CN206051553U - The preparation system of low-polymerization-dammonium ammonium polyphosphate - Google Patents

The preparation system of low-polymerization-dammonium ammonium polyphosphate Download PDF

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Publication number
CN206051553U
CN206051553U CN201620845568.8U CN201620845568U CN206051553U CN 206051553 U CN206051553 U CN 206051553U CN 201620845568 U CN201620845568 U CN 201620845568U CN 206051553 U CN206051553 U CN 206051553U
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tube
ammonium polyphosphate
polymerization
ammonia
low
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李兵
江涛
郑义文
韦莎
黄安勇
郑开元
谭伟
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Sinochem Fuling Chongqing Chemical Industry Co Ltd
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Sinochem Fuling Chongqing Chemical Industry Co Ltd
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Abstract

This utility model discloses a kind of preparation system of low-polymerization-dammonium ammonium polyphosphate, the preparation system includes the polymeric kettle of pipeline connection, tubular reactor, recirculation reactor successively, return duct is connected between the outlet of the recirculation reactor and the entrance of tubular reactor, the return duct is provided with APP circulating pumps.Compared with prior art, preparation system of low-polymerization-dammonium ammonium polyphosphate that this utility model is provided and preparation method thereof, contrast it is existing adopt thermal phosphoric acid, full-boiled process polyphosphoric acid, phosphate that middle low-polymerization-dammonium ammonium polyphosphate is produced for primary raw material, greatly reduce production cost;Reaction is carried out under nature, low temperature, normal pressure, it is not necessary to high temperature, no pressure requirements, using continuous process, is greatly reduced processing step and difficulty, is reduced productive labor intensity, improve working condition;Can prevent the ammonium polyphosphate in tubular reactor from piling up and blocking pipeline, keep production continuous, stable, improve product yield and quality.

