the spirality distributing fin that is installed in the reaction section pipeline.
6. tubular reactor according to claim 5 is characterized in that: spirality distributing fin and the anglec of rotation α between the reaction section pipeline axial in the described reaction section are 5～45 °; And the inclination angle beta of reaction section pipeline between radially is 0～30 °.
7. according to claim 5 or 6 described tubular reactors, it is characterized in that: spirality distributing fin in the described reaction section and the anglec of rotation α between the reaction section pipeline axial and and the inclination angle beta of reaction section pipeline between radially press the fluid overall flow direction by little to big variation.
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| Application Number | Priority Date | Filing Date | Title |
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| CN200510134766XA CN1986042B (en) | 2005-12-21 | 2005-12-21 | Improved tubular reactor |
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| CN200510134766XA CN1986042B (en) | 2005-12-21 | 2005-12-21 | Improved tubular reactor |
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| CN1986042B true CN1986042B (en) | 2010-07-14 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111389338A (en) * | 2020-03-26 | 2020-07-10 | 北京理工大学 | Novel multi-channel reactor for toluene and isobutylene alkylation reaction |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102580661A (en) * | 2012-03-12 | 2012-07-18 | 山东鸿瑞石油化工有限公司 | Three-component polymeric monomer feeding device |
| CN102674904B (en) * | 2012-05-18 | 2013-11-06 | 甘肃瓮福化工有限责任公司 | Diammonium phosphate system and production technique for producing diammonium phosphate with single-tube reactor |
| CN204043972U (en) * | 2014-03-07 | 2014-12-24 | 中华人民共和国四川出入境检验检疫局 | A kind of to granulated samples carrying out the chemical detection liquid extraction tube of lixiviate |
| CN103962066B (en) * | 2014-05-13 | 2015-10-28 | 华中科技大学 | A kind of high heating rate heat treatment reactor being easy to tri-state product separation |
| CN106268499A (en) * | 2015-05-29 | 2017-01-04 | 林新吉 | Automatization's granulating system and comminutor thereof |
| CN111905685A (en) * | 2020-07-16 | 2020-11-10 | 上海交通大学 | Thermal compensation type jet reaction system |
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| US3310371A (en) * | 1962-10-30 | 1967-03-21 | Dorr Oliver Inc | Production of ammonium phosphate |
| US3419378A (en) * | 1965-04-01 | 1968-12-31 | Swift & Co | Method of producing monoammonium phosphate by reacting phosphoric acid and ammonia under pressure |
| US3954942A (en) * | 1974-09-16 | 1976-05-04 | Tennessee Valley Authority | Granular ammonium phosphate sulfate and monoammonium phosphate using common pipe-cross-type reactor |
| CN87107538A (en) * | 1986-12-18 | 1988-07-20 | 氮及肥田料化学公司 | new tubular reactor |
| CN1306955A (en) * | 2000-02-01 | 2001-08-08 | 江西贵溪化肥厂 | Process for producing compound N-P-K fertilizer |
| CN2848349Y (en) * | 2005-12-21 | 2006-12-20 | 中国-阿拉伯化肥有限公司 | Improved tubular reactor |
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- 2005-12-21 CN CN200510134766XA patent/CN1986042B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3310371A (en) * | 1962-10-30 | 1967-03-21 | Dorr Oliver Inc | Production of ammonium phosphate |
| US3419378A (en) * | 1965-04-01 | 1968-12-31 | Swift & Co | Method of producing monoammonium phosphate by reacting phosphoric acid and ammonia under pressure |
| US3954942A (en) * | 1974-09-16 | 1976-05-04 | Tennessee Valley Authority | Granular ammonium phosphate sulfate and monoammonium phosphate using common pipe-cross-type reactor |
| CN87107538A (en) * | 1986-12-18 | 1988-07-20 | 氮及肥田料化学公司 | new tubular reactor |
| CN1306955A (en) * | 2000-02-01 | 2001-08-08 | 江西贵溪化肥厂 | Process for producing compound N-P-K fertilizer |
| CN2848349Y (en) * | 2005-12-21 | 2006-12-20 | 中国-阿拉伯化肥有限公司 | Improved tubular reactor |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111389338A (en) * | 2020-03-26 | 2020-07-10 | 北京理工大学 | Novel multi-channel reactor for toluene and isobutylene alkylation reaction |
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