Description

The preparation system of low-polymerization-dammonium ammonium polyphosphate
Technical field
This utility model is related to the phosphate production technical field in inorganic chemistry industry, more particularly to a kind of oligomerization The preparation system of degree APP.
Background technology
APP, also known as ammonium polyphosphate or polycondensation ammonium phosphate (abbreviation APP), is a kind of Quadrafos containing N, according to The difference of specifically used demand, can produce it is oligomeric, in gather and high poly- three kinds different extent of polymerizations product, its degree of polymerization gets over Highly-water-soluble is less, otherwise then water solublity is bigger.Crystalline and amorphous can be divided into by its structure, crystalline state APP is Long chain water-insoluble salt.The general molecular formula of APP is (NH4)(n+2)PnO(3n+1), when n is 2~20, it is water solublity;When When n is more than 20, it is slightly solubility.The long chain APP of high-purity high polymerization degree water-insoluble is used for preparing high-grade fireproof painting Material, flame retardant plastics.
The low-polymerization-dammonium ammonium polyphosphate that water can be dissolved in is important liquid fertilizer basic material, and basic liquid fertilizer can be molten with nitrogen Liquid, potash fertilizer production liquid compound fertilizer.APP as fertilizer major advantage is:Nitrogen phosphorus nutrient content is high, can save packaging fortune Defeated expense;Quadrafos have chelation to metal ion, are difficult to be fixed by metal ions such as Iron in Soil, calcium, can be with soil Invalid trace element in earth forms soluble complexes and is absorbed and used by plants;Quadrafos are not straight by plant in soil Absorption is connect, but is progressively hydrolyzed into orthophosphate and is utilized by plant, be a kind of slow dissolubility controlled availability fertilizer;The chelating of Quadrafos is made Precipitation is formed with the metal impurities that can be prevented in suspension fertilizers, thus is conducive to making high-concentration suspension fertilizer.
The defect of prior art:There is research to prepare high, middle low polymerization degree using thermal phosphoric acid, the production of full-boiled process polyphosphoric acid at present APP, and phosphorous acid production by BEP cost is than Wet-process Phosphoric Acid Production high cost 20% to 40%;Normal wet produces poly- phosphorus Reactor is easily blocked during sour ammonium, is generally blown stifled using steam, and the big multiplex graphite-pipe of inside reactor is made, although stone Ink manages acidproof, heatproof, but is corroded by gas ammonia and concentrated acid for a long time, when steam blows stifled, graphite-pipe easy fracture in reactor, it is impossible to Ensure the carrying out of production long-time stable, and graphite price is higher, increased production cost;Steam is passed through, the energy is wasted, and Easily cause gas ammonia and nitration mixture mixes uneven, reaction temperature disunity, so as to cause APP quality uncontrollable.
Utility model content
To solve above technical problem, this utility model provides a kind of preparation system of low-polymerization-dammonium ammonium polyphosphate, to solve Production cost is certainly reduced, prevents the blocking pipeline of ammonium polyphosphate from causing production be normally carried out, the use of extension reactor The problems such as life-span, stability of the seriality and product quality of holding production.
The technical solution adopted in the utility model is as follows:A kind of preparation system of low-polymerization-dammonium ammonium polyphosphate, it is critical only that: Polymeric kettle, tubular reactor including the connection of pipeline successively, recirculation reactor, the outlet of the recirculation reactor and pipe reaction Return duct is connected between the entrance of device, the return duct is provided with APP circulating pumps.
The beneficial effect of above scheme is that the polyphosphoric acids ammonium salt solution diluted in recirculation reactor can be flowed back by APP circulating pumps To in tubular reactor, form APP circulation regulation system, can prevent ammonium polyphosphate in tubular reactor pile up and Blocking pipeline, keeps production continuous, stable, improves the yield of APP.
Preferably, the polymeric kettle pipeline is connected with feedstock pre-mixing apparatus, and the feedstock pre-mixing apparatus include acid Acid anhydride feed bin, screw(-type) feeder, phosphoric acid storage tank and horizontal-type biaxial mixer, the anhydride feed bin pass through the screw(-type) feeder and institute The connection of horizontal-type biaxial mixer pipeline is stated, the phosphoric acid storage tank is connected with the horizontal-type biaxial mixer pipeline by dosing pump, The recirculation reactor pipeline connects into product storage tank.
The effect of the program is phosphoric anhydride and phosphoric acid respectively by screw(-type) feeder and dosing pump to horizontal-type biaxial mixer Dosing, and being pre-mixed for raw material is realized, it is that the polyreaction of next step is prepared.
Preferably, the tubular reactor includes reaction tube, and described reaction tube one end is provided with mother tube and ammonia-feeding pipe, described Mother tube is coaxially set with the reaction tube, and the annular isocon is arranged near the mother tube, the other end of reaction tube Discharging opening is provided with, the reaction tube is provided with circulation position of splitter, the circulation position of splitter is arranged on the mother tube and ammonia-feeding pipe Same one end of reaction tube, the circulation position of splitter are connected with the reaction tube;The circulation position of splitter includes annular isocon, institute Annular isocon is stated circumferentially about one circle of the reaction tube, the annular isocon be annular arrange semi-circular tube, the semi-circular tube Plane inwardly, cambered surface outwardly, the plane of the semi-circular tube is closely overlapped with the outer wall of the reaction tube, the tube wall of the reaction tube Upper ring uniformly offers point fluid apertures described at least four, and described point of fluid apertures is connected with the annular isocon, the annular point Flow tube is connected with circulation pipe, and the circulation pipe is connected with the annular isocon, and the charging aperture of the circulation pipe is circulated with the APP The discharge opening pipeline connection of pump.
The effect of the program is that nitration mixture and gas ammonia are reacted in tubular reactor from mother tube and ammonia-feeding pipe respectively, The polyphosphoric acids ammonium salt solution flowed back by circulation pipe, into annular isocon, is then entered in tubular reactor by point fluid apertures, So as to wash away the tube wall of tubular reactor, the ammonium polyphosphate in preliminarily diluted tubular reactor, it is to avoid because in tubular reactor Ammonium polyphosphate blocking pipeline and cause production to be not normally functioning, make gas ammonia and nitration mixture mixing it is more abundant.Stable prod matter Amount.
Preferably, the mother tube includes outer tube and the acid inlet tube being located in the outer tube, the acid inlet tube and described outer Ammonia passage is formed between pipe, the ammonia-feeding pipe in communication on the outer tube outer wall, is connected with.
The effect of the program is that acid inlet tube is located in ammonia passage, compact conformation, and it is anti-that nitration mixture falls into tubular type via acid inlet tube Device, ammonia is answered to enter ammonia passage through ammonia-feeding pipe, reacted with nitration mixture.
Preferably, ring baffle is provided between the inwall of the lower end of the acid inlet tube and the outer tube, in the annular gear On plate, ring uniformly offers ammonia guide hole described at least four, and the ammonia passage is connected with the reaction tube by ammonia guide hole Logical, the upper end of the outer tube is provided with closing flange, and the inward flange of the closing flange is connected with the outer wall of acid inlet tube.
The effect of the program is that ammonia is injected by ammonia guide hole is oblique, blows to nitration mixture, is sufficiently mixed reaction beneficial to both.
Preferably, polyphosphoric acid circulating pump, the polyphosphoric acid are provided between the polymeric kettle and the horizontal-type biaxial mixer The charging aperture of circulating pump is connected with the polymeric kettle pipeline, and the discharging opening of the polyphosphoric acid circulating pump is mixed with the horizontal-type biaxial Machine pipeline connects.
The effect of the program is that polyphosphoric acids are pumped in horizontal-type biaxial mixer by polyphosphoric acid circulating pump, with heterogeneous thing It is fed again in polymeric kettle jointly after material mixing, is polymerized, is formed polyphosphoric acids circulation regulation system, production can be kept continuous Property, adjust the content of oligomer in polyphosphoric acids.
Preferably, the ammonia-feeding pipe connects ammonia source of the gas, the recirculation reactor pipeline connection tail gas washing tower and water source.
It is to provide ammonia for the aminating reaction of polyphosphoric acids that the effect of the program is ammonia source of the gas, and water source is poly- for diluting Ammonium phosphate, tail gas washing tower can purify emission, environmental protection.
Beneficial effect:Compared with prior art, the preparation system of the low-polymerization-dammonium ammonium polyphosphate that this utility model is provided, right Thermal phosphoric acid, full-boiled process polyphosphoric acid, phosphate are adopted for primary raw material to produce middle low-polymerization-dammonium ammonium polyphosphate than existing, significantly Reduce production cost;Reaction is carried out under nature, low temperature, normal pressure, it is not necessary to high temperature, no pressure requirements, using continuity method Technique, greatly reduces processing step and difficulty, reduces productive labor intensity, improves working condition;Tubular type can be prevented anti- Answer the ammonium polyphosphate in device to pile up and block pipeline, keep production continuous, stable, improve product yield and quality.
Description of the drawings
Fig. 1 is structured flowchart of the present utility model;
Fig. 2 is the structural representation of tubular reactor 6 in Fig. 1;
Fig. 3 is enlarged drawing at A in Fig. 2.
Specific embodiment
It is to make those skilled in the art be better understood from the technical solution of the utility model, below in conjunction with the accompanying drawings and concrete real Apply mode to elaborate this utility model.
Embodiment 1:
As Figure 1-3, a kind of preparation system of low-polymerization-dammonium ammonium polyphosphate, including the feedstock of the connection of pipeline successively Pre-mixing apparatus, polymeric kettle 5, tubular reactor 6, recirculation reactor 7 and finished product storage tank 8, the feedstock pre-mixing apparatus include acid Acid anhydride feed bin 1, screw(-type) feeder 2, phosphoric acid storage tank 3 and horizontal-type biaxial mixer 4, the anhydride feed bin 1 pass through the screw feeder Machine 2 is connected with 4 pipeline of horizontal-type biaxial mixer, and the phosphoric acid storage tank 3 is mixed with the horizontal-type biaxial by dosing pump 13 4 pipeline of machine connects, and is connected with return duct, the return duct between the outlet of the recirculation reactor 7 and the entrance of tubular reactor 6 It is provided with APP circulating pumps 10;Polyphosphoric acid circulating pump 9 is provided between the polymeric kettle 5 and the horizontal-type biaxial mixer 4, it is described The charging aperture of polyphosphoric acid circulating pump 9 is connected with 5 pipeline of the polymeric kettle, and the discharging opening of the polyphosphoric acid circulating pump 9 is sleeping with described 4 pipeline of formula double-shaft mixer connects;6 pipeline of tubular reactor connection ammonia source of the gas 11,7 pipeline of the recirculation reactor connects Connect tail gas washing tower 12 and water source 14.
It can further be seen that the tubular reactor 6 includes reaction tube 61 in Fig. 2 and Fig. 3,61 one end of the reaction tube is provided with Mother tube 62 and ammonia-feeding pipe 63,63 pipeline of ammonia-feeding pipe connection ammonia source of the gas 11, the mother tube 62 is coaxial with the reaction tube 61 Line is arranged, and the annular isocon 641 is arranged near the mother tube 62, and the other end of reaction tube 61 is provided with discharging opening, described Reaction tube 61 is provided with circulation position of splitter 64, and the circulation position of splitter 64 is arranged on reaction tube with the mother tube 62 and ammonia-feeding pipe 63 61 same one end, the circulation position of splitter 64 are connected with the reaction tube 61;The circulation position of splitter 64 includes annular isocon 641, the annular isocon 641 is enclosed circumferentially about the reaction tube 61 1, the annular isocon 641 for annular setting half Pipe, the plane of the semi-circular tube inwardly, cambered surface outwardly, the plane of the semi-circular tube is closely overlapped with the outer wall of the reaction tube 61, On the tube wall of the reaction tube 61, ring uniformly offers point fluid apertures 642 described at least four, described point of fluid apertures 642 and the ring Shape isocon 641 is connected, and the annular isocon 641 is connected with circulation pipe 643, the circulation pipe 643 and the annular isocon 641 connections, the charging aperture of the circulation pipe 643 are connected with the discharge opening pipeline of the APP circulating pumps 10.
Shown in Fig. 3, the mother tube 62 includes outer tube 621 and the acid inlet tube 622 being located in the outer tube 621, described Ammonia passage 623 is formed between acid inlet tube 622 and the outer tube 621, institute in communication on 621 outer wall of the outer tube, is connected with State ammonia-feeding pipe 63;Ring baffle 65 is provided between the inwall of the lower end of the acid inlet tube 622 and the outer tube 621, in the ring On shape baffle plate 65, ring uniformly offers ammonia guide hole 66 described at least four, and the ammonia passage 623 passes through ammonia guide hole 66 Connect with the reaction tube 61, the upper end of the outer tube 621 is provided with closing flange 67, the inward flange of the closing flange 67 with enter acid The outer wall connection of pipe 622.
Prepare following the steps below for low-polymerization-dammonium ammonium polyphosphate:
Step one, phosphoric anhydride is added after anhydride feed bin 1, drying nitrogen is passed through to anhydride feed bin 1 and is protected, phosphoric anhydride By screw(-type) feeder 2 to 4 dosing of horizontal-type biaxial mixer, strong phosphoric acid of the mass fraction for 85%wt is added into phosphoric acid storage Groove 3, phosphoric acid is by dosing pump 13 to 4 dosing of horizontal-type biaxial mixer;
Step 2, phosphoric anhydride and mass fraction carry out premixing instead in horizontal-type biaxial mixer 4 for the strong phosphoric acid of 85%wt Should, heterogeneous material is formed, heterogeneous material is sent in polymeric kettle 5, polyreaction is carried out;
Step 3, the product in polymeric kettle 5 is pumped into into 4 porch of horizontal-type biaxial mixer by polyphosphoric acid circulating pump 9, with It is fed again in polymeric kettle 5 jointly after heterogeneous material mixing, forms polyphosphoric acids circulation regulation system;
After repeatedly circulating, the polyphosphoric acids obtained in polymeric kettle 5 are sent into tubular reactor 6 and are passed through tubular reactor 6 ammonia carries out aminating reaction, obtains the first mixed thing of APP and polyphosphoric acids;
Step 4, will just mix thing and send into recirculation reactor 7, add water into recirculation reactor 7, further stirring reaction, Mixture blowback tubular reactor 6 in recirculation reactor 7 is formed APP circulation regulation system, Jing by APP circulating pumps 10 After crossing repeatedly circulation, the finished product in recirculation reactor 7 sends into finished product storage tank 8, carries out metering packing.
Finally it is to be appreciated that foregoing description is only preferred embodiment of the present utility model, those skilled in the art is at this Under the enlightenment of utility model, on the premise of without prejudice to this utility model objective and claim, can make as multiple types Represent, such conversion is each fallen within protection domain of the present utility model.

Claims (7)

1. a kind of preparation system of low-polymerization-dammonium ammonium polyphosphate, it is characterised in that:Including pipeline successively connection polymeric kettle (5), Tubular reactor (6), recirculation reactor (7), between the outlet of the recirculation reactor (7) and the entrance of tubular reactor (6) Return duct is connected with, the return duct is provided with APP circulating pumps (10).
2. the preparation system of low-polymerization-dammonium ammonium polyphosphate according to claim 1, it is characterised in that:The polymeric kettle (5) Pipeline is connected with feedstock pre-mixing apparatus, and the feedstock pre-mixing apparatus include anhydride feed bin (1), screw(-type) feeder (2), phosphorus Acid storage tank (3) and horizontal-type biaxial mixer (4), the anhydride feed bin (1) are horizontal double with described by the screw(-type) feeder (2) Axle mixer (4) pipeline connects, and the phosphoric acid storage tank (3) is by dosing pump (13) and horizontal-type biaxial mixer (4) pipeline Connection, recirculation reactor (7) pipeline connection finished product storage tank (8).
3. the preparation system of low-polymerization-dammonium ammonium polyphosphate according to claim 1 and 2, it is characterised in that:The tubular type is anti- Answer device (6) including reaction tube (61), described reaction tube (61) one end is provided with mother tube (62) and ammonia-feeding pipe (63), the mother tube (62) it is coaxially set with the reaction tube (61), the other end of reaction tube (61) is provided with discharging opening, on the reaction tube (61) Circulation position of splitter (64) is provided with, the circulation position of splitter (64) is arranged on reaction tube with the mother tube (62) and ammonia-feeding pipe (63) (61) same one end, the circulation position of splitter (64) are connected with the reaction tube (61);
, including annular isocon (641), the annular isocon (641) is circumferentially about the reaction for circulation position of splitter (64) Pipe (61) one is enclosed, and the annular isocon (641) is the semi-circular tube that annular is arranged, the plane of the semi-circular tube inwardly, cambered surface outwardly, The plane of the semi-circular tube is closely overlapped with the outer wall of the reaction tube (61), and the annular isocon (641) is near the raw material Pipe (62) is arranged, and on the tube wall of the reaction tube (61), ring uniformly offers point fluid apertures (642) described at least four, described point Fluid apertures (642) is connected with the annular isocon (641), and the annular isocon (641) is connected with circulation pipe (643), and this follows Endless tube (643) is connected with the annular isocon (641), charging aperture and the APP circulating pumps of the circulation pipe (643) (10) discharge opening pipeline connection.
4. the preparation system of low-polymerization-dammonium ammonium polyphosphate according to claim 3, it is characterised in that:The mother tube (62) Including outer tube (621) and the acid inlet tube (622) being located in the outer tube (621), the acid inlet tube (622) and the outer tube (621) ammonia passage (623) is formed between, on outer tube (621) outer wall, the ammonia-feeding pipe (63) in communication is connected with.
5. the preparation system of low-polymerization-dammonium ammonium polyphosphate according to claim 4, it is characterised in that:The acid inlet tube (622) ring baffle (65) is provided between lower end and the inwall of the outer tube (621), the ring on the ring baffle (65) Ammonia guide hole (66) described at least four are offered uniformly, the ammonia passage (623) is anti-with described by ammonia guide hole (66) (61) connection should be managed, the upper end of the outer tube (621) is provided with closing flange (67), the inward flange of the closing flange (67) with enter acid The outer wall connection of pipe (622).
6. the preparation system of the low-polymerization-dammonium ammonium polyphosphate according to claim 4 or 5, it is characterised in that:The polymeric kettle (5) polyphosphoric acid circulating pump (9), the charging aperture of the polyphosphoric acid circulating pump (9) are provided between the horizontal-type biaxial mixer (4) It is connected with the polymeric kettle (5) pipeline, the discharging opening of the polyphosphoric acid circulating pump (9) is managed with the horizontal-type biaxial mixer (4) Road connects.
7. the preparation system of low-polymerization-dammonium ammonium polyphosphate according to claim 6, it is characterised in that:The ammonia-feeding pipe (63) Pipeline connection ammonia source of the gas (11), recirculation reactor (7) pipeline connection tail gas washing tower (12) and water source (14).
CN201620845568.8U 2016-08-04 2016-08-04 The preparation system of low-polymerization-dammonium ammonium polyphosphate Active CN206051553U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106044738A (en) * 2016-08-04 2016-10-26 中化重庆涪陵化工有限公司 Low-polymerization degree ammonium polyphosphate preparation system and method

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106044738A (en) * 2016-08-04 2016-10-26 中化重庆涪陵化工有限公司 Low-polymerization degree ammonium polyphosphate preparation system and method

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